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Effects of Thermal History and Microstructure on Segregation of Phosphorus

and Alloying Elements in the Heat-Affected Zone of a Low Alloy Steel

Article  in  Metallurgical and Materials Transactions A · December 2014

DOI: 10.1007/s11661-014-2582-9

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Effects of Thermal History and Microstructure on Segregation
of Phosphorus and Alloying Elements in the Heat-Affected Zone
of a Low Alloy Steel
ZIQING ZHAI, YUICHI MIYAHARA, HIROSHI ABE, and YUTAKA WATANABE

The grain boundary segregation of phosphorus and alloying elements in the heat-affected zone
(HAZ) of a low alloy steel was studied quantitatively with atom probe tomography. Non-
equilibrium segregation mainly occurred during welding and subsequent fast cooling, leading to
remarkable segregation of P, C, Mn, and Mo. The segregation of these four types of solutes
showed similar microstructure-dependence at this stage, in which the segregation levels are
higher in coarse-grained HAZ and intercritically reheated coarse-grained HAZ than in fine-
grained HAZ. After simulated aging, P and Mn showed further enrichment at grain boundaries
through equilibrium segregation, while desegregation was observed for C and Mo. In addition,
it seems that precipitation of Mo at dislocations was greatly promoted during aging, which
probably also contributed to the increase of P and Mn at grain boundaries.

DOI: 10.1007/s11661-014-2582-9
 The Minerals, Metals & Materials Society and ASM International 2014

I. INTRODUCTION quantitatively using atom probe tomography (APT),

with focuses on the effects of thermal history and HAZ
THE toughness of low alloy steels (LAS) can be microstructure. Characteristics of interactive co-segre-
degraded by aging, which increases the ductile–brittle gation between phosphorus and some alloying elements
transition temperature by an amount dependent on were also examined.
material, prior heat treatment, aging temperature, and
time. This embrittlement is associated with segregated
elements at grain boundaries (GB), essentially phospho-
rus (P).[1,2] Due to the specific thermal cycles induced by II. EXPERIMENTAL
multi-pass welding, complex phase transformations take
place in the heat-affected zone (HAZ) of LAS, especially A. Material and Specimen Preparation
in the close vicinity of the fusion boundary, resulting in
The HAZ investigated in this study was fabricated by
coarse-grained (CG), fine-grained (FG), intecritically
filling Ni-base alloy 182 into a machined groove in an
reheated coarse-grained (ICCG), and subcritically
A533B plate using shielded metal arc welding. Two
reheated coarse-grained (SCCG) HAZ.[3,4] Variations
types of Alloy 182 filler metals were used: Inconel 182
of solute segregation at GBs are also expected in these
for the first 4 layers from bottom of the groove up to a
microstructures. Although the fundamentals of the
height of 7.2 mm, and Yawata Weld 182 for the
interactive co-segregation of phosphorus and alloying
subsequent 11 layers. The chemical composition of the
elements in thermally aged ferritic steels have been
Ni-base alloys and LAS are given in Tables I and II,
intensively studied,[5–10] little is known about the actual
respectively. A typical post-weld heat treatment
segregation behaviors in real weldments with complex
(PWHT) was applied to reduce residual stresses present
thermal histories. In order to evaluate and mitigate the
after the welding and fast cooling process, of which the
risks of temper embrittlement, a better understanding on
procedure is shown in Figure 1. An additional step
the segregation in real weldments is necessary. In this
cooling treatment,[11–13] was conducted on part of the
study, the GB segregation of phosphorus and alloying
weld joint to produce enhanced P segregation at GBs
elements in the HAZ of a LAS was investigated
that would be attained after extended exposure at lower
service temperatures on an accelerated basis. The
ZIQING ZHAI, Ph.D. Candidate, HIROSHI ABE, Assistant sequence for this process is detailed in Figure 2. For
Professor, and YUTAKA WATANABE, Professor, are with the the sake of simplicity, the material which had received
Graduate School of Engineering, Tohoku University, 6-6-01-2 Aoba, this additional heat treatment will be denoted as step-
Aramaki, Aoba-Ku, Sendai 980-8579, Japan. Contact e-mail: ziqing.
zhai@gmail.com YUICHI MIYAHARA, Staff Member, formerly with cooled (SC), whereas the rest will be referred to as non-
the Material Science Research Laboratory, Central Research Institute of step-cooled (NSC) hereafter.
Electric Power Industry, 2-6-1 Nagasaka, Yokosuka, Kanagawa 240- The morphology of the CGHAZ, FGHAZ, and
0196, Japan, is now with the Planning Group, Central Research Institute of ICCGHAZ in the dissimilar weld joint revealed by
Electric Power Industry, 1-6-1 Otemachi, Chiyoda-ku, Tokyo 100-8126,
Japan.
etching is presented in Figure 3. The average size of
Manuscript submitted May 30, 2014. prior austenite grains (PAG) measured according to the
Article published online September 30, 2014 General Intercept Procedure described in ASTM-E112-

