Acta Materialia 50 (2002) 1383–1392

www.actamat-journals.com

Prediction of chromium depleted-zone evolution during

aging of Ni–Cr–Fe alloys
H. Sahlaoui a,*, H. Sidhom a, J. Philibert b
a
Laboratoire de Mécanique, Matériaux et Procédés, Ecole Supérieure des Sciences et Techniques de Tunis, 5, Av. Taha Hussein
1008 Montfleury, Tunisia
b
LPCES, Université Paris-Sud, F-91405 Orsay Cedex, France

Received 16 October 2001; received in revised form 26 November 2001; accepted 5 December 2001

Abstract

The phenomenological and analytical study of depleted chromium zone in Ni–Cr–Fe alloys has been carried out in
order to predict the evolution of chromium profiles resulting from carbide precipitation during aging. A diffusional
model has been developed to take into account the two stages of chromium concentration evolution: dechromization
and rechromization. The model has been verified using the available experimental data found in the literature for a
nickel alloy type: Inconel 690. The changes of the chromium concentration at the carbide–matrix interface xiCr(t) and
near the grain boundary xCr(x,t), as a function of annealing conditions, can be assessed with a reasonable accuracy by
the proposed model and compared to the previous thermodynamic and kinetic models.  2002 Acta Materialia Inc.
Published by Elsevier Science Ltd. All rights reserved.

Keywords: Carbides; Nickel alloys; Aging; Depleted zone

1. Introduction concentration in various commercial nickel based

Chromium confers to steels and special alloys in
general and to nickel alloys in particular a good
resistance to intergranular attack IGA and to inter-
granular stress corrosion cracking IGSCC [1–22].
This property requires a minimum chromium con-
tent higher than (or equal to) a critical value xcrit
Cr ,
which is a function of the chemical composition of
these alloys [1–8]. For this reason, the chromium
* Corresponding author. Tel.: +216-1-49-60-66; fax. +216-
1-39-11-66.
E-mail address: Habib.Sahlaoui@ipein.rnu.tn
Sahlaoui).
alloys in the as received condition ranges on the
average from 15 to 30 wt%. These alloys are
homogenized by a standard processing or by high
temperature annealing [8]. The high chromium
concentration destabilizes the solution by generat-
ing complex chromium carbides of type Cr3C2,
Cr7C3, Cr23C6 and intermetallic phases which are
rich in chromium like σ, χ and R phases [1–22].
These compounds precipitate more or less quickly
between 400 and 900°C according to the content
of carbon, chromium and molybdenum of ternary
alloys Ni–Cr–Fe [1–9]. They often respect a
(H. sequence of heterogeneous nucleation, beginning
with intergranular precipitation, then precipitation

