Literature review
Precipitation in creep resistant austenitic
stainless steels
T. Sourmail
Austenitic stainless steels have for some time been used as superheater tubes in the electricity generation industries
in harsh environments with temperatures as high as 650³C at pressures of some 200 atm; they are expected to
provide reliable service for 30 years or more. Their detailed mechanical properties are dependent on the stability
of the microstructure, particularly the formation, dissolution, and coarsening of precipitates. Although the
precipitation processes have been studied extensively, there remain important discrepancies. It is known that small
changes in the chemical composition or thermomechanical processing can profoundly in¯uence the evolution of the
microstructure. This review focuses on precipitation in creep resistant austenitic stainless steels, in particular
wrought heat resistant grades containing niobium and titanium additions. Conventional alloys such as 18 ± 8 and
16 ± 10 are included together with the new NF709 (20 ± 25) and other recent variants. Precipitates forming in age
hardening austenitic stainless steels are only brie¯y presented. Many studies have shown that MX is not a
stoichiometric phase, and that chromium can be incorporated in the metal sublattice. Furthermore, the reported
compositions show considerable variation. These studies are assessed and an explanation is offered, in terms of the
Gibbs ± Thompson effect, for the variation. A rational consideration of all the results suggests a size dependence in
line with capillarity considerations. The MX phase does not form in isolation; its stability also depends on the
formation of M23C6. The literature reveals that NbC is more stable than M23C6 but the case for TiC is less certain.
The formation of Z phase in nitrogen bearing steels is a further complicating factor, and it is concluded that its
formation is not adequately understood. This is unlike the case for M23C6, where there is consistent reporting in the
literature. Finally, work on the M6C carbide in austenitic stainless steels is critically assessed. It is found that its
detailed composition is not well characterised and that there are no general rules apparent about its formation. The
review also covers intermetallic compounds such as s phase. It is clear that chromium concentrations in excess of
18 wt-%, combined with a low carbon concentration, promote the formation of s phase. This has implications
particularly for steels containing niobium and titanium, both of which getter carbon. Other compounds reviewed
include x and G phases, which form at high temperatures and during very long aging such as that encountered in
service.
MST/4721
The author is in the Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge
CB2 3QZ, UK.
# 2001 IoM Communications Ltd.
Introduction
! ! "# $ %
! !
& '
()*+,* % ! -,- )
+ +# . /
! !
! COMPOSITION AND CONSTITUENTS
0 ( * % 1 ! ( 2 3 0 ( ! % 4 5 *1
% 5
0 ( * 60 7 8%9%+
: 8 8 % * ;
( 5 This review was a runner-up in the inaugural MST Literature Review Prize competition, set
up to encourage the preparation of critical literature reviews by students as an essential part
of study for a higher degree in the materials ®eld, and subsequently to make the best of
these available to a wider readership.
ISSN 0267 ± 0836
Materials Science and Technology
January 2001 Vol. 17
1
2 Sourmail Precipitation in creep resistant austenitic stainless steels
1
5 ! ? 8+)(= ! !
% ! % 2
3 %
wt-% Ni
wt-% Cr
GRADES OF AUSTENITIC STAINLESS STEEL
0 )< *0"
! 6%
7<# % 1
0 ( *
% -,- ) 4 ! 67 ! %
+ <
@ A 6) 7 * 6 )=A*7
8 )= )+
)< 8 * % %
! B ,C,) -,- ) 0 ! -,- ) ! )= - ! 5 ! ! ! % ) ! % +( +#* >! ! 6%z
7 6 +=7 ! = % 4
! 5 !
D 6 7 5 wt-% Fe
³
!" # $%
#
# &'()') *+', -
% 4 1
5!
)
*5 ~‰*Šz‰(Šz:#‰8Šz)‰(Šz:)‰(Š
z+#‰*Š 67
(5 ~‰(Šz+:‰,Šz:#‰8Šz#:#‰
Šz:#‰*Š
z:#‰%Šz:#‰Š 67
- ! ! %
4 !
!
! M ,!
