Morphology of Y' and Y" Precipitates and

Thermal Stability of Inconel 718 Type Alloys

R. COZAR AND A. PINEAU

The p r e c i p i t a t i o n of the 7 ' (L12) and V" (DO22) p h a s e s has been s t u d i e d in four a l l o y s
F e - N i - C r - T i - A 1 - N b containing a h i g h e r T i + A1/Nb r a t i o than that of the INCONEL 718 a l l o y .
F o r t h e s e a l l o y s , the p r e c i p i t a t i o n m i c r o s t r u c t u r e v a r i e s r a p i d l y with aging t e m p e r a t u r e
and c o m p o s i t i o n . Bet V " p a r t i c l e s have a l w a y s been found to p r e c i p i t a t e on V' p h a s e . M o r e -
o v e r , by aging t h r e e a l l o y s above a c r i t i c a l t e m p e r a t u r e , a " c o m p a c t m o r p h o l o g y " has been
o b s e r v e d : c u b e - s h a p e d 7 ' p a r t i c l e s c o a t e d on t h e i r s i x f a c e s with a s h e l l of V " p r e c i p i t a t e .
T h i s m i c r o s t r u c t u r e has p r o v e d to be v e r y s t a b l e on p r o l o n g e d a g i n g . A t h e r m a l s t a b i l i t y
b e t t e r than that e n c o u n t e r e d in n o m i n a l INCONEL 718 a l l o y can thus be a c h i e v e d . The i n f l u -
ence of c o m p o s i t i o n and aging t e m p e r a t u r e on the conditions that b r i n g about this " c o m p a c t
m o r p h o l o g y " has b e e n i n v e s t i g a t e d . A m i n i m a l T i + A1/Nb r a t i o b e t w e e n 0.9 and 1 has b e e n
d e t e r m i n e d , allowing the " c o m p a c t m o r p h o l o g y " to be o b t a i n e d .

N I C K E L - b a s e a l l o y s containing t i t a n i u m and a l u m i - T i + A1/Nb r a t i o m a y f a v o r 7 ' r a t h e r than 7 " p r e c i p i -

num a r e u s u a l l y s t r e n g t h e n e d by p r e c i p i t a t i o n of v'
p h a s e (fcc L12 s t r u c t u r e ) . The d e v e l o p m e n t o f I N C O N E L
718 and s i m i l a r a l l o y s has p r o m p t e d i n t e r e s t in the
p r e c i p i t a t i o n r e a c t i o n which o c c u r s when t i t a n i u m and
a l u m i n u m a r e p a r t i a l l y or c o m p l e t e l y exchanged with
niobium.
P h a s e i d e n t i f i c a t i o n has b e e n r e p o r t e d by P a u l o n i s
et al. (I) in INCONEL 718 containing 5 p c t Nb and
s m a l l a d d i t i o n s of t i t a n i u m ( - 1 pct) and a l u m i n u m
(---0.55 pct). The p r i m a r y s t r e n g t h e n i n g p h a s e has
b e e n i d e n t i f i e d a s y~ (bct DO22 s t r u c t u r e ) . The ~" p r e -
c i p i t a t e s a p p e a r a s c o h e r e n t d i s c - s h a p e d p a r t i c l e s and
with the following o r i e n t a t i o n r e l a t i o n s h i p s :
(001)7" II {001}7 and [10017" II (100)7
T h e s e w o r k e r s a l s o found a s m a l l quantity of s p h e r i -
c a l y ' p a r t i c l e s in this a l l o y . With the h e a t t r e a t m e n t
c o n d i t i o n s that they u s e d , V' and V" w e r e g e n e r a l l y
found to be f o r m e d a t r a n d o m with r e s p e c t to e a c h
o t h e r : v e r y few V" p a r t i c l e s w e r e s e e n in c o n t a c t with
V' p r e c i p i t a t e s . M o r e o v e r , the a c t u a l p r e c i p i t a t i o n
s e q u e n c e d u r i n g i n i t i a l aging was not c l e a r and it w a s
not shown w h e t h e r V' and V" a p p e a r s i m u l t a n e o u s l y or
s e q u e n t i a l l y in this a l l o y . F i n a l l y , in studying the
t h e r m a l s t a b i l i t y of INCONEL 718, t h e s e a u t h o r s have
shown that the p r i n c i p a l c a u s e s of o v e r a g i n g a t t e m -
p e r a t u r e s n e a r 760~ w e r e the r a p i d V" c o a r s e n i n g and
the p a r t i a l solution of V" and 7 ' with c o n c u r r e n t f o r m a -
tion of the s t a b l e o r t h o r h o m b i c ~-Ni3Nb p h a s e .
In studying a l l o y s with a b a s e c o m p o s i t i o n of Ni-25
F e - 1 6 C r , K i r m a n and W a r r i n g t o n 2 have shown [hat
both the y ' and y " p h a s e s a r e found when 1.8 T i and
3.5 Nb a r e a d d e d , but when e i t h e r 6 Nb or 3.5 T i a r e
a d d e d to the b a s e c o m p o s i t i o n , only one p h a s e can be
obtained i.e. V" or y ' , r e s p e c t i v e l y . A s t i t a n i u m and
a l u m i n u m a r e both known to p r o d u c e the p h a s e V',
t h e s e o b s e r v a t i o n s s u g g e s t that the i n c r e a s e in
R. COZAR and A. PINEAU are with the Centre des Mat6riaux de
L'Ecole des Mines de Paris, Corbeil Essonnes, France. This paper is
based upon a thesis submitted by R. COZAR in partial fulfillment of
the requirements of the degree of Doctor of Philosophy at the Uni-
versity of Nancy.
Manuscript submitted May 15, 1972.
tation.
The p r e s e n t study r e p o r t s r e s u l t s on an i n c r e a s e in
t h e r m a l s t a b i l i t y of INCONEL 718 type a l l o y s a c h i e v e d
by a c l o s e c o n t r o l of the m o r p h o l o g y of c o m p o s i t e V"
onto y ' p r e c i p i t a t e s , The T i + A1/Nb r a t i o w a s i n -
c r e a s e d with r e s p e c t to that of INCONEL 718 a l l o y .
The a c t u a l p r e c i p i t a t i o n s e q u e n c e d u r i n g i n i t i a l and
s u b s e q u e n t aging u n d e r v a r i o u s t h e r m a l c o n d i t i o n s
was t h o r o u g h l y i n v e s t i g a t e d .
E X P E R I M E N T A L PROCEDURE
I) M a t e r i a l s - - P r e p a r a t i o n and Heat T r e a t m e n t
The a l l o y c o m p o s i t i o n s a r e given in T a b l e I along
with the c o m p o s i t i o n of the s t a n d a r d INCONEL 718.
The T i + A1/Nb r a t i o i n c r e a s e s f r o m a l l o y 1 to 4. The
r a t i o T i / A 1 is g e n e r a l l y s l i g h t l y l o w e r and the r a t i o
T i + A1/~Nb h i g h e r than for the b a s i c a l l o y . The m o l y -
b d e n u m content in a l l o y s 1 and 2 is s i m i l a r to that in
INCONEL 718, while in a l l o y s 3 and 4 it h a s b e e n i n -
c r e a s e d up to 7 p c t in o r d e r to i m p r o v e the s o l i d s o l u -
tion h a r d e n i n g . B e s i d e s the e l e m e n t s given in T a b l e I,
t h e s e a l l o y s c o n t a i n 0, 10 wt p c t Si and about 500 p p m
C.
A l l o y ingots of a p p r o x i m a t e l y 10 kg w e r e p r e p a r e d
by induction m e l t i n g u n d e r v a c u u m f r o m m e t a l s of
e l e c t r o l y t i c p u r i t y . A f t e r about 80 p c t r e d u c t i o n of
a r e a by hot f o r g i n g , b a r s of 30 m m s q u a r e s e c t i o n
w e r e obtained. T h e y w e r e h o m o g e n i z e d for 48 h a t
1200~ in an a r g o n a t m o s p h e r e . S p e c i m e n s of 8 by 8
by 10 m m w e r e then cut f r o m t h e s e b a r s .
A f t e r m a c h i n i n g , a l l the s p e c i m e n s w e r e s e a l e d in
v y c o r c a p s u l e s f i l l e d with h e l i u m , given an a n n e a l i n g
t r e a t m e n t of 30 min a t 1200~ then w a t e r quenched.
T h e s p e c i m e n s w e r e then a g e d at s e v e r a l t e m p e r a -
t u r e s between 650 ~ and 820~ u n d e r v a c u u m in v y c o r
c a p s u l e s . A f t e r a g i n g , they w e r e w a t e r quenched and
t h e i r V i c k e r s h a r d n e s s w a s u s u a l l y m e a s u r e d with a
20 kg load e x c e p t when o t h e r w i s e s t a t e d . T h e t h e r m a l
s t a b i l i t y of a l l o y s 1, 2, 3 w a s i n v e s t i g a t e d by aging
s a m p l e s a t 750~ up to 524 h and c o m p a r i n g our r e -
s u l t s with t h o s e obtained in the n o m i n a l INCONEL 718
alloy.4

