Beruflich Dokumente
Kultur Dokumente
DOI 10.1007/s00339-008-4870-y
Received: 30 April 2008 / Accepted: 6 August 2008 / Published online: 11 September 2008
© Springer-Verlag 2008
Abstract This paper highlights the microstructural features residual porosity, contamination, and small sample dimen-
of commercially available interstitial free (IF) steel speci- sions have been the major barrier in successful utilization of
mens deformed by equal channel angular pressing (ECAP) these nanomaterials in industrial applications [3].
up to four passes following the route A. The microstructure Severe plastic deformation (SPD) methods, in contrast to
of the samples was studied by different techniques of X-ray powder processing based methods, are the methods to pro-
diffraction peak profile analysis as a function of strain (ε). duce bulk nanostructured materials. The basic principle of
It was found that the crystallite size is reduced substantially SPD is the heavy straining of materials under high pres-
already at ε = 2.3 and it does not change significantly dur- sure [3]. Nanomaterials produced by SPD are fully dense
ing further deformation. At the same time, the dislocation and hence there are no chances of contamination, as often
density increases gradually up to ε = 4.6. The dislocation seen in the materials processed through powder based tech-
densities estimated from X-ray diffraction study are found niques. SPD also allows producing nanomaterials with large
to correlate very well with the experimentally obtained yield geometrical dimensions [4]. Equal channel angular pressing
strength of the samples. (ECAP) is one of the major SPD methods widely used to
fabricate bulk nanostructured materials, almost for a decade
PACS 61.05.Cp · 61.72.-y · 61.72.Dd [4–6]. A grain size of the order of few hundred nanometers
is easily achieved in this process. The mechanism of grain
refinement via ECAP has been extensively investigated in
1 Introduction numerous materials [7–12]. It is now well accepted that the
basic underlying mechanism of grain refinement involves an
Nanostructured/ultrafine grain materials have been the sub- increase in the dislocation density by heavily deforming the
ject of intensive investigations in the recent years due to materials. Dislocations form an ordered arrangement giving
their superior mechanical and physical properties. The past rise to dislocation walls. As the deformation continues, these
two decades have witnessed remarkable advancement in dislocation walls finally transform into grain boundaries. In
processing and characterization of materials with ultra- order to achieve the desired goal of the ECAP, it is manda-
fine grains in nanometer and submicrometer range. Several tory to ensure that no restoration process, i.e., recovery of
methods like inert gas condensation [1], ball milling or me- dislocation substructure, occur during the process [13, 14].
chanical alloying [2] are being extensively used to prepare Thus, it is very interesting to investigate the evolution of dis-
nanomaterials. These techniques allow producing ultrafine location substructure at different stages during ECAP.
grains with size ∼10 nm in powder form. However, high The characterization of the microstructural deformation
of materials is a challenging task. In case of SPD processed
materials, this becomes rather complicated due to the pres-
A. Sarkar () · A. Bhowmik · S. Suwas
ence of a large fraction of low angle boundaries plus some
Department of Materials Engineering, Indian Institute of Science,
Bangalore 560012, India special boundaries. Electron backscatter diffraction (EBSD)
e-mail: apu@platinum.materials.iisc.ernet.in is one of the most popular techniques used to investigate the
944 A. Sarkar et al.
microstructure of the materials. However, EBSD has limi- In the present study ϕ was 90◦ . Therefore, the strains after
tations in both spatial and angular resolutions and therefore one, two, three, and four passes were 1.15, 2.30, 3.45, and
cannot be used to reveal the low-angle boundaries and dis- 4.60 respectively.
locations. Transmission electron microscopy (TEM) is the
most powerful technique used for studying the dislocation 2.2 X-ray diffraction
substructure within the material. It provides a direct way to
observe materials’ microstructure within the material. How- For X-ray diffraction study samples were cut from the mid-
ever, it has some serious drawbacks. Only a miniscule vol- plane section (ED-ND plane) and subjected to metallo-
ume of the sample is investigated under TEM which may graphic preparation up to electropolishing. The X-ray dif-
not be representative of the bulk, particularly, when hetero- fraction patterns were recorded from the polished surface
geneities are reported to be present at all levels in ECAP using a PANalytical X’PertPro diffractometer with Cu Kα
processed material [15, 16]. On the other hand, TEM sam- radiation. All the diffraction profiles were obtained by vary-
ple preparation is a tedious task. In this respect, X-ray dif- ing 2θ from 40◦ to 120◦ in a continuous scan mode with a
fraction (XRD) is a superior technique to investigate the mi- step size of 0.017◦ . The time spent for collecting the data
crostructure of plastically deformed samples. XRD gives in- per step was 400 s. Figures 1a and 1b show typical XRD
formation of the bulk properties of a polycrystalline solid, patterns for the starting and the 4 pass deformed samples,
averaged over the sample volume. The sample preparation respectively.
