Beruflich Dokumente
Kultur Dokumente
in Material Science
8, quai du MarchC-Neuf
75004 Paris
Serveur web : http://www.hermes-science.com
ISBN 2-7462-0115-1
All rights reserved. N o part of this publication may be reproduced, stored in a retrieval
system or transmitted, in any form, or by any means, electronic, mechanical, photocopying,
recording or otherwise, without prior permission, in writing, from the publisher.
Disclaimer
While every effort has been made to check the accuracy of the information in this book, no
responsability is assumed by Author or Publisher for any damage or injury to or loss of
property or persons as a matter of product liability, negligence or otherwise, or from any
use of materials, techniques, methods, instructions, or ideas contained herein.
X-Ray Tomography
in Material Science
Jose Baruchel
Jean-Yves Buffiere
Eric Maire
Paul Merle
Gilles Peix
cience
Authors
DERBY B., Manchester Materials Science Centre, UMIST and the University of
Manchester, Grosvenor Street, Manchester, Ml 7HS,UK
DUVAUCHELLE P., Laboratoire CNDI, INSA, Batiment 303, 69621 Villeurbane
Cedex, France
ELLIOTT J., Department of Biophysics in Relation to Dentistry, St Bartholomew's
and The Royal London Scool of Medecine and Dentistry, Queen Mary and
Westfield College, Mile End Road, London, El 4NS, UK
FOROUGHI B., Institute of Materials Science and Testing, Vienna University of
Technology, Karlsplatz 13, A-1040 Wien
FREUD N., Laboratoire CNDI, INSA, Batiment 303, 69621 Villeurbane Cedex,
France
FROYEN L., Department of Metallurgy and Materials Engineering, Katholieke
Universiteit Leuven, De Croylaan 2, B-3001 Heverlee, Belgium
GuiGAY J.-P., University of Antwerp, RUCA Groenenborgerlaan 171, B-2020
Antwerp, Belgium
HEINTZ J.-M., ICMCB, CNRS, 87 avenue du docteur Albert Schweitzer, 33608
Pessac, France
JOSSEROND C., Genie physique et mecanique des materiaux, ENSPG-UJF, BP 46,
F-38402 Saint-Martin-d'Here Cedex, France
JUSTICE I., Department of Materials, University of Oxford, Parks Rd, Oxford, OX1
3PH, UK
KAFTANDJIAN V., Laboratoire CNDI, INSA, Batiment 303, 69621 Villeurbane
Cedex, France
KOTTAR A., Institute of Materials Science and Testing, Vienna University of
Technology, Karlsplatz 13, A-1040 Wien
LUDWIG W., European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble,
France
MAIRE E., GEMPPM INSA Lyon, 20 avenue Albert Einstein, 69621 Villeurbane
Cedex, France
MARC A., LETI-CEA/Grenoble, 17 rue des martyrs, 38054 Grenoble Cedex 9,
France
MARTIN C.F., Genie physique et mecanique des materiaux, ENSPG-UJF, BP 46,
F-38402 Saint-Martin-d'Here Cedex, France
PEK G., Laboratoire CNDI, INSA, Batiment 303, 69621 Villeurbane Cedex, France
PEYRIN F., CREATIS, INSA-Lyon, 69621 Villeurbane, France
ROBERT-COUTANT C., LETI-CEA/Grenoble, 17 rue des martyrs, 38054 Grenoble
Cedex 9, France
SALVO L., Genie physique et mecanique des materiaux, ENSPG-UJF, BP 46,
F-38402 Saint-Martin-d'Here Cedex, France
SAVELLI S., GEMPPM INSA Lyon, 20 avenue Albert Einstein, 69621 Villeurbane
Cedex, France
SCHLENKER M., CNRS, Laboratoire Louis Neel, BP 166, F-38042 Grenoble, France
SUERY M., Genie physique et mecanique des materiaux, ENSPG-UJF, BP 46,
F-38402 Saint-Martin-d'Here Cedex, France
Authors
Table of contents
Foreword
13
15
15
16
20
23
26
26
29
29
30
32
38
38
42
43
45
45
46
10
49
50
51
53
54
55
56
57
57
61
4.1. Introduction
4.2. Description of projection measurements
4.3. Backprojection
4.4. Projection-slice theorem
4.5. Fourier reconstruction methods
4.6. Filtering in Fourier methods
4.7. ART-type methods
4.8. Conclusion
4.9. References
61
62
65
66
67
69
70
74
74
Introduction
Experimental device and procedure
Results on Al-Si alloys
Results on Al-Cu alloys
Conclusion and perspectives
References
,...
77
77
79
80
85
86
87
89
89
90
92
94
100
101
Table of contents
11
103
Introduction
Experimental methods
Results and discussion
Conclusion
References
103
104
107
112
113
115
115
116
121
124
125
127
Introduction
Background
Simulation possibilities
Simulation examples in tomography
Conclusions and future directions
References
127
128
129
132
135
136
Introduction
Production process of Aluminium foams
Mechanics of foams
Non-destructive investigation of Aluminium foams
Conclusion
References
139
139
140
142
144
151
152
11.1. Introduction
11.2. Experimental set-up
11.3. Result
11.4. Conclusions
11.5. References
.*.
155
155
157
158
160
163
12
165
165
166
166
168
172
175
177
177
179
185
187
190
191
193
193
197
198
199
200
203
204
Foreword
This book collects the texts of the lectures given during the Workshop on the
application ofX-Ray tomography in material science which was organised by the
Groupe d'Etudes de Metallurgie Physique et de Physique des Materiaux (GEMPPM)
in Villeurbanne on October 28-29 1999. Researchers from several European
universities, research centres and companies attended the lectures which were given
by experts in both materials science and X-ray tomography. The workshop was
subsidised by the INSA Lyon, the MMC Assess european network and the
Region Rhone Alpes and we would like to acknowledge their support.
The scope of this European workshop was to provide material scientists with a
detailed presentation of X-Ray tomography techniques, including the latest
developments, and to present recent applications of these techniques in the field of
structural materials.
The interest of material scientists in X ray tomography arises from two facts: 1)
most structural materials are opaque, and 2) it is of very crucial importance to
observe what occurs in the bulk of materials when they are subjected to a
mechanical loading. The apparent contradiction between these two facts has been
overcome by recent progress in X Ray tomography which has allowed 3D non
destructive images of structural materials, with a resolution around 1 micron, to be
achieved. Synchrotron radiation sources are necessary to record these very high
resolution images. Moreover, the phase contrast images, easily obtainable with X
ray sources emitting photons with a high spatial coherence, even permits the
visualisation of features with weak attenuation differences. This technique is
especially well adapted for studying metal matrix composites which are among the
most promising structural materials and for which damage development under stress
is of crucial importance.
Within this framework, the workshop was divided into two parts. The first one
included a global description of the technique itself, an introduction to the
14
Chapitre 1
General principles
1.1. Introduction
Tomography is referred to as the quantitative description of a slice of matter
within a bulky object. Several methods are available, delivering specific images,
depending on the selected physical excitation:
- ultrasonics,
- magnetic field (in the case of nuclear magnetic resonance imaging),
- X and gamma-rays (y rays),
- electric field (in the case of electrical impedance or capacitance tomography).
In the field of industrial non-destructive testing (NOT), as well as in the field of
materials characterization, X-ray or y-ray tomography is mostly used today.
Tomography is a relatively "new" technique. The very first images were obtained
in 1957 by Bartolomew and Casagrande [BAR 57]: they characterized the density of
General principles
17
local positon annihilation delivers pairs of 0.51 MeV annihilation photons which are
detected outside. This is the PET technique, used in the medical field.
N l=
Ar0exp[-
v(x,yi)dx]
[1]
path
Measuring the number N0 of photons emitted by the source and the number N, of
photons transmitted throughout a single line across the sample allows to calculate
the integral of ja along the considered path:
[2]
N
path
The term ((x,y) represents the value of the linear attenuation coefficient at the
point (x,y). Repeating such a measurement along a sufficient number of straight
lines within the same slice delivers the Radon transform of the object. Radon
demonstrated in 1917 the possibility to find an inverse to that transform and thus to
reconstruct the n(x,y) map of the slice [KAK 87].
Figure 1.5. Value of the mass attenuation coefficient for carbon and iron
Two main domains appear in Fig. 1.5. Below 200 keV, the photoelectric effect
dominates and jj/p is sharply dependant on E and Z. Equation [3] is often used to
describe this behaviour [ATT 68]:
General principles
19
[3]
where K is a constant. Such an equation implies that, for any given photon energy,
is proportional to p and to Z4. Performing images in the photoelectric domain
implies two main characteristics:
- a comparison of p between two areas of the object (or between two objects)
can be achieved only in the case when Z is constant (same atomic element or same
composition),
- a change in p between two areas can be cancelled by a change in Z in the
opposite direction.
It thus appears that a clear separation between Z and p can not be obtained, in
the photoelectric domain, unless two tomographic images are performed, using two
different energies.
Within the Compton domain, above 200 keV, u can be considered as weakly
dependant on Z and on photon energy. Tomography thus delivers an information
which is nearly proportional to p. However, due to the higher photons energy, and
hence to the lower value of u, the contrast within the object image is lower, as can
be derived from Beer-Lambert law.
Figure 1.6. Different experimental set-ups in the field of industrial tomography: a) first
generation scanner, b fan-beam scanner, c) cone-beam scanner
General principles
21
bed, through the steel wall of the riser (0.85 meter in diametre). A single source and
a single detector (Nal) are used, thus constituting a first generation tomograph, as
shown in Fig. 1.6a. The scan lasts 3 hours [BER 95]. The University of Bergen and
the Norsk-Hydro Company built a static device using a set of five americium 241
sources (energy: 60 keV) distributed around a pipe [JOH 96]. A linear array
comprising 17 semiconductor detectors is set opposite to each source, allowing a
near real-time (0.1 second) imaging of the slice. The purpose is to visualize the
liquid components (oil, water) apart from gas within a pipe. This application is an
example of process tomography, i.e. fast imaging dedicated to the control of a
manufacturing process.
1.3.1.2. Different families of detectors
Four main families of detectors can be found:
1. gas ionisation detectors were used in the early medical scanners. They are still
in use today in some industrial applications. Their main characteristic is their high
dynamic range. Filled with gas having a high atomic number, they can be used even
with high energies. Linear arrays are available.
2. image intensifiers (I.I.) are used in "desktop" scanners for industrial NDT of
small components. Their low dynamic range and the inherent distortion of the image
need some care. Significative 3D images can nevertheless be obtained.
3. scintillation detectors, composed of a fluorescent material (e.g. gadolinium
oxysulphide Gd2O2S, or caesium iodide Csl) are nowadays widely used. Those
detectors are of two kinds: i) the fluorescent material is directly coupled to an array
of photodiodes [KAF 96] or of photomultipliers (in some cases the coupling is
realized using tapered optic fibers), ii) the fluorescent material is spread on a screen,
which is optically coupled to a CCD camera via a lens [CEN 99].
4. arrays of semiconductors (e.g. CdTe or ZnCdTe), which allow a direct photon
detection are promising. High energy applications are possible.
1.3.2. Microtomography
Considering advanced materials characterization, the need of 3D images with a
very high resolution (a few um) obtained through a non invasive method is growing.
Figures 1.7 and 1.8 show two specific examples of 3D tomographic images
performed with two different scanners, conceived and built in our laboratory [KAF
96] [CEN 99]. Such 3D images are then used by the researchers for the modelisation
of the mechanical properties of materials, within finite elements models
computations. For such applications micro-focus X-ray tubes, with a focus size in
the range 5 - 1 0 micrometers, are used. A very low focus size allows to set the
investigated object directly at the window of the tube. A geometrical magnification
Figure 1.9. According to the location of the investigated object between the focus and the
screen, different geometrical magnifications are attained
General principles
23
Designing and building such a kind of scanner implies some care in at least three
domains:
- the low photon flux delivered by the micro-focus X-ray tube results in long
exposure times; the camera must therefore deliver a very low noise,
- the choice of the photon energy is important: low energy photons deliver
images with an higher contrast, but also with an higher relative noise,
- the accuracy of the mechanical setting must be better than the expected image
resolution.
Today, the most powerful tool involves the use of synchrotron radiation. The
European Synchrotron Radiation Facility (ESRF-Grenoble) delivers a huge X-ray
flux and thus allows very short exposure times. A complete scan can be acquired
within a few minutes, with a spatial resolution down to 1 um. On beam-line ID 19,
the source is located far from the working hutch (145 meters), thus delivering
photons with a high spatial coherence. This property of the X-ray flux generates
diffraction features which underline the edges within the sample, and thus
highlighting sharp defects. Such a phenomenon, the so-called "phase contrast" [CLO
97], allows very small defects to be detected. As the beam is non-diverging, the
resolution is set by the detector itself. Transparent luminescent screens are used,
with a 5 jam sensitive layer of an yttrium-aluminium (YAG) or lutetium-aluminium
(LUAG) garnet, epitaxially grown on a YAG monocrystal, 170 jim in thickness;
they allows a high resolution (1 fim) and a 4% to 8% efficiency for 14 keV photons.
energy photons, and hence to the gradual increase of the mean energy along the
path. The reconstruction algorithm uses, for the reconstruction of any single point,
experimental data corresponding to individual rays impinging the point of interest,
but coming from different orientations. The corresponding information therefore
corresponds to different attenuations, and hence different energies, and different
values of ji. Two kinds of artifacts are generated by beam-hardening: i) cupping
effect and ii) streaks. Cupping effect corresponds to measured values of \JL which are
corrupted, thus preventing the measurement of the "true" density. As the measured
values, inside an homogeneous sample, are lower at the center than at the edges, the
name of cupping effect is generally used to describe this artifact. Projections can be
corrected by acquiring an image of a step-wedge, made of the same material, in such
a way to correlate the mesured attenuation to the true material thickness. Streaks
artifact correspond to abnormal values along lines which correspond, inside the
object, to high attenuation. Beam hardening artifacts can be avoided when using
some filter, i.e. a metallic foil, directly set at the window of the X-ray tube and
intended to pre-harden the spectrum [KAF 96]. Figure 1.10 displays an example of
streaks inside the tomographic image of a set of six samples surrounded by air (Fig
l.lO.a); the streaks are suppressed by the use of a copper filter, 0.1 mm in thickness
(Fig. l.lO.b).
Figure 1.10. The reconstructed slice (l.lO.a) is corrupted by streaks due to beamhardening (l.lO.a). Filtration with a foil of copper, (0.1 mm) nearly suppresses the streaks
(l.lO.b). The high voltage used for both images is 100 kV
Beam hardening is also avoided when using a monochromatic y-ray source. But
it must be kept in mind that y-ray sources deliver a very low photon flux (typically
one hundredth of the flux delivered by a tube). Tomography using synchrotron
General principles
25
centered on the pixel corresponding to the location of the rotation axis. On figure
1.12 a great number of concentric rings are visible.
- Spatial distortion of the detector
Distortions of the projections, due for instance to the camera (e.g. distortions due
to the lens) deliver artifacts which can be corrected by software.
- Centering error
The reconstruction requires the knowledge of the location of the projection of
the center of rotation within the detector. Distortions are generated when the
reference to the centre is erroneous.
1.5. Conclusions
X and y-ray tomography allow a great number of potential applications. The
measured quantity is in fact the linear attenuation coefficient \i, and not directly the
density. A careful choice of the photons energy and the selection of a detector with a
high dynamic range allows to lessen the noise to a reasonable level. Coefficient \JL
can be estimated with an accuracy slightly better than 1%.
1.6. References
[ATT 68] Anrx F.H.R., ROESCH W.C., Radiation Dosimetry, Academic Press, 1968.
[BAR 57] BARTHOLOMEW R.N., CASAGRANDE, R.M., "Measuring solids
concentration in fluidized systems by gamma-ray absorption", Industrial and
Engineering Chemistry, vol. 49, n. 3, p. 428-431, 1957.
[BER 95] BERNARD J.R., Frontiers in Industrial Process Tomography, Engineering
Foundation, Ed. DM SCOTT& RA WILLIAMS, New-York, p. 197, 1995.
[CEN 99] CENDRE, E. et al., "Conception of a high resolution X-ray computed
tomography device; Application to damage initiation imaging inside materials",
Proceedings of the 1st World Congress on Industrial Process Tomography,
Umist Univ. (U.K.), p. 362-369, 1999.
[CLO 97] CLOETENS P., PATEYRON-SALOME M., BUFFIERE J.-Y., PEK G., BARUCHEL
J., PEYRIN F., SCHLENKER M., "Observation of microstructure and damage in
materials by phase sensitive radiography and tomography", J. Appl. Phys., vol.
81, n. 9, p. 5878-5886, 1997.
[DUV 98] DUVAUCHELLE P., Tomographie par diffusion Rayleigh et Compton avec
un rayonnement synchrotron: Application a la pathologic cerebrale, these de
doctoral, universite de Grenoble 1, 1998.
[PEL 84] FELDKAMP L.A., DAVIS L.C., KRESS J.W., "Practical cone-beam
algorithm", J. Opt. Soc., vol. 1, n. 6, p. 612-619, 1984.
General principles
27
[HAL 92] HALMSHAW R., "The effect of focal spot size in industrial
radiography",flrif/s/i Journal of NOT, vol. 34, n. 8, p. 389-394, 1992.
[HAR 99] HARTEVELD W.K. et al. "A fast active differencial capacitance
transducer for electrical capacitance tomography", Proceedings of the 1st World
Congress on Industrial Process Tomography, Umist Univ. (U.K.), p. 571-574,
1999.
[ISO 99] iso/TC 135/SC 5 , ISO document "NDT Radiation methods- Computed
tomography", Part I: Principles; Part II: Examination Practices, 1999.
[JOH 96] JOHANSEN G.A, FR0YSTEIN T., HJERTAKER B.T., OLSEN O., "A dual
Chapitre 2
Hard X-ray radiography and tomography are common techniques for medical
and industrial imaging. They normally rely on absorption contrast. However, the
refractive index for X-rays is slightly different from unity and an X-ray beam is
modulated in its optical phase after passing through a sample. The coherence of third
generation synchrotron radiation beams makes a simple form of phase-contrast
imaging, based on simple propagation, possible. Phase imaging can be used either in
a qualitative way, mainly useful for edge-detection, or in a quantitative way,
involving numerical retrieval of the phase from images recorded at different
distances from the sample.
2.1. Introduction
The phase of an X-ray beam transmitted by an object is shifted due to the interaction with the electrons in the material. Imaging using phase contrast as opposed to
attenuation contrast is a powerful method for the investigation of light materials but
also to distinguish, in absorbing samples, phases with very similar X-ray attenuation
but different electron densities. Phase contrast imaging was pioneered in the early
seventies by Ando and Hosoya [AND 72], who obtained images of bone tissues and
of a slice of granite using a Bonse-Hart type interferometer [BON 65]. This technique
developed into a quantitative three-dimensional imaging technique. Because of the
limited quality of available lenses, elaborate forms of phase contrast imaging such as
Zernike phase-contrast [ZER 35] or off-axis holography [LEI 62] are presently ruled
out for hard X-rays. Three methods of phase sensitive imaging exist: the interferometric technique [MOM 95, BEC 97], the Schlieren technique [FOR 80, ING 95] and
the propagation technique [SNI 95, CLO 96]. They are compared in section 3. The
main advantages of the method used in this work, the propagation technique, are the
extreme simplicity of the set-up and the better spatial resolution.
30
This technique was mostly used up to now in the so-called 'edge-detection regime'
to image directly the discontinuities in refractive index in the object. It is however possible to fully exploit the quantitative information entangled in the Fresnel
diffraction patterns towards high resolution quantitative phase tomography. The 'holotomographic' reconstruction is performed in two steps: first the optical phase of the
wave exiting the sample is retrieved numerically from images recorded at different distances from the sample. The refractive index distribution is then reconstructed from a
large number of phase maps using a classical tomographic algorithm. Results of quantitative phase tomography on samples of interest to materials science are discussed.
[1]
A plane monochromatic wave propagating along the z-axis in vacuum is of the form
exp(i^ L z) with A the X-ray wavelength. In a material with refractive index n this
becomes exp(m^ L z). The refractive index decrement 6 results in a phase variation
compared to propagation in vacuum. The imaginary part J3 determines the attenuation
of the wave. The X-ray intensity is the squared modulus of the wave and the absorption
index (3 is simply proportional to the linear absorption coefficient p.