METALLURGICAL TRANSACTIONS VOLUME 4, JANUARY 1973-47

 Table I. Chemical Composition of Alloys

Wt Pct
Alloy Ni Cr Fe Mo Ti AI Nb Ti/A1 Ti + AI/Nb Ti + AI + Nb

Inconel 718 52.4 19 19 3 0.8 0.6 5.2 0.75 0.69 5.51

1 52.51 18.16 19.5 2.96 0.82 0.70 5.18 0.65 0.77 5.74
2 51.98 18.59 21 2.85 0.72 0.63 3.99 0.65 0.89 4.71
3 51.98 18.97 17 7.03 0.59 0.63 3.41 0.53 0.97 4.24
4 52.09 18.90 16.4 7.00 0.90 0.74 3.85 0.68 1.11 5.14

The contents have been expressed in atomic pct to calculate the two ratios and the sum.

2) M e t a l l o g r a p h y X - R a y and E l e c t r o n
Microscope Observations I00

T h e m i c r o s t r u c t u r a l c h a n g e s o c c u r r i n g d u r i n g aging 400,f
w e r e p r i m a r i l y o b s e r v e d by t r a n s m i s s i o n e l e c t r o n
m i c r o s c o p y with a P h i l i p s EM 300 E l e c t r o n M i c r o -
s c o p e . Thin f o i l s w e r e p r e p a r e d by e l e c t r o c h e m i c a l //-.+..o A 700"C 300
thinning a t 0~ in a bath containing 10 p c t P e r c h l o r i c
a c i d in e t h a n o l and u n d e r a p o t e n t i a l of 15 V. P h a s e -.r ~~/650"C .+~+-t~-~++~7+o'c
i d e n t i f i c a t i o n w a s m a i n l y c a r r i e d out u s i n g e l e c t r o n
d i f f r a c t i o n and d a r k field t e c h n i q u e s with the [001]
a x i s of the m a t r i x p a r a l l e l to the e l e c t r o n b e a m . D i f -
f e r e n t i a t i o n b e t w e e n 7 ' and ~" is e a s i l y a c h i e v e d with I
> 2OO 200

this o r i e n t a t i o n a s shown by P a u l o n i s et al. (I).

T h e weight p e r c e n t a g e of p r e c i p i t a t e s w a s m e a s u r e d Alloy 2 Alloy 3
a f t e r anodic m a t r i x d i s s o l u t i o n . An e l e c t r o l y t i c b a t h
(1 p c t t a r t a r i c a c i d + 1 p c t a m m o n i u m s u l f a t e + w a t e r ) 100'0.5 2 8 32 128 5t2 0.5 2 8 32 128 512
700
with 2.5 V p o t e n t i a l w a s u s e d . 3 T h i s s o l u t i o n a l s o Aging Time, hours
p r o v e d to be a s a t i s f a c t o r y e t c h a n t to p r e p a r e e x t r a c -
Fig. 1--Hardness curves of alloys 2 and 3.
tion c a r b o n r e p l i c a s of p r e c i p i t a t e s .
T h e l a t t i c e p a r a m e t e r s of ~ ' and ~ " p a r t i c i e s w e r e
d e t e r m i n e d on t h e s e r e p l i c a s u s i n g the high r e s o l u t i o n
a t t a c h m e n t of the P h i l i p s EM 300 E l e c t r o n M i c r o s c o p e .
400

~,~j~
A thin f i l m of t h a l l i u m c h l o r i d e w a s v a p o r i z e d u n d e r lnconel 718 [4]
v a c u u m o v e r the r e p l i c a containing the p r e c i p i t a t e s
and u s e d a s a s t a n d a r d ; The m a t r i x l a t t i c e p a r a m e t e r
~ ~
w a s m e a s u r e d by X - R a y d i f f r a c t i o n on bulk s p e c i -
m e n s . The b a c k r e f l e c t i o n c a m e r a technique w a s u s e d /~,.'~X,+~+x ~ o Alloy 1
with a high p u r i t y a l u m i n u m s t a n d a r d .
30(J /~ / " \+x~. +Alloy
ffl 4'/+ /zr"---'ATt,--Z - Alloy 3
RESULTS r-
1) H a r d n e s s C u r v e s "1-

H a r d n e s s v a r i a t i o n s of a l l o y s 2 and 3 a f t e r aging O
a t 650 ~ 700 ~ and 750~ a r e shown in F i g . 1. The
>
3: 200 /
r e l a t i v e l y slow aging r e s p o n s e is t y p i c a l of t h e s e
c o m p o s i t i o n s .4 It is to be noted that h a r d n e s s p e a k s
a r e obtained with a l l o y 2 a t 700 ~ and 750~ but not o
with a l l o y 3 aged a t the s a m e t e m p e r a t u r e s . T h i s
b e t t e r t h e r m a l s t a b i l i t y of a l l o y 3 is shown in F i g . 2,
on which the h a r d e n i n g of a l l o y s 1, 2, 3 up to 524 h a t
750~ can b e c o m p a r e d with that of INCONEL 718 a g e d
a t the s a m e t e m p e r a t u r e . The m a x i m u m h a r d n e s s
v a l u e s obtained a r e l o w e r f o r a l l o y s 2 and 3 than for
,0J 0.5
Aging Time, hours
2
Aging Temperature: 750~