1359-6454/02/$22.00  2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
PII: S 1 3 5 9 - 6 4 5 4 ( 0 1 ) 0 0 4 4 4 - X
1384 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392
on incoherent twin boundaries and on the dislo-
cations [2,10]. Their growth, which is controlled
by an intragranular thermally activated diffusional
process, depends on the chromium content in the
adjacent precipitates and on the matrix carbon con-
tent [10–21]. The consequence of the intergranular
precipitation of these phases in general, and of the
carbides in particular, is to create a chromium-
depleted zone near the grain boundaries. These
depleted zones get wider as the temperature and/or
the aging duration is higher [1–9] and reduce the
local resistance to intergranular corrosion IGC.
Furthermore, they increase the susceptibility to
IGSCC in a chlorinated medium [1–8]. For these
reasons many studies have been devoted to a quan-
titative evaluation of the dechromized zones by
experimental analysis or by empirical or analytical
models [1–22]. These models attempt to find by
calculation the chromium concentration profiles
and their evolutions during aging. These results are
of great interest for the evaluation of the stages of
sensitization and desensitization to the IGC during
aging, under the accelerated operating conditions
of the nickel alloys used in industrial equipment
[1–7]. However, the profiles obtained by the ther-
modynamic and kinetic models reveal significant
discrepancies when they are compared to the
increasingly precise experimental determinations
by recent analysis techniques (STEM). These dif-
ferences become more significant as the aging per-
iod is longer [2], and can have risks on the time–
temperature–sensitization (TTS) diagrams predic-
tion and consequently on the protection of equip-
ment against localized corrosion. Simplifying
assumptions seem to be the origin of these discrep-
ancies, particularly the hypothesis that the carbides
nucleation is instantaneous at any exposure tem-
perature and that the chromium content at the car-
bide–matrix interface reaches instantaneously its
thermodynamically equilibrium value [1,2,6]. For
that reason, we propose to reformulate a model
able to accurately predict the chromium content
evolution of the depleted zones during aging of the
Ni–Cr–Fe alloys. The proposed model will be
based on phenomenological and analytical descrip-
tions of the dechromization process. The model
variables will be well identified to take into
account the experimental profiles available in the
literature [2].
2. Phenomenological analysis of depleted zone
It is well established that the time t0 to start
nucleation of chromium carbides in alloys type Ni–
Cr–Fe and Fe–Cr–Ni depends on exposure tem-
perature, chemical composition and particularly on
carbon content and alloy microstructure [8]. Chro-
mium depleted zones were created following the
carbides precipitation at the grain boundary
because bulk diffusivity of chromium is relatively
low compared to that of carbon. Many studies [1–
22] report that the chromium content at the car-
bide–matrix interface or grain boundaries
decreases significantly with nucleation and growth
of the intergranular chromium carbides. The
growth of carbides during annealing will consume
more chromium atoms which will diffuse from the
interior of grains and leads to a thicker depleted
zone which is described by a profile xCr(x,t). This
profile is characterized by the chromium concen-
tration at the carbide–matrix interface xiCr(t) and by
the width of the depleted zone l which depend
maily on the annealing conditions of these alloys.
The evaluation of these characteristics requires pri-
mary a rigorous analysis of the involved physical
phenomena.
2.1. Evolution of chromium concentration at the
grain boundary
The chromium concentration at the carbide–
matrix interface or at the grain boundary xiCr(t)
reaches a critical value xcrit
Cr after annealing duration
ts at temperature T. This critical value corresponds
to the beginning of sensitization at the IGA [1–8].
The concentration xiCr(t) decreases continuously to
reach a minimal value xminCr after annealing duration
t corresponding to a partial thermodynamic equi-
librium between carbides and matrix (Fig. 1). Since
the diffusion of carbon atoms is very fast, com-
pared to that of chromium, the concentration of
carbon decreases uniformly with depth [1].
According to the law of the solubility, the decrease
of carbon activity leads to an increase in local
 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392
Fig. 1. Influence of chromium concentration at the carbide–
matrix interface on the process of sensitization–desensitization
at the IGA during aging.
chromium activity in equilibrium with carbides
that constitute the driving force for chromium bulk
diffusion from the interior of the grain towards the
depleted zones [1]. The last phenomenon involves
a rise in the chromium concentration at the
depleted zones interfaces which leads to the
rehomogenization of alloys. This process of
rechromization acts against the dechromization
process related to the growth of carbide which is
delayed by the reduction of carbon concentration
in the matrix. The desensitization for IGA (self-
healing) can be obtained when the chromium con-
centration at the carbide–matrix interface reaches
the value xcrit
Cr after one duration exposure td (Fig.
1).
2.2. Evolution of the chromium concentration at
the depleted zone
High chromium content xcCr of carbides which
ranges from 60 to 90 at.% [1–9], is obtained at
the expense of the adjacent matrix initial chromium
content x0Cr which depends on the alloy type. A
chromium consumption by carbide growth is bal-
anced by the bulk diffusion of this element that
leads to the increase of the concentration gradient.
This phenomenon can be described by chromium
concentration profile evolution in the direction per-
pendicular to the grain boundaries as a function of
annealing time (Fig. 2). Matrix chromium content
in the depleted zones can be predicted by solution
of Fick’s second law. Through the width of the
depleted zone (l), chromium concentration varies
between the initial alloy chromium content x0Cr and
1385
the interface carbide–matrix content xiCr as a func-
tion of exposure duration.
3. Analytical description of the depleted zone
3.1. Chromium concentration evolution at the
grain boundary
Carbides nucleation and their first growth stages
(stages b and c—Fig. 2) involve atom migration
from the matrix towards the carbides which are
constituted of all metal elements available in the
matrix like carbide formers (chromium and
molybdenum) as well as other elements like nickel,
silicon and manganese [3,8]. The contribution of
these elements to the carbide precipitation modifies
significantly the interface chemical composition
and particularly its chromium content which is the
major element in the carbides. The change of inter-
face chromium content can be described, during
stages of germination and growth, by the fre-
quently used relationship (1):
t
xiCr(t) ⫽ x0Crexp(⫺k ) (1)
t
where xiCr(t) can be considered as the solution of
chemical kinetics equation of a first order interfa-
dxiCr(t)
cial reaction ⫽ ⫺kxiCr(t), with a constant k
dt
typical of interfacial reaction.
The rehomogenization stage (stage d—Fig. 2)
which is controlled by the chromium bulk diffusion
modifies the chromium content at the carbide–
matrix interface and at the grain boundaries. The
change of the chromium concentration can be
described analytically by considering the conser-
vation of matter flow through these interfaces and
assumes an instantaneously exchange of chromium
atoms between the matrix and the carbide through
the interface. This leads to the equality between
the two areas S1 and S2 (stages c and d—Fig. 2).
• The area S1 is given by Eq. (2):
S1 ⫽ xcCrr (2)
Since the growth of carbides is controlled by the
chromium diffusion in the grains, their sizes r can
1386 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392