,=
f>
[2]
The absorption index has a complex energy and composition dependence. It varies
abruptly near the characteristic edges of the elements. The refractive index decrement
6 on the other hand is primarily due to Thomson scattering and has a much simpler
dependency on the energy and the material characteristics. S is essentially proportional
to the electron density in the material. Generally, it can be expressed as
where the sum extends over all atoms p, with atomic number Zp, in the volume V,
rc = 2.8 fm is the classical electron radius, and f'p is the real part of the wavelengthdependent dispersion correction, significant near absorption edges, to the atomic scattering factor. If the composition of the material is known in terms of mass fractions
qp, the following equivalent expressions can be used
31
[5]
with NA Avogadro's number and Ap the mass number. 6P and pp are respectively the
refractive index decrement and mass density of the pure species.
If the dispersion correction fp can be neglected, 6 is proportional to the electron
density pe, i.e. S = r c A 2 p e /(27r). The ratios ZP/AP appearing in Equation 4 are similar for many atomic species ( 1/2), and 6 is thus to a good approximation determined
by the mass density p of the material [GUI 94]
[6]
Both 6 and ft are small, typically 10~5 - 10~6 and 10~8 - 10~9 respectively for light
materials, indicating the power of phase sensitive imaging compared to the absorption. Figure 1 shows the ratio S /ft, a figure of merit for phase effects compared to
attenuation effects, as a function of the X-ray energy E for aluminium. The energy
range includes soft X-rays and hard X-rays. In the soft X-ray range, more precisely
in the 'water window' where soft X-ray microscopes usually operate, a gain exists but
it is relatively modest. On the other hand in the hard X-ray range (energies above 6
keV) this ratio increases with energy to huge values (up to 1000). Practically, if one
selects for example an X-ray energy of 25 keV to be able to cross a thick aluminium
sample, a hole in this metal should have a diameter of at least 20 /zm to produce 1 %
Figure 2.1. Ratio S//3 of the refractive ondex decrement and the absorption index as a
function of the X-ray energy for the element aluminiu. This is a figure of merit for phase
effects compared to attenuation effects
32
absorption contrast. Using the effect on the phase, the minimum detectable hole is
reduced to about 0.05 yum. X-rays are adapted for imaging of thick samples thanks
to their low absorption at high energies. If it is possible to visualise the phase of the
transmitted wave, the sensitivity and spatial resolution remain good.
For inhomogeneous samples the wave at the exit of the sample will be modulated
in both phase and attenuation. Propagation inside the sample itself can usually be
neglected and it is possible to project the object onto a single plane perpendicular to
the propagation direction. The transmission function T(x, y) gives the ratio of the
transmitted and the incident amplitudes. It can be compared to exp( f n(x, y, z)dz)
that gives the ratio of the transmitted and the incident intensities according to LambertBeer's law. This transmission function corresponds to the projection of the refractive
index distribution through
T(x,y) = A(x,y)eirtx>ri
[7]
and
B(x,y} - y j 0(x,y,z)dz
[8]
[9]
(p0 is the phase modulation that would occur in the absence of the object. In classical
absorption tomography the projection of n is determined for a large number of angular positions of the sample. The three-dimensional (3D) distribution of n(x, y, z)
or equivalently of / 3 ( x , y , z} is then reconstructed from the set of projections using a
tomographic reconstruction algorithm. Similarly if the phase map (p(x, y) is known
for a large enough number of angular positions of the object, it is straightforward to
reconstruct the distribution of the refractive index decrement 8(x, y, z).
33
Forster et al [FOR 80] used a double crystal arrangement similar to the one shown in
Figure 2b. The first crystal acts as a collimator in limiting the angular and spectral
range. The angular deviations introduced by the sample change the incidence angle
with respect to the analyser that acts as an angular filter. The variety in the nomenclature for this approach can be noted: Schlieren-imaging [FOR 80, CLO 96], refraction contrast [SOM 91], phase dispersive imaging [ING 95, ING 96], phase contrast
imaging [DAV 95] and diffraction enhanced imaging [CHA 98] are the most com-
34
Figure 2.2. Set-up for phase sensitive methods: (a) Interferometric technique, (b) Schlieren
technique and (c) Propagation technique
mon names. The possibility to visualise phase gradients (occuring for example at
edges) was shown by many groups, but no reconstructed (differential) phase map was
presented and the method was not extended to 3D imaging through tomographic techniques. Compared to the interferometric technique, the experimental set-up is simplified and the stability requirements are less stringent. To obtain a good sensitivity
to phase gradients, the width of the rocking curve for one of the crystals relative to
the other should be small, typically 2-10 yurad, and the angular stability should be
about 0.2 yurad [ING 96]. As the alignment is less critical, the collimator and analyser
crystal do not need to be part of a monolithic block, and the space available for the
sample and its environment increases. The samples are in general not immersed in a
liquid. The spatial resolution is again affected by the passage of the wave through the
analyser crystal. This method is less adapted than the previous one to covering the
low spatial frequency range, and very smooth variations of the phase may introduce a
phase gradient that is too small to be detected. This imaging scheme can be used on a
laboratory X-ray source. Most of the published results were obtained under these conditions, resulting in long exposure times of 15-30 minutes [ING 96] for a radiograph.
This technique corresponds to Schlieren imaging in classical optics [HEC 98].
35
with / the source sample distance. In the case of the long ESRF beamline ID 19 (d <C
/ = 145m), the defocusing distance and the sample-detector distance are practically
equal. The absorption radiograph corresponds of course to an image recorded close to
the sample (D 0). The region of the object mainly contributing to the corresponding
point of the image (the first Fresnel zone) has a radius equal to
36
the 'holographic regime', give little direct information on the sample. However, combining such images recorded at different distances with a suitable numerical algorithm
gives access to the phase modulation (cf. section 5). For the largest distances, rarely
accessible with X-rays, one reaches the Fraunhofer limit (rp a). Figure 3 shows as
an example four radiographs of a 0.5 mm thick piece of polystyrene foam at increasing
distances D. The beam is monochromatised to 18 keV. As the distance increases, the
contrast and width of the Fresnel fringes both increase. The radiographs are recorded
with a CCD based detector involving X-ray / visible light conversion in a transparent
YAG:Ce screen [KOC 98], with an effective pixel size of 0.95 //m.
The most striking advantage of this method is the extreme simplicity of the setup. It is essentially the same as for absorption radiography. The transition between
absorption and phase radiography or between the different regimes of phase imaging is
simply obtained by changing the sample detector distance. The stability requirements
on the (few) elements downstream of the monochromator, i.e. the sample and the
detector, are easily met. The monochromator can be well upstream of the sample and
the sample detector distance can often be chosen quite large. The free space around
the sample can be used for all kinds of devices for in-situ and real-time observations.
However the optical elements of the beamline have to be carefully prepared to avoid
spurious phase images.
It can be shown that for a given defocusing distance the image is most sensitive
to a specific frequency range. The optimum distance to be sensitive to phase features
with spatial frequency / is such that
This frequency selectivity will intrinsically limit the accessibility to the low frequency
range, i.e. the smooth variations in the object's phase. The optimum distance, increasing as the square of the object size, will not be reached for these frequencies due to
physical limitations (size of the experimental hutch) or the coherence conditions. The
image is not spoiled by the passage of the modulated wave through a crystal as is the
case in the interferometric and Schlieren techniques. The resolution in the propagation technique depends on the image processing after recording. For untreated images
recorded in the edge-detection regime the resolution is limited by the fringe spacing
to about 2rp. When the fringes are disentangled in a holographic reconstruction, the
spatial resolution is limited essentially by the detector. The stringent requirements on
the beam incident on the sample explain why this technique emerged only recently
[HAR 94, SNI 95, CLO 96, NUG 96] with the appearance of partially coherent X-ray
beams delivered by third generation synchrotron radiation sources. The geometrical
resolution in the Fresnel diffraction pattern is equal to Dsa with sa f the angular source size and s the source size. The condition for observation of the spatial
frequency / is
37
Figure 2.3. Phase sensitive radiographs of a 0.5 mm thick piece of polystyrene foam, with the
detector at various distances dfrom the sample. X-ray energy 18 keV. (a) d= 0.03 m, (b) d =
0.2 m, (c) d = 0.5 m and (d) d = 0.9 m. The contrast and the width of the interference fringes
increase trough the series
The blurring due to source size and detector resolution explains why no interference
fringes are observed with classical laboratory sources although the propagation distances are also non-zero in projection radiography. Alternatively, the interference pattern involves the coherent superposition of laterally separated portions of the incident
beam. The interfering waves must originate from points that are mutually coherent,
and thus laterally separated by a distance smaller than the transverse coherence length
/t that can be defined as l[ = A/(2s a ). The incident beam must be coherent over the
first Fresnel zone for optimum conditions.
The conditions on the monochromaticity are less stringent. The beam is usually
monochromatised using a monochromator based on perfect silicon crystals. The en-
38
ergy spread AA/A 10~4 is thus very small. The thickness of the samples that
can be investigated is not limited to the longitudinal coherence length (= A 2 /AA)
[CLO 96]. An increase in energy spread by one or even two orders of magnitude can
still correspond to quasi-monochromatic conditions. This allows to increase considerably the flux using a multi-layer monochromator with a very high substrate quality.
Using the same propagation principle but working with the polychromatic radiation
delivered by a laboratory X-ray microsource to retain some flux, deflection sensitive
images were obtained [WIL 96, POG 97]. This seems promising for work in the edge
detection regime as the main contrast, a white and black fringe, is unchanged over a
large spectral range.
39
projection from a set of in-line holograms. In a second step (toraographic reconstruction), the Radon transform is inversed using a classical tomographic reconstruction
method, such as the filtered backprojection method. Details on the phase retrieval
method are given elsewhere [CLO 99a, CLO 99b]. Here we only give two examples:
the first is a non-absorbing polymer foam and the second an absorbing metal alloy that
introduces very large phase shifts.
Figure 2.4. Phase map retrieved with an algorithm that combines images recorded at several
(here four) distances. The sample is a 0.5 mm thick piece of polystyrene. The X-ray energy is
18 keV.
A piece of polystyrene foam with a rather complex 3D structure was used to test
the method. It had a cross-section of 0.5 x 0.7 mm2 and negligible attenuation. Four
tomographic scans of 700 views each were automatically recorded at defocusing distances D of 0.03, 0.21, 0.51 and 0.9 m. The radiographs for a given angular position
are those of Figure 3. The corresponding reconstructed phase map is shown in Figure 4. The phase retrieval included correction for the detector response and the partial
coherence. The phase varies between about 0 and -7 rad. This phase map has a
straightforward interpretation: it is a projection along the X-ray path of the electron
density in the sample. Cells with sizes on the order of 100 ^m are clearly revealed.
The holographic reconstruction was repeated for the 700 angular positions of the
sample. The phase maps, projections of the refractive index decrement, were used to
determine the 3D distribution of 6 in the sample with a filtered backprojection algorithm. Figure 5a shows a slice of the reconstructed volume. The gray scale is linear
with respect to the index decrement 8(x, y, z), darker corresponding to a higher electron and mass density. The interpretation of the reconstructed slices is thus straightforward. The contrast of the polymer foam is excellent. This would certainly not be
40
Figure 2.5. (a) A slice of the reconstructed distribution of the refractive index decrement 8 of
a polystyrene foam. S is essentially proportional to the electron and mass density in the
polymer. A phase map was determined for each of 700 angular positions using images at four
distances. From the projections the 3D distribution was determined with a filtered
backprojection algorithm. (b) Magnified portion of the reconstructed slice shown in a (a). (c)
Profile along the arrow shown in (a). E = 18 keV.
the case in absorption tomography, the ratio of the refractive index decrement and the
absorption index S/j3 being 2500. Figure 5c shows a profile of the index decrement
along a line segment shown in Figure 5b. The air/polymer transition is abrupt and from
this profile the spatial resolution is estimated to be about 2.5 jum (fwhm). In regions
that apparently contain only polymer the refractive index decrement is 6.6 10~7, corresponding to a mass density of 0.96 g/cm3, in agreement with the expected density
value for polystyrene of about 1 g/cm3. The tomographic slice of Figure 5a intersects
a cell of the foam. It is completely enclosed by a polymer wall. The thin walls were
not evident in the projection images, but they appear correctly after tomographic reconstruction. The shape of the cell is irregular and very distorted. This is probably
due to a crushing process. The magnified portion of the slice shown in Figure 5b, indicates an excellent 3D isotropic spatial resolution that can be obtained thanks to the
detector resolution, but also because the holographic reconstruction disentangled the
object information from the defocused images.
41
Figure 2.6. Three tomographic slices of an aluminium-silicon alloy quenched from the semisolid state, obtained (a) using absorption contrast, (b) using phase contrast and a single
propagation distance, (c) using phase contrast and holotomography based on four distances.
E = 18 keV.
42
2.6. Conclusion
Phase sensitive images are experimentally simple to obtain. Third generation synchrotron radiation facilities, such as ESRF, can easily produce the necessary coherent
beam. A first approach is to use the phase radiographs directly or in combination
with the algorithm for absorption tomography. In many cases this gives useful results,
for example the detection of cracks or reinforcing particles in composite materials.
A new approach, called 'holotomography' is now operational. It allows to perform
quantitative phase contrast tomography with a simple set-up. We used for the holographic reconstruction, in analogy with electron microscopy, a numerical procedure
based on images at different distances from the sample. The feasibility of this method
was demonstrated on a polystyrene foam. The results are in quantitative agreement
with the known sample composition. The study of a metal alloy, with metallographic
phases that are not distinguishable in the absorption mode, demonstrates the usefulness of this technique for materials sciences. A drastic improvement in sensitivity and
resolution is obtained compared to usual X-ray tomography.
43
2.7. References
[AND 72] ANDO M., HOSOYA S., "An attempt at X-ray phase-contrast microscopy", SHINODA G., KOHRA K., ICHINOKAWA T., Eds., Proc. 6th Intern. Conf. on X-ray Optics and
Microanalysis, p. 63-68, Univ. of Tokyo Press, Tokyo, 1972.
[BEC 95] BECKMANN R, BONSE U., BUSCH F., GUNNEWIG O., BIERMANN T., "A novel
system for X-ray phase-contrast microtomography", HASYLAB Annual Report II, p. 691692, 1995.
[BEC 97] B E C K M A N N F., BONSE U., BUSCH F., GUNNEWIG O., "X-ray microtomography
(//CT) using phase contrast for the investigation of organic matter", J. Computer Assist.
Tomography, vol. 21, 1997, p. 539.
[BON 65] BONSE U., HART M., "An X-ray interferometer", Appl. Phys. Lett., vol. 6, 1965,
p. 155-156.
[BOR 80] BORN M., WOLF E., Principle of Optics, 6th ed., Pergamon Press, Oxford, New
York, 1980.
[BUF 99] BUFFIERE J. Y., MAIRE E., CLOETENS P., LORMAND G., FOUGERES R., "Characterisation of internal damage in a MMCp using X-Ray synchrotron phase contrast microtomography", Acta Mater., vol. 47, 1999, p. 1613-1625.
[CHA98] CHAPMAN D., THOMLINSON W., ZHONG Z., JOHNSTON R. E., PISANO E.,
WASHBURN D., SAVERS D., SEGRE C., "Diffraction Enhanced Imaging Applied to Materials Science and Medicine", Synchrotron Radiation News, vol. 11, 1998, p. 4-11.
[CLO96] CLOETENS P., BARRETT R., BARUCHEL J., GUIGAY J. P., SCHLENKER M.,
"Phase objects in synchrotron radiation hard x-ray imaging", J. Phys. D, vol. 29, 1996,
p. 133-146.
[CLO 97] CLOETENS P., PATEYRON-SALOME M., BUFFIERE J. Y., PEIX G., BARUCHEL J.,
PEYRIN F., SCHLENKER M., "Observation of microstructure and damage in materials by
phase sensitive radiography and tomography", J. Appl. Phys., vol. 81, 1997, p. 5878-5886.
[CLO 99a] CLOETENS P., LUDWIG W., BARUCHEL J., VAN DYCK D., VAN LANDUYT J.,
GUIGAY J. P., SCHLENKER M., "Holotomography: Quantitative phase tomography with
micrometer resolution using hard synchrotron radiation x rays", Appl. Phys. Lett., vol. 75,
1999, p. 2912-2914.
[CLO99b] CLOETENS P., LUDWIG W., VAN DYCK D., GUIGAY J. P., SCHLENKER M.,
BARUCHEL J., "Quantitative phase tomography by holographic reconstruction", BONSE
U., Ed., Developments in X-Ray Tomography II, vol. 3772, 1999, p. 279-290.
[DAV 95] DAVIS T. J., GAO D., GUREYEV T. E., STEVENSON A. W., WILKINS W., "Phasecontrast imaging of weakly absorbing materials using hard X-rays", Nature, vol. 373, 1995,
p. 595-598.
[FOR 80] FORSTER E., GOETZ K., ZAUMSEIL P., "Double Crystal Diffractometry for the
Characterization of Targets for Laser Fusion Experiments", Kristall und Technik, vol. 1,
1980, p. 937-945.
[GUI 94] GUINIER A., X-Ray Diffraction In Crystals, Imperfect Crystals, and Amorphous
Bodies, Dover Publications Inc., New-York, 1994.
[HAR 75] HART M., 'Ten years of X-ray interferometry", Proc. R. Soc. Lond. A, vol. 346,
1975, p. 1.
44
[HAR94] HARTMAN Y. M., SNIGIREV A., "Some examples of high energy X-rays phase
contrast", ARISTOV V. V., ERKO A. I., Eds., X-ray Microscopy IV, p. 429-432, Bogorodskii Pechatnik Publishing Company, Moscow, 1994.
[HEC 98] HECHT E., Optics, Srded., Addison-Wesley, 1998.
[ING 95] INGAL V. N., BELIAEVSKAYA E. A., "X-ray plane wave topography observation of
the phase contrast from a non-crystalline object", J. Phys. D: Appl. Phys., vol. 28, 1995,
p. 2314-2317.
[ING 96] INGAL V. N., BELIAEVSKAYA E. A., "Phase dispersion radiography of biological
objects", Physica Medico, vol. 12, 1996, p. 75-81. .
[KOC 98] KOCH A., RAVEN C., SPANNE P., SNIGIREV A., "X-ray imaging with submicrometer resolution employing transparent luminescent screens", / Opt. Soc. Am. A, vol. 15,
1998, p. 1940-1951.
[LEI 62] LEITH E. N., UPATNIEKS J., "Reconstructed Wavefronts and Communication Theory", J. Opt. Soc. Am., vol. 52, 1962, p. 1123.
[MOM 95] MOMOSE A., "Demonstration of phase-contrast X-ray computed tomography using an X-ray interferometer", Nucl. Inst. Meth. A, vol. 352, 1995, p. 622-628.
[MOM 96] MOMOSE A., TAKEDA T., ITAI Y., HIRANO K., "Phase-contrast X-ray computed
tomography for observing biological soft tissues", Nature Medicine, vol. 2, 1996, p. 473475.
[NUG96] NUGENT K. A., GUREYEV T. E., COOKSON D. F., PAGANIN D., BARNEA Z.,
"Quantitative Phase Imaging Using Hard X Rays", Phys. Rev. Lett., vol. 77, 1996, p. 29612964.
[POG 97] POGANY A., GAO D., WILKINS S. W., "Contrast and resolution in imaging with a
microfocus x-ray source", Rev. Sci. Instrum., vol. 68, 1997, p. 2774-2782.
[SNI95] SNIGIREV A., SNIGIREVA I., KOHN V., KUZNETSOV S., SCHELOKOV I., "On the
possibilities of x-ray phase contrast microimaging by coherent high-energy synchrotron
radiation", Rev. Sci. Instrum., vol. 66, 1995, p. 5486-5492.
[SOM 91] SOMENKOV V. A., TKALICH A. K., SHIL'SHTEIN S. S., "Refraction contrast in
x-ray introscopy", Zh. Tekh. Fiz., vol. 61, 1991, p. 197-201.
