[go: up one dir, main page]

0% found this document useful (0 votes)
16 views16 pages

Статья по S17400

The study investigates the effects of quenching temperature and tempering time on the microstructure of UNS S17400 precipitation-hardening stainless steel. It finds that quenching at lower temperatures leads to higher reverted austenite, while tempering time increases the formation of various precipitates. The research employs multiple microscopy techniques to analyze microstructural changes and their implications for mechanical properties.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
16 views16 pages

Статья по S17400

The study investigates the effects of quenching temperature and tempering time on the microstructure of UNS S17400 precipitation-hardening stainless steel. It finds that quenching at lower temperatures leads to higher reverted austenite, while tempering time increases the formation of various precipitates. The research employs multiple microscopy techniques to analyze microstructural changes and their implications for mechanical properties.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 16

See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/362809289

Effect of Quenching Temperature and Tempering Time on the Evolution of


Microstructure in UNS S17400 Stainless Steel

Article in Journal of Materials Engineering and Performance · August 2022


DOI: 10.1007/s11665-022-07228-y

CITATIONS READS

2 185

2 authors:

Nidhi Gupta Rajesh K. Khatirkar


Texas A&M University Visvesvaraya National Institute of Technology
2 PUBLICATIONS 2 CITATIONS 98 PUBLICATIONS 2,181 CITATIONS

SEE PROFILE SEE PROFILE

All content following this page was uploaded by Nidhi Gupta on 04 November 2022.

The user has requested enhancement of the downloaded file.


JMEPEG ASM International
https://doi.org/10.1007/s11665-022-07228-y 1059-9495/$19.00

TECHNICAL ARTICLE

Effect of Quenching Temperature and Tempering Time


on the Evolution of Microstructure in UNS S17400
Stainless Steel
Nidhi Gupta and Rajesh K. Khatirkar

Submitted: 2 February 2022 / Revised: 30 April 2022 / Accepted: 17 June 2022

In the present work, the effect of quenching temperature and tempering time on the evolution of
microstructure in UNS S17400 precipitation-hardening (PH) stainless steel has been investigated. Two
temperatures, 950 and 1050 °C, were selected for quenching followed by tempering at 620 °C for different
times ranging from 15 min to 6 h. Optical microscope (OM), electron backscattered diffraction (EBSD) and
scanning electron microscope (SEM) were used to obtain the microstructural information. Energy-dis-
persive spectrometer (EDS) attached to SEM was used to obtain the localized chemical composition of
various phases/precipitates. X-ray diffraction (XRD) was used to quantify the reverted austenite, coherently
diffracting domain size and lattice strain. There was little change in the grain size with the increase in
quenching temperature. On the other hand, tempering resulted in formation of precipitates of various
types, which increased (as expected) with increase in tempering time. Lower quenching temperature re-
sulted in higher reverted austenite.

