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X-Ray Determination of Retained Austenite in Steel With Near Random Crystallographic Orientation
X-Ray Determination of Retained Austenite in Steel With Near Random Crystallographic Orientation
INTRODUCTION
The volume percent of retained austenite (face-centered cubic phase) in steel is determined by
comparing the integrated chromium or molybdenum X-ray diffraction intensity of ferrite (body-
centered cubic phase) and austenite phases with theoretical intensities. This method should be applied
to steels with near random crystallographic orientations of ferrite and austenite phases because
preferred crystallographic orientations can drastically change these measured intensities from
theoretical values. Chromium radiation was chosen to obtain the best resolution of X-ray diffraction
peaks for other crystalline phases in steel such as carbides. No distinction has been made between
ferrite and martensite phases because the theoretical X-ray diffraction intensities are nearly the same.
Hereafter, the term ferrite can also apply to martensite. This practice has been designed for unmodified
commercial X-ray diffractometers or diffraction lines on film read with a densitometer.
Other types of X-radiations such as cobalt or copper can be used, but most laboratories examining
ferrous materials use chromium radiation for improved X-ray diffraction peak resolution or
molybdenum radiation to produce numerous X-ray diffraction peaks. Because of special problems
associated with the use of cobalt or copper radiation, these radiations are not considered in this
practice.
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TABLE 1 Calculated Theoretical Intensities Using Chromium Kα RadiationA
hkl Sinθ/λ θ f ∆f' ∆f9 /F/2 LP P TB N2 R
(α iron, body-centered cubic, unit-cell dimension ao = 2.8664Å):
110 0.24669 34.41 18.474 −1.6 0.9 1142.2 4.290 12 0.9577 0.001803B 101.5C
200 0.34887 53.06 15.218 −1.6 0.9 745.0 2.805 6 0.9172 0.001803B 20.73C
211 0.42728 78.20 13.133 −1.6 0.8 534.6 9.388 24 0.8784 0.001803B 190.8C
(γ iron, face-centered cubic, unit-cell dimension a o = 3.60Å):
111 0.24056 33.44 18.687 −1.6 0.9 4684.4 4.554 8 0.9597 0.0004594B 75.24C
200 0.27778 39.52 17.422 −1.6 0.9 4018.3 3.317 6 0.9467 0.0004594B 34.78C
220 0.39284 64.15 14.004 −1.6 0.8 2472.0 3.920 12 0.8962 0.0004594B 47.88C
A
Data from “International Tables for X-Ray Crystallography,” Physical and Chemical Tables, Vol III, Kynoch Press, Birmingham, England, 1962, pp. 60, 61, 210, 213;
Weighted Kα1 and Kα2 value used (λ = 2.29092Å).
B
Temperature factor (T = e−2M) where M = B(sin 2 θ)/λ2 and 2B = 0.71. Also N is the reciprocal of the unit-cell volume.
C
Calculated intensity includes the variables listed that change with X-ray diffraction peak position.
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3.3.3 The volume fraction of austenite ( Vγ) for the ratio of metallographic sample preparation. Standard chromic-acetic
measured integrated intensities of ferrite and austenite peak to acid for electropolishing 0.005-in. (0.127 mm) from samples
R-value is: ground to 600 grit or specific chemical polishing solutions for
V γ 5 ~ I γ / R γ !/ @ ~ I α /R α ! 1 ~ I γ /R γ ! # (1) a particular grade of steel polished to a 2.36 × 10-4in. (6-µm)
finish can be used to verify the metallographic polish. Hot-acid
3.3.4 For numerous ferrite and austenite peaks each ratio of etching is not recommended because of selective etching of
measured integrated intensity to R-value can be summed: one phase or along a preferred crystallographic direction.
Vγ 5 S 1
q
q
(I
j51
γj D FS
⁄R γj /
1
P
P
(I
i51
αi /R αi D S
1
1
q j51
q
(I γj /R γj DG (2)
4.1.5 If retained austenite content on the surface of a sample
is desired and the sample can be mounted in the diffraction
system, no preparation is needed.
3.3.5 If carbides are present: 4.1.6 Sample size shall be large enough to contain the Xray
V α 1V γ 1V c 51 beam at all angles of 2θ required for the X-ray diffraction
analysis to prevent errors in the analysis. In most cases, an area
3.3.6 Then the volume fraction of austenite ( Vα) for the of 1 in.2 (645.16 mm2) is sufficient, but sample size depends
ratio of measured ferrite and austenite integrated intensity to upon the dimensions of the incident X-ray diffraction. When
R-value is: using molybdenum radiation, select peaks in the range from 28
Vγ 5 ~1 2 V c ! ~ I γ /R γ ! / @ ~ I α /R α ! 1 ~ I γ /R γ ! # (3) to 40° 2θ for best results.
