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Comparison of different methods for measuring

strain induced a9-martensite content in austenitic


steels
J. Talonen, P. Aspegren and H. Hänninen

Several techniques for measuring the strain induced a9-martensite content in EN 1.4318 (AISI 301LN) and
EN 1.4301 (AISI 304) austenitic stainless steels were compared in order to determine a correlation curve between
Ferritescope measurement results and actual a9-martensite contents. The studied methods involved Satmagan
measurement, magnetic balance measurement, X-ray diffraction, density measurement and quantitative optical
metallography. Satmagan, magnetic balance and density measurements were found to give equal a9-martensite
contents. X-ray diffraction results were affected by the texture but averaging of several diffraction peaks improved
the reliability of the results. It was shown that a9-martensite can be detected by means of optical metallography, but
quantitative analysis is time consuming and inaccurate. The relationship between the Ferritescope results and actual
a9-martensite contents measured with the other techniques was found to be linear. According to the results, the
Ferritescope readings can be converted to actual a9-martensite contents by multiplying with a correction factor of
1.7. MST/6120

Keywords: Strain induced martensite, Austenitic stainless steel, Ferritescope


Published by Maney Publishing (c) IOM Communications Ltd

Mr Talonen and Dr Hänninen are in the Laboratory of Engineering Materials, Helsinki University of Technology, PO Box
4200, FIN – 02015 HUT, Finland (Email: hannu.hanninen@hut.fi). Mr Aspegren is with Outokumpu Stainless Oy, FIN – 95400
Tornio, Finland. Manuscript received 26 January 2004; accepted 24 August 2004.
# 2004 Institute of Materials, Minerals and Mining. Published by Maney on behalf of the Institute.

Correction terms to calculate corrected a9-martensite


Introduction content were derived from the texture functions. In addition
to the problems caused by the texture, X-ray diffraction
Strain induced e- and a9-martensite phases form during measurements are also expensive, time consuming and
plastic deformation of metastable austenitic stainless steels. cover only a thin layer on the specimen surface. For c(111)
The formation of a9-martensite affects significantly the peaks, the depth at which 95% of X-rays are scattered was
mechanical behaviour of the steels by enhancing the work calculated to be 2.6, 6.2, 8.7 and 8.7 mm when using Cu
hardening.1 The mechanisms of martensitic transformations Ka, Co Ka, Cr Ka and Mo Ka radiations, respectively.12
have been studied extensively. It has been established that In addition, for most X-ray diffraction equipment a
a9-martensite is nucleated in the austenite phase at the small specimen must be cut from the material for the
intersections of shear bands that consist of e-martensite, measurement.
stacking fault bundles and mechanical twins.2 – 4 The Measurements based on ferromagnetism of a9-martensite
amount of a9-martensite increases with increasing plastic phase involve measurement of magnetic force acting on the
strain at the expense of austenite and e-martensite phases. specimen placed in a magnetic field1,5,13 – 15 and measure-
The extent of a9-martensite transformation depends ment of magnetisation.7,16,17 As in the case of X-ray
strongly on the steel composition and the temperature at diffraction, these methods normally require that the speci-
which the deformation takes place.5 The strain rate,1,6,7 mens are cut from the test material. The easiest magnetic
grain size8 and the type of the applied deformation6,7 also technique to measure the a9-martensite content is by using a
affect the rate of a9-martensite formation. Ferritescope, a device that is normally used to measure the
Because the cAa9 transformation plays an important role d-ferrite content of austenitic stainless steel weldments. The
in the mechanical behaviour of steels, measurement of the measurement is non-destructive, takes only a few seconds
strain induced a9-martensite content is an important and can be performed in situ. The operational principle of
requirement when investigating the plastic deformation of the Ferritescope is based on the determination of the
austenitic stainless steels. Several techniques are available magnetic permeability of the material. This causes an error
for this measurement. The most common methods involve in the measured values because the magnetic permeability of
X-ray diffraction and techniques based on the ferromagnet- a9-martensite is a function of strain.7 Therefore, the results
ism of the a9-martensite phase. a9-martensite contents have obtained with a Ferritescope have to be converted to actual
also been determined by density measurements.6 a9-martensite contents by using a calibration curve.
X-ray diffraction can be used for quantitative phase Calibration curves have been determined by using different
analysis, because the austenite and a9-martensite phases measurement techniques.7,14,18,19 Comparison of the curves
have different crystal structures. A disadvantage of X-ray is shown in Fig. 1, where it can be observed that there is a
diffraction is inaccuracy because of the texture that is disagreement between the references. The method by which
present in the sheet materials especially after plastic the actual a9-martensite content has been determined does
deformation.9 The effect of texture can be reduced by not explain the differences, because a Satmagan equipment
averaging intensities of several diffraction peaks.10 Cheary was used by Rintamaa,14 a magnetometer by Hecker et al.7
and Ma-Sorrell11 corrected the effect of texture by and X-ray diffraction by Peterson18 and Hünicke.19
determining texture functions by measuring the intensities The aim of this paper is to determine a reliable correlation
of the c(111) and a9(110) reflections as a function of y angle between the Ferritescope measurement results and actual
(the angle between the specimen surface and X-ray beam). a9-martensite contents. To confirm the reliability of the