! ! M M 60 (7~#+{‰(Š{+)‰*Š{)‰8Š{)‰*Š
{+‰(Š{#<‰(Š{=‰8Š
67
)< M >! 1 ! M % M) # ) M) 60 (7~<"{<=+‰(z*Š{":+‰,Š{:‰8Š{+‰*Š
{):‰(Š{:#‰8Š
ROLE OF ALLOYING ELEMENTS
8 1
1 % 1
! < + = 8
>! ! 8 8
-
! - 67
! ! (
+ * >! % '
- # % !
Type 304 (Ref. 4)
NF709 (Ref. 5)
C
Si
Mn
P
Cr
Mo
Ni
B
N
Nb
Ti
Fe
f0.07
0.06
y0
0.40
f2.00
1.00
0.04
0.006
17 ± 19
20
y0
1. 5
8 ± 10
25
y0
0.005
y0
0.167
y0
0.26
y0
0.05
Bal.
Bal.
Materials Science and Technology
January 2001 Vol. 17
Sourmail Precipitation in creep resistant austenitic stainless steels
3
'
- )* . /
K # % !
301
302
304
310
316
321
347
E1250K
20 ± 25 Nb
A286
C max.
Si max.
Mn max.
Cr
Mo
Ni
Al
Nb
Ti
V
Fe
0.15
0.15
0.08
0.25
0.08
0.08
0.08
0.1
0.05
0.05
1.00
1.00
1.00
1.50
1.00
1.00
1.00
0. 5
1. 0
1. 0
2.00
2.00
2.00
2.00
2.00
2.00
2.00
6.0
1.0
1.0
16 ± 18
17 ± 19
18 ± 20
24 ± 26
16 ± 18
17 ± 19
17 ± 19
15.0
20.0
15.0
¼
¼
¼
¼
2.0 ± 3.0
¼
¼
¼
¼
1.2
6±8
8 ± 10
8 ± 12
19 ± 22
10 ± 14
9 ± 12
9 ± 13
10.0
25.0
26.0
¼
¼
¼
¼
¼
¼
¼
¼
¼
y0.18
¼
¼
¼
¼
¼
¼
106%C min.
¼
0. 7
¼
¼
¼
¼
¼
¼
56%C min.
¼
¼
¼
y1.9
¼
¼
¼
¼
¼
¼
¼
0.25
¼
y0.25
Bal.
Bal.
Bal.
Bal.
Bal.
Bal.
Bal.
Bal.
Bal.
Bal.
KE1250 is Esshete 1250.
>! s A! ,
* % ; ! 4 >! % ! % ! ( * % ; * - ? 1 - ! ! < >!
8+)(=
Carbides and nitrides
MX PRECIPITATES
% 8E F 6% *
; ' % 7 % !
,
?
4 < "³( !
! 8 2 3 8(
+ .! ? 4
! ! 8E ,5 ) = +#³(
% 8 ! 8E % 8E '
- . 0
&1 MX
a, nm
Ref.
NbN
NbC
TiN
TiC
0.439
0.447
0.424
0.433
JCPDS
JCPDS
JCPDS
JCPDS
38 ± 1155
38 ± 1364
38 ± 1420
32 ± 1383
! Structure and features of precipitation
% 8E ! *(
67
! %
) :
! !
/ % 8E 1 6 %(7 % ! 4 Solubility of MX carbides in austenite
,
! 1 G
? H A H
‰8Š‰EŠ~A{
T
H8I 6
HEI7 T $ % H8IHEI ,
1 H $2
% 6 J ) <7
=
‰%Š‰(Š~+:"{
T
")#
:
‰*Š‰(Š~< ##{
T
% !
+ 0 + +# $1 et al." %( H~ <# $2
A~)<+ *( H~" $2 A~<"+ !
! + +# 1 ! % 8 E 8E 8E "
>! 8 E 8E - 1 8E >! 66%z*7 6*z;7 7 ! 6 6%*76(*77
J
! Materials Science and Technology
January 2001 Vol. 17
4 Sourmail Precipitation in creep resistant austenitic stainless steels
+ 0 J *6(*7
:
:
:
6*7‰6(7=K( # z6*7=K* # Š ~
K( ~DG0*(: =RT
K* ~DG 0** : =RT
K 5
DG³ R !
>! 8E - 1
4
' % ' 6(**7 4 - = * )< ' )
8! ( * 8E ! <#
* ! ' - ' ! ,4 @
% G 6,@%G7 8%9% %(
Formation and stoichiometry of
MX precipitates
! ! 5 8 E !