Fig. 2. Chromium profile concentration evolution during aging.

be expressed according to Zener’s empirical rt ⫽ b冑Dt (5)

relation [5], by Eq. (3):
Combining relations (2) and (5), S1 can be
r ⫽ b冑Dt (3) expressed by:
where b is a constant determined by Zener method S1 ⫽ xcCrb冑Dt (6)
[5] and D is the chromium diffusion coefficient,
which depends on the temperature as a thermally • The area (S2) can be approximated by a tri-
activated process (4): angular shape where the chromium concentration

冉 冊
near the grain boundaries is assumed to have a lin-
⫺Q
D ⫽ D0exp (4) ear profile as:
RT
S2 ⫽ (x0Cr⫺xiCr)l / 2 (7)
D0 is equal to 0.08 cm2/s and Q is equal to 58,500
cal/mol according to [1,4]. the exact value of area S2 can be determined by a
During the annealing period of t, the carbon solution of Fick’s second law equation according
activity in the matrix decreases significantly and to relation (8):
the interface chromium content reaches a minimal

冕
L0
value xmin
Cr , then the growth of carbides is suf- x
S2 ⫽ (x0Cr⫺xiCr) (1⫺erf(
2冑Dt
ficiently slowed down to be neglected and its size )) dx (8)
rt can be considered constant and expressed by: 0
 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392 1387

L0 is a constant higher than or equal to the width

冪t
t
of the depleted zone and could tend to infinity. In xiCr(t) ⫽ x0Cr⫺xcCrb (13)
this study L0 is approximated to half of a grain size.
The finite difference method can be used to cal- It is important to specify that evolution of the inter-
culate accurately the area S2 according to the fol- face chromium concentration, during isothermal
lowing expression (9): exposure, is described by the relation (1) during

冘冋 册
the depletion stage and by the relation (13) during
(xCr(xj) ⫹ xCr(xj+1)
S2 ⫽ x0Cr⫺ ⌬x (9) the self healing (desensitization) stage. Moreover,
2 the size (rt) is not the real carbide final size but
where xCr(xj) ⫽ xiCr(t) ⫹ (x0Cr⫺ its size when the chromium concentration at the
xj interface reaches its minimal value indicating the
xiCr(t)).erf( ),xCr(xj ⫽ xiCr(t) ⫹ (x0Cr⫺ beginning of self healing stage. In this last stage,
2冑Dt it is possible to temporarily neglect the carbide
xj ⫹ 1 growth (and not to infinite) because other phenom-
xiCr(t)).erf( ), ⌬x ⫽ xj ⫹ 1⫺xj. xj values can vary
2冑Dt ena of precipitation can occur such as:
between 0 and L0. The chromium concentration at
the carbide–matrix interface can be obtained by 앫 The precipitation of new inter and intragranular
writing the equality between the two areas obtained carbides and intermetallic phases which are
by Eqs. (6) and (7) or for a better accuracy by (6) more stable for long annealing periods.
and (8 or 9) which gives: 앫 The redissolution of chromium carbides in favor
of more stable other phases such as the σ-
xcCrb冑Dt phase, etc.
xiCr(t) ⫽ x0Cr⫺ L ⬵x0Cr (10)

冕
0
x This assumption could be accepted to determine
(1⫺erf(
2冑Dt
)) dx
the sensitization time (ts) and desensitization time
0
2xcCrb冑Dt
(td) which are principally related to the chromium
⫺ carbide precipitation.
l
the value of integral is calculated by the following 3.2. Evolution of the chromium concentration in
expression (11): the depleted zones

冕 冋
L0

x The evolution of the chromium concentration

(1⫺erf( )) dx ⫽ x
2冑Dt
(11) near the grain boundaries can be obtained by the
numerical or analytical resolution of Fick’s second