8 32 128 512

INCONEL 718. T h i s b e h a v i o r is m a i n l y due to the
s m a l l e r a m o u n t of p r e c i p i t a t e d p a r t i c l e s s i n c e the
T i + A1 + Nb content i s l o w e r for a l l o y s 2 and 3 than
f o r the b a s i c a l l o y . The weight p e r c e n t a g e of p r e c i p i -
t a t e s c o n t a i n e d in a l l o y s 2 and 3 aged at 750~ for 17 h
h a s b e e n m e a s u r e d . V a l u e s of 11.5 and 8 p c t have b e e n
d e t e r m i n e d , r e s p e c t i v e l y . T h e r e p o r t e d value p r e c i p i -
t a t e d in INCONEL 718 is 15 p c t . 1
Fig. 2--Comparison between hardness curves of alloys
INCONEL 718,1, 2, and 3 aged at 750~
2) P h a s e I d e n t i f i c a t i o n and P r e c i p i t a t e M i c r o s t r u c t u r e
2.1) ANNEALED ALLOYS
The high a n n e a l i n g t e m p e r a t u r e a l l o w s a g r a i n s i z e
of about 300 ~ m and c o m p l e t e d i s s o l u t i o n of a l l the

4 8 - V O L U M E 4, J A N U A R Y 1973 METALLURGICAL TRANSACTIONS

i n t e r m e t a l l i c compounds to be achieved. However there for 30 min up to 524 h. The m i c r o s t r u c t u r e observed
r e m a i n l a r g e inclusions (d - 3 ~m) which have been after aging at 700~ for 524 h is shown in Fig. 3. The
identified as TiC by X-Ray and m i c r o p r o b e a n a l y s i s . b r i g h t field m i c r o g r a p h suggests that two types of c o -
h e r e n t p a r t i c l e s have p r e c i p i t a t e d , F i g . 3(a). The d i f -
2.2) INTERMETALLIC 7' AND 7" PRECIPITATION
DURING ISOTHERMAL AGING TREATMENTS
Aging at 650 ~ 700~ Alloys 2 and 3 show a s i m i l a r
p r e c i p i t a t e morphology a f t e r aging at 650 ~ and 700~

(c)

(b)
Fig. 3 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s of alloys 2 and 3
aged at 700~ for 524 h. Alloy 2: (a) b r i g h t field image,
(b) diffraction p a t t e r n , (c) d a r k field image using spot 1 of
the diffraction p a t t e r n , (d) alloy 3, d a r k field image. (d)

METALLURGICAL TRANSACTIONS VOLUME4, JANUARY 1973-49

 Fig. 4--Dark field electron micrographs of (a) alloy 1 aged at 750~ for 128 h and (b) alloy 2 aged at 750~ for 152 h.
f r a c t i o n p a t t e r n , F i g . 3(b), and the d a r k field a n a l y s i s ,
F i g . 3(c), a r e a l s o r e p r o d u c e d . T h i s technique u s e d
p r e v i o u s l y by P a u l o n i s et al. (I) a l l o w s the u n a m b i g u o u s
i d e n t i f i c a t i o n of 7 ' and Y" p a r t i c l e s when the zone a x i s
of the m a t r i x is [001]. With this o r i e n t a t i o n the d i f -
f r a c t i o n p a t t e r n shows s u p e r l a t t i c e r e f l e c t i o n s b e l o n g -
ing to 7 ' and 7" p r e c i p i t a t e s . T h u s , the spot l a b e l l e d
1 on F i g . 3(b) is c o m p o s e d of a point which is a {100} v'
r e f l e c t i o n and a s t r e a k which i s a (002)7" r e f l e c t i o n .
A d a r k f i e l d m i c r o g r a p h using this s p o t shows a l l the
~ ' p r e c i p i t a t e s and only one of the two s y s t e m s of y "
p a r t i c l e s s e e n on edge on the b r i g h t field m i c r o g r a p h
of F i g . 3(a). T h e following t r a n s m i s s i o n e l e c t r o n
m i c r o g r a p h s showing the 7 ' and 7 " m o r p h o l o g i e s have
a l w a y s b e e n taken with a [001] v zone a x i s and in a l l
the d a r k f i e l d i m a g e s such a s p o t a s 1 on F i g . 3(b) was
used.
The b c t DO22 p a r t i c l e s have a d i s c - s h a p e d m o r p h o l -
ogy with the "~ a x i s n o r m a l to the plane of the d i s c .
The ~ " p a r t i c l e s a r e a l w a y s s e e n a d j a c e n t to the 7 '
p r e c i p i t a t e s . The m o s t t y p i c a l m o r p h o l o g i e s p r o d u c e d
in a c o m b i n e d 7 ' / 7 " p r e c i p i t a t e a r e d r a w n s c h e m a t i c -
a l l y on F i g . 17(c). Two p e r p e n d i c u l a r 7 ~ p a r u c l e s
a d j a c e n t to the s a m e 7 ' p r e c i p i t a t e s a r e s e l d o m o b -
served.
Aging at 750~ A f t e r aging at 750~ the m i c r o -
s t r u c t u r e s obtained in a l l o y s 1 and 2 is quite d i f f e r e n t
f r o m the one obtained in a l l o y 3. In a l l o y s 1 and 2 the
m o r p h o l o g y of ~ ' and 7 ~ p a r t i c l e s is s i m i l a r to that
o b s e r v e d at l o w e r t e m p e r a t u r e s , F i g . 4. The m i c r o -
s t r u c t u r e s of a l l o y 3 a f t e r aging at 750~ for 2, 4, 8,
and 64 h a r e shown in F i g . 5.
A f t e r aging for 2 h, only c u b e - s h a p e d ~ ' p a r t i c l e s
can be i d e n t i f i e d , F i g . 5(a). The p r e c i p i t a t e f a c e s a r e
p a r a l l e l to {001~v. A f t e r aging for 4 h a few y " p a r t i -
c l e s f o r m i n g on the ~ ' p r e c i p i t a t e s a p p e a r (see e.g. A
on F i g . 5(b)). A f t e r aging for 8 h, F i g s . 5(c) and (d),
n e a r l y a l l the y ' p a r t i c l e s have t h e i r s i x f a c e s c o a t e d
with a s h e l l of y " w h i c h can be s e e n for e x a m p l e a f t e r
aging f o r 64 h, F i g s . 5(e) and (f). T h i s m o r p h o l o g y
w i l l be r e f e r r e d to a s c o m p a c t .
T h i s c o m p a c t m o r p h o l o g y h a s p r o v e d to be v e r y
s t a b l e d u r i n g f u r t h e r aging at 750~ F i g s . 6(a) and (b).
50-VOLUME 4, JANUARY 1973
F o r c o m p a r i s o n , the m i c r o s t r u c t u r e s of a l l o y s 1 and 2
a g e d in the s a m e conditions a r e shown on F i g s . 6(c) and
6(d). In a l l o y s 1 and 2, the y ' and 7 " p a r t i c l e s , which
are initially adjacent, gradually separate as their sizes
i n c r e a s e and the 7" p r e c i p i t a t e s have a growing
t e n d e n c y to a l i g n in (001} 7 d i r e c t i o n s . T h e s e m i c r o -
s t r u c t u r a l o b s e r v a t i o n s a r e in a g r e e m e n t with the l o s s
of s t r e n g t h shown in a l l o y s 1 and 2, F i g . 2. On the
o t h e r hand, in a l l o y 3, b e t w e e n 8 h and 524 h, the s i z e
of the p a r t i c l e s i n c r e a s e s only s l i g h t l y .
T h e k i n e t i c s of Y' and Y" c o a r s e n i n g a t 750~ was
d e t e r m i n e d in a l l o y s 2 and 3. The s i z e v a r i a t i o n s of the
7 ' and y " p a r t i c l e s a r e shown on F i g . 7. The m e a s u r e d
d i m e n s i o n s L a r e s c h e m a t i c a l l y i n d i c a t e d on this s a m e
f i g u r e . In a l l o y 3, the i n i t i a l c o a r s e n i n g of the 7 ' p a r -
t i c l e s o c c u r s r e l a t i v e l y r a p i d l y . A s i z e of about 300A
is r e a c h e d a f t e r an aging t i m e of 4 h. V" p r e c i p i t a t i o n
with the c o m p a c t m o r p h o l o g y then s l o w s down the
g r o w t h of 7 ' p r e c i p i t a t e s . In a l l o y 2, the n e a r l y c o n -
c u r r e n t 7 ' and y" p r e c i p i t a t i o n a t the beginning of the
aging t r e a t m e n t r e s u l t s in s m a l l e r L v a l u e s . F o r
l o n g e r aging t i m e s , p a r t i c l e s f o r m e d bv a s i n g l e v "
d i s c a d j a c e n t to a ~ p r e c i p i t a t e c o a r s e n m o r e r a p i d l y .
The p e r i p h e r y of ? " p r e c i p i t a t e s in f a c t , has a t e n d e n c y
to g r o w beyond the 7 ' p r e c i p i t a t e s on which they w e r e
f i r s t l o c a t e d . D i f f e r e n t L v a l u e s a r e then obtained for
7 ' and y " ~ r e c i p i t a t e s , and s o m e 7 " p a r t i c l e s up to m o r e
than 3000A a r e s e e n a f t e r an aging for 524 h.
Aging at Temperatures Higher than 750~ The four
a l l o y s w e r e aged at h i g h e r t e m p e r a t u r e s to s e e w h e t h e r
the c o m p a c t m o r p h o l o g y o b s e r v e d in a l l o y 3 at 750~
could be obtained. The m a x i m u m t e m p e r a t u r e s (TM)
s t u d i e d for e a c h a l l o y a r e t h o s e at which 7 ' and 7" p r e -
c i p i t a t e s a r e s e e n to be p r e c i p i t a t e d uniquely on d i s -
l o c a t i o n s . T h e s e t e m p e r a t u r e s , and a l l the d a t a of
F i g . 8, have b e e n d e t e r m i n e d by m e a n s of e l e c t r o n
microscope observations.
In o r d e r to d e t e r m i n e w h e t h e r the c o m p a c t m o r p h -
ology was only f o r m e d when s i n g l e ~ ' p a r t i c l e s of a
c r i t i c a l s i z e L w e r e p r e c i p i t a t e d , the T T T c u r v e c o r -
r e s p o n d i n g to the beginning of Y" p r e c i p i t a t i o n was
d e t e r m i n e d f o r e a c h a l l o y , F i g . 8. On this f i g u r e , the
m e a n s i z e s of s i n g l e c u b e - s h a p e d 7' p a r t i c l e s p r e c i p i -
METALLURGICAL TRANSACTIONS
 ~a) (b)