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 45A, DECEMBER 2014—6163

 Table I. The Chemical Compositions of the Ni-Base Weld Metals (Weight Percent)

Element C Si Mn P S Ni Cr Cu Co Ti Nb + Ta Fe
Inconel 182 0.053 0.44 6.50 0.004 0.002 68.90 14.70 / / 0.52 1.55 7.23
Yawata Weld 182 0.033 0.65 5.70 0.011 0.006 69.95 13.85 0.01 0.01 0.60 1.70 6.98

Table II. The Chemical Compositions of the A533B Base Material

Element C Si P S Mn Mo Ni Cr Cu Ti V Fe
Concentration (wt pct) 0.20 0.24 0.009 0.004 1.41 0.54 0.65 0.13 0.12 0.001 0.001 bal.
Concentration (at. pct) 0.91 0.24 0.016 0.007 2.75 0.31 0.61 0.14 0.10 0.001 0.001 bal.

polishing method, GBs can only be found through

random encounters and their exact natures are
unknown. Since P is one of the targeted segregants in
this study and it is reported that P tends to favor PAGBs
and high angle packet boundaries for segregation,[16,17]
it seems reasonable to assume that the boundaries found
with enriched P by APT tests belong to these two
categories (hereafter referred to as grain/packet bound-
aries (G/PB)).

Fig. 1—Schematic of the PWHT procedure.

B. The APT Tests and Analysis

Fig. 2—Procedure of the step cooling treatment.
10[14] in each microstructure is also listed in the figure.
The CGHAZ consists of enlarged PAGs from the
second weld pass that grow rapidly due to being
reheated to a temperature close to the melting point.
Upon cooling, the prior austenite grains transform to
martensite or a martensite/lower bainite mix. The
FGHAZ results from fine-grain prior austenite that
form during slower austenitic grain growth at lower
temperatures above Ac3 and usually transform to ferrite
upon cooling. The ICCGHAZ is formed by reheating
material into the Ac3 and Ac1 (intercritical) transforma-
tion zone. It features precipitation of very fine ferrite/
austenite along prior austenite GBs (PAGB).
Most of the APT samples from the CGHAZ,
FGHAZ, and ICCGHAZ were prepared separately by
a modified two-stage electropolishing method. The
sample preparation procedure is detailed elsewhere.[15]
It should be noted that by using the two-stage electro-
APT tests were performed using a Cameca local-
electrode atom probe (LEAP) 3000HR operating in high
voltage mode, with a pulse repetition rate of 200 kHz, a
15 pct pulse fraction, and a sample temperature of 50 K.
The total number of G/PBs observed in the base
material (BM), CGHAZ, FGHAZ, and ICCGHAZ of
NSC and SC samples are 2, 4, 3, 5 and 2, 2, 1, 2,
respectively. 3D reconstruction and data analysis of
these samples were performed with Imago Visualization,
and Analysis Software (IVAS), version 3.6. Background
correction in the software was used to estimate chemical
concentrations from the mass spectra.
In order to quantify solute segregation at G/PBs, a
minimum of 7 cylinders with identical diameters of 3 nm
were sampled randomly over the interface and normal
to the local interfacial plane. One-dimensional (1D)
compositional profiles were plotted along the axial
direction of these cylinders at a bin size of 50 atoms.
These profiles were further transformed to ladder
diagrams,[18] which display the variation between the
accumulated solute atoms along the 1D volume as
related to the total accumulation of all atoms (Figure 4).
Segregation of the solutes of interest was then quantified
in terms of Gibbsian interfacial excess (GIE).[19–21] This
method is based on the assumption that the composi-
tions of the two adjacent regions are constant up to the
dividing surface and that the interface has negligible
volume, which is adequate for the estimation of equi-
librium segregation (ES). However, welding/PWHT and
subsequent cooling that occur in materials can lead to
non-equilibrium segregation (NES), a mechanism rely-
ing on the formation and diffusion of vacancy-solute
complexes[22] which strongly depends on grain size, start
temperature, cooling rate, and time.[23] This process
does not only influence the composition at a GB but also