冉冑 冊册
0

⫺2冑Dt
x x 1 x2 L0 law for the unidirectional diffusion with the fol-
) ⫹ exp(⫺ )
2 Dt 2冑Dt
erf(
冑p 4Dt 0
lowing initial and limit conditions:
tⱕt0⇒xCr(x,0) ⫽ x0Cr∀x
The relation (10) can be simplified by substituting
the width (l) by its approximate expression: x ⫽ 0⇒xCr(0,t) ⫽ xiCr(t)
l⬇2冑Dt (12) xⱖl⇒xCr(x,t) ⫽ x0Cr
This equality is obtained from the random-walk The chromium concentration xiCr(t) at the car-
theory according to Stawström et al. [1] and Bor- bide–matrix interface is determined, according to
ello et al. [4]. The substitution of l in Eq. (10) model described in the previous paragraph
allows us to write: (Section 3.1).
1388 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392

3.2.1. Carbide precipitation stage 1 x

xCr(x,t) ⫽ (xiCr(t)⫺x0Cr).erfc( ) ⫹ x0Cr
2冑Dt
During the carbide precipitation (nucleation and (15)
2
growth, stages b and c—Fig. 2), the chromium
concentration profile is computed assuming dif- In this equation, the origin (x ⫽ 0) is always
fusion in a semi-infinite medium, in accordance to taken on the plane p, which intercepts the diffusion
the original work of Stawström and Hillert [1] fol- direction at coordinate l / 2 (with l ⫽ 2冑Dt) and x
lowed by other authors [2–6]. This assumption is ⫺l l
justified by chromium exchange between the car- varies in the interval [ , ].
2 2
bides and the matrix through their common inter-
face during precipitation stages. Consequently, the 3.3. Identification of model constants
chromium concentration profile can be given with
a good approximation by Eq. (14), which is derived Constant t can be given by an empirical relation
from the exact solution of the Fick’s second law: (16) derived from Eq. (5).

冉冊
x
xCr(x,t) ⫽ xiCr(t) ⫹ (x0Cr⫺xiCr(t)).erf( 1 rt 2

2冑Dt
) (14)
t⫽ (16)
D b

3.2.2. Self healing stage
Eq. (14) cannot be adopted during desensitiz-
ation stage (stage d—Fig. 2), where chromium
exchange through carbide–matrix interface
becomes sufficiently slow to be neglected. Conse-
quently, we propose a model based on an interdif-
fusion mechanism through a plane p so-called Mat-
ano plane. This plane divides the depleted zone
into two equal areas A1 and A2 (Fig. 3). The trans-
port of the chromium atoms, through this plane p,
from area A2 towards area A1 will take place with-
out accumulation. This diffusion leads to an evol-
ution of chromium concentration as a function of
healing time xCr(x,t) described by the approximate
Eq. (15). The last equation is derived from the
Fick’s second law exact solution, which supposes
In this relation, rt is the average value of the car-
bides size at the end of precipitation, which can be
estimated by micrographic observation. The value
of t, which corresponds to the required duration to
reach the minimal chromium concentration at the
carbide–matrix interface xmin Cr can be assessed
directly from experimental measurements of the
chromium concentration evolution as a function of
annealing. Since diffusion phenomenon is a ther-
mally activated process, the relation time–tempera-
ture equivalence of Arrhenius type (17), can be
used to derive the value of t for any temperature
exposure.
t2 ⫽ t1exp 冋 Q 1 1
( ⫺ )
R T2 T1 册 (17)

a constant interface chromium concentration: Constant k is given by relation (18) and determined

Fig. 3. Chromium profile evolution as a function of exposure condition during desensitization.