(c) ~)

(c) (~

Fig. 5 - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s of alloy 3 aged at 750~ for (a)2 h (dark field image), (b) 4 h (dark field image),
(c) and (d) 8 h [(c) b r i g h t field image and (d) d a r k field image] (e) and (f) 64 h [(e) b r i g h t field image and (f) d a r k field image].

METALLURGICAL TRANSACTIONS VOLUME 4, JANUARY 1973-51

 (a) (b)

(c) (d)
Fig. 6-Comparison between the mierostructures of alloys 1, 2, 3 aged at 750~ for 524 h. Alloy 3 (a): bright field image,
(b): dark field image. Alloy 1 (c): dark field image. Alloy 2 (d): dark field image.

tared a t v a r i o u s t e m p e r a t u r e s and a f t e r d i f f e r e n t aging 3) L a t t i c e P a r a m e t e r s and R a t i o s of the

times are also plotted. Volume F r a c t i o n s of 7 ' and 7"
In a l l o y 3, w h a t e v e r the aging t e m p e r a t u r e b e t w e e n
T h e l a t t i c e p a r a m e t e r s of the m a t r i x and p r e c i p i -
750 ~ and 780~ the c o m p a c t m o r p h o l o g y was a l w a y s
t a t e s w e r e m e a s u r e d in a l l o y s 2 and 3, T a b l e II. In
o b s e r v e d . H o w e v e r by a g i n g too n e a r TM, l a r g e 7 '
a l l o y 3 aged at 750~ it was not p o s s i b l e to d e t e r m i n e
p a r t i c l e s e l o n g a t e d in the (111) d i r e c t i o n s w e r e o b -
the 7 " l a t t i c e p a r a m e t e r s . Indeed with the c o m p a c t
tained.
m o r p h o l o g y , c o h e r e n c y s t r a i n s b e t w e e n 7 ' and 7" p r o -
In a l l o y 1, aging at 780 ~ and 800~ did not p r o d u c e
duce b r o a d d i f f r a c t i o n r i n g s . The v a l u e of a T " and c 7 I'
the c o m p a c t m o r p h o l o g y of a l l o y 3. In this a l l o y 1, the
for a l l o y 2 a r e c o n s i s t e n t with t h o s e r e p o r t e d bYo
o b s e r v e d p r e c i p i t a t i o n i s a l w a y s s i m i l a r to that p r e v i -
W a g n e r and H a l l 5 i.e. a7 "= 3.624.~; c7 "= 7,406A in
ously d e s c r i b e d a t l o w e r t e m p e r a t u r e s .
INCONEL 718 a l l o y .
In a l l o y s 2 and 4, on the o t h e r hand, the c o m p a c t
The r a t i o of the volume f r a c t i o n s of 7 ' and 7 "
m o r p h o l o g y could be obtained by aging b e t w e e n 770 ~ to
(F 7 ' I F 7'1 p r e c i p i t a t e d a t v a r i o u s t e m p e r a t u r e s w a s
795~ and 775 ~ to 815~ r e s p e c t i v e l y , F i g . 9. It is
e s t i m a t e d in a l l o y s 1, 2 and 3, T a b l e III. The v o l u m e
w o r t h noting t h a t , a s in a l l o y 3, this m i c r o s t r u c t u r e
of about 30 p a r t i c l e s was m e a s u r e d . 71 p r e c i p i t a t e s
i s obtained when aging c o n d i t i o n s (time and t e m p e r -
w e r e a s s u m e d to be e x a c t l y cubic when they have the
a t u r e ) allow s i n g l e 7 ' p a r t i c l e s with L > 200A to be
c o m p a c t m o r p h o l o g y or in the o t h e r c a s e s to be p o r -
p r e c i p i t a t e d . H o w e v e r , in a l l o y 2, 7" p a r t i c l e s a r e
tions of a s p h e r e . The a c c u r a c y of t h e s e m e a s u r e -
s o m e t i m e s o b s e r v e d growing beyond the s i d e s of 7 '
m e n t s is r e l a t i v e l y p o o r b e c a u s e the 7" p a r t i c l e s w e r e
c u b e s (e.g. A in F i g s . 9(a) and (b)). In a l l o y s 3 and 4,
s o thin. It should be n o t i c e d that F 7 ' I F 7" i n c r e a s e s
the c o m p a c t m o r p h o l o g y without any o v e r l a p p i n g of 7 '
when the r a t i o T i + A1/Nb i n c r e a s e s . T h i s b e h a v i o r
p r e c i p i t a t e s by 7 ~ p a r t i c l e s h a s a l w a y s been o b s e r v e d .
is c o n s i s t e n t with the o b s e r v a t i o n s of K i r m a n and