6164—VOLUME 45A, DECEMBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 3—HAZ microstructures in the immediate vicinity of the FB revealed by etching using picric acid-based aqueous solution: (a) CGHAZ, (b)
FGHAZ, and (c) ICCGHAZ.
Fig. 4—Example of the ladder diagram obtained from a 1D profile
across a G/PB.
its vicinities, resulting in a wider spread of segregation
compared to ES. Therefore, the width of the solute
segregated zone Wseg, represented by the highest solute
concentration region in ladder diagrams, was also
measured in order to investigate the segregation mech-
anism of the solutes of interest, as presented in Figure 4.
III. RESULTS AND DISCUSSION
A. Effects of Welding/PWHT and Subsequent Cooling
on Solute Segregation at G/PBs
Segregation of various solutes at G/PBs was found in
the BM and all HAZ microstructures both before and
after step cooling. Figure 5 displays examples of the
two-dimensional (2D) concentration distribution of
solutes across a G/PB in CGHAZ, FGHAZ, and
ICCGHAZ in NSC materials, respectively. While Ni
and Si only show ambiguous or marginal segregation, P,
C, Mn, and Mo are clearly enriched at the interface. No
evidence of Cr, Cu, or S segregation is observed. Similar
phenomena are also found in SC materials.
Figure 6 summarizes the observed relationship
between the Wseg and u, the angle between the local
G/PB plane and the axial direction of the sample, in all
microstructures for P, C, Mn, and Mo. Trendlines were
METALLURGICAL AND MATERIALS TRANSACTIONS A
also extrapolated using least square method in order to
facilitate the visualization of the relation between Wseg
and u. The results show that for all the solutes
examined, the Wseg gradually decreases with u and
becomes smallest when u = 90 deg. This is in agree-
ment with the work of Maruyama[24] and is attributed to
the local magnification effect.[18] Despite this artificial
effect, an approximately constant difference in the Wseg
of P and Mo as a function of u is visible between NSC
and SC materials. On the contrary, the Wseg of C and
Mn show little change before and after step cooling. In
order to investigate effect of microstructure on the
distribution of Wseg of solute i (i = P, C, Mn, or Mo),
the measured width of the solute segregated zone Wi ðu0 Þ
at u = u0 was corrected to unify the effect of u by the
following equation:
wiðcorrectedÞ ¼ wiðu0 Þ  ½fi ðu0 Þ  fi ð90 degÞ; ½1
where fi ðu0 Þ is the function of the trendline of solute i
shown in Figure 6. The results are displayed in Figure 7.
It is clearly shown that the width of segregation zone of
P and Mo dropped significantly after step cooling, while
no uniform trend was observed in that of Mn and C. It
is interesting to note that for all the segregant except C
in NSC materials, the width of segregation zone in the
BM is wider than that in HAZ. This indicates that the
fast cooling after PWHT may have caused NES in the
materials. It should also be noted that the value of Wseg
differs with solute species, where the Wseg of P is
evidently narrower than the Wseg of C, Mn, and Mo.
This may be associated with the difference in atomic
misfit of these solutes at interfaces.
The average GIE of P, C, Mn, and Mo at G/PBs with
respect to microstructure are presented in Figure 8. For
NSC materials, the segregation level of P, C, Mn, and
Mo are more elevated at the G/PBs in CGHAZ and
ICCGHAZ than in FGHAZ. These features are consis-
tent with NES, which is believed to be microstructure-
dependent.[23,25] The NES in the observed materials
probably occurred during the phase transformation
induced by welding and subsequent cooling, as well as
PWHT followed by fast cooling from 888 K to 588 K
(615 C to 315 C). Since the G/PBs in the BM exhibit
similar segregation level with those in FGHAZ for
almost all the solutes examined, welding seem to have
VOLUME 45A, DECEMBER 2014—6165
Fig. 5—Examples of solute segregation at G/PB in NSC-CGHAZ, NSC-FGHAZ, and NSC-ICCGHAZ: (a) P atom map showing the sampling
volume and orientation of the cube for plotting 2D concentration maps. (b) Cumulative 2D concentration maps of various solutes across a G/
PB along the x and y direction of the cube. (c) The maximum and minimum concentration of every solute presented in the 2D concentration
maps in (b).