in this case is easy and safe. The observed line profile is the convolution of instrumen-
Microstructural studies of deformed polycrystalline sam- tal and specimen (microstructural) broadening. Therefore
ple from X-ray diffraction line profile analysis (XRDLPA) the first step before any attempt to analyze diffraction line
have been a topic of renewed interest for the last two broadening is to correct the observed line profile for instru-
decades. Many new methods of XRDLPA have been pro- mental effects. A careful scan of suitable standard sample,
posed to extract microstructural information from the XRD showing minimal physical broadening, defines the instru-
peaks [17–19]. XRDLPA has been recently used in several mental contribution to the broadening [26]. We have used
studies to investigate the microstructural evolution during standard silicon sample to correct the instrumental broaden-
ECAP of different materials [20–23]. However, most of the ing. The peaks of the silicon sample were fitted with pseudo-
previous studies were focused on the face-centered cubic Voigt (pV ) function. A pV function is basically a linear
(fcc) and hexagonal close-packed (hcp) materials. In this combination of Loretzian (L) and Gaussian (G) functions
study, we extend the application of XRDLPA to characterize and is expressed as:
the microstructure of SPD processed body-centered cubic
(bcc) interstitial free (IF) steel material. pV = ηL + (1 − η)G (2)
where η is the mixing parameter. From the fit the full width
2 Experimental details at half maximum (FWHM) and η are calculated for all the
peaks. The Caglioti relation [27]
2.1 Material and method
(FWHM)2 = U tan2 θ + V tan θ + W and (3)
Interstitial free (IF) steel, with chemical composition given (1 − η) = a + bθ (4)
in Table 1, was processed through equal channel angular
pressing up to 4 passes without rotation around the axis of are used to characterize the instrumental broadening. Five
the billet (route A) in a specially designed die [24]. Details parameters U , V , W , a, and b are used to synthesize the
of the pressing parameters are given in the reference [25]. instrumental broadening profile at any particular angle cor-
For a die with interchannel angle ϕ without any rounding responding to the peak position of the sample. Finally the
of a corner, the total strain, εn imparted to the specimen after instrumental broadening is deconvoluted from the observed
N passes can be estimated as [4]: profile using the Stokes deconvolution method [28].
ϕ
εn = 1.15N cot (1) 2.3 Mechanical testing
2
4 Results and discussions It is to be mentioned here that for bcc materials the (110)
peak is the highest intensity diffraction peak. From the ana-
Figure 2 shows typical WH plots for the starting and the lyzed data, the typical fourth order moment divided by q 2
2 pass deformed sample. The values of integral breadth is presented in Fig. 4a for the 1 pass and the 4 pass de-
as obtained from the XRD patterns clearly indicate an formed samples. Figure 4b shows the representative plot of
anisotropic broadening for the 2 pass deformed sample M2 for the typical (110) peak for the 1 pass and the 4 pass
(Fig. 2). This anisotropic broadening of the XRD profile samples. The asymptotic regions of the curves of M2 and
is attributed to the presence of dislocations in the mater- M4 /q 2 are fitted with (7) and (8), respectively. From the
ial. Figure 3 shows the (110) peak of the starting mater- above analysis, the regime was chosen for which both M2
ial and the 3 pass deformed sample. It is evident that for and M4 yielded the same surface weighted mean crystallite
the 3 pass deformed sample the XRD peak is broadened size (Ds ) values. The dislocation densities ρ in the differ-
and asymmetric, the latter gives the indication regarding the ent samples are determined from the M4 /q 2 vs. q curve.
formation of subgrains or dislocation cell structure in the The variation of the Ds with strain is shown in Fig. 5a.
material [33]. The variance method has been proved to be It can be seen that Ds is reduced to 48 ± 5 nm already
very effective to account this kind of anisotropic broadening after the second pass, i.e., after a strain of 2.30. There-
and asymmetric peak shape of the XRD profile. We have after, the crystallite size does not change significantly for
applied this method to the (110) peak of all the samples. higher strains. It is worth mentioning that for severely de-
formed materials, the mean crystallite size determined by
X-ray line profile analysis is usually lower than the grain
size observed in TEM. The grains in severely deformed ma-
terials are divided into subgrains or dislocation cells which
Fig. 2 Williamson–Hall plot for the starting and 2 pass deformed sam-
ples
5 Conclusions
Fig. 5 Variation of (a) crystallite size and (b) dislocation density with
strain
Microstructural evolution during equal channel angular
pressing of interstitial free steel has been reliably as-
are separated from each other by low-angle grain bound-
sessed by X-ray diffraction line profile analysis using the
aries. The crystallite size obtained from XRD is equivalent
Williamson–Hall plot technique and the variance method.
to the mean size of domains which scatter X-rays coher-
ently. Consequently, X-ray diffraction makes a difference The anisotropic broadening of the line profile of the de-
between dislocation cells or subgrains even if the misori- formed sample provided an estimate of dislocations, while
entations are very small. The variation of dislocation den- the asymmetric peak shape confirmed the formation of sub-
sity with strain is shown in Fig. 5b. It can be seen from grain or cell structure in the deformed samples. Crystallite
the figure that the dislocation density increases to 3.6 × size decreased with strain up to a strain level of 2.3 beyond
1014 m−2 after the first pass, i.e., at a strain of 1.15. Dur- which it reached saturation. The dislocation density consis-
ing further deformation, dislocation density increases rather tently increased with the increasing strain, indicating that no
slowly. dynamic restoration processes occurred during equal chan-
To correlate the yield strength of the samples with the dis- nel angular pressing. Yield strength of the samples measured
location density obtained from the XRDLPA, we have cal- by mechanical tests are found to correlate very well with the
culated the yield strength using Taylor’s equation dislocation density obtained from the X-ray diffraction line
profile analysis.
σTaylor = σ0 + αMGbρ1/2 (9)
where σ0 is the friction stress, α a constant (α is taken Acknowledgements The authors are thankful to Dr. D. Bhattachar-
jee, Dr. N. Gope, and Prof. R.K. Ray, R & D Division, Tata Steel for
as 0.33), G the shear modulus, b the length of the Burg- their encouragement and support to this work. The financial support
ers vector, and M is the Taylor factor (M = 3 for untex- from Tata Steel through a collaborative project “Investigation on Ultra-
tured polycrystalline materials). For pure Iron, G = 82 GPa, fine Grain Steels” is duly acknowledged.
948 A. Sarkar et al.