dimensional accuracy (Ref 8). Some of the most advanced


Keywords microstructure, precipitation hardening, quenching,
reverted austenite, UNS S17400 steel martensitic stainless steels are UNS S17400, UNS S15500,
UNS S13800, and UNS S46500 (Ref 8). The present study is
focused on the UNS S17400 alloy (also known as 17-4 PH
stainless steel or Grade 360 steel). The solution treatment of the
alloy results in the formation of martensitic structure which
doesnÕt possess sufficiently high hardness. The aging treatment
1. Introduction of the alloy results in the precipitation of coherent Cu
precipitates, which improves the hardness and the strength of
Owing to excellent corrosion resistance properties, stainless the material (Ref 9). The aging treatment serves the dual
steels have witnessed a tenfold increase in world production in purpose of stress relieving and precipitation hardening. The
the past 5 decades (Ref 1). One of the highly specialized grades aging temperature for these alloys typically ranges from 510 to
of stainless steel is precipitation-hardening (PH) stainless steel, 620 C (Ref 8). The properties and the microstructures of the
developed in 1940s (Ref 2). These steel grades exhibit good alloy are significantly impacted by the variation in various
corrosion resistance along with high strength and toughness parameters such as aging time and temperature.
(Ref 3), making them desirable as structural materials for There are a few studies on the development of microstruc-
biomedical applications (Ref 4), chemical industries (Ref 5), ture and mechanical properties for PH stainless steels. Rack
marine construction (Ref 6), and nuclear power plant applica- et al. (Ref 10) initially concluded that aging resulted in the
tions (Ref 7). One of the factors contributing to the final formation of copper-rich clusters, which later transform to
properties of the PH stainless steel is the initial microstructure incoherent FCC -copper precipitates upon further aging.
of the matrix. Based on the initial matrix, the three classes of Viswanathan et al. (Ref 11) reported the effect of aging
PH steels produced are martensitic, semi-austenitic, and fully treatment at varying temperatures and for varying aging times.
austenitic PH stainless steels, of which the martensitic grades They reported the formation of internal twin free lath martensite
are considered as the workhorse of PH steels(Ref 8). The with high dislocation density when quenching treatment is
martensitic PH grades comprise of the matrix of low carbon performed from the solutionizing temperature of 1040 C. The
martensite, which is obtained from solution-annealing treatment aging of the alloy resulted in the dislocation rearrangement in
followed by quenching. These alloys possess a unique feature the lath martensite. Wang et al. (Ref 12) reported that the 17-4
where they can be fabricated into the desired shape in the soft PH alloy, after aging treatment attained a peak bulk hardness
state and can be hardened before the service while maintaining after which the hardness decreased with increase in aging time.
They also concluded that the formation of Cu and M23C6
precipitates were responsible for the strengthening of the alloy
Nidhi Gupta and Rajesh K. Khatirkar, Department of Metallurgical at 595 C. Murayama et al. (Ref 13) reported the presence of
and Materials Engineering, Visvesvaraya National Institute of BCC coherent Cu precipitates, when aged for 4 h at the
Technology (VNIT), South Ambazari Road, Nagpur, Maharashtra temperature of 580 C. They showed that aging for a prolonged
440010, India. Contact e-mails: nidhigupta7900@gmail.com,
rajesh.khatirkar@gmail.com, and rajeshk@mme.vnit.ac.in. period, even at temperatures as low as 400 C, results in the