! 8E % 1 $1 et al."
)# -# - 2
- 3. 4 # .. 4" #
2
r%
$ - r~pB'2qA'% p q ) 5 # )5% A' B' 6
Materials Science and Technology
January 2001 Vol. 17
% ! H8IHEI - 1 / 5
et al.= 5! 5 8 E 60 +7 C $ .1 ! *F( *<() 6 + 7
: " *F( ? + +# 7
% 1 $1 et al." 4 ? + ? ! !
! >
! 8 ! ? ? 6!
? < ? )7 4 ? *( ? + +# - !
6 ! 7 *
4 8! 8 E 8E 4
! ! % 8E +
4 <# % 8E 6
) #³(7
8 6% * ; 7 % 8E / ! 8E % 8 8! !
8 ! %
8E
1
! - (
1
5
! - D
% 4 5
/ % / 8E ! !
! ! - D >! ! % L et al. ! 8E
<
Z PHASE
% ' !
!
- ! B1
B1 "+" Sourmail Precipitation in creep resistant austenitic stainless steels
! 6 J )7 ! ! ! Structure and composition
% ' B1 B1?" 6 P4Fnmm7 a~)) c~)" % ( * * (+*+*+ ;L1+ ' )=A*
67' E67c
‰
Š E‰Š
'
c
- 8E ' ! 6 7 J! et
al.+ ! (*6(*7 ! ! %
(*( ! ' 4 5 ' *( Occurrence
% ' ! % ! 8E - ! ++ 4 6see J ) + ++7
1 % ++ 1<
% ' ? J! et al.+ 6 ) $7 + ) * " * == $ 0 8+)(= s % #) $
4 ! ' & 1 J B1++ ! ' #) =+) $ J B1++ ' +( "* ) * + *
³( ³( ' 4 - ) ³( = ;L1+)
' )=A* D = + =#³( + ) " %!
9
+< + < ; ) * <) * # #³( ' 6*;76(*7 L et al.< ! 8E 8E# 6*z;7
>! !
' 5
Considerations on stability of Z phase
- ' >) )< = $
+# 4 ' + +# < * + * F 1
% 1 *(
' ; ! * ( * *( (** C et al.+= ' + 5 % ' 4 *( (** 1
: $
+# *6(*7 + #³( + +# ' 0 ! *0"# ' < #³( 8+)(= 8=( ' *( ! 5 >! J! et al.+ )< 6 + *
(7 )<. 6 + ) *
" * " (7 *( ' *( % Conclusions about Z phase
@
' . 64
7& ! - 4
! ! 1 ! - ' 8E $
+# L et al.< J B1++ % ! ! ! +( * ++ 4
+ % ' ( * * !
5 M23C6
Structure and composition
% 8+)(= (+)(= * 8 0 - & (+* - 6 Fm3m7
! # = - fgc Efg8+) (=
STc EST8+) (=
- 8+)(= Materials Science and Technology
January 2001 Vol. 17
6 Sourmail Precipitation in creep resistant austenitic stainless steels
! Morphologies and locations
% 8+)(= ? - ! 6
7 @
8+)(= MN MN % O1 (
1+
! Precipitation on grain boundaries % 8+)(= !
! : 8+)(= - ! 6) #³( 6J +7 !
- ! MN % 60 )7 8+)(= )
4
1 : 8+)(= Precipitation
on
incoherent
and
coherent
twin
boundaries :
8+)(= 60 <a7 % 8+)(= MN
MN % MN .
. % P !
O1 (
1+ ,1
>! !
! ,
8) 1
4 & 8+)(= ,1
. 7
&.6 -#
3
Materials Science and Technology
January 2001 Vol. 17
1 1 O 6 1 7 ,
)+ * ,
8+)(=
!
- / ? ! 8+)(= 5!
Intragranular precipitation - 8+)(= % !
6see 0 <a7 % % 8+)(= O1 (
1+
! ? 8+)(= % 1 ,
)) .