1506 Materials Science and Technology December 2004 Vol. 20 DOI 10.1179/026708304X4367
Talonen et al. Measuring strain induced a9-martensite in austenitic steels 1507

The device was calibrated with d-ferrite samples and its


measurement range was 0 – 60% d-ferrite. Five measure-
ments were performed on each sample at arbitrary locations
on the specimen surface. The results measured from thin
specimens were corrected with a correction curve provided
by the manufacturer.20

X-RAY DIFFRACTION MEASUREMENTS


Two different types of X-ray diffraction (XRD) equipment
were used in this investigation. One consisted of a Siemens
Kristalloflex 710H X-ray generator, Co Ka tube and INEL
CPS120 position sensitive detector. With this equipment,
five austenite peaks and four a9-martensite peaks could be
detected. To eliminate the effect of texture, the intensities of
the measured diffraction peaks were averaged and the
1 Comparison of the calibration curves between the Fer- specimen was rotated in w angle during the measurement.
ritescope and actual a9-martensite contents presented The other equipment was Stresstech XSTRESS 3000 X-ray
in literature stress analyser with Cr Ka tube and a semiconductor
detector. With this equipment, only c(220)- and a9(211)-
results several different measurement techniques were peaks were detected. In order to eliminate the effect of
compared. The studied methods were Satmagan measure- texture, the X-ray beam was tilted ¡45u in w and y angles
ment, X-ray diffraction, density measurement and quanti- during the measurements. The dimensions of the XRD
Published by Maney Publishing (c) IOM Communications Ltd

tative optical metallography. Furthermore, a magnetic specimens were 10610 mm2.