Journal of Materials Engineering and Performance


decomposition of the martensite and an increase in the hardness For microstructural observations, the specimens were cut
and yield strength of the material. This indicates that aging time from center, ground, and mounted using epoxy resin. Further,
can have a significant impact on the improvement in the specimens were mirror-polished on emery paper followed
microstructures and consequently on the properties. However, by cloth polishing with a suspension of alumina in water, and
aging treatment, when performed for excessive durations can then etched with KellerÕs reagent (2 mL HF, 3 mL HCl, 5 mL
lead to the deterioration of the mechanical properties. Wang HNO3, 190 mL H2O) (Ref 17). Microstructures of all the
et al. (Ref 14) observed a rapid rate of hardening at 350 C after specimens were observed with Zeiss, Germany optical micro-
aging for 8400 h. However, extending the aging hours to scope (OM, bright field mode) and JEOL (model 6380A),
11,000 h resulted in the formation of abundant reversed Japan scanning electron microscope (SEM, secondary electron
austenite, leading to rapid softening. Rack and David (Ref imaging mode). Chemical composition of specific features like
10) showed that increment in the aging temperature, beyond precipitates was obtained with Bruker, Germany energy
620 C, results in the formation of incoherent FCC-Cu dispersive spectrometer (EDS) attached to SEM. Selected
precipitates (Ref 10) in the matrix and the reversal of the samples were also subjected to orientation imaging microscopy
martensite to austenite along the lath martensite boundaries with EDAX, USA electron backscattered diffraction (EBSD)
(Ref 11). The literature states that the presence of very high system attached to a FEI, The Netherlands Quanta 3D field
levels of austenite tends to reduce the mechanical properties, emission gun SEM. EBSD scans were acquired with a step size
specifically the yield strength and toughness of the alloy of 0.5 lm using an accelerating voltage of 20 kV. The beam
making it undesirable (Ref 8). However, a contradictory and video conditions were kept identical for all the samples.
observation was made by Bhambroo et al. (Ref 15) that, The EBSD data were post-processed using TSL OIM software
austenite reversal does not affect the strength and the impact version 7.2. For analysis, all the points/pixels with confidence
toughness of the material, and that the Cu-rich precipitates index (CI) less than 0.1 were excluded from the analysis. CI
control the mechanical properties of the alloy. Wee-Do Yoo typically represents accuracy of a typical EBSD scan (Ref 18).
(Ref 16) reported that the long-term aging phenomenon could For EBSD measurements, samples were electropolished after
lead to spinodal decomposition in martensitic matrix and Cu standard metallographic polishing using an electrolyte consist-
precipitate nucleation. The studies on the long-term aging of ing of a mixture of ethanol (80%) and perchloric acid (20% by
17-4 PH stainless steel are relatively few. The understanding of volume) at  10 C. For electro-polishing, time was 20 s and
aging behavior with varying quenching temperature is impor- voltage used was 15 V DC. X-ray diffraction (XRD) patterns
tant as it has a direct impact on the microstructure, mechanical were also measured for all the samples on a PANalytical, The
properties, and corrosion resistance. The present work inves- Netherlands XÕPert Pro MPD diffractometer in Bragg–Brentano
tigates the effect of aging time (long term) and quenching configuration. The radiation used were CuKa, and the x-ray
temperature on the microstructure and mechanical properties of tube was in line focus mode. The XRD patterns were acquired
UNS S17400 martensitic stainless steel. with a step size of 0.03 with an integration time of 20 s at each
step. Point detector fitted with curved crystal graphite
monochromator was used to remove fluorescent and Kb
radiation. For instrumental broadening correction, a fully
2. Experimental recrystallized silicon sample was used as a standard. The x-
ray data were post-processed using the XÕPert HighScore
software. The instrumental peak broadening was obtained using
A rod with initial diameter 10 mm of 17-4 PH stainless steel
the Caglioti formula (Eq 1) (Ref 19):
was used in the present investigation. The samples were cut in
dimension of /10 mm 9 15 mm by electrical discharge b2 ¼ U tan2 h þ V tan h þ W ðEq 1Þ
machining (EDM) from the initial rod. The composition of
the alloy (as determined by optical emission spectroscopy where b denotes the integral breadth of each hkl peak of
(OES)) is specified in Table 1. The as-received specimens (as standard sample, i.e., binst, h is the corresponding Bragg angle,
shown in Fig. 1) were solution treated at 950 C and at and U, V, W, are the constants. The values of the constants (U,
1050 C for 45 min (followed by oil quenching (OQ)). The first V, W) were obtained by fitting Eq 1 to the fully recrystallized
set of the sample (hereafter (referred to as set-A) comprised of silicon sample data. The integral breadth obtained for each peak
samples solution treated at 950 C followed by aging at 620 C (bobs.) for each experimental condition was then corrected using
for times ranging from 15 min to 6 h. The second set (hereafter Eq 2:
(referred to as set-B) comprised of samples solution treated at rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 ffi
1050 C followed by aging at 620 C for times ranging from bcorr ¼ ðbobs  binst Þ b2obs  b2inst ðEq 2Þ
15 min to 6 h. Before the aging treatment, all the samples were
vacuum-sealed in a quartz tube to avoid oxidation during the The quantification of reversed austenite was performed
aging process. All the specimens were air-cooled post-aging using the direct comparison method developed by Averbach
treatment. The heat treatment operations performed in the and Cohen (Ref 20). The diffraction intensity was calculated
present study are schematically represented in Fig. 2. from Eq 3:

Table 1 Chemical composition (in weight %) of 17-4 PH stainless steel used in the present study
C Mn Si Cr Ni P S Cu Nb + Ti Fe

0.04 0.30 0.60 16.39 4.32 0.023 0.013 3.40 0.60 Balance

Journal of Materials Engineering and Performance


Fig. 1 A schematic diagram showing the sample designation used in the present study

Fig. 2 A schematic of the heat treatment operations involved in the present study

martensite also. The measurement of the bulk hardness of all


K2 R the samples was done with a Vickers macro-hardness tester
I¼ ðEq 3Þ
2l (Blue Star, India) using 30 kg load.
where K2 is a constant independent of the diffracting material,
R is dependent on h, hkl, and material (Ref 21). For a two-
phase material (austenite (c) and ferrite (a) in the present 3. Results and Discussion
investigation), Eq 3 can be written as:
K 2 R c cc 3.1 Microstructures
Ic ¼ ðEq 4Þ
2l Figure 3 shows the optical and secondary electron SEM
images of the as-received sample. The microstructure shows
K2 Ra ca ferritic matrix with uniformly dispersed second phase particles
Ia ¼ ðEq 5Þ
2l throughout the matrix. The second phase particles are coarse
Cu. In the magnified SEM image, pits are observed due to the
Therefore, removal of Cu particles during sample preparation, i.e.,
cc Ic Ra metallographic polishing. Figure 4 and 5 show the optical
¼ ðEq 6Þ microscopy images of the samples oil quenched from 950 C/
ca I a R c
aged at 620 C and oil quenched from 1050 C/aged at 620 C,
After obtaining the ratio cc/ca, fraction of austenite can be respectively. The low carbon ferrite matrix transforms to
calculated, since ca þ cc ¼ 1, where c is the concentration (Ref martensite (lath) due to the quenching operation. The
21). Other details regarding austenite quantification can be microstructure shows the presence of lath martensite and
found in (Ref 21). Similar procedure can be adopted for precipitates. As the aging time increases, new fine precipitates