3.3.7 For numerous ferrite and austenite peaks the ratio of 4.2 X-Ray Equipment:
measured integrated intensity to R-values can be summed: 4.2.1 Any diffraction system may be used that consists of an
x-ray source, an angular measurement capability, and an x-ray
V γ 5 ~ 1 2 V c! (4) detection system. The system must be capable of obtaining the
entire diffraction peak along with adjacent background levels,
FS 1
q
q
( ~ Iγj/Rγj !
j51
DG F/
1
P (
p
i51
~ I a i/R a i ! 1 q
1 q
( ~I
j51
r i/R r i ! G capable of detecting at least two separate austenite reflections
and a ferrite reflection, and capable of normalizing any
3.4 The volume fraction of carbide, Vc, should be deter- equipment-specific intensity biases not accounted for by
mined by chemical extraction or metallographic methods. R-factors.
Adequate X-ray diffraction peak resolution for the identifica- 4.2.2 A chromium X-ray source with a vanadium metal or
tion of carbide peaks is required to avoid including carbide compound filter to reduce the Kβ radiation is recommended.
peaks in the retained austenite measurement. Chromium radiation produces a minimum of Xray fluorescence
of iron. Chromium radiation provides for the needed X-ray
4. Procedure diffraction peak resolution and allows for the separation of
4.1 Sample Preparation: carbide peaks from austenite and ferrite peaks.
4.1.1 Samples for the X-ray diffractometer shall be cut with 4.2.3 Other radiation such as copper, cobalt, or molybde-
a minimum amount of heat effect. Since most steels containing num can be used, but none of these provide the resolution of
retained austenite are relatively hard, abrasive cutoff wheels chromium radiation. Copper radiation is practical only when a
are frequently used. If adequate cooling is not used, heat effects diffracted-beam monochromator is employed, because iron
from abrasive cutoff wheels can be substantial and, in some X-ray fluorescence will obscure the diffracted peaks.
cases, can transform retained austenite. Saw cutting rather than 4.2.4 A molybdenum source with a zirconium filter is used
abrasive wheel cutting is recommended for sample removal to produce a large number of X-ray diffraction peaks.
whenever it is practical. 4.3 X-Ray Method—X-ray diffraction peaks from other
4.1.2 Rough grinding using a milling tool or high-pressure crystalline phases such as carbides shall be separated from
coarse grinding can deform the surface and transform some of austenite and ferrite peaks. The linearity of the chart recorder
the retained austenite to a depth that is greater than the surface or photographic film shall be verified prior to utilizing this
depth analyzed. Final milling or rough grinding cuts limited to method for older systems using these recording media.
a depth of 0.010-in (0.254 mm). or less should reduce the depth 4.3.1 Entire diffraction peaks minus background under the
of deformation. peaks shall be recorded to obtain integrated peak intensities.
4.1.3 Standard metallographic wet-grinding and polishing Peaks without carbide or second phase interference can be
methods shall be used to prepare samples for X-ray analysis. scanned, and the total peak plus background recorded. Back-
Grit reductions of 80, 120, 240, 320, 400, and 600 silicon ground counts are obtained by counting on each side of the
carbide or alumina abrasives may be used but other valid grit peak for one-half of the total peak counting time. Total
combinations may also be used. A final surface polish of 2.36 background is subtracted from peak plus background to obtain
× 10-4in. (6-µm) diamond or an equivalent abrasive polish is the integrated intensity. Alternatively, software supplied with
required. Sample etching, observation for heat effects, and the diffractometer can be used. In general, a diffractometer
repolishing is a recommended safeguard. scanning rate of 0.5°2θ/min or less is recommended to define
4.1.4 Since deformation caused by dull papers or over- the peaks for austenite contents of less than 5 %.
polishing can transform some of the retained austenite, elec- 4.3.2 Where carbide or other phase X-ray diffraction peak
trolytic polishing or chemical polishing of initial samples of interference exists, planimeter measurements of area under the
each grade and condition should be used to verify proper austenite and ferrite peaks on X-ray diffraction charts can be
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used to obtain integrated intensity. Alternatively, software profile can be doubled with some error in background. A
supplied with the diffractometer can be used. Carbide interfer- densitometer reading of film from a Debye Scherrer camera
ence with austenite and ferrite peaks of the more common may also be used. In many cases, the (111) austenite and (110)
carbides is shown in Fig. 1. ferrite peaks interfere with each other and cannot be resolved.
