S T E M- E D S X - Ra y Microanalysis of

Small Precipitates in Iron Base Thin Foils

P. DOIG and P. E. J. FLEWlTT
The experimental conditions for detection of segregated elements in the X-ray spectrum recorded from
small precipitates _< 100 nm diameter contained within a thin foil of an iron base alloy using STEM-
EDS X-ray microanalysis are described. The influence of precipitate size, position and composition,
foil thickness, electron accelerating voltage, and X-ray emission intensity on its detectability are
evaluated. Optimum experimental conditions for microanalysis of these precipitates are established
and the limitations of current techniques discussed.
I. INTRODUCTION
SMALL precipitates, -<100 nm diameter, are important
microstructural features in controlling the mechanical and
chemical properties of many commercial ferrous and non-
ferrous alloys. Interpretation of such properties requires a
description of their morphology, distribution, and crys-
tallography, as well as their chemical composition. The
most widely available technique for undertaking micro-
analysis of these small precipitates is that of scanning
transmission electron microscopy combined with energy
dispersive X-ray spectroscopy (STEM-EDS) of thin foil
samples. This technique, however, suffers practical limi-
tations in that small precipitates with diameter less than
the foil thickness must be analyzed simultaneously with
the surrounding matrix. Thus, it is desirable, whenever pos-
sible, to examine either very thin regions of foil or utilize
techniques for extracting the precipitates from the matrix. In
practice, it is not possible to prepare foils -< 50 nm thickness
such that precipitates with diameter less than this value
will always be contained within the foil. The alternative of
examining precipitates which have been extracted from the
matrix may introduce spurious artifacts into the microanal-
ysis and prejudice any correlation with the microstructure.
Since the X-ray spectrum recorded from small precipi-
tates contained within the foil volume is derived from both
the precipitate and matrix, the relative proportions of the
total signal from each will depend on the foil thickness,
the precipitate size, and its depth within the foil together
with the local volume electron flux intensity distribution
within the sampling electron probe. Intuitively, use of
smaller incident sampling electron probes with higher inci-
dent energies and thinner foils will result in a larger propor-
tion of the recorded X-ray quanta being derived from the
precipitate and therefore optimize the microanalysis. These
conditions, however, serve to reduce the total number of
emitted X-ray quanta thereby decreasing the statistical
confidence in the recorded data. These two competing
effects are nonlinearly related in that the relative benefits
of increasing the proportion of X-rays emitted from the
precipitate are not directly complemented by an equivalent
decrease in the statistical confidence of the data. Thus,
there exists some compromise between these competing
P. DOIG and P. E. J. FLEWI TT are bot h Resear ch Offi cers wi t h Cent ral
Electricity Generat i ng Board, Sout h East ern Regi on, Scientific Servi ces
Depart ment , Gravesend, Kent , Uni t ed Ki ngdom.
Manuscri pt submi t t ed November 18, 1982.
effects that results in a maximum sensitivity for any micro-
analysis which may be achieved by adjustment of the experi-
mental variables.
The purpose of this paper is to examine the influence of
the experimentally adjustable variables of incident electron
probe size, total electron flux, electron accelerating voltage,
foil thickness, and precipitate position within the foil on the
sensitivity of microanalysis of small precipitates contained
within thin foils.
II. THEORETICAL ANALYSIS OF THE X-RAY
EMISSION FROM A SMALL PRECIPITATE
In this work we assume spherical precipitates with a uni-
form concentration, Co, of a particular element and diameter
d positioned at a depth t ' in a foil of thickness t~ shown
schematically in Figure 1. The measured characteristic
X-ray intensity from a given microstructural feature, I ' ,
is a convolution of the volume electron flux, l ( v ) , and the
solute composition, C ( v ) , distributions within the total
sampled region of foil:
I ' = K I v I ( V ) C ( v ) d v [1]
where K is a constant describing the efficiency of X-ray
generation, emission, and detection for the particular ele-
ment of interest. An analytical expression which approxi-
mates the electron flux distribution within the foil, I (v), has
been given by the authors: 1'2
I ( r , t) = Ie[Tr(2o "2 + / 3 / 3 ) ] - 1 . exp[_rZ/ (2cr 2 + /3t3)] [2]
for a total incident electron flux of Ie where I ( r , t ) is the
electron flux at a distance r from the center of the probe at
a depth t in the foil, o, is a measure of the incident electron
probe size such that the probe diameter, B (FWHM) -~
2.35~r, and/3 is a parameter defining the electron scattering
characteristic of the foil material given by:
/3 = ( 4 Z / E o ) 2 " p / a . 500 [3]
Here Z, A, and p are the atomic number, the atomic
weight, and density of the foil material and E0 is the electron
accelerating voltage in eV;/3 is then given in units of nm -1.