[WIL96] WILKINS S. W., GUREYEV T. E., GAO D., POGANY A., STEVENSON A. W.,
"Phase-contrast imaging using polychromatic hard X-rays", Nature, vol. 384, 1996, p. 335338.
[ZER 35] ZERNIKE F., Z. Tech. Phys., vol. 16, 1935, p. 454.
Chapitre 3
The use of the modern synchrotron radiation sources for monochromatic beam
microtomography provides several new possibilities. They include, in addition to
reduced signal-to-noise ratio and enhanced spatial resolution, the easy setup of
sample environment for in-situ experiments, the quantitative measurements, and the
rapidly increasing field of phase imaging. Other topics, such as the present state of
'local' microtomography, and some new approaches like diffraction and
fluorescence microtomography, are also briefly described.
3.1. Introduction
Since their discovery X-rays have been used to image the bulk of materials
which are non transparent for visible light, by taking advantage of their
inhomogeneous absorption. A tremendous progress was obtained, 25 years ago,
when three-dimensional (3D) visualization became available. This computerassisted tomographic approach provides the 3D information, from the many twodimensional (2D) images (radiographs) recorded at various angular positions of the
object, and via appropriate algorithms ("filtered back-projection", described for
instance in references [KAK88] and [PEY96]) and software. From the reconstructed
3D data cuts, projections, or perspective renditions of the object can be obtained at
will.
Microtomography, with spatial resolution better than 20 um, recent emerged in
years [FLA87]. Several laboratory instruments have been developed [SAS98,
RUE96], are commercially available, and produce good results. However, the best
quality images, in terms of signal-to-noise ratio and spatial resolution, are obtained
46
Figure 3.1. Schematic representation of a synchrotron radiation facility, showing the linear
accelerator (LA) and the booster (B). In these two elements the electron beam energy is
raised to the wished value (6 GEV at the ESRF). Then the electron beam is introduced in the
storage ring (SR), where it produces, when accelerated by the magnetic fields which modify
its trajectory, the X-ray beams. The X-ray beams are used at the level of the beamlines (EL),
tangent to the storage ring
47
accelerated by a magnetic field (figure 3.1). This field is uniform over a portion of
the trajectory in the bending magnets. It oscillates spatially in the insertion devices
(wigglers and undulators) which can be set on the straight sections between two
bending magnets.
Figure 3.2. Relative brilliance (arbitrary units, logarithmic scale) of the X-ray sources from
the discovery of X-rays to 3rd generation SR facilities
The X-ray beam produced is tangent to the curved trajectory of the electrons in
the storage ring: the beamlines are thus located all around the storage ring, as
indicated on figure 3.1. Along with all synchrotron radiation sources, the ESRF
features very high intensity of the emitted beam (figure 3.2) and, when the source is
a bending magnet or a wiggler, a continuous spectrum, spanning the whole range
from the infra-red to X-rays.
The original features of third generation synchrotron radiation facilities, and
more particularly the ESRF, when considering the microtomographic applications,
are:
a) the very high intensity of the X-ray beam (fig. 3.2)
b) the high energy (6 GeV) of the electrons producing the radiation, which
implies the availability of high energy photons (beyond 100 keV)
c) the policy of providing each beam-line, through appropriate choice of the
insertion device, with the spectrum best suited to the experiment it is dedicated to,
and
d) the small size of the electron beam cross-section (< 100 um). This leads to
high brilliance, but also to a very small angular extension of the source as seen from
a point in the specimen, hence to a sizeable lateral coherence of the X-ray beam.
48
49
When using the tomographic setup of the ID 19 beamline the total acquisition
time is of the order of half an hour for recording 900 projections images, and around
one hundred reference images for flat-field correction. Data acquisition for one
sample typically represents 2 Gigabytes, and enables the reconstruction of a (1024)3
tomographic image. Due to the parallel geometry, the 3D reconstruction problem
may be solved using a sequence of Filtered Back Projection algorithms run on each
slice of the volume, after rearranging the data in a set of corrected sinograms. To
avoid the duplication of the 2 Gigabytes of data, and save some computations, a
reconstruction program directly handling the radiographic images acquired during
experiment was developed. The program includes both pre-processing, and a 3D
version of the FBP algorithm adapted to 2D parallel projections. This algorithm was
parallelized on the workstation cluster of the ESRF, to speed up the reconstruction.
Using 4 machines, the mean reconstruction time obtained for (512) 3 volumes, is
approximately 2 hours, and depends on the workload of the system, since the system
is multi-user. Reduced reconstruction times are presently reached by devoting an
optimized computer to the reconstruction task.
50
Figure 3.4. Images of a vertebra sample obtained using the ESRF Micro-CT and the IBT
Micro-CT: a)-b): 2D slices extracted from the 3D images, c) d) 3D displays
51
required number of photons grows as the third power of the number of pixels in the
image [PEY96]. As an illustration of the capabilities of micrometer synchrotron
micro tomography, figure 3.5 represents a reconstructed slice of a three dimensional
image of a fetal mouse bone, recorded with a voxel size of 1.8 um. An inferior
spatial resolution would not allow to observe micro-structures within this bone.
Figure 3.5. Reconstructed slice of a fetal mouse bone, pixel size : 1.8 \jan
52
Figure 3.6. Reconstructed slice through a human bone biopsy, showing different gray levels
within the cortical region, indicating differents levels of mineralization (voxel size: 10 /jm)
53
Figure 3.8. Two reconstructed slices of the same sample a) with a 2 jam voxel size (local
tomography, region of 2mm in diameter), b) with a 6.6 jum voxel size ( 6 mm diameter sample
completely immersed into the beam)
Since the 2D detector is based on a 1024x1024 CCD, the size of the field of
view is determined by the pixel size in the image. Tomographic acquisition
theoretically requires that the field of view encompasses the entire transaxial extent
of the object at every angle. When the sample is only partly illuminated by the
beam, the projections are truncated, and the reconstruction problem is known as
'Local Tomography'.
Many efforts are devoted to obtain reliable Local
Tomography images, in spite of the missing information. Among them, let us
mention a wavelet-based algorithm for multiresolution tomographic reconstructions
[PEY99].
However if the region of interest is centered, and if the sample is globally
homogeneous, a good approximation in the center of the structure of the sample can
be obtained. Figure 3.8 shows that in this case the reconstructed image from
truncated projections is close to the image reconstructed from the complete data.
The projections from a 'composite with fibers' sample were recorded both with a
6.65 urn, and 2 urn, pixel size on the detector. In the second case the projections are
54
truncated, which generates the important circular artifact at the border of the image.
However we may notice that even if the values in the center of the image may not
be used quantitatively, they provide an accurate information on the structure of the
sample.
Figure 3.9. Snow samples resulting from the evolution of fresh snow, collected on the field a)
obtained by immersion in water at 0C, well-rounded grains, b) displaying faceted
crystallites, obtained by transformation under the action of a temperature gradient (lC/cm).
10 keV'X-rays.
Figuer 3.9 corresponds to a quite common porous medium, snow, which requires
to remain at low temperature to be investigated. The sample was located in a
cryostat especially designed for microtomography, featuring X-ray absorption that is
weak and independent of the angular position of the sample during its rotation. The
snow was maintained at -60C, in a regulated temperature nitrogen flow. It sitted
within a cylindrical enclosure with polished double plexiglass walls, 0.5 mm thick .
This device allows to establish a catalog of snows: fig. 3.8 shows that tomographic
methods provide data on the three-dimensional microstructure of snow that is
statistically significant because it represents a large number of grains, and at a high
resolution compared to the grain's scale [BRZ99]. Indeed, snow is a mixture of ice
particles, air and occasionally liquid water which can take different aspects. In most
cases, recent snow is a very loose powder, which can transform into hard, crusted or
pasty material, according to weather conditions and exposure. The growth of ice
particles is caused by vapor diffusion in dry snow and melt-freeze exchanges in wet
snow. Normally, dry snow covers are warmer at the bottom than on the top. The
value of the temperature gradient determines whether rounded (small gradient) or
faceted (large gradient) crystals will grow. These transformations have huge
consequences: changes over several order of magnitude in the physical and
55
mechanical properties of the different snow layers are commonplace. In some cases
the snow crystals are able to stick on vertical rocks, whereas under some conditions
a single skier can release a slab avalanche. The shape (specific area, local grain
curvature) and arrangement (grain connections) of the grains, and the quality of the
ice bonds will govern the snow properties. These parameters cannot be directly
derived from classical two-dimensional observations.
Other examples where the sample environment is a crucial part of the scientific
case are 1) the investigation of fatigue failure in silicon carbide particle reinforced
aluminum based composites, ([BUF97] and present volume), which employs a
traction machine specially designed for microtomographic experiments, or 2) the
'local tomography' in-situ investigation of an open-cell polyurethane foam at
several levels of compressive strain. This work correlates the macroscopic
behaviour (stress/strain curve) with the local structure modifications. It shows,
during the initial phase of compression (linear elastic response) the struts bending,
and, on a further compression stage (plateau in the stress/strain curve) the collapse a
whole band of cells [WINOO].
3.8. Phase Imaging
It is shown, in another paper of the present volume [Cloetens et al.], that the Xray beams produced at third generation synchrotron radiation facilities exhibit a
high degree of coherence. This allows to use them to record "phase images" by just
varying the sample-to-detector distance ("propagation technique"). The great
advantage of this new type of imagery is the increased sensitivity it provides, in
particular for light materials such as polymers, or for composites made up of
materials with neighboring densities (for example Al and SiC). This implies, of
course, that the spurious contrast due to inhomogeneities of the beamline
components has been eliminated [ESP 98]
Phase microtomography based on the visualisation of the edges was used, for
instance, to understand the mechanisms of degradation in aluminum-SiC
composites. It is possible not only to easily visualize the SiC reinforcing particles,
but also to observe the nucleation and propagation of cracks when the material is
submitted, in situ, to tensile stress. The cracks appear first in the elongated particles,
and this imaging technique has shown that their number is 50% more than suggested
by surface investigations [PEI 97, BUF 97].
Another example of application is the work on quasicrystals. These materials are
non-periodic solids with long-range order, discovered in 1984. Their growth
mechanism and stability is still a controversial topic. While they are not usually
considered as porous materials, the phase images show all the investigated high
quality icosahedral Al-Pd-Mn quasicrystals to contain internal holes, with
dodecahedral shape and orientation reflecting the icosahedral point symmetry of the
host [MAN98]. Their sizes exhibit a discrete distribution. The jump from one size to
56
the next is consistent with the factor t3, where T is the golden mean, a basic
ingredient in all theoretical approaches of quasicrystals. The 3D reconstruction
resulting from phase microtomography shows that the average distance between
neighbouring holes is, again, about T3 times the hole size. The observed features are
in fair agreement with a geometrical approach which describes the quasicrystalline
structure in terms of a hierarchical self-similar packing of overlapping atomic
clusters, such that an inflation scale factor x3 preserves long range order but
generates a hierarchy of holes [JAN 99]. This geometrical approach appears to be
controversial among the concerned scientific community, and further experiments
are being performed to better understand the physical implications of these
observations.
Phase imaging based on the visualisation of the edges is not a quantitative
technique, and its spatial resolution is limited by the occurrence of the fringes used
to visualize the borders. A more quantitative approach of phase imaging and
tomography was recently developed. It is based on the combination of several
images recorded at different distances. An algorithm, initially developed for electron
microscopy by the Antwerp group, was successfully adapted to the X-ray case, and
allows the "holographic" reconstruction of the local phase, well beyond the images
of edges [CLO99a].
Once the phase maps are obtained through holographic reconstruction, there is
no conceptual difficulty in bringing together many maps corresponding to different
orientations of the sample, and in producing the tomographic, three-dimensional,
reconstruction. This combined procedure was applied to a polystyrene foam: for
each of 700 angular positions of the sample, the phase map was retrieved using
images recorded at four distances. The highest accessible spatial frequency is
determined by the resolution of the detector (~2 um our case). Quantitative phase
mapping and tomography ("holotomography") are now operational, and provide a
new approach to the characterization of materials on the micrometer scale
[CL099b].
3.9. Other new approaches in microtomography
The high intensity beams available at third generation synchrotron radiation
facilities are very favorable for X-ray scanning microscopies. In this approach, one
or more selected features of the sample's scattering diagram (diffraction,
fluorescence...) is plotted as a function of the position of the specimen as the latter
is scanned across the beam, to produce a mapping sensitive to crystalline phases,
impurities... Resolution in the micron range is obtained by focusing the beam.
Various focusing elements are currently used (curved mirrors or crystals, Fresnel
zone plates, refractive lenses, tapered capillaries...) to produce very small beams.
This kind of experiments is being extended to three-dimensional diffraction
tomography [KLE98] as well as to fluorescence microtomography, in which trace
57
elements can be mapped inside a sample [SIM99]. These techniques, and their
applications, will surely exhibit a rapid expansion in the next years, in connection
with the enhanced availability of the modern synchrotron sources.
3.10. Conclusion
X-ray microtomography is an invaluable tool to obtain 3D data on a large variety
of materials. The use of a third generation synchrotron radiation source, such as
ESRF, opens up new possibilities. The most important features, as far as absorption
microtomography is concerned, are the very broad choice available of photon
energy (typically between 6 and 120 keV), the quantitative evaluation of the
experimental data made possible by the beam being monochromatic and parallel,
and the improved spatial resolution. Obviously, some of the applications require an
even better spatial resolution. The detection of X-rays is performed through visible
light scintillators. The system is then diffraction limited. A possible way to
overcome this limitation is to use a lens to magnify the image before the scintillator.
Promising attempts have been performed using asymetrically cut crystals, or
parabolic refractive lenses [LEN99].
These techniques are well adapted to in-situ experiments, where the material, in
an adequate sample environment, is imaged as a function of an external parameter
(temperature, stress...). The very small angular size of the source provides, in an
instrumentally simple way, phase images which reveal phenomena hardly visible by
other means. Other approaches, using focus beams, and where diffraction or
fluorescence are measured, are also being developed.
3.11. References
[BRZ99] BRZOSKA J.B., et al. 3D Visualization of snow samples by
microtomography at low temperature. ESRF Newsletter 32, 22-23 (April 99)
[BUF97] BUFFIERE J.Y., et al.. Damage assessment in an Al/SiC composite during
monotonic tensile tests using synchrotron X-ray microtomography Mat. Science
and Engineering A234-236, 633-635 (1997)
[CLO97] CLOETENS P., et al. Observation of microstructure and damage in
materials by phase radiography and tomography J. Appl. Phys. 81, 5878-5886
(1997)
[CLO99a] CLOETENS P., et al. Hard X-ray phase imaging using simple
propagation of a coherent synchrotron radiation beam J. Phys. D: Appl.
Phys.32, A145-A151 (1999)
[CLO99b] CLOETENS P., et al. M Holotomography: quantitative phase
tomography with micrometer resolution using hard synchrotron radiation X-rays
Appl. Phys. Lett., 75, 2912-2914 (1999)
[COL98] COLES M.E., et al. Pore level imaging of fluid transport using synchrotron
X-ray microtomography J. Petroleum Science and Engineering 19, 55-63 (1998)
58
59
Chapitre 4
4.1. Introduction
The purpose of a computed tomography (CT) system is to build a 2D or 3D
representation of the inner structures of an object, from a set of projection
measurements, acquired from a number of points of view. In the case of
transmission CT with X-rays or gamma-rays, the parameter that is reconstructed in
order to represent these structures is the linear attenuation coefficient u of the
object. It is assumed to be proportional, in most non-destructive testing (NDT)
applications, to the mass density (p in g/cm3) regardless of the chemical nature of
the object. Calibration procedures are usually necessary to transform the raw
measurements into quantitative projection data and to correct for X-ray
polychromaticity effects, but they are beyond the scope of this paper. In this paper
we intend to illustrate the basic concepts of reconstruction methods in parallel-beam
geometry, through a simulated example, rather than going into the details of
mathematical developments. References for this paper have been found in
[AMA85], [LEW 83], [CEN 83] and [HER80]. The reader can find a description of
recent developments including cone-beam or spiral CT in, for instance, [HIR97],
[GRA99] or [NAT99].
62
In most NOT systems the source-detector system is fixed and the object moves,
but in order to explain reconstruction methods it is easier to place oneself in a
reference system attached to the object. Let (x,y) be the coordinates of a point M in
the reference system attached to the object. The origin O of this reference system is
at the axis-of-rotation. A source-to-detector ray is defined by parameters (r, 0) where
9 is the angle of the x axis with the perpendicular to the ray, and r is the algebraic
distance from the axis-of-rotation to the ray.
If $) is the number of photons delivered by the source, and <f> is the number of
photons after attenuation by the object, the Beer-Lambert law states that:
[1]
and
Note that (r, o) do not correspond exactly to polar coordinates since generally :
p(o,
for
63
[3]
p(r,o,) = p(-r,0 + x)
[4]
The linear and angular sampling must be fine enough so that the projection data
can be mathematically considered as a satisfactory sampled version of the
continuous Radon transform, and function u, must be null outside the circle
defined by the acquisition system when it rotates. Obviously, real measurements are
not acquired with infinitely thin rays, but each ray has a width that is determined by
the focal spot size of the X-ray source, the detector width, the source-to-object
distance and the source-to-detector distance. Accordingly, the translation step must
be small enough to be consistent with this ray width and with the size of the
structures in the object. The number of angular projections must be between
and 1 4 times the number of pixels per projection.
The simulated phantom is made of a disk with /j = 1 including two elliptic
inserts with // = 2 . The simulation code is based on an analytic computation of the
lengths crossed by the rays in each component of the object. It does not include any
beam-hardening effect or other physical considerations such as scattering or energydependent detector efficiency. Such a realistic simulation code is available in our
laboratory [GLI98], but for the purpose of reconstruction, possible distortions due to
physical effects are supposed to be corrected for by adequate pre-processing of the
projections. We simulated 180 projections of 128 rays per projection, equally
spaced over 180. The reconstructed image is made of 128 x 128 pixels. Figure 4.2
shows the reconstructed image, which can be considered as the reference
representation of the object.
64
If the projections are displayed in grey levels, one below the other, then the 2D
representation which is obtained (figure 4.3) is called a "sinogram" because a point
of the object describes a sinusoid in this representation, in effect, from figure 4.1 it
can be deduced that:
Figure 4.3. Right: sinogram or set of projections over 180 - Left: three projections
It can be seen on the sinogram that the long objects inside the main cylinder are
better detected when they are seen through their longest direction.
Let us assume now that projection data are available, and that the image whose
Radon transform corresponds to these measurement data is unkown.
65
4.3. Backprojection
The first intuitive operation which can be implemented is backprojection. It
consists in assigning to each point of the object the average value of all the
projections at the corresponding location, as illustrated in figure 4.4. The result of
backprojection of the sinogram of figure 4.3 into a 128 x 128 pixels matrix is shown
in figure 4.5.
66
This is illustrated by figure 4.6 and 4.7: figure 4.6 is a horizontal profile of
figure 4.7. Note that for this object the 2D Fourier transform contains 2 principal
components (one vertical and one horizontal) which correspond to the direction the
two ellipses inside the object. The representations of figure 4.6 and 4.7 are discrete
Fourier transforms; they are a valid representation of the continuous Fourier
67
transform only if the Nyquist sampling conditions are satisfied. Let us recall that, if
Ar is the sampling step on the projections, and Nr the number of pixels per
projection, then the discrete Fourier transform of the projection is made of Nr points
and the maximum frequency which can be represented is :
[8]
RdR dO
[9]
The change of variables may seem a little tricky since R varies over ]-oo,oo[ in
the ID Fourier transform of the projection p(R,0} , while R > 0 in the expression
of u(v 1 ,V2)in polar coordinates. Taking into account symmetry properties,
eventually, it comes :
which is the formula of the FBP reconstruction method. The first step of this
methods is :
68
\R\dR
[12]
This is a filtering operation applied to the projection p(r, 6}, the filter being
represented in the frequency domain by /(/?) = R\ . This filter is noted HD because
it is the Hilbert transform of the first derivative. It is also known as the "ramp filter".
69
This filtering operation has the effect of creating negative components on the
filtered projection (see figure 4.8), which will compensate for the contribution of
other projections in the backprojection step (see figure 4.9).