4.3.3 Another method of determining integrated intensity Four peak ratios of the resolved ferrite to austenite peaks are
involves cutting peak areas from the charts and weighing them adequate to determine the retained austenite content of near
with an analytical balance. randomly oriented samples.
4.3.4 Assuming a 10 % variation in each peak intensity, 4.3.8 Calculated theoretical intensities, R, for ferrite and
chromium peak ratios of integrated intensities (areas under the austenite peaks are listed in Table 1 using chromium Kα
peaks minus background) for the (220) austenite peak relative radiation and in Table 2 using molybdenum Kα radiation.
to (200) austenite peak shall range from 1.1 to 1.7 to satisfy the 4.3.9 The retained austenite content can be estimated from a
requirement of this practice for a near-random orientation of number of ferrite and austenite intensity to R-value ratios using
austenite. Equivalent molybdenum peak ratios range from 0.7 Eq 2 assuming no carbides are present.
to 0.5. 4.3.10 If the volume fraction of carbide has been
4.3.5 Assuming a 10 % variation in each peak intensity, determined, the volume fraction of austenite can be determined
chromium peak ratios of integrated intensities for the (211) from Eq 3 for a single set of peaks or from Eq 4 for more than
ferrite peak relative to the (200) ferrite peak range from 8 to 11 one set of peaks using the theoretical intensities listed in Table
to satisfy the requirement of this practice for a near-random 1 for chromium radiation or in Table 2 for molybdenum
orientation of ferrite. Equivalent molybdenum peak ratios radiation.
range from 1.5 to 2.2.
4.3.6 When either the austenite peak ratio or the ferrite peak 5. Example
ratio is above or below the specified range, this method cannot 5.1 Using chromium radiation, the integrated intensity (area
be used. of peak above background) for ferrite peaks (200) and (211)
4.3.7 Three austenite peaks (111), (200), and (220) and three and for retained austenite peaks (200) and (220) were deter-
ferrite peaks (110), (200), and (211) can be obtained with mined. Values of R for each peak were obtained from Table 1.
chromium radiation on most X-ray diffractometers. Chromium 5.1.1 The measured integrated intensities and values of R
X-ray diffraction limitations may prevent obtaining the entire are illustrated in Table 3.
peak profile for the (211) peak. In this case, the half-peak 5.1.2 From Eq 1 for the α (200) and γ (200) peaks:
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TABLE 2 Calculated Theoretical Intensities Using Molybdenum Kα RadiationA
2
hkl Sinθ/λ θ f ∆f' ∆f9 /F/ LP P TB N2 B RC
(α iron, body-centered cubic, unit-cell dimension ao = 2.8664Å):
110 0.24669 10.10 18.474 0.4 1.0 1428.9 62.15 12 0.9577 0.001803 1840
200 0.34887 14.36 15.218 0.4 0.9 978.9 29.71 6 0.9172 0.001803 288.6
211 0.42728 17.68 13.133 0.4 0.9 735.8 18.95 24 0.8784 0.001803 530.0
220 0.49338 20.53 11.652 0.3 0.9 574.6 13.62 12 0.8413 0.001803 142.5
310 0.55161 23.08 10.542 0.3 0.9 473.4 10.47 24 0.8057 0.001803 172.8
222 0.60426 25.43 9.685 0.3 0.9 402.0 8.396 8 0.7716 0.001803 37.56
321 0.65268 27.64 9.012 0.3 0.9 350.1 6.949 48 0.7390 0.001803 155.6
400 0.69774 29.73 8.480 0.3 0.9 311.6 5.892 6 0.7078 0.001803 14.06
330 0.74006 31.73 8.054 0.3 0.9 282.4 5.099 12 0.6778 0.001803 21.12
411 24 42.23
420 0.78010 33.67 7.713 0.3 0.9 260.1 4.489 24 0.6492 0.001803 32.80