6166—VOLUME 45A, DECEMBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 6—Distribution of the Wseg of P, C, Mn, and Mo at G/PBs before and after step cooling with respect to u. The two dashed lines are the
trendlines obtained using least square method on the measured data of NSC and SC materials with respect to microstructure.
more profound impacts on the segregation level of
solutes at G/PBs than PWHT. Larger grains, higher
start temperature, and faster cooling rate tend to result
in higher segregation level at G/PBs. One explanation is
that the smaller grain size in BM and FGHAZ increases
the total volume of G/PBs, thus provide more defect
sinks for segregation. It is also possible that desegrega-
tion takes place at the smaller grain sizes, leading to
lower segregation level at G/PBs in these regions.
Additionally, in contrast to the large amount of PAGBs
existing in CGHAZ and ICCGHAZ, most PAGBs in
FGHAZ transform into ferrite GBs by heating up the
material during the second weld pass to over approx-
imately 1173 K (900 C) and cooling at a slower rate
from a lower start temperature.[4,23] As higher segrega-
tion level of Nb at PAGBs than at ferrite–ferrite GBs
has been reported,[26] it seems that segregation level of
solutes may vary with the type of GB. More detailed
study is needed to clarify this.
METALLURGICAL AND MATERIALS TRANSACTIONS A
B. Effects of Step Cooling on Solute Segregation at G/
PBs
Step cooling showed opposite effects on P, Mn
compared to C, Mo. While slight increase in the
segregation level is observed for P and Mn, significant
decrease occurs in the segregation level of C and Mo in
almost all the microstructures. Correlation between
Figures 6(a), 7(a) and 8(a) reveals that some P atoms
close to the interface after NES incurred by welding/
PWHT and subsequent cooling (as in NSC materials)
reach the G/PB plane during ES induced by step cooling
(as in SC materials), leading to a narrower Wseg of P.
Meanwhile, some long range diffusion also takes place,
resulting in higher segregation level of P after step
cooling. On the other hand, Figure 6(c) suggests that the
influence of ES on Mn in SC materials is not very high
although increased segregation level of Mn was found
after step cooling. A possible explanation is that the
enrichment of P at G/PBs during ES promotes Mn
VOLUME 45A, DECEMBER 2014—6167
Fig. 7—Average Wseg of P, C, Mn, and Mo corrected using Eq. [1] with respect to microstructure.
segregation through interaction. In contrast, the content
of C and Mo at G/PBs decrease during step cooling. It
may indicate that the maximum ES level of C and Mo
are lower than the segregation level resulted by the prior
heat treatments, thus causing these two types of solute
to desegregate and reducing their final amount at G/
PBs. The noticeable difference in the Wseg of Mo before
and after step cooling is indicative of a faster desegre-
gation rate compared to that of C, which shows little
change in the Wseg during NES and ES. This may also
be attributed to the different diffusion mechanism of
interstitial (C) and substitutional (Mo) atoms.[27]
In addition, C and Mo have been identified as the two
principal segregants at dislocations encountered in the
APT tests. The dislocations probably form on slip
planes within individual grains and usually appear in
long, thin, and slightly curved strip shape, as presented
in Figure 9. Although the exact density of dislocations is
unknown, such features are quite commonly encoun-
tered in almost all microstructures including BM and
HAZ in both NSC and SC materials. As shown in
Figures 9(b) and (c), the concentrations of C and Mo at
dislocations vary from site to site, which may depend on
the type of dislocations.[28] To investigate the effects of
step cooling on the composition of dislocations, a
0.3 atoms/nm3 C + Mo iso-density surface was selected
6168—VOLUME 45A, DECEMBER 2014
to delineate the dislocations, and the concentration of C
and Mo enclosed by the iso-density surfaces were
measured. In total, 43 and 49 dislocations were mea-
sured for NSC and SC materials, respectively. The
average concentration before and after step cooling are
0.94 ± 0.38 and 0.66 ± 0.22 at. pct for C, and
0.55 ± 0.39 and 1.12 ± 0.36 at. pct for Mo. While