The second step of the FBP reconstruction is :
70
Apodisation tends to reduce noise but also to blur the edges of the structures.
There is a trade-off to find between noise and spatial resolution as shown in
figure 4.11 (a gaussian random noise has been added to the projection data before
reconstruction)
Figure 4.11. FBP reconstruction of noisy data (all three images are displayed
with the same gray scale)
[15]
where p is the vector made of the measurement data,
x is a vector made of all the pixels of the image,
M is the projection matrix.
This can be written :
71
Even though many m^ coefficients are null, the size of the system is generally
huge, and the system is not inverted directly, but using a method iterative by blocks.
A block is a set of rays (or a set of rows in the matrix). Very often, a block will be
equivalent with a "projection", that is to say all the rays for the same rotational angle
(then the method is called the SART technique for "simultaneous algebraic
reconstruction technique"). At iteration q, one block of rays is taken into account,
and the current estimate x^' of x is refined in order to minimize the quadratic
error for the rays of this block :
estimate and the actual measurement Phiock for this block is backprojected in order
to update the image estimate. This can be written :
where
Pi
72
is a relaxation factor, which prevents from going too fast towards the
solution corresponding to the current block, regardless of the other blocks,
mi
is the ilh row of matrix M, it corresponds to the projection along ray i.
This algorithm is made of two basis modules which are projection and
backprojection.
Projection : pi (q) = <mi,x ( q ) > = mij xj(q}
[22]
j
is the computed projection of the estimate X
along ray / (at the iteration q)
Backprojection :
[23]
[24]
k on ray i
Figure 4.14. Horizontal profiles across the images reconstructed from 3 projections
73
74
The vertical ellipse, which is in the direction of the projections used for the
reconstruction, can be seen on projection 9 = 0 (see figure 4.3), on the SART
reconstructed image (profile 1), and hardly on the backprojected image (profile 1).
The backprojected image is not quantitative, it has been divided arbitrarily by 50 in
order to be comparable to the other profiles. The SART reconstruction provides a
value of // which is at least of the good order of magnitude. The backprojected
image, and in a better way the SART reconstruction, also provide an information
about of the depth of this ellipse within the object. The quality of this information is
very dependent of the maximum angle between the projections (here, 60).
The horizontal ellipse cannot be located nor quantified since measurement data
along its main axis have not been used for this reconstruction.
This example is of course very simple, but it shows the potentialities of
reconstruction from few view angles, for instance for the detection of defects in
homogeneous media.
4.8. Conclusion
This paper has introduced basic FBP and ART methods in parallel beam in 2D
for the reconstruction of an image from its projections. Adaptations of these
algorithms are necessary in most applications in order to use ID or 2D detectors.
Simulated results for conventional CT and for very few (3) projections have been
shown.
4.9. References
[AMA 85] AMANS J.L., CAMPAGNOLO R.E., GARDERET P., Imagerie medicale :
methodes de reconstruction et techniques instrumentales, Note technique
CEA/LETI/MCTE N1511 du 10 dec 85.
[CEN 83] CENSOR Y., "Finite Series-Expansion Reconstruction Methods",
Proceedings of the IEEE Vol 71 N3 March 1983 p 409-419
[GLI 98] GLIERE A., "Sindbad: From CAD model to synthetic radiographs", Rev.
Of Progress in Quantitative Nondestructive Evaluation, Vol. 17A, 1998, pp 387394.
[GRA 99] GRANGEAT P., "Fully three-Dimensional Image Reconstruction in
Radiology and Nuclear Medicine", to be published in Encyclopaedia of
Computer Science and Technology.
[HER 80] HERMAN G.T., Image reconstruction from
projections: the
fundamentals of computerized tomography, Academic Press, New York, NY
1980.
[HIR 97] HIRIYANNAIAH H.P., "X-ray Computed Tomography for Medical
Imaging", IEEE signal Processing magazine, p 42-59, march 1997.
75
Chapitre 5
Study of materials
in the semi-solid state
A synchrotron X-ray source (ESRF, FRANCE), has been used to investigate the
microstructure of semi-solid materials. Two kinds of materials have been
investigated, Al-Cu alloys with a high volume fraction of solid to study hot tearing
and an industrial 356 alloy (Al-Si) which is the common material used for semisolid forming. Two imaging modes have been used, the absorption mode for the AlCu material and the phase contrast mode for the Al-Si. Discussion is presented on
the interest of such a technique to characterise semi-solid microstructures.
5.1. Introduction
The semi-solid state is a specific state in which the solid and the liquid phases
coexist. This state is obtained for every alloy with a solidification interval when it is
solidified from the liquid state (such as in the continuous cooling of metals), or
when it is reheated from the solid state (such as in semi-solid forming). In the first
case, during the solidification of the material, cracks can be generated in some alloys
(Al-Cu alloys in particular) owing to the deformation of the solid phase [FRE 79]
which leads to hot tearing. This phenomenon is not fully understood from a
theroretical point of view. The second case (reheating from the solid phase) is
related to the forming in the semi-solid state which is a competitive forming process
compared with liquid injection [Gffl 96]. This process involves the forming when
the material is reheated between the solidus and the liquidus with a solid fraction
close to 0.5. For the moment the alloys used in this technique are aluminum-silicon
alloys like 356 and 357 which are hypoeutectic alloys. The main advantage of this
process is to provide laminar filling of the mould during injection which avoids any
78
porosity formation and therefore allows to produce thin parts which can be heat
treated in addition to increase their mechanical properties.
Figure 5.la presents the microstructure of an Al-Cu alloy quenched from the
semi-solid state (T=570C). At this temperature the volume fraction of the solid
phase was 0.8. The solid phase is in grey and the black phase is the eutectic mixture
which was liquid when the material was in the semi-solid state. In the following the
eutectic will often be designated by the liquid. In this material, the solid phase can
be described as globules surrounded by the liquid. Figure 5.1b presents the
microstructure of an Al-Si alloy also quenched from the semi-solid state. The solid
phase is also surrounded by the fine eutectic mixture (which was liquid in the semisolid state). As previously, the solid phase can be described as globules embedded in
the eutectic liquid. Some liquid droplets are also observed in the solid phase.
Figure 5.1. Typical microstructure of (a) an Al-Cu alloy (b) an Al-Si alloy
79
connections between particles. However, it must be noticed that this paper presents
the very first 3D images of a reasonable volume. Finally the last study published on
3D images of semi-solid materials is by [NlR 98]. This paper shows 3D images of
some solid particles obtained from an 2xxx alloy. The technique employed is the
same as that of the other papers except that the precision is higher, around 10
microns for the section spacing. However, there is no attempt in this paper to study
the connectivity of the solid phase and only few solid particles have been
investigated. Therefore, 3D characterisation of solid phase in semi-solid materials is
now becoming necessary to better understand microstructural evolutions, like
Ostwald ripening and coalescence processes, and deformation mechanisms. The aim
of this paper is to present a new technique which allows to get 3D images of any
semi-solid materials with a high resolution. This technique is high resolution X-ray
tomography carried out at ESRF. This paper will first present the experimental
device and then the materials under study. Finally 3D characterisations of these semi
solid materials will be presented.
80
81
Figure 5.2. Influence of the sample / camera distance on the contrast in Al-Si alloys
82
box in figure 5.3 and connection between globules can appear also as illustrated by
the arrow. Therefore a resolution of 2 microns is at least necessary to get complete
information on the connectivity of the solid phase of industrial semi-solid materials.
83
The last experiment which was conducted was designed to study the evolution of
the microstructure during partial remelting with the same sample. As explained
earlier, it is not possible to perform in situ scan of these materials since the evolution
of the microstructure is very fast. Therefore, we decided to do what we call
84
interrupted in situ scans. A sample is scanned, then partially remelted during five
minutes, quenched and scanned again, remelted again for some time and so on. The
important point here is to put marks on the sample to be able to image the same part
of the sample after the remelting experiments. The sample was studied in the as
received conditions, after 5 minutes remelting at 587C and after 10 minutes. Figure
5.5 presents 2D sections of reconstructed volumes of the same region in the
specimen. It is therefore possible to see the evolution of the microstructure within 10
minutes remelting at 587C. It indicates that the evolution of the microstructure
during the time required for a complete scan is too important to perform real in situ
measurements. The microstructure evolves very rapidly during the 5 first minutes so
that it is difficult to follow the same region. Indeed coalescence of dendrite arms
occurs as generally observed which leads to the entrapped liquid [SEC 84]. Between
5 and 10 minutes, the evolution becomes slower and it is then easy to follow some
groups of globules as those underlined in black in figure 5.5.
85
The main mechanism of this evolution is the well known reduction of the
liquid/solid interface area [VOO 84] and this figure is a real 3D representation of this
mechanism.
We also performed an interrupted in situ test for the Al-Cu alloy. For this alloy,
the air furnace temperature was 555C (the eutectic temperature is 548C) and four
86
cumulated times were analyzed: 5, 15, 30 and 60 min. Figure 5.8 presents a 2D
section of the same sample after 30 and 60 min of partial remelting. As already
mentioned for the Al-Si material, there is an evolution of the microstructure which
obeys the Ostwald ripening process [Voo 84] but the evolution is lower since the
solid fraction is higher. During the partial remelting treatment, the liquid fraction
decreases from the Scheil equation value (0.19) to the equilibrium value given by
the phase diagram (0.1).
87
5.6. References
[FRE 79] H.FREDRIKSSON and B.LEHTINEN, Solidification and Casting of Metals,
1979, p. 260-267
[GHI 96] G. GHIARMETTA , Conference Proceedings of the 4th International
Conference on Semi-Solid Processing of Alloys and Composites, 19-21 June
1996 Eds D.H. Kirkwoodand P. Kapranos, p204-208
[ITO 92] Y. ITO, M.C. FLEMINGS, J. A., Cornie Nature and Properties of Semi-Solid
Materials, eds J.A. Sekhar and J.A. Dantzig, 1992, p3-17.
[VOL 97] T.L. VOFLSDORF, W.H. BENDER, P.W. VOOHREES, Acta Mater. vo145,
n6, 1997, p 2279-2295
[Nm. 98] B. NlROUMAND , K. XlA, Conference Proceedings of the 4th International
Conference on Semi-Solid Processing of Alloys and Composites, June 1998
p637-644
[BUF 98] J.-Y. BUFFIERE, E. MAIRE, P. CLOETENS, J. BARUCHEL, R. FOUGERES,
Chapitre 6
6.1. Introduction
In this study we have investigated the evolution of void volume fraction during
the plastic tensile straining of a particle reinforced metal matrix composite (MMC)
using X-ray microtomography (XMT). Previous studies of void evolution in MMCs
using conventional absorption contrast XMT have been unable to distinguish
between the contribution of void and reinforcement populations [MUM 93a, 95].
Recent work using coherent synchrotron X-radiation has been able to use phase
contrast to image individual reinforcement particles in model MMCs [BUF99].
However, this was only achieved with a model MMC containing very large SiC
reinforcement of diameter > 200 am.
90
91
where p is the density of the component in the voxel, r is the specimen thickness and
I and I, are the intensities of the incident and transmitted beam respectively. Note
that because a void has a mass absorption coefficient taken to be zero, it is not
included in the above calculation. Equation 2 can be rewritten for the second X-ray
energy E2 and combined to give a solution for the local particle component density:
This calculation is carried out on the X-ray intensity values collected at each
specimen position. This results in "intensity of density" values on which
reconstruction is carried out directly yielding voxel particle density:
Ip=exp-[Joppdx|
[4]
The above equations 2-4 can also be solved for pm. Once the values of pm and
pp are known for an individual voxel, the void content of that voxel can also be
calculated by
[5]
Pp
Pm
where pp' and pm' are the theoretical densities of the particles and reinforcement.
92
Dual energy XMT reconstruction was carried out on data collected at X-ray
energies of 17.4 keV and 19.6 keV. These energies correspond to the MoKa and
MoKp characteristic X-ray energies and were chosen because the characteristic count
rates are high. The strong X-ray absorption of ZrO2 restricts the maximum diameter
and reinforcement volume fraction of the specimens that can be examined. Thus, a
maximum reinforcement volume fraction of 7.5% was used which allows a
maximum specimen thickness of about 1mm. The typical data collection time on
these specimens was 14 hours per slice; a minimum of 20 slices with 50 urn
separation between each slice were reconstructed for each specimen examined.
Figure 6.1. Variance of local area fraction of ZrO2 particles in a 7.5% ZrO2 reinforced Al
6061 matrix, plotted against the size of the area used for measurement (logarithmic scale for
both axes)
93
94
Figure 6.3. Reconstruction of a single slice obtained from dual energy XMT measurements on
a fully dense, extruded bar of 7.5vol% ZrO2 reinforced Al 6061 MMC. a) Single energy
reconstruction of absorption density from 17.4 keV and 19.6 keVX-rays either side of the Zr
K-edge. b) Reconstruction of Al and ZrO2 density computed from the data in (a)
95
reconstruction for each of the Al and ZrO2 distribution data sets obtained from the
data of figure 6.3a. It is clear that regions of high ZrO2 density correspond with
regions of low Al density. The reinforcement volume fraction averaged across this
slice was measured at 4.5%. The maximum reinforcement volume fraction of a
single voxel was 56%, which is attributed to a combination of the interpolation
carried out during back-projection reconstruction and the similarity between
reinforcement particle size and voxel linear dimension. The void content averaged
over this slice was measured as 0.4%.
Figure 6.4 shows images of ZrO2 density distribution and total material density
distribution. The void density distribution is the inverse of the total relative density.
These have been calculated from two slices of a dual energy XMT reconstruction
from beneath the fracture surface in the peak aged 7.5% ZrO2 Al 6061 MMC. Slice
numbering is arbitrary with increasing number towards the fracture surface. Both
images in slice 16 show a common feature corresponding to a section of the fracture
surface intersecting the slice. Regions of high void density correlate with regions of
low ZrO2 density as expected.
Figure 6.4. Dual energy XMT reconstructions from a peak aged 7.5vol% ZrO2 reinforced Al
6061 MMC showing ZrO2 particle distribution and totsl density distribution. Two slices are
shown, slice 12 is from the bulk of the specimen while slice 16 intersects the fracture surface:
a) total density distribution (light regions are voids), b) ZrOz density distribution
96
Figure 6.5. Maximum ZrO2 volume fraction measured in an individual voxel on each
reconstructed slice as a function of distance from the fracture surface
97
Figure 6.6 shows the results of variance analysis on both reinforcement and void
distribution within each slice of an XMT reconstruction. The resulting straight lines
have gradients between ~ -0.8 and - 0.5. These are similar, if a little further from the
ideal case of -1, to those found for the distribution of particles on optical crosssections. Thus, we might infer there to be no significant clustering of voids.
However, the algorithm used during filtered back projection reconstruction of an
XMT slice introduces a correlation between adjacent voxels, hence leading to a
reduction in variance at small sampled areas, as can be clearly seen from the gradual
change in slope as the sampled area decreases. This reduces the utility of variance
analysis with this form of tomographic reconstruction algorithm, however, the
absence of any abrupt change in slope suggests that there is no clustering within the
length scales sampled.
Figure 6.6. Variance analysis with gradient of plot, b, shown of a) Zr02 distribution and b)
void distribution, determined from dual energy XMT slice reconstruction data
98
Figure 6.7. Local void content as a function of local reinforcement volume fraction measured
from a dual energy XMT reconstructed slice 300 fjmfrom the fracture surface of a peak aged
7.5vol% ZrO2 reinforced Al 6061 MMC. Linear regression plots are shown for two different
sampled areas
Distance
4x4
6x6
Annealed 7.5% ZrO2 Al 1100
0.25
0.18
50
0.38
0.33
100
0.34
150
0.35
0.29
0.39
200
250
0.35
0.33
0.12
300
0.18
350
0.16
0.27
0.24
0.32
400
0.04
450
0.05
0.21
500
0.05
0.14
550
0.00
0.05
600
0.01
650
0.20
0.09
0.34
0.20
700
0.04
750
0.01
Peak Aged 7.5% ZrO2 Al 6061
50
0.45
0.50
100
0.34
0.35
150
0.42
0.41
200
0.44
0.38
250
0.31
0.30
300
0.60
0.65
350
0.44
0.42
400
0.46
0.43
450
0.37
0.27
500
0.51
0.53
550
0.41
0.46
600
0.01
0.05
650
0.33
0.32
700
0.33
0.29
750
0.33
0.20
99
12x12
16x16
24x24
0.22
0.29
0.41
0.40
0.34
0.09
0.22
0.46
0.08
0.19
0.18
0.02
0.29
0.44
0.07
0.29
0.28
0.21
0.44
0.34
0.19
0.12
0.40
0.18
0.07
0.16
0.18
0.48
0.54
0.06
0.46
0.29
0.25
0.39
0.03
0.22
0.11
0.50
0.08
0.07
0.22
0.10
0.45
0.40
0.23
0.52
0.09
0.04
0.38
0.58
0.43
0.39
0.52
0.38
0.74
0.02
0.71
0.97
0.47
0.79
0.59
0.44
0.43
0.35
0.37
0.70
0.50
0.43
0.33
0.58
0.51
0.13
0.32
0.47
0.20
0.57
0.33
0.18
0.41
0.36
0.85
0.24
0.61
0.15
0.65
0.76
0.30
0.06
0.33
0.88
0.88
0.45
0.60
0.40
0.27
0.89
0.43
0.43
0.08
0.73
0.74
0.32
0.30
0.57
0.24
0.81
0.38
0.83
0.66
0.89
0.95
0.34
0.99
0.24
0.74
0.90
0.37
0.89
0.32
0.62
Table 6.1. Linear correlation coefficient between local reinforcement volume fraction and
local void fraction as a function of distance from the fracture surface and different sampling
areas
100
Let us now consider the evidence for any relationship between local particle
volume fraction and local void volume fraction in these materials after straining.
These materials were produced by powder metallurgy and our analysis of the
particle distribution using a Richardson (variance) plot indicates a self similar
distribution with fractal dimension between 2 and 3. There is no apparent change in
slope seen on the plot over the range of sampled areas selected and thus no
significant change in distribution character. Similar random distributions are seen
when the XMT data of void and particle distribution are analysed, with the caveat
concerning possible autocorrelation introduced during reconstruction. Linear
regression analysis indicates a significant correlation between void fraction and
reinforcement content. However, this correlation is independent of plastic strain and
sampled area. Thus there is no evidence for either an increased void nucleation rate
or growth rate in regions of higher local reinforcement content. Our results are
consistent with a model of random void nucleation at particles and subsequent
growth independent of local environment; i.e. there is greater void volume in regions
of high reinforcement content purely because there are more nucleation sites.
These results only apply to our materials with random particulate distributions
and may not apply to highly clustered MMCs obtained by casting routes [LLO 91].
There is some evidence from acoustic emission experiments that artificially
constructed MMC microstructures with reinforcement clusters nucleate damage at
lower strains than random microstructures [BUR 97]. Indeed, there is some very
limited evidence from our results that might support this hypothesis. Highly
clustered regions of reinforcement are rare in our material, but their presence was
identified in the undeformed material where some voxels in the tomographic
reconstruction had reinforcement contents in excess of 50%. Beneath the fracture
surface, we never found any voxels with reinforcement contents greater than 20%.
Thus, the albeit rare regions of high reinforcement disappear after straining. Clearly
more work is required to address the fracture behaviour of more clustered
microstructures during tensile straining.
6.5. Conclusions
Dual energy XMT has been used successfully to determine the spatial
distribution of voids and reinforcement in model ZrO2 reinforced Al alloy MMCs. It
has not been possible to demonstrate the equivalence of reconstructed XMT sections
with coincident metallographic sections, because the system resolution was below
that required to image individual ZrO2 reinforcement particles. However, the ability
to measure local reinforcement density in each reconstructed voxel allowed the
analysis of local particle clustering.
The initial ZrO2 reinforcement distribution appears to be random and with no
significant clustering as determined by variance analysis. Void distributions after
straining had similar properties. Unfortunately because of correlations introduced by
101
[BUF 99] BUFFERS J.-Y., MAIRE, E., CLOETENS P., LORMAND G. and FOUGERC R.,
Acta Mater, vol. 47, p. 1613 (1999).
[BUR 97] BURDEKIN N.A., STONE I.C. AND MUMMERY P.M., presented at 4th Inter.
