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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.

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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


  
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Type 304 (Ref. 4) f0.07 y0 f2.00 0.04 17 ± 19 y0 8 ± 10 y0 y0 y0 y0 Bal.


NF709 (Ref. 5) 0.06 0.40 1.00 0.006 20 1. 5 25 0.005 0.167 0.26 0.05 Bal.

Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 3

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301 0.15 1.00 2.00 16 ± 18 ¼ 6±8 ¼ ¼ ¼ ¼ Bal.


302 0.15 1.00 2.00 17 ± 19 ¼ 8 ± 10 ¼ ¼ ¼ ¼ Bal.
304 0.08 1.00 2.00 18 ± 20 ¼ 8 ± 12 ¼ ¼ ¼ ¼ Bal.
310 0.25 1.50 2.00 24 ± 26 ¼ 19 ± 22 ¼ ¼ ¼ ¼ Bal.
316 0.08 1.00 2.00 16 ± 18 2.0 ± 3.0 10 ± 14 ¼ ¼ ¼ ¼ Bal.
321 0.08 1.00 2.00 17 ± 19 ¼ 9 ± 12 ¼ ¼ 56%C min. ¼ Bal.
347 0.08 1.00 2.00 17 ± 19 ¼ 9 ± 13 ¼ 106%C min. ¼ ¼ Bal.
E1250K 0.1 0. 5 6.0 15.0 ¼ 10.0 ¼ ¼ ¼ 0.25 Bal.
20 ± 25 Nb 0.05 1. 0 1.0 20.0 ¼ 25.0 ¼ 0. 7 ¼ ¼ Bal.
A286 0.05 1. 0 1.0 15.0 1.2 26.0 y0.18 ¼ y1.9 y0.25 Bal.

KE1250 is Esshete 1250.

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Materials Science and Technology January 2001 Vol. 17


4 Sourmail Precipitation in creep resistant austenitic stainless steels

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Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 5

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Materials Science and Technology January 2001 Vol. 17


6 Sourmail Precipitation in creep resistant austenitic stainless steels


     
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Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 7

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Materials Science and Technology January 2001 Vol. 17


8 Sourmail Precipitation in creep resistant austenitic stainless steels

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Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 9


  
 

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 ³(  8  et al.<<  ! 
  
6y#  7  =³(   6y+ 7  ³( 67c E6
7s
%   5 

   0 == % %  !   


 
    4
  !
  
          -  
 0  
 B 
. #"   
  
     5      



    67  s  +  +#


         ! 6
%
  
 
   !   <# 
J << 
  )<  )*  =%  = ? 6)#  <)70  6  7,  6  "78  6+  )+7( 
( 677 6  =78  6  #7* 0  )= 
)" 

- +  +#

   ! 8=(  @     6  


  !7 <<0 
 !  
    6  
 J =+7  +"+(  )8

    4  
  E   
 
  
 -  4
  
   
    

 J     =)   8=( Occurrence


 +  +# 

 
  6) 7     !  s       (  *
    @   6

 
   
      O 1= %  
<   7    4    
        
      6 )<  +  +# 
7 
         6   #   
4 5  '        4
  ) $7 
         
    
 
!  8=(   

 %    
  


    !   



    

Cr3Ni2SiX and G phase % @      d    8+)(=   
    ,
    
  
  ! 
   !           

   ( )*+,(   !   8+)(= 
 
< -    
 ( )*+,(  !  
          
 
?  )< )= 687 )+

   %   

   !    6%  


7  )< 6*  
7 6see   

       
  
    J <<7 >!        %
 )=      *  % #< +#(  +* 
         +   s
  ! !=<   @      
  

 
       ! 

 -  
             
- +  +#        
 !   8  et al.<<       s 
.

et al.= =#  G et al.==  !  @       ³(   )<  )+ 6)<    s
  !   * (  

     @    

     )+7 - )< )=  %
 s
 -   
       +  +# 
@      4  5  
    
    
     ( )*+,(  
 60 7 -       %
   
   
 1
  
   * F(   = 
   
>!  *0" 6J #  !  <   )< 
 %  
 

     
%
 7 ( )*+,(    %    s        

 
  
!

