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
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E975 − 22
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 test method 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 test
method.
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hkl
1 ~ /F/ pLPe
2 22M
! 3.3.3 The volume fraction of austenite (Vγ) for the ratio of
Rα 5 measured integrated intensities of ferrite and austenite peak to
v2
R-value is:
where:
V γ 5 ~ I γ / R γ !/ @ ~ I α /R α ! 1 ~ I γ /R γ ! # (1)
Iα hkl = integrated intensity per angular diffraction peak
(hkl) in the α-phase, 3.3.4 For numerous ferrite and austenite peaks each ratio of
Io = intensity of the incident beam, measured integrated intensity to R-value can be summed:
µ = linear absorption coefficient for the steel,
e,m
r
= charge and mass of the electron,
= radius of the diffractometer,
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 (I
j51
q
γj /R γj DG (2)
2
Retained Austenite and Its Measurement by X-ray Diffraction , SAE Special
3.3.6 Then the volume fraction of austenite (Vα) for the ratio
Publication 453, Society of Automotive Engineers (SAE), 400 Commonwealth Dr., of measured ferrite and austenite integrated intensity to R-value
Warrendale, PA 15096-0001, http://www.sae.org. is:
j51
1 p
i51
a i/R a i ! 1
1
q
q
( ~I
j51
r i/R r i ! G entire diffraction peak along with adjacent background levels,
capable of detecting at least two separate austenite reflections
3.4 The volume fraction of carbide, Vc, should be deter- and a ferrite reflection, and capable of normalizing any
mined by chemical extraction or metallographic methods. equipment-specific intensity biases not accounted for by
Adequate X-ray diffraction peak resolution for the identifica- R-factors. Two separate ferrite reflections should be measured;
tion of carbide peaks is required to avoid including carbide however, in alloys with known carbide interference, only the
peaks in the retained austenite measurement. unaffected ferrite reflection may be measured.
4.2.2 A chromium X-ray source with a vanadium metal or
4. Procedure compound filter to reduce the Kβ radiation is should be used.
4.1 Specimen Preparation: NOTE 4—Chromium radiation produces a minimum of X-ray fluores-
4.1.1 Specimens for the X-ray diffractometer shall be cut cence of iron. Chromium radiation provides for the needed X-ray
with a minimum amount of heat effect. Saw cutting rather than diffraction peak resolution and allows for the separation of carbide peaks
abrasive wheel cutting should be for specimen removal when- from austenite and ferrite peaks.
ever it is practical. 4.2.3 Other radiation such as copper, cobalt, or molybde-
num may be used, but none of these provide the resolution of
NOTE 1—Since most steels containing retained austenite are relatively
hard, abrasive cutoff wheels are frequently used. If adequate cooling is not
chromium radiation.
used, heat effects from abrasive cutoff wheels can be substantial and, in NOTE 5—Copper radiation is practical only when a diffracted-beam
some cases, can transform retained austenite. monochromator is employed, because iron X-ray fluorescence will ob-
NOTE 2—Rough machining using a milling tool or coarse grinding can scure the diffracted peaks.
deform the surface and transform some of the retained austenite to a depth
that is greater than the surface depth analyzed. Final milling or rough 4.2.4 A molybdenum source with a zirconium filter may be
grinding cuts limited to a depth of 0.010-in (0.254 mm) or less will reduce used to produce a large number of X-ray diffraction peaks.
the depth of deformation.
4.3 X-Ray Method—X-ray diffraction peaks from other
4.1.2 Standard metallographic wet-grinding and polishing crystalline phases such as carbides shall be separated from
methods shall be used to prepare specimens for X-ray analysis. austenite and ferrite peaks. The linearity of the chart recorder
Grit reductions of 80, 120, 240, 320, 400, and 600 silicon or photographic film shall be verified prior to utilizing this
carbide or alumina abrasives may be used, but other valid grit method for older systems using these recording media.
combinations may also be used. 4.3.1 Entire diffraction peaks minus background under the
4.1.2.1 The final surface polish shall be 2.36 × 10-4in. peaks shall be recorded to obtain integrated peak intensities.
(6-µm) diamond or an equivalent abrasive polish. Peaks without carbide or second phase interference may be
4.1.2.2 Specimen etching, observation for heat effects, and scanned, and the total peak plus background recorded. Obtain
repolishing should be conducted as a safeguard. background counts by counting on each side of the peak for
4.1.3 Since deformation caused by dull papers or over- one-half of the total peak counting time. Subtract the total
polishing can transform some of the retained austenite, elec- background from peak plus background to obtain the integrated
trolytic polishing or chemical polishing of initial specimens of intensity. Alternatively, software supplied with the diffracto-
each grade and condition should be used to verify proper meter may be used. In general, the diffractometer scanning rate
metallographic specimen preparation. Standard chromic-acetic should be 0.5°2θ/min or less to define the peaks for austenite
acid for electropolishing 0.005-in. (0.127 mm) from specimens contents of less than 5 %.
ground to 600 grit or specific chemical polishing solutions for 4.3.2 Where carbide or other phase X-ray diffraction peak
a particular grade of steel polished to a 2.36 × 10-4in. (6-µm) interference exists, planimeter measurements of area under the
finish may be used to verify the metallographic polish. Hot- austenite and ferrite peaks on X-ray diffraction charts may be
acid etching should not be used because of selective etching of used to obtain integrated intensity. Alternatively, software
one phase or along a preferred crystallographic direction. supplied with the diffractometer may be used.
4.1.4 If measurement of the retained austenite content on the NOTE 6—Details of the correction techniques are outside the scope of
surface of a specimen is desired and the specimen can be this test method. Carbide interference with austenite and ferrite peaks of
mounted in the diffraction system, no preparation is needed. the more common carbides is shown in Fig. 1.