balance based on a permanent magnet was constructed. The X-ray diffraction data was analysed with Microcal
Origin software. The a9-martensite volume fractions were
determined from X-ray diffraction data by using the
equation21
Experimental procedure
Ic Rc Vc
~ : : : : : : : : : : : : : (1)
TEST MATERIALS AND SAMPLE Ia 0 Ra0 Va0
PREPARATION where Ic and Ia9 are the integrated intensities of austenite
The test materials were commercial austenitic stainless and a9-martensite reflections, Rc and Ra9 are constants and
steel grades EN 1.4301 (AISI 304) and EN 1.4318 Vc and Va9 are volume fractions of austenite and a9-
(AISI 301LN). The chemical compositions of the steels martensite phases, respectively. By assuming that
are given in Table 1. VczVa9~1, the volume fraction of a9-martensite can be
The specimens were strained in tension or by cold rolling at solved as
room temperature to obtain different a9-martensite contents. Ia0 Rc
The pre-straining was assumed to produce a uniform Va0 ~ : : : : : : : : : : : (2)
Ic Ra0 zIa0 Rc
distribution of strain induced a9-martensite in the samples.
Specimens for destructive a9-martensite measurements were The constants Rc and Ra9 are determined by the crystal
cut from the strained sheets with an abrasive cutting machine structure, composition and lattice parameters of the studied
and the edges of the specimens were finished with SiC emery phases, given by22
paper. It was not possible to perform the measurements with  
1
different techniques on the same samples because specimens R~ 2 F 2 p(LP) exp ({2M) : : : : : : : (3)
v
with different dimensions were required for Satmagan and
X-ray diffraction measurements, and in the density measure- where v is the unit cell volume, F2 is the structure factor, p is
ments maximising the specimen size was preferable in order the multiplicity factor, LP is the Lorentz polarisation factor
to obtain best possible accuracy. and exp(22M) is the temperature factor. Values of these
Ferritescope and X-ray diffraction measurements were factors were taken from Refs. 22 and 23. The R values of
performed mainly on electropolished surfaces. Some trials the measured XRD peaks for Co Ka and Cr Ka radiations
were carried out also on as received surfaces. Surface are presented in Table 2. For Cr Ka radiation, the R values
treatment was considered to have no effect on Satmagan, were not calculated but taken from Ref. 24.
magnetic balance and density measurements, as these
techniques cover the whole volume of the specimen.
Electropolishing was performed with a Struers Lectropol- SATMAGAN MEASUREMENTS
5 equipment using A2 electrolyte (78 mL perchloric acid, A series of specimens was measured with a Satmagan
120 mL distilled water, 700 mL ethanol and 100 mL butyl device. The Satmagan is a magnetic balance that is used to
cellosolve) at 20 V at room temperature. determine the content of the ferromagnetic phase in a
specimen. In a Satmagan measurement a saturating
magnetic field is applied to the specimen that is placed in
FERRITESCOPE MEASUREMENTS a sample holder. The magnetic field causes a force that is
The a9-martensite content of all specimens was measured recorded by adjusting a potentiometer. The relation
with a Ferritescope (Helmut Fischer GmbH, model MP3C). between the potentiometer reading S and the content of

Table 1 The chemical compositions of the test materials (mass %)


Grade Thickness C N Si P S Cr Mn Ni Cu Mo

EN 1.4318 1 mm 0.019 0.094 0.48 0.028 0.002 17.6 1.61 6. 6 0.22 0.14
EN 1.4318 2 mm 0.024 0.106 0.52 0.027 0.001 17.5 1.23 6. 4 0.28 0.17
EN 1.4301 2 mm 0.046 0.050 0.38 0.031 0.002 18.1 1.73 8. 1 0.23 0.24

Materials Science and Technology December 2004 Vol. 20


1508 Talonen et al. Measuring strain induced a9-martensite in austenitic steels

the ferromagnetic phase is expressed as14 DENSITY MEASUREMENTS


ca0 Msat Because austenite and a9-martensite phases have different
S~K : : : : : : : : : : : : : (4) crystal structures, their densities are not equal. If the
r
densities of both phases are known, the content of a9-
where K is constant, ca9 is the mass percentage of the martensite phase can be determined by measuring the
ferromagnetic phase, Msat is the saturation magnetisation of density of the specimen. However, this requires that a9-
the ferromagnetic phase and r is density. The value of martensite content is assumed to be a linear function of the
constant K is determined by empirical calibration. In this density, which is not exactly true owing to the crystal defects
investigation the calibration constant determined by in both phases. The densities of the austenite and a9-
Rintamaa14 was used. Assuming that the saturation martensite phases were determined by using the equation
magnetisation of a9-martensite is 1.65 T (in fact, the value
of saturation magnetisation depends on the steel composi- nA
r~ : : : : : : : : : : : : : : (6)
tion and density, but this error was regarded as negligible), VNA
the a9-martensite content ca9 can be calculated from the where n is the number of atoms in a unit cell (two in a9-
potentiometer reading S by using equation14 martensite, four in austenite), A is the atomic weight, V is
ca0 (mass%)~0:1266|S : : : : : : : : : : (5) the volume of a unit cell and NA is Avogadro’s number. The
volume of the unit cell was calculated by using X-ray
The size of the Satmagan samples was 9610 mm2. diffraction data (Co Ka radiation, using the same equipment
as for a9-martensite measurements). Average atomic
weights were derived from the chemical composition data
MAGNETIC BALANCE that was given in mass percentages. The density measure-
The principle of measuring the force acting on a ments were performed utilising the Archimedean principle.
The mass of the samples was first measured with a Mettler
Published by Maney Publishing (c) IOM Communications Ltd