slight decrease is observed in the average C concentra-
tion at dislocations after step cooling, the average Mo
concentration at dislocations is more than doubled. The
concentration ratio of C:Mo changes from ~1:0.6 to
~1:1.7 after step cooling, which is indicative of the
onsetting of Mo2C precipitation. In addition, the
measured average concentration of the onsetting pre-
cipitation after step cooling at dislocations
(~2.25 wt pct) is of the same order compared to the
equilibrium solubility product of Mo2C in ferrite at step
cooling finishing temperature 741 K (468 C)
(~1.33 wt pct) calculated using the method proposed in
Reference 28. This suggests that the hypothesis of the
onsetting of Mo2C precipitation is reasonable.
On the other hand, comparison between the average
bulk composition before and after step cooling reveals
that the average bulk C content in the vicinity of G/PBs
(<±100 nm from the G/PB plane) increases from
0.031 ± 0.001 to 0.044 ± 0.002 at. pct, while the aver-
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 8—The estimated GIE of P, C, Mn, and Mo at G/PBs before and after step cooling with respect to microstructure.
age bulk Mo content decreases from 0.125 ± 0.003 to
0.077 ± 0.002 at. pct. This is consistent with the com-
positional fluctuation of C and Mo observed at dislo-
cations before and after step cooling. It seems that
during step cooling, competition takes place between
equilibrium segregation and precipitation of Mo, and
that dislocations act as stronger sinks for Mo than G/
PBs. Mo has been reported to reduce temper embrittle-
ment by either tying P atoms up in the grain interior or
by counteracting the embrittlling effect of segregated P
atoms at GBs.[29] It is likely that in this case, the
solubility of Mo in iron is reduced during step cooling
due to its affinity for C, thus hampering its scavenging
action on P segregation at G/PBs. However, the
precipitation/coarsening of Mo-rich carbides is strongly
dependent on the nominal Mo content, aging time and
temperature.[5] It is necessary to verify these findings by
isothermal aging the material at service temperatures,
which are lower than the temperatures applied during
step cooling.
C. Implications on Synergistic Co-segregation
In order to investigate the existence of co-segregation
between different solutes, all G/PBs were extracted from
METALLURGICAL AND MATERIALS TRANSACTIONS A
the original APT dataset using a 0.2 atoms/nm3 C + P
iso-density surface, which was chosen because it forms a
relatively smooth shell near the inflection point between
the interface and the matrix. Examples of the cumulative
2D concentration map of C, Mn, Mo, and P plotted
along the direction giving the maximum projection area
of the interface are displayed in Figure 10. Obviously,
the distributions of all the solutes examined are inho-
mogeneous at the interface. Analysis employing radial
distribution function (RDF)[18] was implemented on P
atoms in all the extracted G/PBs. It examines the
average local neighborhood as a function of distance
extending radially outwards from each P atom in the
datasets and compares the concentration of C, Mn, or
Mo in concentric shells around each P atom to their
bulk concentration. Values of the RDF >1 indicate
attractive interactions/clustering, while values <1 indi-
cate repulsive interactions between atoms. In this study,
the thickness of the concentric shells built around each P
atom is set as 0.5 nm, which approximately equals to the
average 1-order nearest neighbor distance[18] between P–
P atoms (~0.5 to 0.75 nm) at G/PBs. Figure 11 displays
the RDF of pair correlation between P-C, P-Mn, and P-
Mo with respect to microstructure. It is shown that the
concentration of C in the vicinity of P atoms is slightly
VOLUME 45A, DECEMBER 2014—6169
Fig. 9—(a) C enrichment at dislocations in a NSC-BF sample. The brown dots represent C atoms, and the brown surfaces correspond to 0.3 atoms/
nm3 C + Mo iso-density surface. The large precipitate in the middle left is of Mo2C type. (b) and (c) present the 1D compositional profile across the
dislocation site enclosed by the upper (size: 30 9 8 9 30 nm) and lower cube (size: 40 9 8 9 30 nm), respectively (Color figure online).