Conf. Compos. Eng. (1997), unpublished.
[ELL 90] ELLIOT J.C., ANDERSON P., DAVIS G.R., DOVER S.D., STOCK S.R.,
BREUNIG T.M., GUVENILIR A. AND ANTOLOVICH S.D., /. X-Ray Sci. Tech. vol.
2, p. 249(1990).
[ELL 94] ELLIOTT J.C., ANDERSON P., DAVIS G.R., WONG F.S.L., and DOVER S.D.,
JOM-J. Min. Met. Mater. Soc. vol.46, p. 11 (1994).
[HIL 61] BILLIARD J.E., CAHN J.W., Trans. Metall Soc. AIME vol. 221 p. 344, 1961.
[KOZ 99] KOZUL N., DAVIS G.R., ANDERSON P. AND ELLIOT J.C., Meas. Sci.
Technol. vol. 10, p. 252 (1999).
[LI 92] LlQ.F., SMITH R., McCARTNEY D.G., Mater. Char. vol. 28 p.189 1992.
[LLO 91] LLOYD D.J., in Metal Matrix Composites - Processing, Microstructure and
Properties, Proceedings of the. 12th Ris0 Inter. Symp. Mater. Sci., p. 81 1991
Ris0 National Lab., Roskilde, Denmark.
[MUM 93a] MUMMERY P.M., ANDERSON P., DAVIS G.R., DERBY B. and
ELLIOTT J.C., Scripta Metall. Mater, vol. 29, p. 1457 (1993).
[MUM 93b] MUMMERY P.M. and DERBY B., in Prcoeedings of the 9th International
Conference on Composite Materials. , Vol. 1, Metal Matrix Composites, p. 424,
1993, Woodhead Publishing, Cambridge, UK.
[MUM 95] MUMMERY P.M., ANDERSON P., DAVIS G.R., DERBY B. and
ELLIOTT J.C., J. Micros, vol. 177, p. 399 (1995).
[WOR 96] WORRALL C.M., WELLS G.M. Proceedings of the European Conference
on Composite Materials, London, p. 247 1996.
Chapitre 7
Characterisation of MMCp
and cast Aluminium alloys
This paper describes recent results on the application of high resolution X-ray
tomography to the study of metal matrix composites and cast aluminium alloys. The
advantage of phase contrast X-ray tomography over classical attenuation X-ray
tomography is shown in the case of an Al/SiC metal matrix composite. The
possibility of studying in situ damage initiation and development within a material
under stress is also illustrated. Finally, examples of quantitative results extracted
from reconstructed three dimensional images are given with respect to
microstructure and damage characterisation of different structural materials.
7.1. Introduction
Almost all structural materials contain micro-heterogeneities such as precipitates,
reinforcing particles, holes, etc. Generally the mechanical properties of those
heterogeneities are different from those of the base material (the matrix). Therefore,
those heterogeneities form a preferential site for the nucleation and development of
damage inside structural materials under stress.
Ceramic reinforcements can be added, for instance, to a metal matrix in order to
obtain a Metal Matrix Composite (MMC) with a high specific elastic modulus.
However, the co-existence of a brittle material with a very ductile matrix induces
some elastic and plastic incompatibilities which result in poor fracture properties. A
lot of attention has been paid to the investigation of the damage mechanisms of
Metal Matrix Composites (MMC) under stress. However, most of the work carried
out so far relies on surface observations of samples mainly because experimental
104
evidences of the damage mechanisms occurring in the bulk of the samples are rather
difficult to obtain.
Another example of micro-heterogeneous structural materials are cast aluminum
alloys. These materials offer various advantages over wrought aluminium alloys
when one is concerned with the manufacturing of an object with a very intricate
shape, like, for example, hollow shapes. However, aluminium, like other metals,
contracts when it solidifies and besides, hydrogen dissolves very easily in the molten
metal. Therefore, unless special (expensive) processing methods are used, aluminium
cast objects always contain a certain amount of porosity. These pores are a major
problem because of their detrimental effect on the mechanical properties of the
finished object. For this reason, a lot of research is being carried out on the study of
porosity in cast aluminium alloys and on its influence on mechanical properties.
However, like in the case of MMCs, the characterisation of porosity in cast alloys is
quite difficult to achieve experimentally through classical metallographic
examination.
For the moment, X-ray Computed Tomography (XRCT) is the only non
destructive characterisation technique which provides direct images of the bulk of
heterogeneous materials. As a matter of fact, this method has been used extensively
in medicine for years, but the low resolution of the images obtained (around 100 um)
impeded its use in materials science. In the last ten years, however, the use of
synchrotron X-ray radiation coupled with new detectors has opened new possibilities
in this field. 3D images of the interior of micro-heterogeneous materials have been
obtained with a resolution of a few microns (see for example [CLO 97] for a
review).
In this paper we present some recent results in the study by XRCT of damage
initiation and development inside a notched sample of MMC. The aim of the
experiment is to evaluate the influence of the non uniform stress state on damage
development within the material. Moreover, the same technique has also been used
for the characterisation of model cast alloys. Some quantitative results on the
description of the pore population in these alloys are shown.
7.2. Experimental methods
7.2.1. Materials.
7.2.1.1. Al/SiC composite
The composite studied in this work was a 6061 Al alloy reinforced by a 10 %
volume fraction of SiC particles. The average size of the reinforcement, 120 fam, was
large compared to industrial material. This size had been chosen in relation with the
resolution of the 3D imaging technique (see below). The average aspect ratio of the
particles was 1.6. The material was processed through a rheocasting route under
105
nitrogen and was subsequently extruded at 813 K with an extrusion ratio of 16 and a
ram displacement rate of 100 um.s"1. The extruded bars were solutionised at 803 K
for 2 hours, quenched in water and matured at room temperature for 2 weeks (T4
heat treatment) before testing.
7.2.1.2. Al cast alloys
Three different model Al cast alloys have also been studied and characterised by
X-ray tomography. The nominal composition of the three alloys is given in table 7.1.
Those alloys were chill mould cast by Pechiney. Different amounts of hydrogen (H2)
and Argon (Ar) gases were introduced in the melt thanks to a propeller. At the
beginning of solidification, part of the gas content was rejected and formed artificial
pores. By varying the H2/Ar ratio (2%, 7% and 10%) three different average sizes of
pores were obtained for each alloy (alloy A, B and C, respectively). Thin cylinders
(diameter 3mm) were machined from the ingots for XRCT characterisation. The
volume of material investigated during each scan was around 170 mm3.
Si
Fe
Mg
Ti
Sb
6.6-7.0
0.09-0.14
0.29-0.34
0.11-0.14
0.12-0.14
Cr
<0.01
Others
<0.01
Figure 7.1. Schematic view of the experimental set up used for the tomography experiments
on line ID 19 at ESRF. Note the unusual large distance between source and detector which
results in a large coherence of the X ray beam.
106
studied specimen which stands on a rotating stage. The transmitted X-ray beam, is
converted into visible light before being recorded by a 1024*1024 CCD detector
specially designed at ESRF. A tomographic scan comprises 600 2D projections of
such type. They are obtained by a 180 rotation of the sample around its vertical
axis with a 0.3 step. Those projections are used to reconstruct a 3D numerical
image of the sample through a classical filtered back projection algorithm [ROB 99].
The voxel size in the reconstructed volume, fixed by the experimental setting of the
detector, was about 6.5*6.5*6.5 um3 for the materials studied in this work.
In classical tomography, the contrast obtained on the reconstructed images
comes from differential X-ray attenuation between the constituents of the studied
material. The pores in the studied cast al alloys show an X-ray attenuation very
different from the matrix. Therefore, they give a good contrast on the 2D projections
and in the reconstructed images.
The case of the Al/SiC composite is slightly more problematic as the X ray
attenuation of the SiC particles is very close to that of the matrix. Thus, the contrast
of the SiC particles in the reconstructed images is very faint. This is illustrated on
figure 7.2a. To circumvent this problem, the so called phase contrast tomography
has been used. This technique, which is based on the high coherence of the X-ray
beam on line ID 19, greatly improves the detection of SiC particles (see figure 7.2b).
It has been shown, besides, that the phase contrast also enhances the detection of
damage (cracks) within reinforcements in MMCs [BUF99].
Figure 7.2. Reconstructed images of two different cross sections of the studied Al/SiC
composite obtained by a) attenuation tomography and b) phase contrast tomography. On the
left, the contrast given by the SiC particles is very faint because of the small difference in Xray attenuation between SiC and Al. Reconstruction rings are also visible because the
contrast of the image has been enhanced to visualise the SiC particles. On the right, thanks to
the phase contrast technique available on ID 19 beamline at ESRF, the contrast between
matrix and reinforcement is enhanced by the presence of bright/dark fringes at each
particle/matrix interface. Those fringes are obtained by simply setting the CCD detector at 83
cm behind the sample
107
108
already observed for the same material during tensile test on a smooth sample [BUF
99]. The evolution of the cracked particles spatial distribution within the sample, all
along the test, is shown on figure 7.4.
Figure 7.3. Reconstructed images of the same internal section of the AlSiC sample at step 0,
1 and 2. The arrows indicates the presence of a crack in a SiC particle at the root of the
notch where the stress level is high
It can be seen, on that figure, that the particles tend to break first near the root of
notch where a higher stress level is obtained. When the stress is increased, however,
the size of the volume containing the cracked particles steadily increases.
The presence of a tri axial state of stress in the studied sample is generally
believed to alter the mode of damage, by promoting particle matrix decohesions
[CLY93]. In our case, however, the mode of damage ( mode I particle cracking)
seems to be the same as that observed in a smooth sample in the same deformation
conditions. At least two effects can account for this observation. One is related to the
phase contrast technique. A thin interfacial crack between matrix and reinforcement
would give an extra fringe in the reconstructed image which would probably be quite
difficult to detect with a 6.65 urn resolution. The second reason is related to the
material itself. In MMCs indeed, a large size of the reinforcements is known to
promote particle cracking at the expense of other damage modes. Thus, the large size
of the SiC particles studied here are likely to favour only the particle cracking as
damage mechanisms in the early stages of straining. Further work with a material
109
containing smaller particles (around 20 urn) and with a higher (2 urn) resolution
should help to clarify this point.
Figure 7.4. 2D projection (as indicated by the arrows on the 3D sketch on the right) of the
SIC particle centroids in the reconstructed volume of the material. The different symbols used
on the figure indicate at which step a particle broke. The tensile stress was applied vertically.
The superimposed square indicates approximately the zone where a higher number of broken
particles was found at the first stages of deformation
110
111
images. The binary images have been studied by automatic 3D image analysis. Two
stereological parameters have been defined to try and characterise the shape and size
distributions of the pores. The first one, called the equivalent size, is defined as the
diameter of a sphere which would have the same volume as the considered pore.
The second one, called the sphericity s, is defined from the ratio of the volume of
the pore to its surface. A perfect sphere would have a sphericity parameter of 1
while a pore with a very tortuous shape would have a sphericity much smaller than 1
[SAV 98].
Figure 7.5. Reconstructed images of internal pores in two model cast aluminum alloys.
Artificial pores have been obtained by introducing H2 and Ar gases in the melt metal. As the
solubility of hydrogen decreases with temperature, when the metal solidifies, H2 is rejected
and forms gas pores which are easily visualised using X-ray tomography. Two different
H/Ar ratio have been used: 2% (left) and 7% (right). The edge size of both cubic boxes is
1.33 mm
Figure 7.6 shows a plot of those two parameters for the three investigated alloys.
It can be seen from this figure that at least two population of pores (cooresponding
to two clouds of points on the plot) can be found in the material. The first one, in the
lower part of the plot (equivalent size lower than 50 um), shows a weak correlation
between shape and sphericity and is represented for the three alloys. The second one
on the contrary can be found for sizes larger than 50 um and shows a strong
correlation between size and shape. The volume fraction of the pores belonging to
this last population can be seen to increase when the amount of hydrogen introduced
in the liquid metal is increased.
The two populations have different origins. One corresponds to microshrinkages when the metal solidifies while the other corresponds to artificial gas
pores. The latter appears during the whole solidification process while the former
appear at the end of it. Both types of pores have to form between the growing
dendrite arms network. Thus the growth of large pores is geometrically hindered by
112
the dendrites and the resulting shape is tortuous (low sphericity). By analysing
carefully the data it is possible to show [SAV 00] that the volume fraction of microshrinkage pores remains roughly constant for the three investigated alloys while the
volume fraction of gas pores increases exponentially with the H2 content as already
observed in the literature.
Figure 7.6. Plot of the equivalent size of the pores inside alloys J, K and L, as a function of
their sphericity. Two populations of pores can be seen respectively below and above an
equivalent size of about 50 jam. Those two populations correspond to artificial gas pores
(equivalent size larger than 50 pm) and to micro-shrinkages (below 50 /jm)
7.4. Conclusion
We have shown in this paper how X-ray tomography can be used to study
quantitatively structural micro heterogeneous materials. Two examples have been
given corresponding to the case on an Al/SiC particulate metal matrix composite
and to model cast aluminium alloys. Although 3D X-ray images of internal pores in
cast alloys are quite easy to obtain thanks to the large X-ray attenuation difference
between gas pore and aluminium matrix, the visualisation of the SiC reinforcements
in an aluminium matrix is not possible with classical tomography. In that case, it is
necessary to use phase contrast tomography which can be obtained with a coherent
X ray beam like the one delivered on the ID 19 beamline at ESRF. This technique
also improves the detection of damage in reinforcements.
With regard to the composite material, it was possible to follow the initiation and
development of damage inside a notched sample during in situ tensile deformation.
113
No influence of the tri axial stress state could be found on the mode of damage
(mode I cracking of the particles) which appears to be localised near the notch root
at the begining of the deformation process. By coupling the 3D data on the SiC
particles and analytical calculation a Weibull analysis of the particle fracture was
carried out, leading to Weibull modulus of 3.2 and a a0 constant of 1000 MPa.
For the model cast aluminium alloy, the 3D data obtained by tomography has
been used to characterise the pore population for three different processing
conditions. From this characterisation it is possible to distinguish between degassing
pores and micro-shrinkage pores.
7.5. References
[CLO 97] CLOETENS P., et al. Observation of microstructure and damage in
materials by phase sensitive radiography. Journal. Appl. Phys. 81,9 p.5878,
1997.
[ROB 99] ROBERT-COUTANT C, et al. Introduction to reconstruction methods
This Workshop.
[BUF 99] BUFFIERE J.-Y., et al. Characterisation of internal damage in a MMCp
using X-Ray synchrotron phase contrast microtomography Acta Mater. 47, 5,
pp.1613-1625, 1999.
[CLY 93] CLYNE T.W., WITHERS P.J., An Introduction to Metal Matrix
Composites Cambridge University Press, 1993.
[MIC 98] MICHOUD P., DARSONVILLE F., Segmentation et visualisation d'images
3D application par croissance de region a I'imagerie medicate dentaire PhD
thesis Saint EtienneUniversity June 1998.
[LEW 95] LEWIS C.A., WITHERS P.J., Weibull modelling of particle cracking in
metal matrix composites Acta metall. mater., 43, 10 1995.
[SAV 98] SAVELLI S., et al. Characterisation by synchrotron X-ray
microtomography of internal features and their detrimental effects with respect
to the fatigue properties in aluminium cast alloys Proc. of ICAA 6 Toyobashi
Japan p.529 1998 .
[SAV 00] SAVELLI S., PhD thesis INS A Lyon 2000 to be published.
Chapitre 8
The High resolution X ray tomography technique has been used to investigate
the internal structure during the deformation of two very different materials : an Al
foam and a SiC fibre reinforced titanium matrix composite. The observations show
that the metallic foam deforms via local buckling events. This collapse mechanism
is also studied by means of a modelling technique based on the finite element
method. The microstructure of the metal matrix composite is also easily revealed
with a sifficient resolution despite the high attenuation of the matrix. Cracks can be
observed during the straining on a fibre touching the surface of the sample. It was
not possible to show if this preferencial rupture was due to the weakness of this fibre
or to the stress field which is different close to the surface.
116
117
slice. For the present application, N was set to 900. A second stepping motor then
generates a translation of the sample along a direction parallel to the rotation axis
and a new adjacent slice can thus be imaged. The acquisition of the data
corresponding to a single slice lasts about 3 min.
Figure 8.1. Schematic description of the experimental setup for the tomograph used
Reconstruction is achieved using a C-language program written by the CEALETI (Commissariat a 1'Energie Atomique - France) and based on the Feldkamp
algorithm [FEL 84]. A ramp filter is selected, thus preserving the spatial resolution.
A DEC 500 MHz workstation is used to reconstruct the entire volume, slice by slice.
Reconstruction of the complete volume (350 x 340 x 128 voxels) lasts
approximately 1 hour.
We have translated the sample of 300 (jm between each slice in z, a value which
corresponds to the height of the diodes. In order to get an isotropic 3D
representation of the sample (i.e. reduce the resolution in the z direction to 150 |jm ),
we have numerically added extra slices in between the slices in z. We calculated the
grey level in these extra slices by linearly interpolating the grey levels in the
corresponding x, y voxels of the two adjacent slices.
8.2.1.2. Results
The sample was scanned for tomographic analysis in its initial state. It was then
compressed at three increasing values of remnant strain (true strain measured after
unloading). The internal microstructure was imaged using tomography at these three
steps after removal of the compression load. We then have a picture of the interior
118
of the sample at four values of the remnant true strain in compression: 0, 0.065, 0.2
and 0.6.
A 3D view of the analysed sample is shown in figure 8.2. The cell walls are
clearly imaged and the 3D structure can be analysed. However, it is quite difficult to
visualise the deformations with this kind of representation especially in the of closed
cells for which the outer walls hide the inner ones. In what follows the qualitative
results will be shown under the form of 2D reconstructed slices which are easier to
analyse. Figure 8.3 (a and b) show a set of 2 D images of the same zone of the
sample numerically extracted from the volume at 0 to 6.5 % of remnant strain
respectively. These slices are parallel to the compression axis which is vertical on
the figure. One can clearly observe the deformation mechanism of the studied foam
in compression by comparing these two figures. The large value of the plastic strain
at this stage is obviously not due to a homogeneous plastic straining of the whole
sample, but to the local buckling of several walls like these surrounded by circles on
the picture. From the observation of the entire population of buckled walls, we have
observed that they are located in a band perpendicular to the loading axis (see figure
8.3b) i.e. the centre of gravity of these buckled walls is located in a narrow range in
the z dimension (roughly between z=60 and 100 pixel compared to a total height of
255 pixel for the sample).
Between the second and the third step, the number of new buckled walls is
small. The deformation process leads to the complete closing of the already
collapsed cells instead of the appearance of new ones. Some new collapsed cells can
be seen in step 3, but even at this very large plastic strain, some regions of the
sample are not deformed at all.
119
Figure 8.3. Part of a 2D reconstructed slice of the same zone at two deformation steps
initial state (left) and 6 % (right)
120
121
122
123
The sample used for this study was made of three layers of monofilamenatry SiC
fibers embedded into a titanium matrix. The schematic geometry of the sample is
shown in figure 8.5. The initial state was characterised using the tomographic setup
described above. The results are shown in figures 8.6 and 8.7 under the form of 2D
reconstructed tomographic slices along the 3 principal directions of the sample
according to the geometry defined in figure 8.5. The internal structure of these
composites can be clearly imaged at the resolution of 6.65 um used for the present
study.
8.3.1.3. Tensile rig and testing procedure
A tensile rig has been especially designed to allow the observation of damage by
tomography during the deformation of materials [BUF 99]. This rig can be set on
the turntable. In order to avoid the frame of the machine to hide the beam when
rotation is necessary (for the tomographic inspection) a PMMA tube is used to
transmit the load between the upper mobile grip and the lower fixed grip. This tube
was carefully polished and gave negligible attenuation nor phase contrast on the 2D
radiographs. The force and the crosshead displacement were recorded on a
computer and monitored during the test.
A crosshead displacement rate of 150 um.mn 1 was used for the tests
corresponding to an average strain rate of 5.10 s'1. Once sample 1 was set in the
machine, a first radiograph was recorded in order to characterise the initial state.
The sample was then loaded step by step in tension : during the test, the crosshead
displacement was stopped at increasing values of the deformation and a radiograph
was recorded during each of these steps.