52 VOLUME 4, JANUARY 1973 METALLURGICAL TRANSACTIONS

 ii ii i = i i i I

T a b l e I I . L a t t i c e Parameters M e a s u r e d in A l l o y s 2 and 3

Alloy2 Alloy3
Heat Treatments aT, A a'}",A aT", A c3/',A a%A aT',h
(I) 1200~ 1 h, WQ 3.601 + 0.001 3.605 + 0.001
(I) + 770~ 1 h, WQ 3.594 • 0.001 3.607 • 0.002
(I) + 750~ 2 h, WQ 3.603 + 0.001 3.605 • 0.002
(I) + 750~ 524 h, WQ 3.594 + 0.002 3.605 • 0.002 3.626 + 0.002 7.416 + 0.010

ALLOY 2 AL~ 3
I
I
TMI

+'`

• tr
z

L ~')
.J

t
7001 ,
O,S
++7
Alloy,3/
1
,
2
,
S
,
4
, ,
S S
,
|
,
10
,
24
Aging Time , hours

Fig. 8--TTT curves for appearance of 7" phase and highest

'2 4 e 16 32 64 t ~ 24545 ~ 2 4 e 16 32 64 126 2~6 $12 temperatures TM for homogeneous precipitation in alloys
AG4NG TIME , ~ R S
1,2,3 and 4. On this diagram curves showing the TJsize be-
fore appearance ofT" are also indicated for alloys 2, 3, and 4.
Fig. 7--Alloys 2 and 3 aged at 750~ upper (mean size plus
standard deviation) and lower (mean size minus standard
deviation) limits for T J and T" size L as a function of aging
time. The meaning of L is indicated above the curves in each the h a r d n e s s r e m a i n s r e l a t i v e l y c o n s t a n t and, a f t e r
case. 524 h, is found to be a p p r o x i m a t e l y 15 hV h i g h e r than
that obtained a f t e r a d i r e c t t r e a t m e n t a t 700~ Thus
W a r r i n g t o n ~ who have shown that ~," p r e c i p i t a t i o n is the b e n e f i t s of a duplex t r e a t m e n t s u c h a s no. 1 a r e
p r o m o t e d by Nb a d d i t i o n s . c l e a r l y shown: tt p r o d u c e s a good p r e c i p i t a t e s t a b i l i t y
(due to the c o m p a c t m o r p h o l o g y ) and good m e c h a n i c a l
p r o p e r t i e s (due to the i n c r e a s e d v o l u m e f r a c t i o n of
4) T h e r m a l S t a b i l i t y of the C o m p a c t M o r p h o l o g y at
p r e c i p i t a t e s a v a i l a b l e at the l o w e r t e m p e r a t u r e ) . T h i s
Lower Temperatures
t r e a t m e n t h a s p r o v e d p o s s i b l e b e c a u s e the p r e c i p i t a -
The c o m p a c t m o r p h o l o g y obtained by aging a l l o y 3 tion which o c c u r s on c o o l i n g , o r d u r i n g the l o w e r t e m -
n e a r 750~ h a s been shown to be s t a b l e d u r i n g f u r t h e r p e r a t u r e a g i n g , has a l s o the c o m p a c t m o r p h o l o g y .
aging a t t h i s t e m p e r a t u r e ( | 2). In this a l l o y , the s t a -
b i l i t y of the c o m p a c t m o r p h o l o g y d u r i n g aging at l o w e r 5) P r e c i p i t a t i o n of P h a s e s O t h e r T h a n ~ ' and ~ ~
t e m p e r a t u r e s w a s a l s o e x a m i n e d . The a p p l i e d t h e r m a l
t r e a t m e n t ( t r e a t m e n t no. 1) w a s the following: 745~ - 24h, In a d d i t i o n to the i n t e r m e t a l l i c c o m p o u n d s p r e v i o u s l y
cooling down to 700~ at about 100~ aging at d e s c r i b e d , s e v e r a l o t h e r p h a s e s w e r e found.
700~ f o r 524 h. T h e r e s u l t i n g m i c r o s t r u c t u r e w a s In a l l a l l o y s and w h a t e v e r the aging t r e a t m e n t ,
c o m p a r e d with that obtained by aging d i r e c t l y at 700~ C h r o m i u m C a r b i d e s (M23 CB) and N i o b i u m C a r b i d e s
f o r 524 h ( t r e a t m e n t no. 2). (NbC) w e r e i d e n t i f i e d a t g r a i n b o u n d a r i e s . Along t h e s e
In t r e a t m e n t no. 1, p a r t i c l e s p r e c i p i t a t e d d u r i n g b o u n d a r i e s , an about 0.5 /~m b r o a d zone was s e e n to
cooling and aging at 700~ have the c o m p a c t m o r p h - be d e p l e t e d in ~" p r e c i p i t a t e s , F i g . 11. S m a l l NbC p a r -
ology, F i g s . 10(a)and (b}. By f u r t h e r aging a t 700~ t i c l e s (~b ~ 200A) w e r e a l s o p r e c i p i t a t e d h e t e r o g e n -
this c o m p a c t m o r p h o l o g y p r o v e s to be t h e r m a l l y e o u s l y on d i s l o c a t i o n s punched out f r o m l a r g e TiC
s t a b l e , F i g . 10(c). c a r b i d e s d u r i n g the quench f r o m 1200~
T r e a t m e n t no. 2 d o e s not p r o d u c e a c o m p a c t m o r p h - Moreover, numerous extrinsic stacking faults were
ology (~ 2). By aging i s o t h e r m a l l y a t 700~ for 50 h, o b s e r v e d , F i g . 12. T h e y a c t a s s i t e s for the n u c l e a -
s m a l l p a r t i c l e s a r e p r e c i p i t a t e d (L ~ 100~,). On f u r t h e r tion of y ' and y " p a r t i c l e s , but not f o r the p r e c i p i t a t i o n
aging for 524 h a t 700~ m e a n s i z e s l a r g e r than t h o s e of NbC. P r e c i p i t a t i o n of ~ ' on E S F was p r e v i o u s l y
obtained through t r e a t m e n t no. 1 a r e o b s e r v e d , F i g s . o b s e r v e d by O b l a k et all
10(c) and (d). In a l l o y 1, which h a s the h i g h e r niobium content, a
On the o t h e r hand, a f t e r the t r e a t m e n t a t 750~ for s i g n i f i c a n t a m o u n t of ~-NiaNb p h a s e ( o r t h o r h o m b i c , D O a
24 h which p r o d u c e s the c o m p a c t m o r p h o l o g y , an i n - s t r u c t u r e ) was o b s e r v e d a f t e r aging at 750~ for 100 h.
c r e a s e of 30 to 40 hV can be obtained by s u b s e q u e n t T h e ~ - p h a s e p r e c i p i t a t e s a s laths along { l l l } T p l a n e s
aging a t 700~ T a b l e IV. D u r i n g this l a t t e r t r e a t m e n t , with the following o r i e n t a t i o n r e l a t i o n s h i p :