8+)(= ! 60 <b7 - MN MN % ! !1
Role of other alloying elements
-
8+)(= ( 0 >! ! 0 ++#( 8 8+)(= y)0 )( 8 ++( 6
7 )< <0 =#( 8 ++( % ! ! 8+)(= A >
+ 5 .
et al.)< 8() 0F( 1 ,
8
< 5 )# < 0 8+)(= - !
! - ! / 5
% ! 1 !
/ 6
!& see J )= )7
- ! 5
O 8+)6(O7= % !
Sourmail Precipitation in creep resistant austenitic stainless steels
a
7
b
3
8 7
&.6 a -#
b # -%" Solubility and kinetics of precipitation
% 8+)(=
<
=++
‰(Š ~:{
T
0 # !
+
4 1
- - 1 8+)(= ? + ( (
! 4 8+)(= 4
- !
1 1 % 1 : 1 8+)(= !
<" >!
9
0< ! 8 !
! 8+)(= Relative stability of M23C6
- )< 8+)(= 8=( <+ 8+)(= 8=( 6 )=7 8+)(= 8=( 6see 7& ! 8+)(=
! - 8+)(= 8=( E#(*8)
6( )* #8 677 % et al.<) % !
! 8=( <<
- 0 8+)(= 4 8E %!
9
+<<#<= ! TEMPERATURE °C
!
! 8+)(= % 8+)(= 4
6.0-8& J )7 % - ! ! 8+)(= 6 J )"7 >!
ab initio D 8+)(= G 4 8+)(= - 6 7
CARBON wt-%
*#- # &.6 % #
# &'()')% #
% &.6% &.% 9# % % %
:.*% :& !" -; % 9#
8
Materials Science and Technology
January 2001 Vol. 17
8 Sourmail Precipitation in creep resistant austenitic stainless steels
8+)(= %( *( % @ ,
< 8+)(= )+
$1
et al." + +# % %( 8+)(= : O
A1< )+ ! =³(
4 8+)(= %( A<" ! 8+)(= )+ 6= +" =³(7
:!
! 1 4 8+)(= % 8+)(= 5
5 % *( 8+)(= >! 8+)(= M 6C
% 8=( 1 g 8=( ! g 6A! 7 -
! !
-
!
8! 1 4
6%%.7 Structure and composition
% 8=( ! "# + -
Fd3m 8+)(= @
! Fm3m % g ,
J # % ! % 8=( 660(7+8)(=7 60)*)(7 % 0)8)( 6a~ 7 ! # -
6a~"# 7# %
O et al.#+ )= 1
! 8=(? <#, =#8 % )( #8 +=0 )* 67
,
! 8#,( ! :
8 * % ( - *0" 6 + +# *7 ()*+,(& #) )= % #< 6<==³(7 ! =³( -
1 1 % =+ 6B(.9, ))7 1 8+)(= ! ()*+,( 6see %
<7 #) 6(87)6*07+,(
B
.## 6()*+,*7 +( +#* #8 +* - # ) #³(
5
-
! +# 8 6
7
Occurrence and stability
Mo rich compositions - )= 8=( 60(7+8)(= ,1
# 8+) (= ?60(7+ 8) (= ?8= (
- 8 et al.<< #³( 6 x 7 A 81#= = =#³( O1# "³(
>! ,# )=
! =#³( + = ! 8+)(=
* ! / 8=(
% et al.<) 4 )= ) * "³( =" @!
P1 O B
.#" ! +( +#* <#8 67 ! 8=( >! 8=( ,@%G &
g - g - B
.
#" 8#,* ! - g ! 0 )+ 6 7 8=(
Nb rich compositions - )< 8=( ( 1 .
et
al.= @ 8=( !
>! !
'
- 8 * .* .6 % : ! <: ."
Temperature, ³C
Cr
Mo
Si
Ni
Fe
500
600
35
32
11
15
20
20
24
24
10
10
Materials Science and Technology
January 2001 Vol. 17
6 7
9# &6 - /% - &
et al.6
Sourmail Precipitation in creep resistant austenitic stainless steels
0)*)( ()*+,( 6 *0"7 *=*=,
% 1 ! - 8=( $1
et al." ³( + +# - =
³( 8 et al.<< ! 6y# 7 =³( 6y+ 7 ³(
% 5 0 == %
-
5 ! 6
%
J << )< )* =% ( 677
- + +# ! 8=( @ ! 6 J =+7 4 E - 4
J =) 8=(
+ +# 6) 7 @ 6
< 7
6 )< + +# 7 4 5 ' 4
! 8=(
Cr3Ni2SiX and G phase % @ ! ()*+,( ! ()*+,( ! % ! )= * % #<
! !=< @ !