The assumption of uniform precipitate composition C (v) =
Co in Eq. [1], and a matrix composition = 0 reduces this
convolution to a simple integration of I (v) over the volume
of the precipitate. Thus, integration of Eq. [2] over the
METALLURGICAL TRANSACTIONS A VOLUME 14A, OCTOBER 1983 - - 1943
(a)

O
u
. - d. ~
1
t'
(b)
Co
0
(c)
Fig. 1- - ( a) Transmission electron micrograph showing a typical small
second phase precipitate, P, contained in a thin foil sample. (b) Schematic
diagram showing the position of the included precipitate within the thin
foil. (c) Schematic composition profile across a small precipitate.
precipitate volume gives the total electron flux within
the precipitate and thereby from Eq. [1] its contribution
to the total X-ray signal.
The accuracy of this X-ray measurement is given by a
statistical consideration of the finite number of detected
X-ray quanta. The significance of the measurement is re-
lated to the counting statistics in the characteristic X-ray
energy peak, Np, compared with those in the background of
the spectrum Nb (Figure 2). Confidence in any measured
peak intensity (or integrated counts) is dependent on both
the peak and background such that for a large number of
counts where Gaussian statistics may be assumed (N - 20):
Peak intensity = Np "+" (Np) I/2 [4]
Background intensity = Nb + (Nb) ~/2 [5]
Detection of a peak requires its magnitude to be greater than
the error in its estimation such that:
Up >-- (Up + Ub) ''2 + (Ub) 1/2 [6]
1944--VOLUME 14A, OCTOBER 1983
I---
Z
I - - I
I
[
/
/
1
/ \
i ~ Np
[
N b
I
ENERGY
Fig. 2- - Schematic diagram defining the number of X-ray counts recorded
in the characteristic peak, Np, and in the background, No.
For any given electron source the total incident electron
flux, le, is related to the incident probe size, B, by: 3'4'5
l e oc B 8/3 [7]
Thus, the total emitted X-ray intensity, I ' , increases with
beam size. The background X-ray intensity in a recorded
spectrum is proportional to the electron probe current, Ie, the
foil thickness, tl, and the total recording time, T, such that: 6
N b = K' BS/ 3hT [ 8]
where K' is a constant for the particular X-ray energy
and electron illumination system which characterizes the
"effective" electron intensity for X-ray generation and
detection. The X-ray intensity, Np, from the precipitate
is given by the volume integral:
Up = K'RB8/3T JvI(V) dv [9]
where R is the characteristic X-ray peak-to-background
ratio (Np/Nb) in the spectrum obtained from a thin foil
sample of unit composition, and V is the volume distribution
of the precipitate. Here, the integral term represents that
fraction of the foil volume which contributes to the charac-
teristic X-ray peak.
The inequality in Eq. [6] defines the condition for de-
tecting a characteristic X-ray energy peak from the pre-
cipitate in a recorded X-ray spectrum. Nb and Np may be
calculated from Eqs. [8] and [9] for given values of foil
thickness tl and material /3, spectrum recording time T,
electron probe size B, "effective" electron intensity K' , pre-
cipitate composition Co, depth t ' , and diameter d. Thus,
from Eqs. [6], [8], and [9], we may establish conditions for
detecting the segregated element in the X-ray spectrum from
a precipitate of given composition contained within a thin
foil using STEM-EDS X-ray microanalysis.
III. RESULTS OF THE
THEORETI CAL ANALYSIS
For a given precipitate geometry, the volume integral
component of Eq. [9] decreases with increasing incident
METALLURGICAL TRANSACTIONS A
low
Io w fd v

Np/ N b
Detected
!
low N b
d
~
d
Fig. 3- - Sc he ma t i c diagram showing the range of electron probe size, B,
required for the X-ray detection of a small precipitate of diameter, d,
contained within a thin foil. d* is the mi ni mum precipitate diameter whi ch
may be detected in the recorded X-ray spectrum requiring a critical electron
probe size, B*.