METALLURGICAL TRANSACTIONS VOLUME 4, JANUARY 1973-53

 (c)
Fig. 9-Transmissionelectron micrographs of (a) and (b) alloy 2: heat treatment (a) 770~ 19 h (darkfield image), (b) 780~
17 h (brightfield image) and (c) and (d) alloy 4: heat treatment 775~ 8 h (c) bright field image, and r dark field image.
(010)/3 II {111}~, and [100]/3 l{ <I10>T
Around these particles V"precipitates are dissolved
and only $' phase remains, Fig. 13. On the other hand,
by aging alloys 2 and 3 at 750~ for up to 524 h this
phase has never been found.
In alloys 3 and 4, which contain 7 pet Mo, platelets
often parallel to {111}~/planes are precipitated after
Iongoaging times (---100 h). These thin platelets (I00 to
500A thick and up to 1 {~m long) have been identified
as Laves phases (hexagonal, C 14 structure). Numerous
two-dimensional faults were found in these particles,
Fig. 14. Similar faults have been observed by Yagisawa
and Fujita7 in Fe2 Mo precipitates. The lattice param-
eters wereo
determined
o
by electron diffraction as:
a = 4.76A, c = 7.79A. These values are between those
reported for Fe2 Mo (a = 4.745A, c = 7.734A)8 and
o o 9
Fe2Nb (a = 4.822A, c = 7.877A). This last observation
suggests that the chemical composition of this phase is
of the type Fez(Mo, Nb). We found the following orienta-
tion relationship:
5 4 - V O L U M E 4, JANUARY 1973
(d)
(0001)Fe2(Mo, Nb)II {III}~ and (10i0)Fe2(Mo,Nb) 11{II0}~
DISCUSSION
As in INCONEL 7181 both V' and )," precipitates have
been identified in our four alloys. Since similar obser-
vations have been made in alloys 2 and 3 having a dif-
ferent molybdenum percentage, the molybdenum effect
on ~' and 7"precipitation is thought to be of secondary
importance. Chemical analysis of precipitates ex-
tracted from different Nickel base alloys have shown
that this element remains essentially in the matrix
after aging treatments,s
Although we have performed no chemical analysis
of 7' and 7" precipitates, several previously mentioned
observations suggest that the DO22 phase is richer in
niobium than the Llz phase is: i) zones around fi par-
ticles (stable phase in Ni-Nb system) and around NbC
particles are depleted in T"precipitates; ii) the
Fv'/FT"ratio increases with the Ti + Al/Nb ratio.
We have shown that the rate of coarsening of the
METALLURGICAL TRANSACTIONS
 (a; Ib)

(c) (d)
Fig. 10--Dark field e l e c t r o n m i c r o g r a p h s of alloy 3. Heat t r e a t m e n t : (a) 745~ 24 h, (b) 745~ 24 h + 700~ 8 h,
(c) 745~ 24 h + 700~ 524 h, (d) 700~ 524 h.

p r e c i p i t a t e s i s s t r o n g l y d e p e n d e n t on t h e p a r t i c l e s
m o r p h o l o g y . T h e r e f o r e , t h e n u c l e a t i o n of 7" on Y'
p a r t i c l e s a n d t h e e f f e c t of a g i n g t e m p e r a t u r e a n d c o m -
p o s i t i o n on p r e c i p i t a t i o n m o r p h o l o g y w i l l f i r s t b e
d e a l t w i t h . T h e t h e r m a l s t a b i l i t y of t h e o b s e r v e d c o m -
pact morphology will be subsequently discussed.
1) N u c l e a t i o n of y " P a r t i c l e s on 7 ' P r e c i p i t a t e s
S e c o n d l y , i n s t u d y i n g t h e b e g i n n i n g of t h e a g i n g
r e a c t i o n , we h a v e s h o w n t h a t 7 " p r e c i p i t a t e s a r e
s y s t e m a t i c a l l y a s s o c i a t e d w i t h y ' p a r t i c l e s : L12 p a r -
t i c l e s a r e t h e n p o t e n t i a l n u c l e a t i o n s i t e s f o r DOe2
phase.
Table III. Ratio of the Volume Fractions of 7' and 3"'

T w o m a i n d i f f e r e n c e s a r e to b e n o t e d w i t h r e s p e c t Alloy Heat Treatments FT'/FT"

to t h e o b s e r v a t i o n s r e p o r t e d by P a u l o n i s e t al. on 750~ 128 h 0.4 -+0.08
I N C O N E L 718:1 770~ 19 h 1.5 -+0.3
F i r s t , t h e Y' v o l u m e f r a c t i o n s f o u n d i n o u r a l l o y s 780~ 17 h 1.25 -+0.15
750~ C, 64 h 2.7 -+0.5
a r e h i g h e r t h a n t h a t f o r m e d in t h e b a s i c a l l o y . T h i s 750~ 524 h 2.4 -+0.2
b e h a v i o r i s t h o u g h t to b e m a i n l y d u e to t h e h i g h e r 745~ 24 h + 700~ 524 h 2.5 -+0.5
T i + A 1 / N b r a t i o s u s e d in o u r a l l o y s .

METALLURGICAL TRANSACTIONS VOLUME4, JANUARY 1973-55

 Table IV. Alloy 3 Influence of Duplex Heat Treatments on HardnessValues

Heat Treatments hV 100 g

750~ 24 h 318
750~ 24 h + 700~ 8 h 361
750~ 24 h + 700~ 120 h 351
750~ 24 h + 700~ 524 h 349
700~ 524 h 334

Fig. 1 1 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s h o w i n g g r a i n ~)
b o u n d a r y p r e c i p i t a t i o n of M23 C 6 and NbC carbides. A zone
f r e e f r o m y ' p a r t i c l e s is o b s e r v e d near the boundaries
(alloy 3--745~ 24 h + 700~ 120 h).

Fig. 1 2 - - D a r k field e l e c t r o n m i c r o g r a p h s h o w i n g "y'and 7 "

p r e c i p i t a t i o n on a e x t r i n s i c stacking fault s e e n on edge
alloy 3--770~ 8 h).