Journal of Materials Engineering and Performance


Fig. 3 (a) Optical and (b) secondary electron SEM images of the as-received sample

Fig. 4 Optical microscopy images of set-A 17-4PH stainless steel samples (a) as-quenched condition, and aged at 620 C for (b) 15 min, (c)
30 min, (d) 1 h, (e) 2 h, (f) 4 h, and (g) 6 h. The micron bar applies to all the images

are formed and old precipitates became coarse. Similar trend is Figure 6 and 7 show the secondary electron SEM micro-
observed for both the set of samples. However, there was a graphs of the specimens from set-A and set-B, respectively.
slight difference in the grain sizes; set-B had a slightly coarser Figure 6(a) and 7(a) show the presence of lath martensite in the
microstructure. as-quenched samples with some precipitates. The precipitates
were coarse having irregular shapes, which are probably the

Journal of Materials Engineering and Performance


Fig. 5 Optical microscopy images of set-B 17-4PH stainless steel samples (a) as-quenched condition, and aged at 620 C for (b) 15 min, (c)
30 min, (d) 1 h, (e) 2 h, (f) 4 h, and (g) 6 h. The micron bar applies to all the images

undissolved precipitates. After aging, new fine precipitates also show the presence of Cr, which is probably from the
started to appear. There was no correlation of the size adjoining matrix.
distribution, since new precipitates were formed and it was The precipitates were mostly rich in Cr content. The
very difficult to judge the exact kinetics due to sluggish nature depletion of Cr from the matrix results in the loss of corrosion
of the phase transformation. resistance of the alloy. Therefore, the aging treatment has to be
EDS attached to SEM was used to obtain the chemical optimized to get a balance of corrosion resistance and
composition of the various precipitates that formed at different mechanical properties. This is also reflected in the hardness
stages of the aging treatment for both set-A and set-B. Tables 2 curve. Figure 9 shows the variation of Vickers Hardness with
and 3 provide the summary of the major elements present in the aging time for set-A and set-B samples. The hardness of the
various types of precipitates. The precipitates were classified initial oil-quenched specimen was  320 Hv. As the specimen
into different morphologies based on secondary electron SEM from set-A was aged for 15 min, the hardness reached the peak
imaging. In most of the precipitates, the major elements found value. With further increase in the aging time, the hardness
by EDS analysis were Fe, Cr, and Cu. For a better understand- decreased gradually. The initial increase in the hardness was
ing of the precipitates, Fig. 8 illustrates some of the morpholo- attributed to the presence of copper-rich zone (Ref 11). After
gies provided in Tables 2 and 3. the peak is reached, the hardness decreased possibly because of
It needs to be noted that the signals detected by the EDS two reasons. First, the interface nature changes from coherent to
come from a large interaction volume of the electron beam with incoherent which results in distortion of atomic structure at the
the sample. Therefore, the chemical composition of the interface, thus reducing the hardness. Second, coalescence of
precipitates determined by the EDS may also consist of signals previously formed Cu precipitates takes place which results in
from the neighboring matrix. The Cu-rich precipitates therefore the reduction of hardness value in both the sets. To confirm the

Journal of Materials Engineering and Performance


Fig. 6 Secondary electron SEM images of set-A 17-4PH stainless steel samples (a) As-quenched condition, and aged at 620 C for (b) 15 min,
(c) 1 h, (d) 2 h, (e) 4 h, and (f) 6 h. The micron bar applies to all the images

above observation, EDS measurements were performed for hardness observed in set-B can be attributed to higher
larger precipitates. At the highest aging time of 6 h, the dissolution of Cu precipitates which would in turn result in
hardness was lowest, even less than the hardness of the initial the formation of more Cu precipitates during the aging
as-received sample. The trend of the hardness was similar for operation.
set-B; however, the peak hardness reached was higher. Higher