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       -
    
   -   
      )<


    
    
        !     * ( 
 
     %

 !
( )*+,(    -!             
 %      )+ 

      5       


        
      

      !   !    @  
   
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Intermetallic phases

s PHASE
%  

1  

       
0  (    0(  - 




    ! 
 -    
    
 -     
 s
     
       
        

   
     



Structure and composition


 7  
   s    
 
# 
% s      
 

6    P42F 


  
 ³ ' 
 )     
mnm7  a~   c~<#<  60( 7 %    -= 
   :6% 
 .8  
 
  


  )  J     


 :8>  
 

  - 4?@ <: 88"

Materials Science and Technology January 2001 Vol. 17


10 Sourmail Precipitation in creep resistant austenitic stainless steels


 
1    
  %(     -    
        0+% 
8+)(= %     8+)(=
      !     
    )+ 

     % 
  @   8  et al.<<          
, 

<      s         #    =  #³(   )+ 

+    )+ % s   
   +  +# >!     O   > 
+   += 
60 7 ;           s  

   = ( += *   %


G
   ( * %  8  1        #³( %   
 
  

s    ,
    
             
   
- 
     s       
)+



      (5
     d   -    
 
 0+*   5
  

  s   = 
         
     !
    et al.=      0)* )(   -       
   s     

     )<   *  # (   

  !     N Å!  =#  ³(     
 ! ~:==‰*Šz:‰(Šz+:==‰0Šz<:==‰( z8zŠ #    << >!       
N
 ! 

    -     
z#:==‰;Šz=:==‰' Šz:==‰* Š 6 :7 %
 6    ) *   (7
Å !     +#+ 

 
   s
-  !
  N      A !        
  +#   -  
 * (   6see 0 =7 %
  
     J  !  et al. +  
LAVES PHASE * (  A !     )< 
  *
A !      !       
   ( 6   y=³(7  
 '   

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      5   
       
    * (  '     

     #    A !     


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1
   A ! x PHASE
    
  

      8=(


6see 
7 %        

   - 
 
    )= 
! #³(
Structure and composition
Structure and composition
A !     
       P63Fmmc
 a~<)   c~+        % x         6 7     
        
!  D     14Å3m %  

  #    


        

   !       


 B 
. #"       
  0)=( +8      
A !    +  +#

  # 8    


   
   %  
  

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     1         8(
 -  
   0+*  0+% 6  
7   - 
         
       
   

  
 
9   ,
1="    0+*  


   
 Occurrence
670+ * E67c 
    6  
7    !  

5   )+ 


<< x    4    
 
6
70+ * E6
7c  )=          0
 
      8  et al.<<    
+#          #³(  
Occurrence A         s  #  #³( 
-  )< 
A !            #     , #  +  
  8 *  % -  )=    =    =#³(


 +  +# 8     


!


  8  et al.<<       
     =+#  ³( %    G PHASE


  A        
 % @    
      
 

 0+8 ! ³( ( 
   A 8   
       -   4    
     A !       =< O   ;  )  "#=   +=  
 
 ³(      "    ,1
 #       +=*  #(

  ! 

  

        A ! 6  +) 7   
  -  

     )=       #³( -  
!    
      
  
      !       s  )     +  +# 
 >! .

et al.=
x   0  
     d   
    "        
  +  +#
            s  x      


      

'
-        0
2 
%  ! <: 3"
Fe Mo Cr Ni Mn Si

After 10 min at 850³C 29¡2 36¡2 19¡2 13¡1 1.5¡0.8 1.8¡0.5


After 3000 h at 850³C 37¡1 35¡1 12¡1 14¡1 y0 0.7¡0.2

Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 11

#  #³(         4  Ti rich G phase -    4    @
8=(  
      
   +     @       
+=  
 -   
     
              
Structure and composition   
    >! @     
% @     
 
=9=(       

   
  , 
9    
  (    -; 
&==         !
   
 

 1
 9  

  = =# ==        


   +  
 <" G et al.==    
 
        @   %
   

5   9 6     1


 
 
     
 7        .

et al.=   
1      )     @  
    

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<#0  #( 67 % 
        @    
A <"      @     )+ )+ 
 5 !<" %   !  )+ 


 !   
   1
?  @    =   #    =³( %
=))*  +"%  ++,  )<0  )( 67 *            )+ 
    
    

        @        

  D
9           
              
% @         
       >!  
 
 + &       =   << <     @  
 

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Nb rich G phase - +  +#     
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J <"  +7 -  
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6see J = =#  ==7  

  


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et al.=   1  ,


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@     4  8=(  
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+#¡#     
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    4  
!   
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et al.=     1  %%.   


!         
   

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  6GGA,7 6   J =7   !