The e x a m i n a t i o n of the two unit c e l l s drawn on

F i g . 15 s h o w s that the y ' / m a t r i x i n t e r f a c e s can be
v e r y favorable nucleation s i t e s for 7" phase. Except
for the m e a s u r e d slight d i s t o r t i o n along the a V" a x i s
and the higher one along the c y " a x i s , the two p h a s e s
r e p r e s e n t o r d e r e d v a r i a t i o n s of the fcc lattice. In the
L12 p h a s e , Nb, A1, and Ti a t o m s a r e located at the (b)
cube c o r n e r s , while in the DO22 p h a s e , niobium a t o m s Fig. 1 3 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s showing the
occupy the c e n t e r and the c o r n e r s of a c e l l f o r m e d by d i s s o l u t i o n of the ~/" particles near the p-Ni3Nb laths. Alloy 1
aged a t 750~ f o r 524 h (a) b r i g h t field i m a g e , (b) d a r k field
putting two fcc c e l l s one upon the other. image.

56-VOLUME 4, JANUARY 1973 METALLURGICAL TRANSACTIONS

 2) E f f e c t of Aging T e m p e r a t u r e and C o m p o s i t i o n on the
S t r u c t u r e of the P r e c i p i t a t e s
S e v e r a l f a c t o r s can p r o m o t e the f o r m a t i o n of the
c o m p a c t m o r p h o l o g y . A m o n g s t t h e m , the i n i t i a l shape
oK the i s o l a t e d 7 ' p r e c i p i t a t e s is an i m p o r t a n t one.
T h e f l a t f a c e s of cube s h a p e d p a r t i c l e s p r o b a b l y f a v o r
the n u c l e a t i o n and g r o w t h of 7" on 7 ' . H o w e v e r t h i s
f a c t o r i s thought to be of s e c o n d a r y i m p o r t a n c e . I n -
d e e d , if a l l o y 3 is a g e d a t 730 ~ and 740~ for a s h o r t
t i m e (t < 2 h), i s o l a t e d cube s h a p e d 7 ' p r e c i p i t a t e s a r e
o b s e r v e d . T h e s e p a r t i c l e s do not allow the c o m p a c t
m o r p h o l o g y to be a c h i e v e d d u r i n g f u r t h e r aging a t
these temperatures.
The e x p e r i m e n t a l r e s u l t s s u g g e s t that the m a i n
f a c t o r might be the i n i t i a l s i z e of 7 ' p r e c i p i t a t e s b e f o r e
the f o r m a t i o n of 7" p a r t i c l e s . It has been shown that
the c o m p a c t m o r p h o l o g y could only be obtained if the
i s o l a t e d 7 ' p r e c i p i t a t e s has r e a c h e d a m i n i m u m c r i t i -
c a l s i z e . By c o n s i d e r i n g the b e h a v i o r of a l l o y 2 a t
770~ a l l o y 3 a t 745~ and a l l o y 4 at 775~ this
Fig. 14--Dark field image of a Fe2(Mo, Nb) particle (laves c r i t i c a l s i z e (L c) h a s been s e e n to be about 200/~.
phase type) extracted on a carbon replica. Note the high A t e n t a t i v e e x p l a n a t i o n of the e x i s t e n c e of such a
density of two-dimensional faults. c r i t i c a l s i z e m a y be given by taking into a c c o u n t the
diffusion zone a s s o c i a t e d with 7 " p r e c i p i t a t i o n in the
A3 B Structures n e i g h b o r h o o d of 7 ' p a r t i c l e s , F i g . 17. L e t us c o n s i d e r
a 7 ' p a r t i c l e a l r e a d y p r e c i p i t a t e d a t a given t e m p e r a -
o A atoms t u r e . L e t us s u p p o s e this 7 ' p r e c i p i t a t e has a s m a l l
~I 0 . s i z e when a 7 " p a r t i c l e is n u c l e a t e d on it, F i g . 17(a).
9 B atoms !
T h e p r e c i p i t a t e 7" is p r e f e r e n t i a l l y f o r m e d on one of
a u aY' 0 the s i x f a c e s of 7 ' (the p r o b a b i l i t y of 7" n u l c e a t i o n m a y
cy"=2au 0 not be the s a m e on the s i x f a c e s ) . F o r a s m a l l i n -
c r e a s e in d i m e n s i o n L , the V" p a r t i c l e t e n d s v e r y
r a p i d l y to o v e r l a p the 7 ' p r e c i p i t a t e , F i g . 17(b).
P, A r o u n d this 7" p a r t i c l e the n i o b i u m c o n c e n t r a t i o n is
i
I 0 l o w e r e d in the diffusion zone s c h e m a t i c a l l y d r a w n on
F i g . 17(b) (hatched zone). The l o w e r i n g of n i o b i u m
~ o 0
content at A o r B d e c r e a s e s the p r o b a b i l i t y of 7 "
I o 0
p r e c i p i t a t i o n in this r e g i o n . The r e s u l t i n g m i c r o -
I
s t r u c t u r e s a r e , then, those o b s e r v e d when s m a l l p a r -
o t i c l e s a r e f o r m e d , F i g . 17(c), ( e . g . a l l o y s 2 and 3 at
ay" 650 ~ and 700~ A t h i g h e r aging t e m p e r a t u r e s , l a r g e r
l= ay' --I i s o l a t e d Y' p r e c i p i t a t e s can be f o r m e d , and p r e c i p i t a -
-a- -b- tion can o c c u r m o r e e a s i l y (and independently) on the
Fig. 15--Unit cells of FCC and bct structures of y'and 7" s i x f a c e s of the c u b e - s h a p e d 7 ' p a r t i c l e s , F i g s . 17(c),
phases. (d), and (f).
T h i s a r g u m e n t s u g g e s t s that the c o n d i t i o n s n e c e s -
The p o s s i b i l i t y of s t a c k i n g (001)7" p l a n e s o v e r one s a r y to p r o d u c e the c o m p a c t m o r p h o l o g y a r e d i r e c t l y
of the (llree {001}~,, p l a n e s without i n t r o d u c i n g a s t a c k - d e p e n d e n t on i) the r e l a t i v e p o s i t i o n s of the T T T
ing fault e x i s t s . M o r e o v e r the 7 ' l a t t i c e p a r a m e t e r is c u r v e s c o r r e s p o n d i n g to the s t a r t of V' and V " p r e -
b e t w e e n those of 7" and the m a t r i x , T a b l e II. c i p i t a t i o n and ii) the k i n e t i c s of 7 ' growth. Such T T T
It should be noted h e r e that t h i s coupled 7 ' and 7" c u r v e s a r e s c h e m a t i c a l l y d r a w n on F i g . 18. A c u r v e
p r e c i p i t a t i o n can o c c u r f o r c o m p o s i t i o n s d i f f e r e n t of the aging t i m e n e c e s s a r y to r e a c h L c a s a function
f r o m those p r e v i o u s l y d e s c r i b e d such a s the one of of t e m p e r a t u r e is a l s o shown. A m i n i m u m c r i t i c a l
706 a l l o y , a new F e - N i s u p e r a l l o y , in which the i r o n t e m p e r a t u r e T c below which the c o m p a c t m o r p h o l o g y
content is h i g h e r than in INCONEL 718 The s t r e n g t h - cannot be obtained is thus d e f i n e d . E x p e r i m e n t a l T c
ening p h a s e in this a l l o y w a s r e c e n t l y i d e n t i f i e d a s 7 ' v a l u e s , F i g . 8, c o r r e s p o n d i n g to L c = 200A a r e the
by Moll e t al. 1~ following:
H o w e v e r the e x a m i n a t i o n of t h e i r b r i g h t f i e l d m i c r o -
g r a p h s s u g g e s t s that two p h a s e s w e r e p r e c i p i t a t e d .
- a l l o y 2 ~ Tc2 - 770~
D i f f r a c t i o n p a t t e r n and d a r k field a n a l y s i s p r e s e n t e d
- a l l o y 3 - - T c 3 ~- 745~
on F i g . 16 u n a m b i g u o u s l y show that, with the s a m e
- a l l o y 4 ~ T c 4 - 775~
a g i n g c o n d i t i o n s a s those u s e d by t h e s e a u t h o r s , V"
p a r t i c l e s a r e n e a r l y a l w a y s a d j a c e n t to 7 ' p r e c i p i t a t e s . In a l l o y 1, we have not been a b l e to obtain 7 ' p a r t i -
T h e two o b s e r v e d m i c r o s t r u c t u r e s a r e v e r y s i m i l a r c l e s with a s i z e L c b e f o r e the s t a r t of the 7 " p r e c i p i -
to t h o s e of our a l l o y s 2 and 3 aged at 700~ F i g . 3. tation.