ferromagnetic sample placed in a magnetic field was applied


by constructing a magnetic balance using the original idea Toledo AG204DR balance having the repeatability of
of Livitsanos and Thomson.15 The equipment consisted of 0.0001 g. The volume of the specimen was then determined
an analytical balance, an AlNiCo permanent magnet by immersing the specimen in distilled water placed on the
attached to the stage of the balance and a stage made of balance. The specimen was supported with 0.1 mm thin
aluminium on which the sample was placed for the fishing line. A small amount of wetting agent was added to
measurement. The tip of the magnet was conical to the water to improve its wettability. The density of the
minimise the effect of size and surface roughness of the specimen was calculated by using equation
specimen. The force acting between the specimen and mA rW
the magnet (the force needed to disconnect the sample from r~ : : : : : : : : : : : : : : (7)
mW
the magnet) was measured by lifting the stage by adjusting a
screw. The measured force is proportional to the mass where mA is the mass of the specimen weighed in air, mW is
content of a9-martensite. Therefore, a9-martensite content the mass of the specimen weighed in distilled water and rW
can be calculated by dividing the measured force with the is the density of distilled water.25 The specimens were about
force characteristic of a fully martensitic sample. 10 mm wide and 50 mm long and, depending on the sheet
The main difference between the magnetic balance and thickness, their mass ranged between 7 and 14 g. Therefore,
Satmagan is that in a Satmagan measurement the sample is the accuracy of the balance enabled the martensite contents
fully saturated by the applied magnetic field – a situation to be measured with the accuracy of ¡0.5 mass %. The
that is not present when using a relatively weak permanent measurements were performed at room temperature, which
magnet. Therefore, the size of the specimen, especially the varied about ¡2uC during the measurements. The tem-
thickness, affects the force acting between the sample and perature of the water was recorded during the measure-
the magnet. In this investigation, all measurements were ments and the effect of the temperature on the density of
performed on originally 20 mm wide and 220 mm long water was taken into account in the analysis.25 The effect of
tensile test specimens. The changes in the dimensions temperature on the density of the phases was neglected. The
because of plastic straining were found to have no effect of the volume of the line used to support the specimen
significant influence on the results. The thickness of the was also considered negligible. All samples were measured
samples varied between 0.9 and 2.0 mm. The thickness three times.
calibration was performed by determining an experimental
calibration curve by measuring fully martensitic specimens
of different thicknesses. X-ray diffraction was used to OPTICAL METALLOGRAPHY
confirm the fully martensitic microstructure of the calibra-
a9-martensite was detected by means of optical metallo-
tion samples. Both cold rolled and tensile strained samples
graphy using Ferrofluid. The cross-sections of the test
were used for calibration and no difference between them
materials, cut with an abrasive cutting machine, were
was found. With both the Satmagan device and the
ground with SiC emery paper up to a roughness of 2500 grit
magnetic balance the effect of steel composition was
and then electropolished with the procedure described
neglected.
above. The grain boundaries were etched electrolytically
with aqueous nitric acid (60 vol.-% HNO3 and 40 vol.-%
Table 2 The values of R for the austenite and a9-
H2O) at 1.5 V for 30 s. To colour the a9-martensite phase,
martensite reflections
Ferrofluid (Ferrotec Corporation EMG 308) was used.
XRD peak R (Co Ka) R (Cr Ka) Ferrofluid is a water based liquid that contains small
magnetic particles with an average diameter of 10 nm. The
c(111) 138.4 Ferrofluid was diluted with water (1 part Ferrofluid, 30
c(200) 62.7
c(220) 36.8 47.9
parts water) and a small amount of wetting agent was added
c(311) 56.9 to the solution. The solution was applied to the polished
c(222) 19.5 and etched specimen surfaces with a syringe. As a result, the
a9(110) 206.2 small magnetic particles were attached to the ferromagnetic
a9(200) 29.1
a9(211) 65.0 190.8
a9-phase, which was coloured dark. After the preparation,
a9(220) 32.1 the specimens were investigated with a Nikon Epiphot
microscope.