O
(a)
0
3
0
10
1
log d
\
electron probe size, i.e., a smaller proportion of the total
electron flux interacts with precipitate. Conversely, the
total electron current increases rapidly (Eq. [7]) such that
the resulting total electron flux which interacts with the
precipitate will tend to increase. Therefore, from these two
competing effects it is possible to define a range of electron
probe diameter over which the inequality in Eq. [6] may be
satisfied such that the intensity of characteristic X-rays emit-
ted from the element segregated to the precipitate may be
detected in the recorded spectrum. Clearly, for very small
precipitates the inequality will never be satisfied in that the
volume integral term (Eq. [9]) tends to zero and the segre-
gation cannot be detected. This overall behavior is shown
schematically in Figure 3 where the electron probe size
range for detection is given as a function of the precipitate
diameter. For small electron probes the overall X-ray count
rate is low such that statistical noise in the recorded spec-
trum precludes detection whereas for large probes the vol-
ume integral term decreases such that the measured Np/Nb is
reduced to a level below that for which the increasing statis-
tical confidence in the data is able to compensate. The form
of the curve defining the bound for detectability displays a
minimum at a precipitate diameter d*. This diameter is a
measure of the overall sensitivity for microanalysis.
Calculated curves defining the limits of probe size B for
detection of a segregation to a precipitate with diameter
d are shown in Figure 4 as a function of (a) the product
METALLURGICAL TRANSACTIONS A
2
t ~
O
1
0
0 1 2
(b) l og d
Fig. 4- - Ca l c ul a t e d plots showing the range of electron probe size, B, for
detection of a precipitate wi t h di amet er d in the X-ray spectrum as a
function of: (a) product Ro = RCo = 10, 1, 0.1. (b) ' Effect i ve' electron
flux K' T = 10 -I, 10 2, 10 3, 1 0 - - 4 nm-ll/3.
VOLUME 14A, OCTOBER 1983-- 1945
o
(c)
0
(e)
n
m
m
0
I I I I i I i I I |
1
log d
I I I I I I I I ]
1
log d
,00
100
0 0
_ 2 0 0
I I I l I
I I I I I
I !
o
3
t 1
0 1 2
( d ) l og d
Fig. 4--Calculated plots showing the range of electron probe size, B, for
detection of a precipitate with diameter d in the X-ray spectrum as a
function of: (c) foil thickness h = 1 0 0 , 2 0 0 , 300 nm. (d) Precipitate depth
t ' = top, center, and bottom of foil. (e) Electron accelerating voltage
E0 = 100, 200, 300 kV for standard conditions given in the text.
Ro = RCo, (b) "ef f ect i ve" el ect ron flux, K' T, (c) foil thick-
ness, tl, (d) precipitate dept h, t ' , and (e) el ect ron accel er-
ating vol t age, E0. These cur ves are eval uat ed for t ypi cal
standard condi t i ons whi ch relate t o the operat i on of a t ypi cal
100 kV STEM i nst rument fitted wi t h an ener gy dispersive
X- r ay spect romet er:
(i) i ron base f o i l s - - d e f i n i n g / 3 in Eq. [3]
(ii) foil t hi ckness = 200 nm
(iii) el ect ron accel erat i ng vol t age = 100 kV
(iv) "ef f ect i ve" el ect ron flux, K' T = 0. 01 nm -11/3
(v) an assumed pr oduct R0 = RCo = 1
(vi) with t he preci pi t at e dept h = t l / 2, i. e. , at t he cent er of
the foil.
Al l curves have the f or m shown schemat i cal l y in Fi gure 3
wi t h a mi ni mum in t he precipitate di amet er, d*, at a critical
val ue of el ect ron pr obe size, B*. Fi gure 4(a) shows t he
i nfl uence of precipitate composi t i on. The val ue of d* de-
creases by a fact or of - 2 . 5 for a t enfol d i ncrease in peak-
t o- backgr ound rat i o, R0, wi t h an associ at ed but smal l er
decrease in el ect ron pr obe size, B*. B* tends to a l ower
limit with i ncreasi ng R0 whi ch for t he above st andard con-
ditions is - 2 0 nm.