- + +# !
.
et al.==# G et al.== ! @ ! *( @ - + +# @
()*+,( 1
>! *0" 6J # ! %
7 ()*+,( % 5 ! @ - ! ()*+,( -! 5 ! ! @ ()*+,( g 9
<
67c E67s
6
7 E6<7
c
s
67c E67s
67
E6
7
c
s
% ! 4
!
0 B
.#" 67 s + +#
! <# = ? 6)# <)70 6 7, 6 "78 6+ )+7( 6 =78 6 #7* 0 )= )" 6 !7 <<0 +"+( )8
Occurrence
! s ( *
O1= % 4 6 # ) $7 % ! d 8+)(= ,
! 8+)(= < - ? )< )= 687 )+
6% 7 )< 6* 7 6see J <<7 >! %
+#( +* + s
- 8 et al.<< s ³( )< )+ 6)< s
)+7 - )< )= %
s
4 5 60 7 - %
*F( = < )< % s !
5!
-
)< *( %
!
% )+ Intermetallic phases
s PHASE
% 1 0 ( 0( - !
- - s
Structure and composition
% s 6 P42F
mnm7 a~ c~<#< 60(7 % ) J 7
s #
³ '
) -= :6% .8 :8> - 4?@ <: 88"
Materials Science and Technology
January 2001 Vol. 17
10
Sourmail Precipitation in creep resistant austenitic stainless steels
1 %( 8+)(= % 8+)(= % @ ,
< s + )+ % s + +#
60 7 ; s G
( * % 8 1 s ,
- s (5
d s =
!
et al.= s Å!
! N
! ~:==‰*Šz:‰(Šz+:==‰0Šz<:==‰(z8zŠ
N
z#:==‰;Šz=:==‰'Šz:==‰*Š 6:7
Å ! +#+ s
- !
N
LAVES PHASE
A! ! - - 5 # A! -
! 1
A!
8=(
6see 7
Structure and composition
A! P63Fmmc
a~<) c~+ ! D B
.#" A! + +# # 8 ! %
# % A! 5
- 0+* 0+% 6 7
9 ,
1=" 0+* 670+ * E67c
6
7
E6
7
0+ *
c
Occurrence
- )< A! 8 * % - )= + +# 8 !
8 et al.<< =+# ³( % A 0+8 ! ³( (
A 8
A! =<
³( " ,1
#
A!
)= #³( -
! s x 0 d s x - 0+% ! )+ 8 et al.<< # = #³( )+ >! O >
+ += = ( += * %
#³( % )+ - 0+* 5
0)*)( - )< * # ( =# ³( # << >! !
- %
6 ) * (7
A! +# - *( 6see 0 =7 %
J! et al.+ *( A! )< *
( 6 y=³(7 ' 4 )< ) * " * - *( ' 0+*
x PHASE
% - )= ! #³(
Structure and composition
% x 67 14Å3m % # ! 0)=(+8 % 1 8(
- Occurrence
6 7 ! 5 )+ << x 4 )= 0
8 et al.<< +# #³( A s # #³( # ,# + = =#³(
G PHASE
% @ - 4 O ;) "#= += +=* #( !
6 +) 7 - ! ) + +# >! .
et al.=
" + +#
'
- 0
2 % ! <: 3"
After 10 min at 850³C
After 3000 h at 850³C
Fe
Mo
Cr
Ni
Mn
Si
29¡2
37¡1
36¡2
35¡1
19¡2
12¡1
13¡1
14¡1
1.5¡0.8
y0
1.8¡0.5
0.7¡0.2
Materials Science and Technology
January 2001 Vol. 17
Sourmail Precipitation in creep resistant austenitic stainless steels
# #³( 4 8=( Structure and composition
% @ =9=( 9 ( -; &== 1
9 ==#== <" G et al.== 5 9 6 7 .
et al.=
? #* +"* <, <#0 #( 67
A<" @ )+
! 1
?