Journal of Materials Engineering and Performance


Fig. 7 Secondary electron SEM images of set-B 17-4PH stainless steel samples (a) As-quenched condition, and aged at 620 C for (b) 15 min,
(c) 1 h, (d) 2 h, (e) 4 h, and (f) 6 h. The micron bar applies to all the images

It is known that the hardness increases after the initial aging coarsening of precipitates. In order to substantiate the
treatment due to the formation of coherent Cu precipitates. microstructure further, EBSD was carried out. Figure 10 shows
Upon further aging, the precipitation of incoherent Cu clusters the EBSD normal direction (ND) inverse pole figure (IPF)
begins along with coarsening of existing precipitates, resulting maps of the samples for two extreme conditions (OQ and aged
in decrement in the hardness values (Ref 22-24).Thus, the for longest time) for both sets. There was no significant
decrease in hardness beyond the aging treatment for 30 min can variation in the grain size of the samples; however, sample aged
be attributed to the onset of precipitation of incoherent Cu and for 6 h after oil quenching from 1050 C shows a slight

Journal of Materials Engineering and Performance


Table 2 Chemical composition (major elements) of precipitates as determined by SEM–EDS for set-A samples
Major elements, in weight %
Sr. No Condition Morphology Fe Cr Ni Nb Cu Mn Ti

1 As-received Circular 15.7 8.5 … 5.6 13.8 …


Oval 14.3 10.5 … … 4.6 17.1 0.4
Elongated 70.7 21.1 2.3 … 5.4 … …
Square 77.1 17.4 4.8 … … … …
Small (< 0.5 lm) 31.9 7.3 1.3 … 7.4 1.7 …
2 950 C-OQ Oval 39.8 8.5 2.1 15.8 3.2 … …
Circular 51.9 11.8 2.1 0.5 1.7 … 0.6
Triangular 79.9 17.7 1.0 … 1.3 … …
Elongated 72.0 19.2 1.4 … … … …
3 950 C-15 min Irregular 60.4 12.9 2.4 … 2.6 … …
Small 48.8 10.9 2.6 2.8 … …
Circular 45.2 9.9 2.0 4.8 1.6 … …
4 950 C-1 h Small 58.8 11.0 3.3 0.2 4.6 … …
elongated 10.3 2.2 … 61.0 1.1 … …
Triangular 77.6 17.6 1.3 … 2.4 … …
Circular 68.2 14.1 4.0 0.8 6.0 … …
5 950 C-2 h Big 65.1 18.2 1.4 … … … …
Small 45.7 9.1 2.7 … 2.5 … …
Circular 33.7 7.5 2.2 9.2 3.0 … …
6 950 C-4 h Irregular 56.7 12.1 3.3 1.2 3.0 … …
7 950 C-6 h Irregular 49.0 9.5 2.3 … … … …
Elongated 55.6 11.2 4.3 … 3.5 … …

Table 3 Chemical composition (major elements) of precipitates as determined by SEM–EDS for set-B samples
Major elements, in weight %
Sr. No Condition Morphology Fe Cr Ni Nb Cu Mn Si Ti

1 1050 C-OQ Rectangular 48.8 15.6 … … 22.3 13.0 … …


Coarse 5.4 46.3 … … 1.5 33.8 … 2.8
Triangle 83.7 14.4 … … 0.9 … …
Small 62.3 12.7 2.8 … 3.3 2.4 … …
Elliptical 21.4 8.2 1.6 … 10.9 27.7 … …
2 1050 C-15 min Elliptical 53.7 11.8 2.5 4.3 3.2 … … …
Coarse 39.3 10.2 1.8 … 9.2 8.6 … …
3 1050 C-1 h Irregular 30.1 10.5 … 0.7 8.4 21.1 … …
Big 77.3 17.7 1.5 … 2.1 … … …
Small 50.1 11.3 2.3 6.9 2.8 … … …
Circular 52.9 11.0 3.0 … … 3.9 … …
Triangular 57.1 10.8 2.9 … 2.8 … …
4 1050 C-2 h Irregular 9.9 9.6 … … 4.8 19.6 … …
Circular 54.2 10.7 2.6 1.3 … … … …
Dendritic 53.7 10.4 2.9 … 3.5 … … …
5 1050 C-4 h Irregular 34.7 8.3 … … … … 5.4 …
Elongated 56.5 9.5 4.8 … 3.2 … …
6 950 C-6 h Irregular 67.3 3.9 3.2 … … … 2.7 …
Elongated 63.7 10.7 3.5 … 3.0 … … …