Fi gure 4(b) shows t he effect of changes in the "ef f ect i ve"
el ect ron flux, K' T, whi ch i ncl udes bot h t he r ecor di ng t i me,
1 9 4 6 - - V O L U M E I 4 A , O C T O B E R 1 9 8 3 M E T A L L U R G I C A L T R A N S A C T I O N S A
T, and the intensity parameter K' . This latter term is de-
pendent on the electron source brightness, the geometry and
design of the electron optical illumination system and the
efficiency of X-ray generation, emission and detection for
the element of interest. The particular value of K'T for a
microanalysis experiment is reflected in the background
i nt ensi t y val ue Nb (Eq. [8], Fi gure 2). The results in
Figure 4(b) show that increasing K'T by a factor of ten
decreases d* by about 30 pct with, as before, a decrease
in B* t oward a l ower l i mi t i ng val ue of - 2 0 nm f or
K'T = 1 0 - 3 nm -H/3.
The influence of the experimental variables of foil thick-
ness, tl, precipitate depth, t ' , and electron accelerating volt-
age, E0, are shown in Figures 4(c) to (e). Figure 4(c) shows
that increasing the foil thickness, tl, over the range 100 to
300 nm increases d* nonlinearly by a decreasing amount
from 12 to 17 nm only with a corresponding change in B*.
The minimum value of B* for a 100 nm thickness foil is
15 nm. Figure 4(d) shows the effect of precipitate depth, t ' ,
for three positions within the foil: the top, center, and bot-
tom. Here, d* increases with depth into the foil as a result
of the increasing effect of the electron scattering within the
foil reducing the proportion of the total electron flux inter-
acting with the precipitate. For these conditions d* increases
from 12 to 18 nm with an associated change in B* from 15
to 60 nm.
Changes in the electron accelerating voltage, E0, influ-
ence the electron scattering behavior described by /3 in
Eqs. [2] and [3], and also the parameters K' and R0. Consid-
ering firstly the influence on/ 3, increasing the electron ac-
celerating vol t age from 100 to 200 kV reduces d* by
- 1 0 pct and is again accompanied by a corresponding
change in the associated electron probe diameter from 20 to
12 nm (Figure 4(e)). This improvement in detectability with
increasing electron accelerating voltage is evaluated for a
constant "effective" electron flux, K'T. For a constant true
electron probe current, however, since the X-ray ionization
cross section, Q, and therefore K' is proportional to the
factor ln(E~/Eo)/(E~Eo) where Ec is the characteristic X-ray
energy, 6'7 increasing the accelerating voltage from 100 to
200 kV decreases the "effect i ve" electron flux by - 4 0 pct.
Complementing this decrease, however, is the associated
change in peak-to-background ratio, R, for this increase
in electron accelerating voltage. Theoretically, 6,8 an im-
provement of up to 40 pct may be achieved, 8 but in practice
this is difficult to realize because of increasing contributions
to the background from spurious X-rays within the micro-
scope and detector. Thus, for a constant current in the elec-
tron probe, increasing the electron accelerating voltage from
100 to 200 kV has almost no effect on the value of d*. For
a constant electron source geometry, the electron probe cur-
rent increases linearly with electron accelerating voltage. 3,4,9
However, for instruments with variable electron acceler-
ating voltage, the illumination system geometry is not nec-
essarily constant and this simple linear relationship will
rarely apply. Nevertheless, the results of Figure 4(b) show
that even a twofold increase in the "effective" electron flux
will have little effect on d*.