=))* +"% ++, )<0 )( 67 * 9 % @ + & = % Fm3m - 1
*=*=, 6see J = =#7 *=%=, 6see
J <" +7 - ,
*=+ + +# +#¡# 4 8=(
! .
et al.= ! @ 4 8=( 1 + +#
! 4 ! == ! 6GGA,7 6 J =7 !
! ,G8 6 J <"7
5 1 5! 6( *7 % !
4 @ Occurrence of G phase in
austenitic stainless steels
Temperature (˚C)
% @ ?
67 ! 6 7
67 + +# 67 )+ 11
Ti rich G phase - 4 @
+ @ += - >! @ , !
+ @ %
1 1 ) @ % @ )+ 5 !<" % ! )+ @ = # =³( %
)+ @ D
>! <<< @ Nb rich G phase - + +# @ 6see J = =# ==7 .
et al.= 1 ,
*=+
9 et al.< !
@ 8=( @ - J =+ +#¡# @ .
et al.= 1 %%. 0 - 6= *
) ( = ,7 @ #
#³( 4 *( ! *( % 5 G et al.== @ + +# ! *( @ % *( ! @ !
! *( % !
@ - + +# ! ! 8=( ()*+,* @
* - + @ #)#< - = @ ! !
!
()*+,( * @
+ Ni3Ti AND RELATED PRECIPITATES
' # 7 et al.6 ''7"
. *)% *)6%
7 ? += #( +#* % % 5 ) c9 * % F Materials Science and Technology
January 2001 Vol. 17
12
Sourmail Precipitation in creep resistant austenitic stainless steels
ALUMINIUM, wt-%
- a~)+ c~+ COPPER PRECIPITATES
A
!
% 8 ) %
)< % % 4
TITANIUM, wt-%
3 , ) ' 9#-# ³ # 0 " 6J #7 >! ! !
!
6see
J =7 0 ! J #
! % ?
67 c9 *)
*)6%
7 )= & *)%
67 g 6a~#" c~)+ 7
5
*)%
67 b *
6
³(7 6 7
Other precipitates
>! Cr2N
% 6+ "³( + *7< - 1 67 a~< c~<<< <
P ' ! J p NITRIDE
% B
.###" + +# + * % #³( 6¡+7, 6¡)78 6<¡7( 6+¡7* 6)¡78 6"¡70 67 -
a~=) ##
TITANIUM CARBOSULPHIDES
% %<(+,+ A<" ! )+ y=³( = #) 8 et al.<< % Materials Science and Technology
January 2001 Vol. 17
CHROMIUM PHOSPHIDES
% (). J
*
" ) . - a~"= c~<## Concluding remarks
! .
! / % 1
% ' ,@%G 1 8%9% %
(
% 1 - 8=( ! g g ,
!
g : ,@%G 0)*)( ()*+,E
% 8E 1
1 ( * * ! *E
! ' %
= ! !! Acknowledgements
% 9 @ *
. P ! > 1 1 . C! ( ! ! . > $ 9 >
O Sourmail Precipitation in creep resistant austenitic stainless steels
13
'
- 6 ## # Precipitate
Structure
Parameters, nm
Composition
NbC
NbN
TiC
TiN
Z phase
M23C6
M 6C
s phase
Laves phase
x phase
G phase
fcc
fcc
fcc
fcc
tetragonal
fcc
diamond cubic
tetragonal
hexagonal
bcc
fcc
a~0.447
a~0.440
a~0.433
a~0.424
a~0.3037, c~0.7391
a~1.057 ± 1.068
a~1.062 ± 1.128
a~0.880, c~0.454
a~0.473, c~0.772
a~0.8807 ± 0.8878
a~1.12
NbC
NbN
TiC
TiN
CrNbN
Cr16Fe5Mo2C6 (e.g.)
(FeCr)21Mo3C, Fe3Nb3C, M5SiC
Fe ± Ni ± Cr ± Mo
Fe2Mo, Fe2Nb
Fe36Cr12Mo10
Ni16Nb6Si7, Ni16Ti6Si7
References
f. b. pickering? 2,
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Materials Science and Technology
January 2001 Vol. 17
14
Sourmail Precipitation in creep resistant austenitic stainless steels
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Materials Science and Technology
January 2001 Vol. 17
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