Materials Science and Technology December 2004 Vol. 20


Talonen et al. Measuring strain induced a9-martensite in austenitic steels 1509

3 a9-martensite contents (in mass %) measured by


2 X-ray diffraction spectra of as received and electropol- means of X-ray diffraction and plotted as a function of
ished EN 1.4318 2B steel specimens Ferritescope reading

Results SATMAGAN MEASUREMENTS


Published by Maney Publishing (c) IOM Communications Ltd

The relationship between the Ferritescope readings F


RESULTS OF THE X-RAY DIFFRACTION and the a9-martensite contents ca9 measured with Satmagan
MEASUREMENTS is shown in Fig. 4. The relationship seems to be linear and
no difference can be observed between tensile strained and
Effect of surface condition
cold rolled specimens. Fitting of a linear function to the
The first X-ray diffraction measurements performed on the as data gives the following equation with R2~0.992
received steel surfaces revealed that in unstable EN 1.4318
steel a9-martensite was present even on the surface of 2B ca0 (mass%)~0:261z1:714|F : : : : : : : (11)
(cold rolled, soft annealed and skin pass rolled) material.
Measurement on the electropolished surface showed that
almost all a9-martensite disappeared after removal of a surface MAGNETIC BALANCE
layer with thickness of a few microns. Further polishing did The correlation between the sheet thickness t and the
not affect the results. Also Ferritescope results measured on balance reading B for fully martensitic specimens is shown
the as received surfaces were slightly higher than those in Fig. 5. It can be observed that the effect of thickness is
measured on the electropolished surfaces. Examples of X-ray significant with low sheet thicknesses. The results can be
diffraction spectra, measured with Co Ka radiation before and expressed with an equation
after electropolishing, are shown in Fig 2. a9-martensite is
B~{560:6z123:5|½1{exp ({t=2:3)z968:5
transformed on the steel surface probably as a result of surface
roughness of the skin pass rolls. Although the cold rolling |½1{exp ({t=0:22) (12)
reduction is very low, considerable plastic deformation occurs The relation between the Ferritescope measurement results
in a very thin layer of the steel surface during rolling. F and the a9-martensite contents ca9 obtained with the
Therefore, it was concluded that to obtain the results magnetic balance is shown in Fig. 6. As with Satmagan, the
representing the average a9-martensite content of the specimen dependence is linear except for the Ferritescope readings
volume with X-ray diffraction, the measurements must be above 55.
performed on the electropolished surfaces. Fitting a linear function to the data gives the following
equation between the Ferritescope reading F and actual a9-
Measurement of a9-martensite content with martensite content ca9 with R2~0.993
X-ray diffraction
ca0 (mass%)~{0:03z1:766|F : : : : : : : (13)
Almost no evidence of the presence of e-martensite was
found from the X-ray diffraction results. Therefore, all the
samples were considered to contain only austenite and a9-
martensite phases. The a9-martensite contents ca9 measured
with X-ray diffraction are shown as a function of
Ferritescope results F in Fig. 3. The X-ray diffraction
technique gives the contents in volume percentages, which
were converted to mass percentages. Probably because of
differences in the texture, the samples deformed by tensile
straining and by cold rolling show different slopes. The
linear fitting gives the following equations
Cold rolled material, Cr Ka radiation (R2~0.973)

ca0 (mass%)~1:203z2:676|F : : : : : : : (8)


2
Cold rolled material, Co Ka radiation (R ~0.992)
ca0 (mass%)~4:140z1:845|F : : : : : : : (9)
2
Tensile strained material, Cr Ka radiation (R ~0.961)
4 a9-martensite contents (in mass %) measured with Sat-
ca0 (mass%)~0:696z1:422|F : : : : : : : (10) magan and plotted as a function of Ferritescope reading