The influence of the "effective" electron flux term, K'T,
on the minimum diameter, d*, is more clearly illustrated in
Figure 5. Here, d* is plotted as a function of the term K'T
over the range 10 4 to 10 -1 nm 11/3 for R0 values of 0. 1, 1,
and 10, and the other conditions as defi ned above for
Figure 4. In addition, results are shown for R0 = 10 and foil
thicknesses of 100 and 300 nm. The data for 200 nm thick
foils are described by the empirical equation:
log(d*) = 0.75 - 0.18 log (K' T) - 0. 37 log ( Ro) [10]
Thus, a tenfold increase in the "effect i ve" electron flux
decreases d* by a factor of - 1 . 5 whereas a similar increase
in R0 decreases it by a factor of - 2 . 3 . In practice R0 is
limited primarily by the resolution of energy dispersive
spectrometers. The "effect i ve" electron flux term, K' T, how-
ever, may be increased most significantly by using higher
brightness electron sources such as LaB6 or field emission
tips where improvements of up to X100 in electron current
density may be achieved 4 for smaller probe sizes. Any in-
crease in K'T by extending the spectrum acquisition time, T,
is limited by the mechanical and electrical stability of the
microscope. For these small precipitate sizes, - 1 0 nm, a
realistic period for microanalysis is - 1 0 0 seconds.
IV. DI SCUSSI ON
The above theoretical consideration of STEM-EDS X-ray
microanalysis of small precipitates illustrates the compro-
mise between reducing spatial resolution and improving
counting statistics associated with increasing the elec-
tron probe size. For given experimental conditions of foil
thickness tl, precipitate di amet er (d), position ( t ' ) and
segregated element concentration (Co oc R0), electron accel-
erating voltage (E0), effective flux intensity in the probe
(K' ), and recordi ng time (T) there exists an opt i mum
incident electron probe diameter (B*) for detection of the
particular element of interest within the X-ray spectrum
recorded from that precipitate. For iron base foils, electron
scattering within the foil, characterized by the term /3 in
Eqs. [2] and [3], results in optimum electron probe di-
ameters in the range 10 to 60 nm for the standard conditions
considered in the present work. For precipitates located at
the center of a foil of thickness >- 100 nm the optimum probe
size is >-20 nm regardless of the "effective" electron flux
parameter K'T. This beam diameter is larger than usually
obtained in current STEM instruments when operating in the
1.o
0 , i i i I i I 1 [ i i i I I I i l l I i I i i i i 1 [ i
- 4 - 3 - 2 - I
1o9 K'T
Fi g. 5 - - Ca l c u l a t e d pl ot s o f mi n i mu m pr e c i pi t a t e d i a me t e r , d*, wh i c h ma y
be de t e c t e d i n t he X- r a y s p e c t r u m as a f u n c t i o n o f t he e l e c t r o n f l ux, K' T
( nm it/3) f o r R0 = 0, 1 a n d 1, t~ = 2 0 0 n m a n d Ro = 10 wi t h t~ = 100,
200, a n d 3 0 0 nm.
C
METALLURGICAL TRANSACTIONS A VOLUME 14A, OCTOBER 1 9 8 3 - 1 9 4 7
normal imaging mode but may be achieved by overriding
the first condenser lens current controls or selection of aper-
ture size. It is noteworthy that the mi ni mum segregated
precipitate diameter in these cases is smaller than the elec-
tron probe size which is required for their detection in the
X-ray microanalysis spectrum. The "effect i ve" electron in-
tensity paramet er K' is proportional to the electron source
brightness. Our JEOL JEM 100CX STEM combi ned with a
Link Model 860 EDS microanalysis system has a value for
K' of - 5 x 10 -5 nm -H/3 s -j for iron K~ X-radiation using
a conventional thermal hairpin tungsten filament at 100 kV
(evaluated using Eq. [8] and the definition for Nb shown
schematically in Figure 2). Thus, for a foil thickness of
200 nm, X- r ay recordi ng t i me of 200 seconds (K' T =
10-2nm-ll/3), and a 10 nm diameter electron probe we ob-
tain a background count Nb = 1000 counts, an integrated
peakNp = 4 x 104 counts (R = 40 for FeK~) with an over-
all X-ray count rate for the total spectrum of 1000 s -~. The
maxi mum count rate which can be accommodat ed by such
an EDS system is - 2 0 0 0 s -~ for a processing time of 40/ zs.