) ( = ,7 @      #
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 5  1 
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* (  
  ! 
   * (  
  
 
 
 6( *7 %   !
    %            
4      

  @  
    5  
     

Occurrence of G phase in G et al. ==       @   
austenitic stainless steels 
+  +#    
 
   


% 
    @      ?  
 
      
67    !    
      
!  
  * (      @  
6   7 %            
 
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       +  +#       
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!    

              
67   
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-    +    
 
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    #) #< -   

   =  
       
Temperature (˚C)

        @    ! !


       ! 

    ( )*+,( * 
     
          @
        + 


Ni3Ti AND RELATED PRECIPITATES


.     *)%  *)6% 
7  
  
 

    
 
?    
     

     
+= #(  +#*  
 % 
 % 
  
  
  5    



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#   
  ''7" 

      )    
  
7 et al.6        c9   * % F 
   

Materials Science and Technology January 2001 Vol. 17


12 Sourmail Precipitation in creep resistant austenitic stainless steels

    
     -    
   
   a~)+  
c~+ 
ALUMINIUM, wt-%

COPPER PRECIPITATES
A
    ! 

       
      
 
 %  
8   )    %
 


 )<     

 
  % 
       
  
         
%        4 
    
     


TITANIUM, wt-%
CHROMIUM PHOSPHIDES
%    ( ).      
3 ,   )
 '  9# - # 
 
 J
  *
"      

³    
#    ) . -    
 


a~"=   c~<## 
   0 " 6J #7 >!    !  
           
  !
 
        ! 

 6see
  
 J =7 0       Concluding remarks
     
    !  J #
         !              !     
 % ?           
 
 
67 c9    *)
 *)6% 
7  

  
       .  
 
   )= &  
        
 
  ! 
       *)%   
 /     
   
67 g    
6a~#"  c~)+ 7      
 

    

   5
      *)%     
          
67 b   *
  
    6          
 
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 %      1
      
    
     

  
      
Other precipitates % '    
  

    
       
 
    
              ,@%G    
    
           
   

  1    8%9%  % 

 >!        (
 % 1      
    
  

 
 -    
  8=(     
      !         
      
   g   
Cr2N     g    
 ,

   
%     
   
 
    
 ! 

   
   
  
     6+   "³(  g    :        
+ *7< -    

  1 67   ,@%G    
 0)* )(  ( )*+,E



    a~<   c~<<< < %     8E     



  P                    

 
 
           
 
     
1
      
 
       
 
  1         (  * 
   
       
 *  
 
   !     * E
        '           

  !     
  

   
 !          '  
  J  %
 = !  ! !       
           
 
 
p NITRIDE        
%     B 
. ## #"     
 
 +  +# 
 + * % 
    #³(  6¡+7,  6¡)78  Acknowledgements
6<¡7(  6+¡7*  6)¡78  6"¡70 67 -
       
   a~=) ##
%    
 9 @  * 
. 
   P   
   !   
TITANIUM CARBOSULPHIDES > 


1   1 .   
  
%    
 %<(+,+     A <"  C!   (      ! 
  
!   )+ 
   y=³(     
    ! .  > $ 9 >
=   #)     8  et al.<<  
O          


 %
          
  

Materials Science and Technology January 2001 Vol. 17


Sourmail Precipitation in creep resistant austenitic stainless steels 13

'
-  6 
# #
     
   
 
#  
   
Precipitate Structure Parameters, nm Composition

NbC fcc a~0.447 NbC


NbN fcc a~0.440 NbN
TiC fcc a~0.433 TiC
TiN fcc a~0.424 TiN
Z phase tetragonal a~0.3037, c~0.7391 CrNbN
M23C6 fcc a~1.057 ± 1.068 Cr16Fe5Mo2C6 (e.g.)
M 6C diamond cubic a~1.062 ± 1.128 (FeCr)21Mo3C, Fe3Nb3C, M5SiC
s phase tetragonal a~0.880, c~0.454 Fe ± Ni ± Cr ± Mo
Laves phase hexagonal a~0.473, c~0.772 Fe2Mo, Fe2Nb
x phase bcc a~0.8807 ± 0.8878 Fe36Cr12Mo10
G phase fcc a~1.12 Ni16Nb6Si7, Ni16Ti6Si7

) h. tanaka m. murata f. abe  k. yagi? Mater. Sci. Eng. A


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) l. k. singhal  j. w. martin? Acta Metall. "= 15 =) 
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 p. rios? Mater. Sci. Eng. A "" A142   "< #
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=#    
 

3   @    ""


) h. hughes? J. Iron Steel Inst. "= 205 #   ##  =& "" :   .  
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15 +)=#  +)=  
 
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  >  $7   "&


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 . %8,-8G
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 s. r. keown  f. b. pickering?  2(     
 # h. h. stadelmaier?  29!
    