8.3.2. Results
Figure 8.8 shows the observation of the evolution of damage during the straining
of the sample. After the first step, one fiber was broken in two locations. After the
second step, the same fiber was broken in a third location. These were the only
visible events detected during the straining which then had to be stopped because
the sample was too strong compared to the limited capacity of the tensile rig. The
fiber which broke was this at the bottom left corner of the sample in figure 8.6. This
fiber was the only one cut by the free surface. It is not clear if the early damage of
this fiber is due to the fact that its intrinsic resistance was reduced because of pre
damage during the sample preparation or if the stress field inside this fiber was
modified by the effect of the presence of the surface.
Figure 8.8. 2D reconstructed tomographic slices showing the evolution of the microstructure
of a same zone for the three steps of the tensile test: inital step, fisrt step (center) and second
step (right)
125
with a much higher resolution (6.65 urn in the resent case). This resolution was
achieved using synchrotron radiation. The observation of damage was carried out in
tension. Unfortunately, the sample was too strong for the tensile rig, but the
observations made during this primarily experiment are promising. We were able to
visualise several ruptures in a same fibre at different steps during the test.
Acknowledgements
The tomographic scans on the Al foam were performed with the help of G. Peix
using the equipment of the CNDRI laboratory in Villeurbanne. The Ti/SiC samples
were provided by Alex Madgewick and Phil Withers from the UMIST in
Manchester and the tomographic scans were made at ESRF in collaboration with
J. Baruchel and P. Cloetens.
8.5. References
[BAR 98] H. BART-SMITH, A.F. BASTAWROS, D.R. MUMM, A.G. EVANS,
DJ. SYPECK, and H.N.G. WADLEY. Acta mater. (1998). 46, N 10, PP 35823592.
[BUF 99] J.-Y. BUFFIERE, E. MAIRE, P. CLOETENS, G. LORMAND, R. FOUGERES.
Characterisation of internal damage in a MMCp using X-ray synchrotron phase
contrast microtomography. Acta Met. (1999) vol. 47, N5 pp 1613-1625.
[CEN 99] CENDRE E., DUVAUCHELLE P., PEIX G., BUFFIERE J.-Y. and BABOT D.
Conception of a high resolution X-ray computed tomography device ;
application to damage initiation imaging inside materials. Proceedings of the 1st
World Congress on Industrial Process Tomography (1999) BUXTON (U.K.),
14-17avril.
[CLO 97] P. CLOETENS, M. PATEYRON-SALOME, J.-Y. BUFFIERE, G. PEIX,
J. BARUCHEL, F. PEYRIN, J. SCHLENKER. J. Appl. Phys. (1997), 81,9.
[DAY 83] G.J. DAVIES and S.J. ZHEN. Mater sci. (1983), 18, 1899.
[PEL 84] L.A. FELDKAMP, L.C. DAVIS, J.W. KRESS. Practical cone-beam
algorithm. J. Opt. Soc. Am. (1984), 1 N 6, pp. 612-619.
[KAK 88] C. KAK, M. SLANEY. Principles of Computerized Tomographic Imaging.
(1988). Cotellessa RF (Editor). New York : IEEE Press (Phs).
[KAF 96] V. KAFTANDJIAN, G. PEIX, D. BABOT and F. PEYRIN. J. of X ray Science
and Technology (1996). 6, 94.
[MCC 99] K.Y.G. McCuLLOUGH, , N.A. FLECK and M.F ASHBY. Toughness of
aluminium alloy foams. Acta Mater. (1999), 47 pp. 2331-2343.
Chapitre 9
Simulation tool
for X-ray imaging techniques
9.1. Introduction
X-ray imaging techniques, such as radiography, radioscopy and tomography, are
used in a wider and wider range of specific applications, notably in the medical field
and in materials science [PEL 89][PEI 97]. To develop new imaging systems, or
optimise existing ones, it is generally necessary to carry out long and expensive
series of tests and measurements. Proceeding in such a way, by trials and errors,
often reveals itself unrewarding because it is practically difficult to study the
influence of the many parameters (beam energy, focal spot size of the X-ray tube,
detector type, geometric parameters, etc) that condition the final image quality.
128
9.2. Background
Our simulation software requires various input data, intended to describe an
experimental situation with maximum accuracy. From the geometric point of view,
we have to define the source (shape, size, position, orientation), the detector
(position, orientation, pixel number and size), and the sample. The use of a
computer aided drawing (CAD) model describing the object offers great advantages:
complex 3D samples can be drawn in a short time with automatic surface mesh
generation (triangular meshes), and with high accuracy. The object may consist of
several parts, possibly of different materials.
Ray-tracing techniques, together with the X-ray attenuation law, are the basis of
our computer code. From each source point, a set of rays is emitted towards every
pixel centre of the detector. Each ray may intersect a certain number of meshes on
the object surface (fig. 9.1). The attenuation path length in every object phase is
calculated by determining the coordinates of all those intersection points. The
photon number N(E) that emerges from the sample and reaches the detector
surface is given by the attenuation law:
N(E) = N0(E) A0Q[])xp[-//,()*,.]
[1]
129
where N0(E) refers to the number of photons with energy E, emitted by the source
per solid angle unit, AQ is the solid angle corresponding to the pixel, observed from
the source point, ui(E) designates the attenuation coefficient associated to the
material i at energy E, and xi the total path length through the material i.
The image computed by using equation [1] does not take into account the
contribution of scattered photons. Moreover, the simulated image does not contain
any photon noise. So far, we have used a perfect detector, in which every pixel is
able to count all of the photons that hit its surface. The Compton and Rayleigh
scattering contributions to the image and the photon interactions with a real detector
will be investigated in a future work [DUV 98].
Figure 9.1. Principle of radiography simulation. A point source, a matrix detector, and a
CAD model of the object with triangular meshes are used
130
Figure 9.2. Simulation of geometric unsharpness. The sample is a thin square plate with a
circular hole 1 mm in diameter. The detector is composed of 80 x 80 square pixels, 0.1 mm
wide. Simulation A: point source (geometric unshrapness UA = 0 mm); B: 1 mm wide square
source (UB = 1 mm); C: 2 mm wide square source (Uc = 2 mm). The grey level profile
corresponding to the central column of the detector is presented in each case. The profile C
reveals a degradation of the image contrast, due to geometric unsharpness
131
132
Figure 9.3. Radiograph simulation of a gate, with a step wedge. A polychromatic beam is
used and the detector is split into 100 energy channels with a 1 keV interval, (a): CAD model
of the gate, (b): Simulated radiograph, (c): Incident beam spectrum, (d): The transmitted
photon spectra associated to the points labelled a to c reveal a beam hardening phenomenon,
stronger where the part is thicker, i.e. close to the edge
133
134
Figure 9.5. Influence of the incident beam spectrum on a reconstructed slice (a):
monochromatic 100 keV beam, (b): polychromatic beam with 100 kV tube voltage. In both
cases, a point source was used, (c): (-n) reconstructed value profiles (n designates the linear
attenuation coefficient). When a monochromatic beam is used (graph A), the baseline of the
profile has a constant value, equal to the value of(-u) associated to aluminium at 100 keV. In
contrast, when the source is polychromatic, the beam hardens itself in the object, causing a
"cupping effect" (graph B)
9.4.2.3D tomography on a complex mechanical part
Finally, we simulated a 3D tomographic system, with a matrix detector,
consisting of 250 x 220 pixels. The whole volume of the object was reconstructed
successfully. As the beam was polychromatic, cupping effect, as well as streaks, are
visible in the reconstructed slices (fig. 9.7).
135
Figure 9.6. Influence of Gaussian photon noise. Gaussian fluctuations have been added to the
sinogram and to the reference image (obtained by performing an acquisition without sample)
before reconstruction, (a): The photon number reaching the central pixel of the detector,
during the first projection, is equal to 50. (b): The photon number is 10 times greater, (c):
Grey level profiles corresponding to the lines labelled A and B
136
Figure 9.7. 3D computed tomography, (a): Schematic view of the simulated setup and CAD
model of the sample. A matrix detector (250 x 220 pixels) and a point source were used. The
dotted lines labelled A, B and C indicate schematically three slices presented on the right (b)
computed images present no photon noise, but Gaussian random fluctuations can be
added afterwards, if needed.
Several issues need further development and will be addressed in the next phase
of our research program. As a priority, we envisage to enrich our simulation tool, by
taking into account the scattering contribution. The 3D mapping of the absorbed
dose in the sample will be broached simultaneously. Modelling and simulating the
influence of the detector response on the image quality will also be an essential task.
Finally, quantitative experimental validations will be necessary.
Possible application areas are numerous. Simulation can be useful, when
developing any specific application, to choose the best components, optimise the
experimental parameters and save time by reducing the number of experimental
tests. Simulation also presents an important potential, to test the performance of
image processing procedures in a virtual environment, where all parameters are
fully controlled.
9.6. References
[BER 88] BERGER, M. J., "MIST Standard Reference Database 8, X-ray and Gamma-ray
Attenuation Coefficients and Cross Sections, XGAM", distributed by Office of Standard
137
"A computer simulation technique to preview the influence of the recording system on
the image sharpness in mammography", Part of the SPIE Conference on Physics of
Medical Imaging, Vol. 3336, p. 602-609, 1998.
Chapitre 10
10.1. Introduction
Metallic foams are porous metals with high porosity (from 50 to 99 %). In the
past few years there has been a considerable increase in interest for metal foams,
especially made of aluminium or aluminium alloys. The unique properties of
aluminium foams like high stiffness to weight ratio, high energy dissipation, low
density, reduced acoustic, thermal and electrical conductivity, chemical resistance,
easy recycling etc..., make them potentially useful in many high technology
industries such as automotive and aerospace. Therefore, they are currently used for
energy impact absorbers [GIB 88, EVA 99], in lightweight structures (in the cores of
sandwich panels) [DAY 83, GIB 88, KRE 99], heat exchangers [GIB 88, BAR 98, EVA
99], sound absorbers or silencers [DAV 83, GIB 88] and filters [GIB 88]. However,
successful thermostructural implementation relies not just on their thermome-
140
141
to the mixture. The content of the foaming agent depends on the metal to be foamed
and the desired density. The mixture, containing the agent, is then compacted by
extrusion. As a result a semi finished product is obtained in which the foaming agent
is homogeneously distributed within a dense, virtually non-porous metallic matrix.
This foamable material is processed into pieces of the desired shape by rolling and
cutting. Finally, foamed metal parts were obtained by heating the material to
temperatures above the melting point of the matrix metal. The metal melts and the
foaming agent releases gas in a controlled way, so that the metal transforms into
foamy mass which expands slowly.
The foaming takes place inside simple closed moulds which are completely filled
by the foam. After the mould is filled, the process is stopped by simply allowing the
mould to cool to a temperature below the melting point of the metal. The density of
the metal foams is controlled by adjusting the content of foaming agent and by
varying the heating conditions. The resulting foamed blocks have closed outer skins
(figure 10.2) which can be removed by cutting them into samples of the desired
dimensions.
Figure 10.2. Aluminium foams made by powder metallurgical process, the right picture
is a sample with closed outer skins, and the left one is a sample without skins.
142
particles. The particle size ranges from 10 to 30 um and their amount in the melt is
comprised in the interval of 10 to 30 vol%.
Figure 10.3. principle sketch of the foam-casting route employed by Nosk Hydro
Figure 10.4. Aluminium foams made by casting process, the right picture is a sample
with density 0.3 g/cm, and the left one is a sample with density 0.18 g/cm
Foams may be produced in densities from 0.1 to 0.5 g/cm3 by this method. The
density is controlled by the process parameters, the most important being the rotor
speed, the gas flow through the rotor and the amount of particles in the melt. At the
present stage the production is directed towards slabs having typically 8-12 cm
thick, 70 cm wide and 200 cm long; however samples of the desired dimensions
(figure 10.4) can be cut out from these slabs.
143
can see an initial quasi-static increase of stress for small deformations followed by a
long collapse plateau, truncated by a regime of densification where the stress steeply
rises.
Figure 10.5. Schematic compressive stress-strain curve for an elastic solid and a foam made
from the same solid, showing the three regimes of compressive behaviour and the dissipated
energy at a given peak stress for both foam and the solid from which the foam is made
Gibson and Ashby [GIB 88] have developed models to describe the typical
mechanisms responsible for the different mode of deformation of foams. The
mechanical properties of foams can be described by equation [1] derived using
dimensional analysis:
[1]
where X and p are the mechanical property and density of the foam, Xs and ps are
those of the solid cell wall material and (|) is the volume fraction of solid contained in
the edges, C and a are constants.
Foams are especially good for energy absorption. Energy absorption in a foam is
related to the area under its stress-strain curve in figure 10.5, energy absorption of a
foam for a given peak stress is compared to that of the solid from which it is made.
For the same energy absorption, the foam always generates a lower peak force, but
the stress is limited by the long flat plateau of the stress-strain curve [GIB 88].
Thereby, by choosing the right cell wall material and relative density, best
combination of the properties can be achieved for energy absorbers.
144
145
146
Figure 10.7. CT images of cross-sections of Norsk Hydro Al-foams; (a) sample with average
density of 0.10 g/cm3, (b) sample with average density of 0.18 g/cm, (c) sample with average
density of 0.31 g/cm
We can also distinguish from figure 10.7 that the cells are oriented in a preferred
direction (perpendicular to the outer skins) and on the other hand that there is a
broad cell size distribution. A qualitative description of the material distribution
between cell walls and cell edges is shown in figure 10.9. Different situations that
influence the mechanical properties of foams through the factor <j> in equation [1] are
specified.
Figure 10.8. CT images of cross-sections of Norsk Hydro Al-foams showing regions of high
density and others of lower density; (a) sample with average density of 0.18 g/cm , (b) sample
with average density of 0.31 g/cm
147
Figure 10.9. CT images of cross-sections of Norsk Hydro Al-foams showing the material
distribution between cell walls and cell edges: (a) concentration of the material in the cell
walls, (b) concentration of the material in the cell edges, (c) equal distribution of the material
between cell walls and cell edges
Cell size distribution seems to be homogeneous but the presence of big holes
around the centre of the structure leads to a broad density distribution through the
specimens. These holes might be caused by the foaming process itself because the
latter is stopped by simply allowing the mould to cool. The temperature in the centre
of this mould is still sufficiently high to enabling the foaming process to continue
while it has stopped elsewhere.
In figure 10.11 the image obtained by a zooming of the circled region (figure
10.11(a)) in the CT slice of the specimen, reveals a significant decrease of the
resolution. To overcome this problem, a scanning of a smaller sample is done (figure
10.1 l(b)). Therefore, the size of the specimen has to be chosen carefully to achieve
the required resolution.
148
Figure 10.10. CT images of cross-sections of LKR Al-foams showing the presence of big
holes in the foam structure: (a) sample with average density of 0.35 g/cm, (b) sample with
average density of 0.22 g/cm3
Figure 10.11. C7 images of cross-sections of Norsk Hydro Al-foams: (a) picture obtained by
a zooming of the circled region, (b) picture obtained by scanning a smaller specimen of 10 x
10 x 30 mm leading to a resolution of 90 [im
149
From figure 10.12 we can see that deformation was concentrated in a local area
having the lowest density of the sample [KRI 99, BAR 98]. The main observed plastic
deformation mechanisms were bending and buckling of cell walls, nodes which are
centre of high concentration of metallic material were left unchanged in most cases,
some of them seemed to undergo a slight rotation. Some cells were even found to be
completely intact, they had only undergone a translation. 10% straining is perhaps
too much to describe the onset of the deformation bands in the specimen, so in
subsequent tests, samples will be strained at lower values (2 - 4 %) to identify the
cells that initiate the bands and to provide a morphological explanation to the
importance of band formation in plastic deformation.
10.4.2.3. Three-dimensional (3D) reconstruction of Al foam structure
CT technique provides 3D information of the scanned specimen concerning cell
arrangement like orientation, gradient, homogeneity, etc. Images of contiguous
planes can be stacked by mean of a reconstruction algorithm, called T3D, to form
3D images of a section or if the entire part has been scanned, a full volumetric image
of the specimen. T3D is a scientific visualisation application for graphically
150
TT
Once data is imported, the reconstruction algorithm can quickly generate slices
in any orthogonal plane or at oblique angles through the 3D data volume (figure
10.13) as well as creating cut-outs in the reconstructed 3D foam structure (figures
10.14, 10.15). The presence of the big holes in the Al-foam specimens produced by
LKR powder metallurgical process is clearly shown in figure 10.15
10.5. Conclusion
Aluminium foams of similar relative density can exhibit a wide dispersion of the
mechanical properties due to various effects, such as, gradient of density
distribution, preferred pore orientation, cell size distribution and cell shape features
[SIM 99, GRA 99, SIM 98, GIB 88]. Therefore a clever characterisation of these
material is required.
Besides the fact that microfocus computed tomography is a non-destructive
technique of investigation, it brings a fundamental change to the microstructure
characterisation by delivering 3D data as well as it provides a powerful tool to
describe the deformation mechanisms within the specimen at different strain values.
152
Future work will focus on the use of microfocus computed tomography for
quantitative characterisation of Al-foams as well as the identification of the cells that
initiate the deformation bands by straining the specimens at lower values (2-4 %).
Furthermore, input parameters to support modelling work can be expected.
Acknowledgements
We wish to acknowledge the financial support of Renault S.A. Company. The
authors would like to thank Claude Peytour-chansac and Christophe Grolleron from
Renault S.A. for their support and useful discussion.
10.6. References
[BUR 92] BURCH S.F., LAWRENCE P.P., "Recent advances in computerised X-ray
tomography using real-time radiography equipment", British Journal of NOT,
Vol. 34, n 3, p. 129-133, 1992.
[CEN 96] CENDRE E. et al., "High resolution X-ray computed tomography applied
to bone structure characterization", Proceedings of the 14th Word Conference on
Non Destructive Testing, p. 1211-1214, 1996.
[SAS 98] SASSOV A., "Desktop X-ray microtomography", Proceedings of the 7h
European Conference on Non Destructive Testing, p. 2837-2836, 1998.
[MAI 89] MAISL M., REITER H., "Non destructive investigation of new materials
and electronics by microfocal radiography and high resolution X-ray computed
tomography", Proceedings of the 12th Word Conference on Non Destructive
Testing, p. 1667-1672, 1989.
[GRO 99] GROTE F., SCHIEVENBUSH A., "Characterization of cast and compressed
foam structures by combined 2D-3D analysis", Proceedings of the International
Conference on Metal Foam and Porous Metal structures, p.227-232, 1999.
[GIB 88] GIBSON L.J., ASHBY M.F., Cellular Solids: Structure and Properties,
Pergamon Press, 1988.
[SUG 97] SUGIMURA Y. et al., "On the mechanical performance of closed cell Alalloy foams", Acta Mater., Vol. 45, n12, p.5245-5259, 1997.
[THO 75] THORNTON P.H., MAGEE C.L., " The deformation of Aluminium foams",
Metallurgical Transactions A, Vol. 6A, p. 1253-1263, 1975.
[BAR 98] BART-SMITH H. et al., "Compressive deformation and yielding
mechanisms in cellular Al alloys determined using X-ray tomography and
surface strain mapping", Acta Mater., Vol. 46, n10, p. 3583-3592, 1998
[GRA 99] GRADINGER R., RAMMERSTORFER F.G., "On the influence of mesoinhomogeneities on the crush worthiness of metal foams", Acta Mater., Vol. 47,
n l , p . 143-148, 1999.
[SIM 98] SlMONE A.E., GIBSON L.J., "Effects of solid distribution on the stiffness
and strength of metallic foams", Acta Mater., Vol. 46, n 6, p. 2139-2150, 1998.
[PRA 95] PRAKASH O. et al., "Structure and properties of Al-SiC foam", Materials
Science and engineering A199, p. 195-203, 1995.
153
[DAV 83] DAVIES G.J., ZHEN S., "Metallic foams: their production, properties and
applications", J. Mater. Sci., Vol. 18, p. 1899-1911, 1983
[SAN 94] SANG et al., "Process for producing shaped slabs of particle stabilized
foamed metal", US Patent 5334236, 1994.