increase in the grain size. The EBSD IPF maps showed a is better for avoiding/minimizing the reversed martensite. There
typical lath martensite (a’) structure. Figure 11 shows the was also no significant change in the grain boundary misori-
EBSD phase maps for 950 C OQ—620 C aged 6 h and entation distribution and grain boundary character distribution
1050 C OQ—620 C aged 6 h samples. It can be clearly seen for samples quenched from 950 C and aged (Fig. 12).
that the reversed austenite (green) was more in samples However, for quenching from 1050 C (Fig. 13), low angle
quenched from 950 C and aged than that quenched from boundaries (boundaries with misorientation < 15) and CSL
1050 C. This indicates that hardening from higher temperature (coincident site lattice) boundary fractions decreased.

Journal of Materials Engineering and Performance


Fig. 8 Various morphologies marked on the secondary electron SEM images

phase. In the present work, precipitates are also present, which


can affect the magnetic measurement. XRD is extensively used
in the literature (Ref 25) for determination of retained and
reversed austenite. In the present work, both x-ray diffraction
(XRD, indirect) and electron backscattered diffraction (EBSD,
direct) were used to obtain and confirm the information
regarding austenite reversal.

3.2 X-ray Diffraction


Figure 14 and 15 show the XRD peak profiles of the
samples from set-A and set-B, respectively. The martensite
peak is indexed as 110a peak. As the aging time was increased,
reversed austenite 111c peak becomes visible. This was due to
the austenite reversal taking place at higher aging times. Table 4
gives the amount of reversed austenite (calculated using the
direct comparison method (Ref 20)). The amount of reversed
austenite was observed to increase with the increase in aging
time. Further, the amount of reversed austenite was higher in
Fig. 9 Variation of hardness (Hv) as a function of aging time (h) set-A samples (quenched from 950 C) than set-B samples
(quenched from 1050 C). The blank spaces in Table 2 indicate
that the austenite peaks for those conditions were too low in
Another method which could be used to calculate austenite intensity to give reliable results or were absent in the XRD
reversal is using the magnetic measurements as used by De pattern altogether. This observation also confirms the results
Oliveira et al. (Ref 25). Magnetic measurements like fer- obtained from EBSD phase maps earlier.
ritescope and vibrating sample magnetometer (VSM) may be Figure 16 and 17 show the instrumental corrected peak
used in the calculation of retained austenite. Both are indirect broadening and Williamson–Hall (WH) plots for 17-4 PH
techniques, in which ferritescope measures the magnetic phase stainless steel samples for selected conditions, respectively.
and VSM relies on the saturation magnetization of the pure

Journal of Materials Engineering and Performance


Fig. 10 EBSD inverse pole figure (IPF) maps of (a) 950 C OQ, (b) 950 C OQ—620 C aged 6 h, (c) 1050 C OQ and (d) 1050 C
OQ—620 C aged 6 h samples. The micron bar applies to all the images

WH plot was used to obtain qualitative information of In Eq 7, K represents shape factor and is taken as 0.9, while
coherently diffracting size and micro-strain. The coherently k is the wavelength. The slope and the intercept of the plot of
diffracting domain size (D) and the micro-strain (e) are obtained Eq 7 give the values of coherently diffracting domain size (D)
from Eq 7. and micro-strain (e), respectively. No particular trend was
observed for the values of D and e from the WH plot. However,
Kk
bcorr: cos h ¼ þ 4e sin h ðEq 7Þ peak broadening, in general, decreased with the increase in
D aging time. The phenomenon is complicated due to the fact that
simultaneous occurrence of the fine precipitates is also seen

Journal of Materials Engineering and Performance


Fig. 11 EBSD phase maps for (a) 950 C OQ—620 C aged 6 h and (b) 1050 C OQ—620 C aged 6 h samples. Red is ferrite/martensite
matrix and green is austenite. The micron bar applies to all the images

Fig. 12 Graphs depicting the variation of grain size, boundary character, and misorientation angle distribution for (a) 950 C OQ, (b) 950 C
OQ—620 C aged 6-h samples