 
  

3 )<  <)& "< A % 8


 

  3 <  & "=" * R 1 .


 . 
, # b. weiss  r. stickler? Metall. Trans. "+ 3 #  ==
 j. m. adamson  j. w. martin? J. Iron Steel Inst. "+ 210 #+ g. brun j. l. naour  m. vouillon? J. Nucl. Mater. "
+  +# 101 "  +)
" d. h. jack  k. h. jack? J. Iron Steel Inst. "+ 210 "  #) t. m. williams?  2, 
 
 <3 <)  <+& "# A
"+ % -  8

+ v. vodLrek? Metall. Mater. "" 25 #<"  ##+ #< j. m. titchmarsh  t. m. williams?  2Q  !
+ a. raghavan c. f. klein  c. n. marzinsky? Metall. Trans.   
    

3 6 @  A 
A ""+ 23A +<##  +<= et al.7 ++)  ++& " A % -  8

++ p. w. robinson  d. h. jack? 2* !
   
 ## r. f. a. jargelius-petterson? Scr. Metall. Mater. "") 28


3 6 J A
7   =& "# 8
 . 1 :> )""  <)
   ,  8
 #= j. k. l. lai  m. meshkat? Met. Sci. " 12 <#  <+
+) v. vodLrek?  2
    
 
 3"+3 6 > # j. barcik? Metall. Trans. A ") 14A =)#  =<
*     B OPS 1
7 ;
  +)  )+& ""+ 8  
 # l. p. stoter? J. Mater. Sci. " 16 )"  #
. 1 :> ,8 -  
 #" r. f. a. jargelius-petterson? Z. Metallkd. "" 79   )
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" " 36 )  +<
+# g. knowles? Met. Sci. " 11   ++ = y. minami h. kimura  m. tanimura?  2* !

+= h. uno a. kimura  t. misawa? Corrosion ""+ 2 <=    
 

3 6 J A
7 +)  +<+& "#
<< 8
 . 1 :>    ,  8

+ f. r. beckitt  b. r. clarck? Acta Metall. "= 15 )  =+ r. sumerling  j. nutting? J. Iron Steel Inst. "=# 203
+" )"  <#
+ m. h. lewis  b. hattersley? Acta Metall. "=# 13 #"  =) v. ramaswamy  d. r. f. west? J. Iron Steel Inst. " 208
= )"  )"<
+" t. sourmail  h. k. d. h. bhadeshia? C
  1 =< t. m. williams  j. m. titchmarsh? J. Nucl. Mater. " 98
C!   (   C$ ++)  ++=

Materials Science and Technology January 2001 Vol. 17


14 Sourmail Precipitation in creep resistant austenitic stainless steels

=# d. j. powell r. pilkington  d. a. miller?  2, 


 # f. b. pickering?  2% 

 
!
   


 <3 )+  )"& "# A % -  8
 
3 6 0 O .1 7 )"  <& A "" %
== r. c. ecob r. c. lobb  v. l. kohler? J. Mater. Sci. " 22 8
 ,
+=  + = d. v. v. satyanarayana m. c. pandey  d. m. r. taplin?
= j. barcik? Mater. Sci. Technol. " 4 #  # Trans. Indian Inst. Met. ""= 49 <"  <+)
= l. r. woodyatt c. t. sims  h. j. beattie? Trans. AIME  e. j. dulis?  2% 

 
!
   
 
3
"== 236 #" 6 0 O .1 7 <+  <<& "" A % 8

=" a. w. denham  j. m. silcock? J. Iron Steel Inst. "=" 207 ,
##  #"+  a. tohyama  y. minami?  2!      

 j. k. l. lai? Mater. Sci. Eng. ") 58 "#  +"    3 6 J ;     B *7
 w. e. white  i. le may? Metallography " 3 #  = <"<  #=& """ A -8 (  A
+ h. j. beattie  w. c. hagel? J. Met. "# "  " " a. f. rowcliffe  r. b. nicholson? Acta Metall. "+ 20
) h. j. beattie  f. l. versnyder? Nature "#= 178 + <)  ##
< r. a. p. dewey g. summer  i. s. brammar? J. Iron Steel Inst.
"=# 203 ")  "<<

Materials Science and Technology January 2001 Vol. 17