[EVA 99] EVANS A.G., HUTCHINSON J.W., "Multifunctionality of cellular metal
systems", Proceedings of the International Conference on Metal Foam and
Porous Metal structures, p.45-56, 1999.
[KRE 99] KRETZ R. et al., "Manufacturing and testing of aluminium foam structural
parts for passenger cars demonstrated by example of rear intermediate panel",
Proceedings of the International Conference on Metal Foam and Porous Metal
structures, p.23-27, 1999.
[ASH 99] ASHOLT P., "Aluminium foam produced by the melt foaming route
process, properties and applications", Proceedings of the International
Conference on Metal Foam and Porous Metal structures, p. 133-140, 1999.
[SIM 99] SlMANClK F., Reproducibility of aluminium foam properties", Proceedings
of the International Conference on Metal Foam and Porous Metal structures,
p.235-240, 1999.
[KRI 99] KRISZT B. et al., "Deformation behaviour of aluminium foam under
uniaxial compression (a case study)", Proceedings of the International
Conference on Metal Foam and Porous Metal structures, p.241-246, 1999.
Chapitre 11
11.1. Introduction
The phenomenon of liquid metal embrittlement (LME) can be defined as the
brittle fracture (or loss of ductility) of normally ductile metals and alloys when
stressed while in contact with a liquid metal [PER 97]. LME leads to a significant
deterioration of the mechanical properties of the solid metal: liquid Ga for example
(melting point Tm= 29.8 C) is known to induce brittle fracture in polycrystalline Al
at stress levels far below the fracture strength of the material in air. Typically this
deterioration is observed only over a limited range of temperatures near the melting
point of the embrittling agent ('temperature trough' [NIC 79]). Strictly speaking,
LME concerns metals and alloys under stress. However, it is known, that for some
particular systems, intergranular penetration occurs even at zero applied stress. The
observed kinetics are far beyond the rates expected for grain boundary diffusion.
There is experimental evidence that the penetration may be considered as a wetting
process which is governed by the ratio of the grain boundary energy ygb and the
156
energy y sl of the liquid metal - solid metal interface. The equilibrium dihedral angle 6
at the solid metal is given by: 9 = 2cos"1(ygb/2ysl). Once the wetting condition
2ysl <ygb is fullfilled, 6 equals zero and the grain boundary will be replaced by the
liquid metal [Str 94].
Figure 11.1. a) grain boundary groove with equilibrium dihedral angle d >0 (T<TJ b)
wetted grain boundary with 9=0 (T>TJ c) Temperature dependance of surface and grain
boundary energies d) resulting temperature dependance of equilibrium dihedral angle for
different grain boundaries [Str 94]
157
Figure 11.2. Schematic view of the experimental set-up showing multilayer monoehromator,
sample rotation and translation stage and the detector system. The sample is rotated stepwise
from 9 0 to 180 and 2D projections are recorded for each angular position 9. The
spatial distribution of the linear attenuation coefficient in the sample can be reconstructed
using a standard tomographic reconstruction algorithm
158
revealed the columnar structure of the material. In the plane perpendicular to the
deformation direction, grain size ranges from tens to hundreds of microns.
Cylindrical samples with a diameter of 0.8 mm were machined from this material,
with the cylinder axis parallel to the major axis of the elongated grains. In order to
promote surface wetting by liquid Ga, the sample was dipped in a 10% NaOH
solution for about 30 seconds in order to remove the Alumina layer covering the
surface and a droplet of Ga was deposited on the surface immediately afterwards.
11.3. Results
Figure 11.3 shows a reconstructed slice of a sample which has been penetrated
by liquid gallium. Lighter gray-levels in the reconstructed images correspond to
stronger absorption. The bright lines, dividing the image into smaller, closed cells
can be clearly attributed to the presence of highly absorbing Ga (Z=31, attenuation
length =19 |jm at 15 keV) layers inside the Al matrix (Z=13, attenuation length =
506 |tim at 15 keV). The spatial resolution of the used optical set-up is restricted to
about 1.7 (am. However it is possible to detect features below this limit ('partial
volume effect'): the locally enhanced absorption in a subregion of a volume element
(voxel) will change the mean attenuation for the entire voxel. The fact that some of
the wetted grain boundaries show only weak contrast might be attributed either to
different composition or density of the absorbing material, or to a different (subpixel) size of the observed features. As Al shows a very limited solubility in Ga at
low temperature [Mon 76] the differences in attenuation can not be explained by
differences in composition of the liquid itself. As a consequence, the amount of
liquid Ga present per unit volume must be different, or in other words, the width of
some wetted grain boundaries is smaller than the pixel size.
11.3.1. Comparison with EBSD surface mapping
As mentioned above, the thickness of the liquid layer varies considerably from
grain boundary to grain boundary. A first attempt has therefore been undertaken to
correlate the information from electron backscattering diffraction (EBSD) mapping
(Fig 11.4c) before application of liquid Ga and microtomographic reconstruction of
the same zone on the sample surface after penetration by liquid Ga (Fig. 11.4a,b).
The sample was penetrated with liquid Ga and a first tomographic scan was
performed after an initial anneal for 30 min at 50C (Fig 11.4a). The second
tomographic scan (Fig 11.4b) followed after an additional anneal of 60 min at
150 C.
159
Figure 11.3. a) Reconstructed tomographic slice (pixel size: 1 \jan) through a cylindrical
Al sample which has been exposed to liquid Ga for 4h at 320K: the wetting of the grain
boundaries by liquid Ga can be clearly detected; the magnified image shows the varying
thickness of the Ga layer
160
A series of circumstances contributes to the fact, that the contours observed with
both techniques do not compare perfectly: a) corrosion and dissolution processes of
excess liquid Ga on the sample surface may lead to changes in the size and shape of
the surface grains, b) the tomographic cut defines a geometrically perfect plane
whereas the (mechanically and electrochemically polished) sample surface analysed
by EBSD does not, c) the spatial sampling rate of 5um in the EBSD mapping
different from the pixel size of Ijam in the tomographic reconstruction d) spherical
aberations of the electron microscope at low magnification leed to distorsions of the
EBSD mapping.
It is interesting to note, that grain boundaries which cannot be observed after the
first anneal at 50C, e.g. boundaries B'-B2 and C'-C2, are preferentially those of
small relative misorientation (close colour codes in the EBSD mapping). These
boundaries become visible after the second anneal at 150 C - in accordance with
the qualitaive model presented in Fig. 1 [Str94].
11.3.2.3D visualization of a polycrystal
The comparison of the tomographic reconstruction after the second anneal at
150C with the EBSD surface mapping (Fig. 7.4b&c) shows, that even with the
above mentioned limitations a good agreement is achieved. The tomographic
reconstruction of a penetrated polycrystal might therefore be used to analyse and
visualize the microstructure of the material in three dimensions. For this purpose the
experimental raw-data need to be refined using morphological image processing
methods. The applied three-dimensional segmentation algorithm, an implementation
of the "watershed" method [Bou 99], transforms the experimetnal raw data (Fig.
7.5a) into binarised volume-data containing closed cells (Fig 7.5b). In a final step, a
"label" (e.g. a number or a specific colour) is attributed to each voxel belonging to
the same cell. The size and the shape of the individual grains in the polycrystalline
material can now easily be analysed and visualized using a dedicated volume
rendering software (Fig 7.5c).
11.4. Conclusions
The present study is a new example showing the interest of synchrotron
radiation X-ray microtomography as a non destructive bulk characterization method
of materials at the micrometer scale. The presence of liquid Ga at the grain
boundaries of polycrystalline Al leads to locally enhanced absorption and standard
tomographic reconstruction methods allow to observe the wetting state of grain
boundaries inside the material. The complementary information provided by
micotomography and EBSD allows to correlate the wetting state of grain boundaries
with the relative misorientation of the adjacent grains. We do not yet have enough
data to draw quantitative conclusions, however we may confirm from our
161
experimental results that, as expected, low angle grain boundaries are less
penetrated than general grain boundaries.
Figure 11.4. Comparison of tomographic reconstructions (a,b) of the sample surface with
electron backscattering diffraction mapping (c). The EBSD mapping was obtained before
application of liquid gallium. Two tomographic scans were taken after the penetration: a)
after an anneal of SOmin at 50 C and b) after additional anneal of 60 min at 150 C. Note
that the low angle grain boundaries B'-B2 and C'-C2 are only detected after the second
anneal
162
163
Acknowledgements
We would like to thank E. Boiler and P. Cloetens for their help during the microtomography experiments. We gratefully acknowledge useful discussions with
J. Baruchel and Y. Brechet.
11.5. References
[PER 97] FERNANDES P.J.L., JONES D.R.H., "Mechanisms of liquid metal induced
embrittlement",International Material Reviews 42, p. 251, 1997.
[NIC 79] NICHOLAS M.G., OLD C.F., " Review Liquid Metal embrittlement",
Journal of Materials Science 14, p. 1-18, 1979.
[Str 94] STRAUMAL B., GUST W., MOLODOV D., "Tie lines of the grain boundary
wetting phase transition in the Al-Sn system", Journal of Phase Equilibria
Vol.15, 4, p. 386-391, 1994.
[Rab 97] RABKIN E., "Coherency strain energy as a driving force for liquid
grooving at grain boundaries", Scripta materialia, vol.39, No.6, pp 685-690,
1998.
[Gli 99] GLICKMAN E., NATHAN M., "On the kinetic mechanism of grain
boundary wetting in metals", J.Appl.Phys.,85, p. 3185-3191, 1999.
[Hug 98] HUGO R.C., HOAGLAND R.G., "In-situ observation of Aluminium
embrittlement by liquid gallium", Scripta Materialia, 38, p., 523-529, 1998.
[Lud 99]LUDWIG W., BELLET D., "Penetration of liquid gallium into the grain
boundaries of aluminium: A synchrotron radiation microtomographic
investigation", J. Mater. Science Eng. A, in press.
[Lab 96] LABICHE J.C., SEGURA-PUCHADES J., VAN BRUSSEL D., MOY J.P.,
ESRF Newsletter 25 p. 41-43, 1996.
[Mon 76] MONDOLFO L.F., Aluminium Alloys: Structure and Properties,
Butterworths, London, 1976.
[Bou 99] BOUCHET S., Segmentation et quantification d'images tridimensionnelles,
rapport de stage 36me annee, Ecole des Mines de Paris, 1999.
Chapitre 12
Closed cell aluminium based foams are chosen for performing digital transmission
radiography and X-ray computed tomography (CT). Transmission radiography yields
information on the heterogeneity of mass distribution, if two dimensional local mean mass
density maps are computed. CT provides data of the three-dimensional mass distribution.
Three-dimensional local mean density maps are proposed to identify hard and soft regions in
a cellular structure and they are used for modeling the mechanical behavior of aluminium
foams. High resolution CT enables a detailed structural analysis of the foam.
12.1. Introduction
Industrial production of foamed metals [ASH 99, BAU 99, HOP 99, KRE 99, MIY 99,
SEE 99] and metal matrix composites [DEC] is in progress for some specific
applications. Being in a developmental stage there are no generally acknowledged
specifications. Quality definitions for heterogenous materials have to be defined.
One of the main structural features correlated to properties is the local distribution of
the second constituent (either reinforcement or pores) within the matrix metal. The
aim of this work is to develop a quantitative description of "heterogeneity" of such
composites which can be applied for quality control. Foamed aluminium is chosen to
demonstrate the determination of local mass distribution by transmission
radiography or computed tomography. The recorded intensity distributions form the
basis for the calculation of local mass density distributions. Since the density is the
most important parameter which correlates the mechanical properties of a foam to
those of the dense bulk material [GIB 97], density distributions can be used for the
simulation of the mechanical behaviour and can be correlated to experimentally
determined properties.
166
12.2. Material
Samples of foamed aluminium with closed cell structure were chosen for testing.
The ALULIGHT material [MEP 96] of AlSiMg (AA 6xxx) wrought and of AlSil2Mg
cast alloys were produced by LK-Ranshofen [KRE 99] and by SAS-Bratislava [SIM 99]
and are originally covered by a skin of the matrix alloy, respectively its oxide.
where g(r ij-r ij) is the weight of each surrounding pixel. In Fig. 12.1bp(;c.) is a
schematic onedimensional representation of the pixel values of the transmission
image. A mean local density function pa(xi)is calculated by averaging over an
intervall of [;t - 34, xi + 35] with a constant weigth function g = 1 /70.
nD efot eloca
r sml idnemas
ant ysi oi t d i s t r i bn u t i o7
16
Figure 12.1. (a) principle of calculating a local density value from a transmission image; (b)
the density
values p(x
scheme) derived from the transmitted intensities
t} (onedimensional
are the result of a physical averaging over the column taversed by the beam.
pa (xt ) illustrates the effect of mathematical averaging over an interval of Ax=70 pixel
is then defined
Figure 12.2. (a) principle of calculating a local density value from a volumetric CT data set;
(b) onedimensional representation p(xt) of a cellular structure and local density p(l(xj).
Limits of the mean local mass density around the overall average density pm are indicated to
discriminate "hard" (pa > pm + Ap) or "soft" (pa < pm - Ap) regions
168
The averageing process neglects fine structural details and allows to determine
local differences in the material distribution. Figure 12.2b shows a onedimensional
model p(xi)of a cellular structure with massive walls of the solid density psand
empty pores in between. Averaging the mass densities over intervals [*, - 34, ;c, + 35]
with g = I/70yields the mean local density function pa(xi).
12.4. Results
12.4.1. Mass Distributions calculated from Transmission Radiographs
Figure 12.3. X-ray transmission of ALL/LIGHT plate: a) transmitted intensity of each pixel
(0.6 x 0.6 mm2); b) contour plot of the 2D mean local mass density
169
170
Fig Ure l 2 4
,
, ' - MaSS dmsity distribution on the surfaces of a parallelepiped recorded by
technical CT: a) CT cross section images from the 3D data set (voxelsize 0.3x0.3x0 3 mm3)
b) contour plots of 3D mean local density maps for an averaging volume of 4.3x4.3x4 3 mm>
(15x15x15 voxels) for the voxels along the planes shown in (a)
The iso-surface presentations of the limits of mean local mass density reveal as
well the 3D arrangement of the corresponding hard or soft regions across the sample
Fig I2.5b shows a V-like interconnection of hard regions across the sample which
will increase the compression resistance in the long direction. The soft regions of
that sample - see Fig. 12.5c, d - are oriented rather parallel to the direction of
compression suggesting, that they will not be identical with deformation bands [KRI
yybj. Consequently the spatial distribution of hard and soft regions has to be
considered too as an additional quality criterion.
High resolution CT reveals details in the cellular structure as shown in Fig 126
The 3D iso-surface representation of the structure shows cell walls down to about
100 Mm thickness as well as tiny shrinkage pores in cell wall nodes. Such CT data
can be used to study deformation mechanisms by computing 3D-displacements of
structural features [FOR 98].
171
Figure 12.5. Iso-surfaces of mean local mass densities in one AISU2-ALULIGHT test sample
(a = b = 22 mm, c = 30 mm) of average density pm= 0.5 g/cm3: a) hard regions of mean
local densities p > 1.67-pm in averaging volumes of 2x2x2 mm3, b) hard region of p >
1.33-pn, within 6x6x6 mm3, c) soft regions of p < 0.67- pm within 6x6x6 mm3, d) same
density limit as c) but within 7 x 7 x 10mm3, i.e. 1/3 of the edge lengths of the sample
172
Figure 12.6. Iso-surface at a level of 50% of pAI computed from high resolution 3D technical
CT data (voxelsize: 40x40x 40 fjm3). The volume of 8x8x8 mm3 within a casting alloy
ALL/LIGHT sample (same as in Fig. 5) shows a few cells, where the roughness of the cell
walls, defects in cell walls, shrinkage pores in nodes and an ensemble of neighbouring cells
can be seen
173
parallel to the loading direction. Density variation limits can be chosen as quality
criteria, but have to be combined with a reasonable choice of averaging volume.
Figure 12.7. Compressive stress-strain curves of Alulight (cast alloy) samples, both having
an average density of 0.48 g/cm3 but different local density distribution as shown by
mappings of these samples in xz and xy planes
Figure 12.8. The sample A: a) The cellular structure along the observed surface recorded by
a digital camera at 2% overall strain. Deformation zones are marked by the white lines; b)
distribution of the corresponding calculated equivalent plastic strain (PEEQ) on this surface
The assessment of the spatial arrangement of such hard and soft regions in
mechanically loaded components can also be used for the meso-mechanical
simulation of heterogeneous materials. The results of this simulation for foamed
aluminium are presented, by demonstrating the calculated elastic-plastic behavior of
a sample. A 3D density mapping which was calculated with an averaging volume of
5 x 5 x 5 mm3 was used in this finite element simulation. The detailed modeling has
174
been described in [KRI]. Fig. 12.8b shows the distribution of the equivalent plastic
strain [HIB 98] occurring on the sample's surface, which was observed in the
experiment.
The calculated maximum strain is in the same position as observed in the
experiment by optical recording (Fig. 12.8a). The capability of the 3D model
enables to follow the forming of deformation bands in the interior of the sample too.
The calculated 3D plastic strain field for this sample is given in Fig. 12.9. Four
stages, showing the growth of deformation bands, are depicted in this figure by
indicating the regions having more than 1% equivalent plastic strain.
Figure 12.9. Simulated 3D propagation of plastic regions in the interior of the sample A at
a) 0.7%; b) 1.0%; c) 1.23% and d) 1.5% overall strain. Direction x is the compression
direction
Acknowledgements
The authors gratefully acknowledge: the provision of ALULIGHT samples by
Leichtmetall-Kompetenzzentrum Ranshofen (A) and Slovak Academy of Science,
Bratislava (SK); the admission to use CT at the Department of Radiology, Division
of Osteoradiology, University of Vienna (A) and the Ferderal Institute for Materials
Research and Testing, Berlin (D). The work was funded by the Austrian Ministry of
Science and Transport.
175
12.6. References
[ASH 99] ASHOLT P., "Aluminium Foam Produced by the Melt Foaming Route Process Properties and Applications", MetFoam99 a>, p. 133-140, 1999.
[BAM 97] "Computertomographie", Leaflet, Federal Institute for Materials
Research and Testing, Berlin (Germany), 1997.
[BAU 99] BAUMGARTNER F., GERS H., "Industrialisation of P/M foaming
process", MetFoam99 a>, p. 73-78, 1999.
[COR 99] CORNELIS E., KOTTAR A., SASOV A., VAN DYCK D., "Desktop X-ray
micro-tomography for studies of metal foams", MetFoam99 a), p. 233-240, 1999.
[COP 94] COPLEY D., EBERHARD A., MOHR A., "Computed Tomography Part I :
Introduction and Industrial Applications", Journal of Materials, vol. 46, no 1, p.
14-26, 1994.
[DAX 99] DAXNER T., BOHM H.J., RAMMERSTORFER F.G., "Influence of microand meso-topological properties on the crash-worthiness of aluminium foams",
MetFoam99 a>, p. 283-288, 1999.
[DEG] DEGISCHER H.P., DOKTOR M., PRADER P., "Assessment of metal matrix
composites for innovations - a Thematic Network within the 4th EUframework", Euromat 99 (to be published).
[DEG 99] DEGISCHER H.P., KOTTAR A., "On the Non-Destructive Testing of
Metal Foams", MetFoam99 a), p. 213-220, 1999.
[EVA 99] EVANS A.G., HUTCHINSON J.W., "Mutifunctionality of Cellular Metal
Systems", MetFoam99 a>, p. 45-56, 1999.
[FOR 98] FOROUGHI B., "Study of cellular deformation of Al-Foam under
Compressive Loading", Junior Euromat, 1998.
[GIB 97] GIBSON L.J., ASHBY M.F., Cellular Solids : Structure and Properties,
2nd Ed., Cambridge University Press, 1997.
[GRO 99] GROTE F., SCHIEVENBUSCH A., "Characterization of cast and
compressed foam structures by combined 2D-3D analysis", MetFoam99 a), p.
227-232, 1999.
[HIB 98] HIBBIT, KARLSSON and SORENSON INC., HKS ABAQUS/Standard
user manual, Version 5.8, 1998.
[HOP 99] HOPLER E., SCHORGHUBER F., SIMANCIK F., "Foamed aluminium
cores for aluminium castings", MetFoam99 a>, p. 79-82, 1999.