Journal of Materials Engineering and Performance


Fig. 13 Graphs depicting the variation of grain size, boundary character, and misorientation angle distribution for (a) 1050 C OQ, (b) 1050 C
OQ—620 C aged 6-h samples

Fig. 14 The x-ray diffraction peak profiles of samples quenched from 950 C (set-A)

Journal of Materials Engineering and Performance


Fig. 15 The x-ray diffraction peak profiles of samples quenched from 1050 C (set-B)

Table 4 Fraction of reversed austenite (calculated using 4. Conclusions


x-ray diffraction) for various conditions
Condition Reversed austenite (%) The effect of quenching temperature and tempering time on
the evolution of microstructure in UNS S17400 martensitic
950 C-OQ … stainless steel can be summarized as follows:
950 C-4 h 23.0
950 C-6 h 24.6 1) Lower amount of austenite reversal was observed for the
1050 C-OQ … samples quenched from 1050 C followed by aging treat-
1050 C-15 min … ment than the samples quenched from 950 C and aged.
1050 C-2 h 2.7 As the aging time increased, more and more austenite
1050 C-4 h 18.8 reversal took place.
1050 C-6 h 21.2 2) The fraction of precipitates increased with the increase in
aging time as new precipitates kept appearing, whereas
the older precipitates coarsened. The major elements
which constituted the precipitates were Fe, Cr, and Cu.
3) Samples quenched from 1050 C and aged for 6 h re-
with the increase in aging time. Precipitates are associated with sulted in decrement of low angle boundaries and CSL
the interfaces and mismatch with the matrix which may also fraction, all other conditions being almost similar. Coher-
give rise to x-ray peak broadening and micro-strain. ently diffracting domain size and micro-strain did not

Journal of Materials Engineering and Performance


Fig. 16 Peak broadening behavior with respect to the annealing time for (a) set-A and (b) set-B

Fig. 17 Williamson–Hall plot of 17-4PH stainless steel quenched from (a) 950 C and (b) 1050 C

show any specific trend due to simultaneous occurrence 6. M. Wu, Z. Zhao, X. Wang, C. Wang and P. Liang, Corrosion behavior
of precipitation, precipitate coarsening, and decomposi- of 17-4 PH stainless steel in simulated marine environment, Mater.
Corros., 2019, 70, p 461–469. https://doi.org/10.1002/maco.2018104
tion of martensite to ferrite. 54
7. D.F.A. Ferreira, R.P. Rezende, T. Turcarelli, Microstructural Charac-
terization Of Stainless Steel 17-4 PH used in the Control Element of
PWR-type, Int. Nuclr. Atlantic Conf., (2017).
8. M.F. McGuire, Stainless Steels for Design Engineers, ASM Int., 2019 h
ttps://doi.org/10.31399/asm.tb.ssde.9781627082860
References 9. J.D. Bressan, D.P. Daros, A. Sokolowski, R.A. Mesquita and C.A.
Barbosa, Influence of Hardness on the Wear Resistance of 17-4 PH
1. Outokumpu, Handbook of Stainless Steel 1-89, (2013). http://www. Stainless Steel Evaluated by the Pin-On-Disc Testing, J. Mater.
outokumpu.com/sitecollectiondocuments/ outokumpu-stainless-steel- Process. Technol., 2007, 5, p 353–359. https://doi.org/10.1016/j.jma
handbook.pdf tprotec.2007.11.251
2. C.N. Hsiao, C.S. Chiou and J.R. Yang, Aging Reactions in a 17-4 PH 10. H.J. Rack and D. Kalish, Strength, Fracture Toughness, and Low Cycle
Stainless Steel, Mater. Chem. Phys., 2002, 74, p 134–142 Fatigue Behavior of 17-4 Ph Stainless Steel, Met. Trans., 1974, 5, p
3. H. Dong, M. Esfandiari and X.Y. Li, On the Microstructure And Phase 1595–1605. https://doi.org/10.1007/BF02646331
Identification of Plasma Nitrided 17-4PH Precipitation Hardening 11. U.K. Viswanathan, S. Banerjee and R. Krishnan, Effects of Aging on
Stainless Steel, Surf. Coat. Technol., 2008, 202, p 2969–2975. https://d the Microstructure of 17-4 PH Stainless Steel, Mater. Sci. Eng. A, 1988,
oi.org/10.1016/j.surfcoat.2007.10.036 104, p 181–189. https://doi.org/10.1016/0025-5416(88)90420-X
4. I. Mutlu and E. Oktay, Characterization of 17-4 PH Stainless Steel 12. J. Wang, H. Zou, C. Li, R. Zuo, S. Qiu and B. Shen, Relationship of
Foam for Biomedical Applications in Simulated Body Fluid and Microstructure Transformation and Hardening Behavior of Type 17-4
Artificial Saliva Environments, Mater. Sci. Eng. C, 2013, 33, p 1125– PH Stainless Steel, J. Univ. Sci. Technol. Beijing Min. Metall. Mater.,
1131. https://doi.org/10.1016/j.msec.2012.12.004 2006, 13, p 235–239
5. J. Nowacki, Weldability Of 17-4 PH Stainless Steel in Centrifugal 13. M. Murayama, Y. Katayama and K. Hono, Microstructural Evolution in
Compressor Impeller Applications, J. Mater. Process Technol., 2004, a 17-4 PH Stainless Steel after Aging at 400 C, Metall. Mater. Trans.
157–158, p 578–583. https://doi.org/10.1016/j.jmatprotec.2004.07.117 A Phys. Metall. Mater. Sci., 1999, 30, p 345–353. https://doi.org/10.
1007/s11661-999-0323-2