332 0.81817 35.55 7.437 0.3 0.9 242.7 4.017 24 0.6217 0.001803 26.23
422 0.85455 37.40 7.211 0.3 0.9 228.9 3.647 24 0.5954 0.001803 21.51
431 0.88945 39.21 7.022 0.3 0.9 217.7 3.360 48 0.5702 0.001803 36.10
510 24 18.05
521 0.95542 42.77 6.719 0.3 0.9 200.3 2.972 48 0.5230 0.001803 26.94
440 0.98675 44.53 6.591 0.3 0.9 193.2 2.853 12 0.5009 0.001803 5.97
433 1.01712 46.29 6.472 0.3 0.9 186.7 2.775 24 0.4797 0.001803 10.75
530 24 10.75
442 1.04661 48.06 6.357 0.3 0.9 180.5 2.735 24 0.4594 0.001803 9.81
600 6 2.45
532 1.07529 49.84 6.244 0.3 0.9 174.5 2.730 48 0.4400 0.001803 18.14
611 24 9.07
620 1.10322 51.63 6.133 0.3 0.8 168.1 2.759 24 0.4214 0.001803 8.46
541 1.13047 53.46 6.022 0.3 0.8 162.4 2.822 48 0.4036 0.001803 16.01
622 1.15707 55.32 5.913 0.3 0.8 157.0 2.922 24 0.3865 0.001803 7.67
631 1.18307 57.22 5.805 0.3 0.8 151.6 3.061 48 0.3702 0.001803 14.87
444 1.20852 59.19 5.700 0.3 0.8 146.6 3.245 8 0.3545 0.001803 2.43
543 1.23344 61.23 5.598 0.3 0.8 141.7 3.484 48 0.3395 0.001803 14.51
550 12 3.63
710 24 7.25
640 1.25787 63.37 5.503 0.3 0.8 137.3 3.792 24 0.3252 0.001803 7.33
552 1.28183 65.64 5.414 0.3 0.8 133.2 4.193 24 0.3114 0.001803 7.53
633 24 7.53
721 48 15.05
642 1.30535 68.08 5.332 0.3 0.8 129.4 4.731 48 0.2983 0.001803 15.80
730 1.32846 70.76 5.258 0.3 0.8 126.1 5.489 24 0.2856 0.001803 8.55
651 1.37350 77.46 5.130 0.3 0.8 120.5 8.796 48 0.2620 0.001803 24.03
732 48 24.03
(γ iron, face-centered cubic, unit-cell dimension a o = 3.60Å):
111 0.24056 9.84 18.687 0.4 1.0 5845.0 65.51 8 0.9597 0.0004594 1351
200 0.27778 11.39 17.422 0.4 1.0 5098.0 48.43 6 0.9467 0.0004594 644.3
220 0.39284 16.21 14.004 0.4 0.9 3332.6 22.88 12 0.8962 0.0004594 376.7
311 0.46064 19.11 12.355 0.3 0.9 2575.3 15.97 24 0.8601 0.0004594 390.0
222 0.48113 19.99 11.908 0.3 0.9 2397.5 14.44 8 0.8484 0.0004594 107.9
400 0.55556 23.26 10.472 0.3 0.9 1869.5 10.29 6 0.8032 0.0004594 42.59
331 0.60540 25.48 9.668 0.3 0.9 1602.7 8.358 24 0.7709 0.0004594 113.9
420 0.62113 26.20 9.438 0.3 0.9 1530.2 7.849 24 0.7604 0.0004594 100.7
422 0.68041 28.92 8.674 0.3 0.9 1301.5 6.270 24 0.7199 0.0004594 64.77
333 0.72169 30.86 8.231 0.3 0.9 1177.4 5.423 8 0.6909 0.0004594 16.21
511 24 48.64
440 0.78567 33.94 7.670 0.3 0.9 1029.3 4.414 12 0.6452 0.0004594 16.16
531 0.82168 35.73 7.414 0.3 0.9 965.1 3.978 48 0.6192 0.0004594 52.42
442 0.83333 36.32 7.339 946.6 3.854 24 0.6108 0.0004594 24.57
600 6 6.14
620 0.87841 38.63 7.080 0.3 0.9 884.4 3.444 24 0.5782 0.0004594 19.42
533 0.91076 40.34 6.918 0.3 0.9 846.6 3.214 24 0.5549 0.0004594 16.65
622 0.92128 40.90 6.869 0.3 0.9 835.3 3.149 24 0.5474 0.0004594 15.88
444 0.96225 43.15 6.691 0.3 0.9 794.9 2.943 8 0.5182 0.0004594 4.46
551 0.99187 44.82 6.571 0.3 0.9 768.3 2.837 24 0.4973 0.0004594 11.95
711 24 11.95
640 1.00154 45.38 6.533 0.3 0.9 760.0 2.811 24 0.4906 0.0004594 11.56
642 1.03935 47.62 6.385 0.3 0.9 728.0 2.742 48 0.4644 0.0004594 20.44
553 1.06683 49.30 6.278 0.3 0.9 705.3 2.728 24 0.4457 0.0004594 9.46
731 48 18.91
800 1.11111 52.15 6.101 0.3 0.8 665.8 2.773 6 0.4162 0.0004594 2.12
733 1.13685 53.90 5.997 0.3 0.8 644.7 2.842 24 0.3995 0.0004594 8.07
644 1.14531 54.48 5.962 0.3 0.8 637.6 2.873 24 0.3940 0.0004594 7.96
820 24 7.96
660 1.17851 56.88 5.824 0.3 0.8 610.3 3.033 12 0.3730 0.0004594 3.81
822 24 7.61
555 1.20281 58.74 5.723 0.3 0.8 590.7 3.199 8 0.3580 0.0004594 2.49
751 48 14.92
662 1.21081 59.37 5.691 0.3 0.8 584.5 3.264 24 0.3531 0.0004594 7.43
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TABLE 2 Continued