Thus, the maxi mum beam diameter which can be efficiently
utilized for microanalysis of iron base foils of this thickness
is =13 nm. The calculated mi ni mum precipitate diameter
detected in the X-ray spectrum vs incident electron probe
size curves for the standard conditions of Figure 4 and
K' T = 5 x 10-~,5 x 10-2,5 x 10-3, and5 x 10 - 4 nm -11/3
are shown in Figure 6. For K' T = 5 x 10 - 3 nm -H/3 char-
acteristic of our JEOL system, we find a mi ni mum diameter
of 19 nm when limited by the X-ray count rate that is ac-
cepted by the X-ray spectrometer. For higher values of K' T
associ at ed wi t h br i ght er el ect r on sour ces, i . e. , fi xed
T = 100 seconds, the X-ray count rate limitation further
reduces the maxi mum electron probe size which may be
used for X-ray excitation. These limits are superimposed as
broken lines on the curves of Figure 6 for count rate limits
of 2000 and 10,000 s ~. Clearly, for higher K' T values the
finite X-ray count rate significantly increases the mi ni mum
diameter, d*, f r om the t heoret i cal l y calculated values.
Typically, a value of K' T = 5 x 10 -~ nm -H/3, which is
100 times greater than that attainable from the present JEOL
tungsten thermal filament, represents an upper limit which
might be achieved with field emission illumination systems.
This would reduce the mi ni mum diameter to 15 nm com-
pared with a theoretical d* of 7 nm and the 19 nm using the
conventional tungsten filament system. Increasing the maxi-
mum acceptable X-ray count rate to 10,000 s -1, however,
decreases d* to 11 nm for this value of K'T. Thus, any
attempt to i mprove the sensitivity of X-ray microanalysis by
increasing K' through i mprovement s in electron flux in-
tensity within the probe must be accompanied by a corre-
sponding i mprovement in the maxi mum X-ray count rate
which may be accommodat ed by the EDS system.
Although the results described in this work have been
developed for iron base foils, the overall principles apply
to other alloy systems and the conclusions concerning the
interaction between precipitate diameter, electron probe
size, "effective" electron intensity, and maxi mum X-ray
count rate apply even to low atomic number elements such
as aluminum base and K' T values up to 100 times that
achieved using conventional thermal tungsten filaments and
accelerating voltages of up to 300 kV. In the present work
130
O
1
0
0 1 2
log d
Fig. 6 - - Ca l c u l a t e d pl ot s of t he el ect ron pr obe size r ange requi red for
X-ray detection of precipitate cont ai ned wi t hi n a t hi n foil base foil as a
f unct i onof pr eci pi t at e di amet er f or val ues of K' T = 5 10 ' , 5 10 2,
5 x 10 3, and 5 x 10 -4 nm - " / 3 usi ng t he st andard condi t i ons for Fig. 3.
Super i mposed on t hese cur ves are br oken lines s howi ng the ma xi mum
pr obe size whi ch ma y be used whe n l i mi t ed by the X- r ay det ect or count rate
of 2000 and 10,000 s ~.
we have used a simple analytical approxi mat i on to describe
the electron flux distribution within the total vol ume of the
thin foil, Eq. [2], and a specific analytical formulation for
the total electron flux as a function of electron probe size has
been assumed (Eq. [7]). Regardless of the absolute accu-
racy of these descriptions, the overall conclusions of the
theoretical analysis depend only on an increase in electron
probe current which is greater than a linear function of
probe size.
V. CONCLUSI ONS
The principal conclusions which may be derived from the
results of the present work are:
1. For precipitates which are contained within a thin foil
there exists an opt i mum electron probe size for their
detection in their X-ray spect rum obtained using STEM-
EDS X-ray spectroscopy.
2. For precipitates contained within iron base foils of thick-
ness ->100 nm the opt i mum el ect ron pr obe size for
their detection in the X-ray spectrum is greater than
10 nm diameter.
1948--VOLUME 14A, OCTOBER 1983 METALLURGICAL TRANSACTIONS A
3. For EDS systems, where the saturation X-ray count rate
is -<10,000 s -l , the optimum electron probe size for
detecting segregations in the X-ray spectrum of small
precipitates in iron base foils produces sufficient counts
to saturate the spectrometer such that in practice a
smaller probe size must be used. Thus, experimental
conditions are optimized by using the largest electron
probe size which just saturates the EDS to produce an
acceptable maximum X-ray count rate.
ACKNOWLEDGMENT
This paper is published by permission of the Director
General, Central Electricity Board, South Eastern Region.
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METALLURGICAL TRANSACTIONS A VOLUME 14A, OCTOBER 1983-- 1949