Fig. 10—(a) A G/PB in SC-ICCGHAZ extracted by a 0.2 atom/nm3 C + P isoconcentration surface. The size of the cylinder for plotting 2D
concentration maps is 30 9 42 9 8 nm. (b) Cumulative 2D concentration maps of P, C, and Mo at a G/PB. The maximum concentration is
1.62, 3.16, 0.96, 1.10 at. pct for C, Mn, Mo, and P, respectively. The minimum concentration is 0 for all the three solutes.

lower than that in the bulk in NSC materials. However,
after step cooling, no uniform trend was observed. This
may indicate that repulsive P-C interaction exists but the
magnitude is rather small. On the other hand, in almost
all the microstructures examined before and after step
cooling, Mn and Mo tend to segregate in close proxim-
ities of P. These are consistent with the attractive
interaction between the metallic alloying element Mn
and Mo and the embrittling impurity P reported in
References 5, 29, 30. The abnormal distribution of RDF
of P-Mo in SC-FGHAZ (Figure 11(f)) is probably due
to the greatly reduced amount of Mo atoms at the
interface. As Mo alone appears as a very weak segregant
at GBs in Fe, [31,32] it seems that the Mo-P interaction is
critical for the segregation of Mo. Although strong
C-Mo affinity has also been reported,[5] such interaction
does not seem to favor G/PBs but prefer C-enriched
dislocations and precipitates instead. As C and Mo
enhance GB strength while P and Mn act oppo-
sitely,[5,30] the results suggest increasing risk of temper
embrittlement with progress in service time of LAS,
especially in ICCGHAZ and CGHAZ.
On the other hand, similar trend in RDFs of P-Mn
and P-Mo are observed in both NSC and SC materials,

6170—VOLUME 45A, DECEMBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 11—Normalized P-centered C, Mn and Mo partial radial distributions from all G/PBs in NSC and SC materials with respect to microstruc-
ture.
indicating that similar interactions between these solutes
occur during the different thermal treatments and
segregation mechanisms.
IV. CONCLUSIONS
In summary, effects of thermal history and micro-
structure on segregation of P, C, Mn, and Mo at G/PBs
METALLURGICAL AND MATERIALS TRANSACTIONS A
in the HAZ of LAS were studied quantitatively using 3D
APT. The main conclusions are listed below:
1. The thermal history of the material, consisting of
welding and quenching after welding (causing
NES), PWHT at 888 K (615 C) for 25 hours (caus-
ing ES), and cooling to 588 K (315 C) (causing
NES), followed by cooling to room temperature (no
significant segregation expected) and step cooling
VOLUME 45A, DECEMBER 2014—6171
 (causing ES), had profound influence on the final
segregation level at G/PBs of all the solutes exam-
ined.
2. NES during welding and subsequent cooling ap-
peared to play a vital role in the microstructure-
dependent segregation of P, C, Mn, and Mo at G/
PBs, resulting in higher G/PB enrichment of all the
solutes in ICCGHAZ and CGHAZ than in
FGHAZ and BM.
3. The ES induced by step cooling further promoted
the segregation level of P and Mn at G/PBs. On the
contrary, it led to the desegregation of C and Mo
at G/PBs.
4. Competition between segregation and precipitation of
Mo occurred during step cooling. The solubility of
Mo in iron appears to be significantly reduced by pre-
cipitating at dislocations, contributing to the observed
changes in the segregation level of solutes at G/PBs.
5. Attractive interactions between P-Mn and P-Mo at
G/PBs seem to have taken place during the entire
thermal history, which showed good agreement with
the interactions observed between these solutes in
other studies. On the other hand, marginal repulsive
interaction between P-C was also observed, espe-
cially in NSC materials.
ACKNOWLEDGMENTS
The authors gratefully acknowledge the Central Re-
search Institute of Electrical Power Industry (CRIEPI)
for providing the LEAP facility, and the technical
assistance of Dr. Masanari Tomozawa and Masaru
Sato. The authors would also like to express their
gratitude to the Innovative Leader Platform of To-
hoku University for the financial support for Ziqing
Zhai to conduct APT tests in CRIEPI.
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METALLURGICAL AND MATERIALS TRANSACTIONS A