2
hkl Sinθ/λ θ f ∆f' ∆f9 /F/ LP P TB N2 B RC
840 1.24226 61.99 5.564 0.3 0.8 560.4 3.585 24 0.3343 0.0004594 7.41
753 1.26534 64.06 5.475 0.3 0.8 543.8 3.905 48 0.3209 0.0004594 15.03
911 24 7.51
842 1.27294 64.78 5.446 0.3 0.8 538.5 4.030 48 0.3165 0.0004594 15.15
664 1.30289 67.81 5.339 0.3 0.8 519.0 4.666 24 0.2996 0.0004594 8.00
931 1.32492 70.32 5.268 0.3 0.8 506.3 5.352 48 0.2876 0.0004594 17.18
844 1.36083 75.27 5.164 0.3 0.8 487.9 7.391 24 0.2685 0.0004594 10.68
755 1.38193 79.15 5.107 0.3 0.8 478.0 10.26 24 0.2577 0.0004594 13.93
771 24 13.93
933 24 13.93
A
Data from “International Tables for X-Ray Crystallography,” Physical and Chemical Tables, Vol. III, Kynoch Press, Birmingham, England, 1962, pp 60, 61, 210, 213;
Weight Kα1 and Kα2 value used (λ = 0.71069Å).
B
Temperature factor (T = e−2 M) where M = B(sin 2 θ)/λ2 and 2B = 0.71. Also N is the reciprocal of the unit-cell volume.
C
Calculated intensity, R, includes the variables listed that change with X-ray diffraction peak position.
TABLE 3 Measured Integrated Intensities and Values of K 6.2 Bias—No bias estimate is available because there is no
Peak − α (200) γ (200) γ(220) α (211) independent test method to determine an accepted reference
I 1.00 1.00 1.41 9.50 value from retained austenite. Use of this practice produces
R 20.73 34.78 47.88 190.8 comparable values from one facility to another while utilizing
I:R 0.04824 0.02875 0.02945 0.0497
a variety of X-ray diffraction instruments.
7. Report
7.1 For this practice, the accompanying report shall contain
1.00 the following:
34.78 7.1.1 Name of the organization and person performing the
Vγ 5 5 0.373 or 37.3 % retained austenite (5)
1.00 1.00 analysis.
1
20.73 34.78 7.1.2 Date the analysis was completed.
5.1.3 From Eq 2 for all four peaks: 7.1.3 Material type.
7.1.4 Specimen description, size, and location.
½ ~ 0.0287510.02945!
Vγ 5 5 0.373 (6) 7.1.5 X ray system used for the analysis.
½ ~ 0.0482410.04979! 1½ ~ 0.0287510.02945! 7.1.6 Radiation used for the analysis.
7.1.7 Beam size or collimator used.
6. Precision and Bias
7.1.8 Depth where analysis was performed.
6.1 Precision—On the basis of an interlaboratory test pro- 7.1.9 Specimen rotation (Yes / No ).
gram this method produces an intralaboratory repeatability of 7.1.10 Specimen translation (Yes / No ).
3 % and an interlaboratory reproducibility of 4 % both at the 7.1.11 The austenite and ferrite peaks used for the analysis.
95 % confidence level.3 These estimates were derived from 7.1.12 Approximate carbide volume percent.
measurements of specimens containing about 2.5 %, 5 %, and 7.1.13 Carbide correction (Yes / No ).
15 % by volume austenite in a medium carbon steel. These 7.1.14 Volume percent retained austenite.
measures of precision will be degraded with increasing alloy 7.2 Any other information regarding the test procedures
content and also near the minimum detectability limit of 2 %. deemed necessary shall be based upon purchaser-testing labo-
ratory agreements.
3
Hinton, R. W., “Interlaboratory Evaluation of ASTM Practice for X-ray 8. Keywords
Determination of Retained Austenite in Steel with Near-random Crystallographic
Orientation” (Practice E975), Journal of Testing and Evaluation, Vol 15, No. 2 8.1 austenite; crystallographic orientation; ferrite; marten-
March 1987, pp. 95–100. site; retained austenite; X-ray diffraction
6
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