Journal of Materials Engineering and Performance


14. J. Wang, H. Zou, C. Li, S. Qiu and B. Shen, The Effect of 22. R. Gerosa, B. Rivolta and A. Sala, Optimization of the Heat Treatment
Microstructural Evolution on Hardening Behavior of Type 17-4PH of a 17-4 PH stainless Steel by Dilatometric Technique, ASTM Spec.
Stainless Steel in long-term Aging at 350 C, Mater. Charact., 2006, Tech. Pub., 2010, 1523 STP, p 1066–1076. https://doi.org/10.1520/
57, p 274–280. https://doi.org/10.1016/j.matchar.2006.02.004 stp49198s
15. R. Bhambroo, S. Roychowdhury, V. Kain and V.S. Raja, Effect of 23. J.W. Martin, Precipitation Hardening: Theory and Applications,
Reverted Austenite on Mechanical Properties of Precipitation Harden- Butterworth-Heinemann, 1998
able 17-4 Stainless Steel, Mater. Sci. Eng. A, 2013, 568, p 127–133. h 24. R. Rice, J. Jackson, J. Bakuckas, S. Thompson (2003) Metallic
ttps://doi.org/10.1016/j.msea.2013.01.011 Materials Properties Development and Standardization, MMPDS,
16. W. Yoo, J. Lee, K. Youn and Y. Rhyim, Study on the Microstructure (2003)
and Mechanical Properties of 17-4 PH Stainless Steel depending on 25. M.P. de Oliveira, J.W. Calderón-Hernández, R. Magnabosco, D.
Heat Treatment and Aging Time, Solid State Phenom., 2006, 118, p Hincapie-Ladino and N. Alonso-Falleiros, Effect of Niobium on Phase
15–20. https://doi.org/10.4028/www.scientific.net/SSP.118.15 Transformations Mechanical Properties and Corrosion of Supermarten-
17. ASM Handbook, Metallography and Microstructure, vol 9, 2004 sitic Stainless Steel, J. Mater. Eng. Perform., 2017, 26, p 1664–1672
18. D.P. Field, Recent Advances in the Application of Orientation Imaging,
Ultramicroscopy, 1997, 67, p 1–9. https://doi.org/10.1016/S0304-399 Publisher’s Note Springer Nature remains neutral with regard to
1(96)00104-0
jurisdictional claims in published maps and institutional affilia-
19. G. Caglioti and A. Paoletti, On Resolution and Luminosity of a
Neutron powder Spectrometer, Nucl. Intrum. Methods, 1958, 3, p 223– tions.
228
20. B.L. Averbach and M. Cohen, X-ray Determination of Retained Springer Nature or its licensor holds exclusive rights to this article
Austenite by Integrated Intensities, Trans. AIME, 1948, 176, p 401–415 under a publishing agreement with the author(s) or other rightsh-
21. B.D. Cullity, Stock SR, 3rd ed. Elements of X-Ray Diffraction, Pearson, older(s); author self-archiving of the accepted manuscript version of
2001 this article is solely governed by the terms of such publishing
agreement and applicable law.

Journal of Materials Engineering and Performance

View publication stats

You might also like