Materials Science and Technology December 2004 Vol. 20


1510 Talonen et al. Measuring strain induced a9-martensite in austenitic steels

7 a9-martensite contents (in mass %) calculated from the


5 Correlation between sheet thickness and balance read- density of the specimens and plotted as a function of
ing for fully martensitic specimen Ferritescope reading

with Satmagan and magnetic balance results, the relation-


Published by Maney Publishing (c) IOM Communications Ltd

ship here seems to be linear, except for the two points that
correspond to the Ferritescope readings above 55. Fitting of
a linear function to the linear part of the data gives an
equation with R2~0.987
ca0 (mass%)~0:004{1:712|F : : : : : : : (17)

OPTICAL METALLOGRAPHY
The microstructure of 15% tensile strained EN 1.4318 steel
is shown in Fig. 8. a9-martensite is coloured in dark grey.
The morphology of a9-martensite phase is in agreement with
the literature. It is very finely dispersed and formed on shear
bands of the austenite phase. Some larger coloured areas
can also be seen. These areas may consist of excess
Ferrofluid that has been distributed non-uniformly and
probably does not indicate the ferromagnetic phase.
6 a9-martensite contents (in mass %) measured with the The a9-martensite content was calculated by means of a
magnetic balance and plotted as a function of Ferrite- point count method.26 The measurements were performed
scope reading on the screen of a microcomputer, which was found to be
the easiest way to distinguish between the finely dispersed
DENSITY MEASUREMENTS a9-martensite phase and the austenite phase. Several
micrographs taken at different locations were counted.
The calculated densities of austenite and a9-martensite The number of points in the grid used was 25. Counting the
phases for the test materials are shown in Table 3. The points in the sample shown in Fig. 8 gave an a9-martensite
following equations were derived from the density values to content of 22.4¡2.4% (volume percentages converted to
calculate the a9-martensite content by assuming a linear mass percentages). The Satmagan measurement for the
relationship between a9-martensite content ca9 and density r same sample gave an a9-martensite content of 18.3%.
of the material
EN 1.4318, 1 mm
ca0 (mass%)~4393{555:6|r : : : : : : : : (14) Discussion
EN 1.4318, 2 mm
ca0 (mass%)~4417{558:7|r : : : : : : : : (15) X-ray diffraction results showed high scatter and different
curves were obtained with different techniques. When
EN 1.4301, 2 mm comparing only one austenite and one a9-martensite
reflection cold rolled and tensile strained materials
ca0 (mass%)~4920{621:1|r : : : : : : : : (16)
showed different correlations with the Ferritescope results.
The density measurement results converted to a9-martensite The results correlated best with the other measurement
contents with equations (14) – (16) are shown as a function techniques studied when several diffraction peaks were
of Ferritescope readings F in Fig. 7. Each data point averaged. It is clear that the discrepancy is caused by the
represents an average of three density measurements. As texture.10 Tilting the X-ray beam in the y angle was not

Table 3 Calculated densities of austenite and a9-martensite phases


Material Thickness Density of austenite, g cm23 Density of a9-martensite, g cm23

EN 1.4318 1 mm 7.908 7.728


EN 1.4318 2 mm 7.906 7.727
EN 1.4301 2 mm 7.922 7.761

Materials Science and Technology December 2004 Vol. 20


Talonen et al. Measuring strain induced a9-martensite in austenitic steels 1511

8 a9-martensite phase coloured by Ferrofluid in EN 1.4318 steel after 15% tensile deformation
Published by Maney Publishing (c) IOM Communications Ltd