[KRE 99] KRETZ R., HOMBERGSMEIER E., EIPPER K., "Manufacturing and
testing of aluminium foam structural parts for passenger cars demonstrated by
example of a rear intermediate panel", MetFoam99 a>, p. 23-28, 1999.
[KRI] KRISZT B., FOROUGHI B., KOTTAR A., DEGISCHER H.P., "Mechanical
Behavior of Aluminium Foam Under Uniaxial Compression ", Euromat 99 (to be
published).
[KRI 99a] KRISZT B., KOTTAR A., DEGISCHER H.P., "Strukturanalyse von
geschaumten
Aluminium
mittels
Computertomographie",
Metalle/Werkstoffwoche 98, Symposium 8, Ed.: R. Kopp, Bd. 6, p. 687-692,
Wiley-VCH, 1999.
176
[KRI 99b] KRISZT B., FOROUGHI B., FAURE K., DEGISCHER H.P., "Deformation
behavior of aluminium foam under uniaxial compression (a case study)",
MetFoam99 a), p. 241-246, 1999.
[MEP 96] "Alulight", Leaflet, Mepura Ges.m.b.H., Ranshofen/Austria, 1996.
[MIY 99] MIYOSHI T., ITOH M., AKIYAMA S., KITAHARA A., "Aluminuim Foam,
'ALPORAS': The Production Process, Properties and Applications",
MetFoam99 a>, p. 125-132, 1999.
[SEE 99] SEELIGER H.-W., "Application Strategies for Aluminum-Foam-Sandwich
Parts (AFS)", MetFoam99 a>, p. 29-36, 1999.
[SIM 99] SIMANCIK F., MINARIKOVA N., CULAK S., KOVACIK J., "Effect of
foaming paramters on the pore size", MetFoam99 a\ p. 105-108, 1999.
a)
Chapitre 13
13.1. Introduction
Understanding the evolution with time of natural or artificial porous materials is
essential for many applications. In this paper, three examples that are presently
studied within the research group CM3D* from Bordeaux, will be considered:
- mineral diagenesis of reservoir rocks for oil exploration and production,
- carbon/carbon (C/C) composites elaboration by vapour-phase densification of
carbon-fibre preforms for thermostructural materials production,
- sintering of advanced ceramics with controlled porosity distribution for
mechanical properties enhancement (strength and toughness).
In porous media physics the concept of "change of scale" is fundamental. The
common objective of all the methods used to perform the change of scale (volume
averaging, homogenisation, etc...) is to move from the local scale (the pore scale for
the cases considered here) to a larger one where the porous material behaves as an
178
179
in the p phase
on the interface A po
[1]
[2]
180
where GRAY's decomposition (equation [5]) of the local concentration has been
used to distinguish the smooth part, the averaged concentration linked to transport at
the large scale, from the spatial deviation produced by the reaction at the interface
and by the interface itself.
181
Assuming that k is constant and introducing the specific surface av defined by:
[8]
f mainly takes into account the effects of the micro-geometry on diffusion and s
takes into account the previous effects plus the effects of the chemical reactions on
the interface. The problems [10] are similar to the closure problems classically
obtained for diffusion-reaction in porous media, the specific effects of local stress
concentration being carried by * Indeed, this term is not an unknown for transport
equations. It is a local property of the interface that has to be calculated by solving
an almost decoupled local mechanical problem.
The transport equation at the large scale can now be written:
182
[12]
The local flux of matter can be expressed by equation [13]. A new version of the
model, taking into account the existence of water films at the grain-to-grain
contacts, is under development. When the new expression of the local flux will be
available, it will be possible to compare the evolutions predicted by both models for
the same starting geometry. In parallel, both models will be confronted to real data
( 13.2.3) looking for arguments supporting a choice between them.
13.2.2. REV size of a Fontainebleau sandstone sample
The concept of Representative Elementary Volume (REV) is central in the
change of scale theory for porous media. However there is no explicit formula for
the REV size ro, the main indication being that it has to be large enough compared to
the local scale characteristic lengths (lp, la) and small enough compared to the largescale characteristic length (L):
[14]
Using tomography data acquired at the ESRF (ID 19) for ELF-EP, the 3D microgeometry shown on Figures 13.3 and 13.4 has been reconstructed. It is the central
zone of cylindrical sample (diameter of 6 mm). The voxels are cubic (edges of 10
jam) and the complete data set comprises 256 x 256 x 256 voxels.
To estimate the REV size of this Fontainebleau sandstone sample for different
physical properties, the following numerical experiments have been performed:
- cubic volumes of different sizes have been extracted from the central region of
the complete data set;
- those volumes being considered as REV, three physical properties have been
computed:
- porosity values from the number of voxels belonging to the fluid phase,
- effective diffusivity values using equation [12] after resolution of problem
[10],
183
184
approximation of the size of a cubic REV for simple granular porous media. The
subsequent and complementary question is now: what is the required size for the
voxel in order to characterise correctly the fluid-solid interface? The importance of
this aspect is obvious when dealing with more complex porous media and with
coupled phenomena like in the following example.
185
section
a NC
clearly
clay
larger scales (no water flow) and the initial state has been frozen by calcite
cementation; it is why the Ellon field is an exceptional case to study.
Examining Figures 13.7 and 13.8, it is evident that this sandstone is more
complex than Fontainebleau sandstone. Porosity is larger but spatial distribution of
this porosity is completely different. Both were rather similar quartz grains packing
at the deposit (Figure 13.7) but the diagenetic mechanisms that took place have been
different. The combination of classical CMT (Figures 13.7, 13.8) and local CMT
(Figure 13.9) seems to be a promising solution to problems where more than one
scale are relevant.
13.3. C-C
Carbon/carbon composites are well known high-performance materials for
thermostructural applications, such as rocket nozzles or aeroplane brakes, and their
market is in appreciable extension. They are usually produced either by
impregnation of a preform made of carbon fibres by pitches or mesophases or by
vapour-phase densification of the same preform [NAS 99]. Chemical Vapour
Infiltration (CVI) is a variant of the Chemical Vapour Deposition (CVD) process
involving the cracking of gaseous species (precursors) which lead to the deposition
of a solid phase on a hot substrate by heterogeneous reaction. For instance, a
mixture of hydrocarbons and hydrogen is used to obtain a pyrocarbon deposit. The
gaseous species are transported inside the preform by viscous flow or by diffusion.
186
187
tips
188
grains with its associated porosity situated on the grain edges [COB 61]. In this
representation the process is completely defined by two parameters: the grain size
and the density. In real systems, grain size distribution and initial packing
inhomogeneities lead to internal stress gradients originating differential
densification phenomena (constrained densification). Pore evolution should be
considered and analysed independently of density and grain size changes.
Sintering of a powder deposited on a dense and rigid substrate (Figure 13.12) of
the same chemical nature, is an interesting model to investigate constrained
sintering at the macroscopic scale.
Figure 13.12. Schematic of (a) a powder sintered without constraints (free sintering)
(b) a powder layer sintered on a rigid substrate (constrained sintering)
189
the sintering times were 15 min, 30 min and 60 min. Due to the large initial grain
size, relative density of the free samples remained low and was 62.5 %, 67 % and
68 % respectively. The constrained samples were assumed to exhibit even lower
relative densities [LET 94].
Figure 13.13. 2D sections of alumina ceramics samples sintered during 30 min. at 1600C
(image size: 512x512 pixels, pixel size: 0.9 /jm2). Free sintering on left and constrained
sintering on right (on left is the sapphire substrate)
Figure 13.14. 60 min. free sintered ceramic. Formation of a denser shell around a large pore
is observed while no change in density can be noticed along the crack. The first effect may be
attributed to differential sintering (localised constrained sintering phenomenon) as it has
been predicted and observed in 2D within ceramic and composites [LAN 96]. Image
processing analysis tools will be used to obtain 3D information on the micro structure around
the pore to relate them to previous studies
190
Acknowledgement
All the micro-tomography data has been acquired at the ESRF (European
Synchrotron Radiation Facility, Grenoble, France) on the ID 19 beamline. 3D
* CM3D is a thematic research group from Bordeaux (Caracterisation et Modelisation 3D de 1'evolution
des milieux poreux reels. Contact: bernard@icmcb.u-bordeaux.fr).
191
13.6. References
[BER 95] BERNARD D., "Using the Volume Averaging Technique to Perform the
First Change of Scale for Natural Random Porous Media", Adv. Methods for
Groundwater Pollution Control, Gambolati & Verri Eds., p. 9-24, Springer
Verlag, New York, 1995.
[CLO 96] CLOETENS P., BARRETT R., BARUCHEL J., GUIGAY J., SCHLENKER
M., "Phase Objects in Synchrotron Radiation Hard-X-ray Imaging", J. Phys. D :
Appl. Phys., vol 29, p. 133-146, 1996.
[COB 61] COBLE R.L., "Sintering Crystalline Solids. I. Intermediate and Final State
Diffusion Models", J. Appl. Phys., vol. 32, p. 787-792, 1961.
[HEI 94] HEINTZ J.M., SUDRE O., LANGE F.F., "Instability of Polycrystalline
Bridges than Span Cracks in Powder Films Densified on a Substrate", J. Am.
Ceram. Soc., vol. 77 [3], p. 787-91, 1994.
[LAN 89] LANGE F.F., "Powder Processing Science and Technology for Increased
reliability", J. Am. Ceram. Soc., vol. 72 [1], p. 3-16, 1989.
[LEE 98] LEE S-B., STOCK S.R., BUTTS M.D., STARR T.L., BREUNIG T.M.,
KINNEY J.H., "Pore Ggeometry in Woven Fiber Structures: 0/90 Plain-Weave
Cloth Lay-up Preform", J. Mater. Res., vol 13(5), p. 1209-1217, 1998.
[LET 94] LETULLIER P., Ph.D. thesis, n1247, University Bordeaux I, 1994.
[NAS 99] NASLAIN R., "Key Engineering Materials", CSJ Series - Publications of
the Ceramic Society of Japan vol. 164-165, Switzerland, Trans Tech Pub., p. 38, 1999.
[HAZ 95], HAZLETT R.D., "Simulation of Capillary-Dominated Displacements in
Microtomographic Images of Reservoir Rocks", Transport in Porous Media, vol
20(1-2), p. 21, 1995.
[QUI 93] QUINTARD M., WHITAKER S., "Transport in Ordered and Disordered
Porous Media: Volume-Averaged Equations, Closure Problems, and
Comparison with Experiment", Chem. Eng. Sci., vol 48, p. 2537, 1993.
[POT 97] POTDEVIN J-L., HASSOUTA L., "Bilan de matiere des processus
d'illitisation et de surcroissance de quartz dans un reservoir petrolier du champ
d'Ellon (zone Alwyn, Mer du Nord)", Bull. Soc. Geol. France, vol 168 (2), p.
219-229, 1997.
[POU 96] POUTET J., MANZONI D., HAGE-CHEHADE F., JACQUIN C.G.,
BOUTECA M.J., THOVERT J-F., ADLER P.M., "The Effective Mechanical
Properties of Reconstructed Porous Media", Int. J. Rock. Mech. Min. Sci. &
Geomech. Abstr., vol 33(4), p. 409-415, 1996.
[VIG 95] VIGNOLES G.L., "Modelling Binary, Knudsen, and Transition Regime
Diffusion inside Complex Porous Media", J. de Physique IV, vol 65(1), p. 159166, 1995.
192
[WHI 99] WHITAKER S., The Method of Volume Averaging : Theory and
Applications of Transport in Porous Media, Theories and Applications of
Transport in Porous Media, V. 13, Kluwer Acad. Pub., Dordrecht, 1999.
Chapitre 14
194
SEM micrograph of a Pb-Sn alloy of which a marker line was drawn on the polished
surface before testing [DUP 97]. After deformation, the marker line inside the grains
is not significantly modified whereas gaps are detected through the grain boundaries,
which indicates that movements of grains are predominant.
m
a = Ke
[1]
195
[2]
with V0 a constant and r|g the cavity growth parameter. Some expressions of the
parameter r)g have been proposed in the past, in particular as a function of the
rheology of the matrix [PIL 85]. However, it must be underlined that, since these
models of cavity growth were initially developed for alloys deforming in creep
conditions, they do not take into account GBS, although it is the predominant
mechanism of deformation in superplasticity.
196
Despite its crucial link with fracture, the coalescence process between growing
cavities has been poorly documented [STO 83, STO 84]. Very limited experimental
data have been reported and few models were proposed. Moreover, these models are
generally based on very strong hypotheses about the spatial distribution of the
cavities through the microstructure and the criteria of coalescence. In particular, they
assume that the cavities are randomly distributed through the microstructure and that
all the cavities have a spherical shape and the same diameter. Lastly, coalescence is
supposed to occur only when cavities impinge.
It is expected that such assumptions are not experimentally satisfied. As already
mentionned, many cavities are preferentially nucleated near grain boundary
particles, which are not randomly distributed through the microstrucutre. Moreover,
the shapes of large cavities after superplastic deformation can be very irregular, as it
is illustrated by figure 14.4, which shows an optical micrograph of the fracture zone
for a superplastically deformed aluminium alloy. This irregularity of the shape of the
cavities is attributed to GBS, which is the main mechanism of deformation in
superplasticity.
Experimental data about strain-induced damage in superplastic conditions are
frequently quantified from the variation with strain of the cavity volume fraction Cv.
Figure 14.5 displays such a variation of Cv with s in the case of superplastic
deformation of Al-Mg alloy. The cavity volume fraction continuously increases with
strain and after a period of apparent incubation in which the level of cavitation
remains limited (less than 1 %), a sharp increase is obtained and the cavity volume
fraction, when fracture occurs, is generally high in the case of superplastic alloys,
typically more than 10 %.
197
[3]
where CVo is a constant and r\app the apparent parameter of cavitation sensitivity. The
logarithm of experimental values of Cv is plotted as a function of strain and in most
cases, a straight line can be roughly obtained in a relatively large strain interval,
which allows the measurement of a slope r|app.
The corresponding value of r)app is then compared to those deduced from the
cavity growth models. Indeed, these models predict also an exponential variation of
the volume of the cavity with strain under two main assumptions : firstly, growth is
controlled by plastic deformation of the matrix which surrounds the cavity;
secondly, the number of cavities is roughly constant in the corresponding strain
interval.
The differences between such predictions and r)app are frequently discussed in
detail and sometimes interpreted in terms of continuous nucleation of cavities during
deformation.
Despite the fact that these assumptions (in particular the constancy of the number
of cavities per unit volume in a large strain interval) appear very questionable, it is
difficult to draw conclusions with data deduced from conventional 2D techniques of
characterisation.
198
199
Figure 14.7 compares the variations with strain of the cavity volume fractions
deduced from density variation measurements and from X-ray micro-tomography. A
good correlation between the results obtained by these two independent techniques
is found. It confirms the validity of X-ray micro-tomography as a fruitful technique
of quantification of strain-induced cavitation in superplastic alloys.
Moreover, this technique allows to get information about the population of
cavities as illustrated by figure 14.8, which displays the reconstructed image of the
spatial distribution of the cavities after an elongation of about 170 %. This condition
corresponds to a mean cavity volume fraction of about 1 %. For this elongation,
most cavities are isolated through the microstructure, although some connections
between cavities can be detected.
200
201
However, as already mentioned, when strain is increased, the cavities become very
irregular and consequently, the interpretation of the associated variation of nA may
be delicate. It appears more reliable to study the variation with strain of the number
of cavities nv per unit volume.
Figure 14.9 shows the variation with elongation of the number nv of detected
cavities per unit volume. Between elongations from 200 % to more than 400 %, a
continuous decrease of nv is obtained, which points out the extent of the coalescence
process. The data obtained for an elongation close to 150 % has to be considered
with caution since it must be kept in mind that only cavities with a volume larger
than 10 voxels were taken into account in the procedure of counting. It means that
an apparent increase of ny with strain can be partially attributed to cavity growth.
From the results presented in figure 14.9, it can be concluded that the effects of
strain on the variation of nv and nA (deduced from SEM observations or from X-ray
micro-tomography data) are contrary. These differences between the dependencies
on strain of nv and nA confirm the fact that a the usual interpretation of the cavitation
processes from 2D characterisations is very hazardous.
The variation with strain of the number of cavities per unit volume is a first
approach to quantify the coalescence process. However, this parameter gives only
limited indications about the mechanism of coalescence. A way to get additional
data is to follow the variation with testing conditions of the largest cavity in the
investigated volume, since it may give indication about the extent of connection
between cavities through the microstructure. In this view, figure 14.10 displays a 3D
observation of the largest cavity obtained after an elongation of about 400 % for
which Cv is about 14.5 %. It can be seen in figure 10 that the largest cavity admits a
very irregular shape and extends beyond the studied volume. Moreover, this cavity
202
corresponds to about 75 % of the total cavity volume fraction, which indicates that
most cavities have connected together.
From this conclusion, a coalescence parameter CP can be defined, according to:
CP =
-x 100
total volume of cavities
Figure 14.11 shows the variation with strain of the coalescence parameter CP.
The value of this parameter remains limited up to a strain of about 1.2 and then
sharply increases. This strain corresponds, for the associated conditions of
deformation (525C and 10"4 s"1) to a value of Cv close to 5 %.
These results confirm the importance of the coalescence process during
superplastic deformation since they point out that coalescence occurs in a large
domain of strain. It must be kept in mind that between 8 1.2 (i.e. an elongation
230 %) and fracture, which is obtained after an elongation 400 %), the mean
cavity volume fraction Cv increases roughly from 5 % to 15 %. Consequently, it
indicates that coalescence takes place not only in a large strain interval but also in a
large domain of Cv.
203
Moreover, from figures 14.9 and 14.11, it seems that two domains of coalescence
may be identified. In a first step (for strains between 1.0 and 1.3), a significant
reduction of nv is obtained whereas the value of the coalescence parameter remains
low. It means that a large number of cavities coalesce but that the volume of the
largest cavity through the volume remains comparable to the mean cavity volume of
the cavities. It is expected that this step of coalescence is associated to a nonuniform spatial distribution of cavities. Indeed, as already mentioned, cavity
nucleation takes place preferentially near intergranular particles which are not
uniformly dispersed in the alloy, as a result of the thermomechanical process
undergone by the material. Indeed, previous work has shown that, as a result of the
thermomechanical process undergone by the material, some stringers of second
phase particles are present in the studied alloy [LAR 98]. In a second step (when 8 >
1.3), the value of CP increases sharply. It indicates that a large fraction of cavities
connect together, leading to one cavity which concentrates the coalescence process.
14.6. Conclusions
High resolution X-ray micro-tomography appears as a very promising technique
to characterise cavitation induced by superplastic deformation of industrial alloys. It
confirms the difficulty to interpret experimental information deduced from
conventional 2D quantitative metallography. In the case of an Al-Mg alloy, the
coalescence process has been preferentially investigated since it is concerned with
large cavities.
204
14.7. References
[BLA 96] BLANDIN J.J., HONG B., VARLOTEAUX A., SUERY M., L'ESPERANCE G.,
Acta Mater., vol. 44, p. 2317-2326, 1996.
[BUF99JBUFFIERE J.Y., MAIRE E., CLOETENS P., LORMAND G., FOUGERES R., Acta
Mater., vol. 47, p. 1613, 1999.
[CHO 86] CHOKSHI A.H., J. Mater. Sc., vol. 21, p. 2073, 1986.
[DUP 97]DUPUY L., DEA INP Grenoble, 1997.
[FRI 96] FRIEDMAN P.A., GHOSH A.K., Metall. Mater. Trans., vol. 27A, p. 3827,
1996.
[HAN 76] HANCOCK J.W., Metal Sc., vol. 10, p. 319, 1976.
[HIR 95] HlRANO T., USAMI K., TANAKA Y., MASUDA C., J. Mater. Res., vol. 10, p.
381, 1995.
[rwA91]IWASAKi H., HIGASHI K., TANIMURA S., KOMATUBARA T., HAYAMI S.,
Proc. of Int. Conf. on Superplasticity of Advanced Materials (ICSAM), p. 447,
1991.
[LAB 96]LABICHE C., SEGURA-PUCHADES J., VAN BRUSSEL D., MOY J.P., ESRF
Imprime en France