 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392
by equating 1 and (13), which expresses the conti-
nuity condition between the two dechromization
and rechromization stages for t ⫽ t
xcCrb
k ⫽ ⫺Ln(1⫺ 0 )
xCr
4. Model validation
The prediction of chromium concentration evol-
ution at the carbide–matrix interface xiCr(t) and near
the grain boundaries xCr(x,t) during aging of Ni–
Cr–Fe alloys requires the determination of the fol-
lowing parameters:
앫 t0: time required for carbide nucleation which is
evaluated from time–temperature–precipitation
diagrams;
앫 t: determined by application of the Eq. (16)
and/or (17) depending on the available data;
앫 k: determined by Eq. (18).
To compute chromium concentration profile during
isothermal exposure at a temperature T, we pro-
ceed, depending on the aging time (t), in the fol-
lowing manner:
앫 t ⬍ t: xiCr(t) is determined by Eq. (1) and the
profile xCr(x,t) is computed using Eq. (14);
앫 t ⬎ t: xiCr(t) is determined by Eq. (13) and the
profile xCr(x,t) is computed using Eq. (15).
This established model was validated using data
for Inconel 690 which is one of the most sensitive
to the phenomenon of chromium carbide precipi-
tation at the grain boundaries and the subsequent
dechromization during aging at their operating
temperature range (vapor generator, exchanger,
turbojet, etc.). Chromium concentration at the car-
bide–matrix interface and near the grain bound-
aries during aging of this alloy evaluated by the
proposed model is in good agreement with the
experimental data (Figs. 4–6).
1389
5. Discussion
The major contribution of the present model lies
the high accuracy prediction of the interface car-
bide–matrix chromium concentration and its evol-
(18)
ution xiCr(t) with annealing time. The value of this
concentration is required for a better prediction of
which is a consequence of intergranular precipi-
tation of chromium carbide in the Ni–Cr–Fe alloys.
The accurate determination of the dechromization
profiles is of particular interest when these alloys
which are usually used in electronuclear, aerospace
and agroalimentary applications, are exposed to
operating conditions which induce dechromization.
This last phenomenon reduces the resistance of Ni–
Cr–Fe alloys to intergranular corrosion IGC and to
intergranular stress corrosion cracking IGSCC [1–
22]. The proposed model gives a rather precise
chromium concentration at the carbide–matrix
interface, which was lacking in many empirical,
thermodynamic and kinetic models proposed in the
literature [1–7]. Moreover, the assumption of semi-
infinite diffusion hypothesis, used by these models
does not seem to be well adapted to account for
the rechromization phenomenon at the end of the
carbide precipitation, leading to the significant dif-
ferences between the calculated and measured pro-
files [1,2,6]. The present model gives a better pre-
diction of chromium profiles during aging, as
shown by the superposition of calculated and mea-
sured chromium profiles for Inconel 690 (Figs. 4–
6). The chromium profiles resulting from the
annealing at 700°C of Inconel 690 measured by
Kai et al. [2] and calculated by the present model
are in good agreement. These profiles diverge as a
function of time from those obtained by the
thermodynamic/kinetic model developed by Was
and Kruger [6] and modified by Kai et al. [2] (Fig.
6). These discrepancies which are more significant
when aging duration is longer, were attributed by
the authors to the intragranular precipitation of car-
bides and to the thermodynamic instantaneous
equilibrium at the grain boundary hypothesis
which is not very founded and in contradictory to
the carbides nucleation and growth kinetics. This is
the reason for which all the thermodynamic/kinetic
model profiles find a carbides–matrix interface
chromium concentration at the carbide–matrix
1390 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392

Fig. 4. Chromium carbides–matrix interface concentration evolution during aging of Inconel 690 at T=600°C (t=50, k=0.57) and at
T=700°C (t=6, k=0.40).

Fig. 5. Comparison between measured data [2] and present model calculated chromium depletion profiles during aging at 24 h, 48
h, 100 h and 215 h of Inconel 690 at 600°C.

interface almost constant (苲20 wt%) for all the
aging duration (Fig. 6). The proposed model,
which takes into account the evolution of the chro-
mium concentration at the carbide–matrix interface
with annealing time is in reasonable agreement
with the experimental results. Moreover, the
hypothesis considered in this study which consists
of neglecting of the carbide–matrix interface dif-
fusion after a duration t and of using an interdif-
fusion solution is justified by the vanishing value
 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392 1391

Fig. 6. Comparison of chromium depletion profiles: measured [2], calculated with former model [2] and with the present model
during aging at 5 h, 10 h, 48 h and 100 h of Inconel 690 at 700°C.

of the horizontal tangent to the profiles at the end
∂C(x,t)
of the precipitation (( ) ⫽ 0). The last
∂x x ⫽ 0
result was not obtained by other models, which are
based on the assumptions of semi-infinite dif-
fusion, although it was observed on experimentally
measured profiles published in the literature [1–7].
6. Conclusion
Chromium concentration evolution at the car-
bide–matrix interface and near the grain bound-
aries (chromium depleted zones) resulting from
intergranular carbides precipitation during aging of
the Ni–Cr–Fe alloys can be accurately predicted by
a two stage model, i.e. dechromization and rechro-
mization. The model constants were identified and
validated for Inconel 690 heat treated for different
periods of time (5 h, 10 h, 24 h, 48 h, 100 h, 215
h) and at two temperatures (600°C and 700°C).
An analytical calculation using approximate sol-
utions of diffusion equations can correctly describe
the phenomena of dechromization and rechromiz-
ation without the need to resort to a heavy numeri-
cal calculation method (finite differences) to solve
the complete equations system describing these
phenomena. This last method would require in any
case several approximations, since the final equi-
librium state of the alloy cannot be simply
1392 H. Sahlaoui et al. / Acta Materialia 50 (2002) 1383–1392
described because of the multiplicity of phases
which can be appear, according to alloy chemical
composition, exposure conditions, etc.
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