found to be an effective way to eliminate the effect of the With all the techniques studied both tensile strained and
texture. In the case of X-ray diffraction, another source of cold rolled materials were tested, and in each case the results
error is that only a small amount of material is covered by followed the same line.
the measurement. Satmagan measurements and density Optical microscopy was shown to be applicable to detect
measurements give an average value of a9-martensite a9-martensite. Point counting gave slightly higher a9-
content whereas the X-ray diffraction measurements martensite content than the Satmagan measurement. The
cover only a very thin layer on the specimen surface. very fine morphology of the a9-martensite phase makes
Therefore, if the distribution of a9-martensite within the point counting difficult. In addition, non-uniform distribu-
specimen is not uniform, comparison of the XRD results tion of Ferrofluid may cause false indications and, there-
with the other methods covering a larger volume or the fore, lead to overestimation of the a9-martensite content.
whole specimen should not be performed. Comparison of the results with the calibration curves
The Satmagan measurements, the magnetic balance presented in the literature shows that the curves presented
measurements and the density measurements showed by Hecker et al.7 and by Peterson18 strongly overestimate
similar correlations between the measured a9-martensite the actual a9-martensite contents. The curves determined by
contents and the Ferritescope measurement results. The Rintamaa14 and Hünicke19 are in a better agreement with
results can, therefore, be considered representative. The the results obtained in this investigation, especially at low
relationship between Ferritescope readings and measured a9-martensite content.
a9-martensite contents was found to be linear when the
Ferritescope reading was below the value of 55 (the
corresponding a9-martensite content is 90%). The measure-
ment range of Ferritescope is 0 – 60% d-ferrite. Therefore, Conclusions
the non-linearity of the correlation curve at the high a9-
contents is most probably caused by the limitation of the A Ferritescope may be used to measure strain induced a9-
Ferritescope. This assumption is supported by the fact that martensite, but a calibration curve is needed to convert the
similar behaviour was observed in the case of all compared results to actual a9-martensite content. The Satmagan
methods. device and density measurements were found to give
The reproducibility of the density measurement technique consistent results and the relation between the measured
was found to be unsatisfactory, but averaging of the results a9-martensite content and Ferritescope readings is linear
from several measurements resulted in a similar curve to the below Ferritescope readings of 55 (a9-martensite content of
magnetic balance technique and the Satmagan measure- 90%).
ments. The accuracy of the density measurements could be A magnetic balance based on a permanent magnet was
improved by using a liquid with higher density for volume found to be a reliable and rapid way to measure a9-
determination and larger specimens. martensite content. The results correlated well with the
The magnetic balance technique proved to be an accurate Satmagan and density measurement results. The limitation
and easy way to measure the a9-martensite content. As of the method is its sensitivity to the size and shape of the
discussed earlier in this paper and by Livitsanos and specimen.
Thomson,15 the method is sensitive to the size of the It was observed that a9-martensite content is higher on
specimen, especially to the thickness of the specimen. Other the steel surfaces than in the interior. Therefore, X-ray
possible sources of error are surface roughness and diffraction measurements must to be performed on the
curvature. When using a magnet with a tapered tip the electropolished surfaces to obtain representative results.
effect of surface roughness is most probably negligible. The Electropolishing is recommended also for other methods
effect of curvature was not studied in this investigation, but that do not cover the whole volume of the specimen
it needs further consideration if curved specimens are to be (Ferritescope and magnetic balance). The results of X-ray
measured. Livitsanos and Thomson15 also discussed diffraction measurements were affected by the texture. The
whether the stress state during deformation or the texture effect of the texture can be reduced by averaging several
affects the magnetic measurement. It was concluded that diffraction peaks.
these factors do not have any influence on the measurement. Optical metallography was found to be applicable to
This is supported by the results presented in this paper. detect a9-martensite. Quantitative analysis by means of

Materials Science and Technology December 2004 Vol. 20


1512 Talonen et al. Measuring strain induced a9-martensite in austenitic steels

point counting is, however, inaccurate and time consuming 9. j. durnin and k. a. ridal: J. Iron Steel Inst., 1968, 206, 60 –
because of the fine morphology of the a9-martensite phase 67.
and the possible false indications caused by non-uniform 10. r. d. arnell: J. Iron Steel Inst., 1968, 206, 1035 – 1036.
distribution of Ferrofluid. 11. r. w. cheary and y. ma-sorrell: J. Mater. Sci., 2000, 35,
1105 – 1113.
According to the results of this investigation, the 12. p. rozenak and d. eliezer: Mater. Sci. Eng., 1984, 67, L1 – L4.
Ferritescope readings F can be converted to the actual a9- 13. c. p. livitsanos and p. f. thomson: Mater. Sci. Eng., 1977, 30,
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