4.1.5 Specimen size shall be large enough to contain the 4.3.3 The integrated intensity may be determined by cutting
X-ray beam at all angles of 2θ required for the X-ray peak areas from the charts and weighing them with an
diffraction analysis to prevent errors in the analysis. analytical balance.
NOTE 3—In most cases, an area of 1 in.2 (645.16 mm2) is sufficient, but 4.3.4 Assuming a 10 % variation in each peak intensity,
specimen size depends upon the dimensions of the incident X-ray chromium peak ratios of integrated intensities (areas under the
diffraction. peaks minus background) for the (220) austenite peak relative
to (200) austenite peak shall range from 1.1 to 1.7 to satisfy the peaks (110), (200), and (211) can be obtained with chromium radiation on
requirement of this test method for a near-random orientation most X-ray diffractometers. Chromium X-ray diffraction limitations may
prevent obtaining the entire peak profile for the (211) peak. In this case,
of austenite. Equivalent molybdenum peak ratios range from the half-peak profile can be doubled with some error in background. A
0.7 to 0.5. densitometer reading of film from a Debye Scherrer camera may also be
4.3.5 Assuming a 10 % variation in each peak intensity, used. In many cases, the (111) austenite and (110) ferrite peaks interfere
chromium peak ratios of integrated intensities for the (211) with each other and cannot be resolved. Four peak ratios of the resolved
ferrite peak relative to the (200) ferrite peak range from 8 to 11 ferrite to austenite peaks are adequate to determine the retained austenite
content of near randomly oriented specimens.
to satisfy the requirement of this test method for a near-random
orientation of ferrite. Equivalent molybdenum peak ratios 4.3.6 Calculated theoretical intensities, R, for ferrite and
range from 1.5 to 2.2. austenite peaks, for a Bragg-Brentano powder diffractometer,
are listed in Table 1 using chromium Kα radiation and in Table
NOTE 7—When either the austenite peak ratio or the ferrite peak ratio 2 using molybdenum Kα radiation. The R values shown are for
is above or below the specified range, this may indicate carbide interfer-
ence and/or preferred orientation which can result in an increase in only one type of steel. R values will vary with the composition
measurement error. of the steel and therefore should be calculated from first
NOTE 8—Three austenite peaks (111), (200), and (220) and three ferrite principles for each steel alloy tested to ensure accurate results.
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.
4.3.7 The retained austenite content may be estimated from measurements of specimens containing about 2.5 %, 5 %, and
a number of ferrite and austenite intensity to R-value ratios 15 % by volume austenite in a medium carbon steel. These
using Eq 2 assuming no carbides are present. measures of precision will be degraded with increasing alloy
4.3.8 If the volume fraction of carbide has been determined, content and also near the minimum detectability limit of 2 %.
the volume fraction of austenite may be determined from Eq 3
for a single set of peaks or from Eq 4 for more than one set of 6.2 Bias—No bias estimate is available because there is no
peaks using the theoretical intensities listed in Table 1 for independent test method to determine an accepted reference
chromium radiation or in Table 2 for molybdenum radiation. value from retained austenite. Use of this test method produces
comparable values from one facility to another while utilizing
5. Example a variety of X-ray diffraction instruments.
5.1 Using chromium radiation, the integrated intensity (area
of peak above background) for ferrite peaks (200) and (211) 7. Report
and for retained austenite peaks (200) and (220) were deter-
7.1 For this test method, the accompanying report shall
mined. Values of R for each peak were obtained from Table 1.
contain the following:
5.1.1 The measured integrated intensities and values of R
are illustrated in Table 3. 7.1.1 Name of the organization and person performing the
5.1.2 From Eq 1 for the α (200) and γ (200) peaks: analysis.
1.00 7.1.2 Date the analysis was completed.
34.78 7.1.3 Material type.
Vγ 5 5 0.373 or 37.3 % retained austenite (5)
1.00 1.00 7.1.4 Specimen description, size, and location.
1
20.73 34.78 7.1.5 X ray system used for the analysis.
5.1.3 From Eq 2 for all four peaks: 7.1.6 Radiation used for the analysis.
½ ~ 0.0287510.02945! 7.1.7 Beam size or collimator used.
Vγ 5 5 0.373 (6)
½ ~ 0.0482410.04979! 1½ ~ 0.0287510.02945! 7.1.8 Depth where analysis was performed.
6. Precision and Bias 7.1.9 Specimen rotation (Yes / No ).
7.1.10 Specimen translation (Yes / No ).
6.1 Precision—On the basis of an interlaboratory test pro-
gram this test method produces an intralaboratory repeatability 7.1.11 The austenite and ferrite peaks used for the analysis.
of 3 % and an interlaboratory reproducibility of 4 % both at the 7.1.12 Approximate carbide volume percent, if determined.
95 % confidence level.3 These estimates were derived from 7.1.13 Carbide correction (Yes / No ).
7.1.14 Volume percent retained austenite.
3
Hinton, R. W., “Interlaboratory Evaluation of ASTM Practice for X-ray
Determination of Retained Austenite in Steel with Near-random Crystallographic 7.2 Any other information regarding the test procedures
Orientation” (Practice E975), Journal of Testing and Evaluation, Vol 15, No. 2 deemed necessary shall be based upon purchaser-testing labo-
March 1987, pp. 95–100.
ratory agreements.
TABLE 3 Measured Integrated Intensities and Values of K
8. Keywords
Peak − α (200) γ (200) γ(220) α (211)
I 1.00 1.00 1.41 9.50
8.1 austenite; crystallographic orientation; ferrite; marten-
R 20.73 34.78 47.88 190.8 site; retained austenite; X-ray diffraction
I:R 0.04824 0.02875 0.02945 0.0497
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