METALLURGICAL TRANSACTIONS VOLUME4, JANUARY 1973-57

 (a)
(c)
Fig. 16--Transmission electron mierographs showing T' and "y" phases in 706 alloy aged at 732~ for 16 h: (a) bright field image,
(b) diffraction pattern, (c) dark field image using spot 1, (d) dark field image using spot 2. (Composition of 706 alloy used:
41.10 Ni; 16.05 Cr; 3.00 Nb; 1.56 Ti; 0.21 A1; balance Fe.)
It should be b o r n e in m i n d that the r e l a t i v e p o s i t i o n s
of T T T c u r v e s a r e s t r o n g l y dependent on c o m p o s i t i o n .
B e c a u s e of the rapid 7 ' p r e c i p i t a t i o n it has not been
p o s s i b l e to d e t e r m i n e p r e c i s e l y the T T T c u r v e s c o r -
r e s p o n d i n g to this p h a s e . However a f t e r 30 m i n at
d i f f e r e n t t e m p e r a t u r e s up to TM, 7' p a r t i c l e s have
always been o b s e r v e d in the four a l l o y s . As for 7"
p r e c i p i t a t e s , the i n c i p i e n t p r e c i p i t a t i o n c u r v e is d e -
p e n d e n t on the a m o u n t of T i + A1 + Nb (Alloys 1, 2, 3,
4) and on the r a t i o T i + A1//Nb (Alloys 1, 4 and 2, 3)
and was p r e c i s e l y d e t e r m i n e d . The influence of the
c o m p o s i t i o n is indicated on F i g . 18.
3) T h e r m a l Stability of the C o m p a c t Morphology
When the c o m p a c t morphology obtained at a given
t e m p e r a t u r e is f u r t h e r aged at the s a m e t e m p e r a t u r e
58 VOLUME4,JANUARY 1973
(b)
(d)
or at a lower t e m p e r a t u r e , two m a i n o b s e r v a t i o n s have
b e e n made: i) the 7 ' growth rate is slowed down a s
soon as 7" a p p e a r s , ii) the o r i g i n a l shape of the p a r t i -
cles is m a i n t a i n e d .
To explain why the c o m p a c t morphology i m p r o v e s
so much the t h e r m a l s t a b i l i t y of the p r e c i p i t a t e s ,
s e v e r a l s u g g e s t i o n s may be made:
F i r s t : with r e g a r d to the c o a r s e n i n g of 7 ' , the dif-
fusion of T i , A1, and Nb through the 7" s h e l l , n e c e s s a r y
to allow the growth of 7 ' , has to be taken into account.
The DO22 phase may be an efficient diffusion b a r r i e r .
C o m p a r a t i v e diffusion r a t e m e a s u r e m e n t s of T i , A1,
and Nb in the stable 13-Ni3Nb phase (in default of 7'1
and in a N i - C r - F e m a t r i x would be u s e f u l to t e s t this
hypothesis.
Secondly: the e l a s t i c d i s t o r t i o n s a s s o c i a t e d with
the c o h e r e n t 7" p r e c i p i t a t i o n may affect the p a r t i c l e
METALLURGICAL TRANSACTIONS
 L < Lc L >i Lc
.a. ~
1 YI/ ,. Y+Y' S*Y'+Y"
.b- oe.
/ \
A IJi*AI/Nb '
.f.
W
Fig. 17--Schematic diagram showing the occurrence of o m -
pact morphology above a given size L of y' particles for
further understanding see text).
s h a p e , An e x a m p l e is g i v e n by the p r e c i p i t a t i o n of 7 "
in F e - N i - N b s y s t e m . 11 T h i s e f f e c t is r e l a t e d to the
d i f f e r e n c e b e t w e e n the m i s f i t p a r a m e t e r s of 7 ' and 7".
L e t us c o n s i d e r a ~," e l l i p s o i d - s h a p e d p a r t i c l e c o -
h e r e n t l y p r e c i p i t a t e d in an i n f i n i t e m a t r i x , t h e r a d i u s
of the g r e a t c i r c l e b e i n g L and the t h i c k n e s s h. T h e
i n c l u s i o n t h e o r y due to E s h e l b y 12 can be u s e d to c a l c u -
l a t e the e l a s t i c e n e r g y ( E e ) p e r u n i t v o l u m e a s s o c i a t e d
w i t h the f o r m a t i o n of t h i s 7 " p r e c i p i t a t e . E e d e c r e a s e s
w i t h h//L a s s h o w n by G, F a i v r e . H
T h e s e r e s u l t s c a n be u s e d to d e m o n s t r a t e t h a t the
s h a p e s t a b i l i t y of the c o m p a c t m o r p h o l o g y is d i r e c t l y
d e p e n d e n t on t h e F T ' / F y " r a t i o . Indeed, particles re-
t a i n i n g the c o m p a c t m o r p h o l o g y w i t h a p p r o x i m a t e l y
the s a m e L v a l u e h a v e an i n c r e a s i n g t h i c k n e s s h w i t h
d e c r e a s i n g F 7 ' / / F 7" r a t i o . T h e e l a s t i c e n e r g y t h u s
i n c r e a s e s up to a m a x i m u m c r i t i c a l v a l u e a b o v e w h i c h
the c o m p a c t m o r p h o l o g y b e c o m e s u n s t a b l e . It h a s b e e n
p r e v i o u s l y s h o w n t h a t the F ~ ' / F ~ " a n d T i + A 1 / N b
r a t i o s a r e s t r o n g l y d e p e n d e n t upon e a c h o t h e r . T h e r e -
f o r e , in o r d e r to m a i n t a i n the s t a b i l i t y of the c o m p a c t
m o r p h o l o g y it i s n e c e s s a r y to h a v e a T i + A1 + N b
r a t i o a b o v e a c r i t i c a l v a l u e . I n v e s t i g a t i o n s of a l l o y s
b e h a v i o r l e a d to a 0.9 to 1 v a l u e f o r t h i s c r i t i c a l
Ti + A1/Nb ratio.
C O N C LUSION
I) I n c r e a s i n g the T i + A 1 / N b r a t i o in N i - C r - F e a l l o y s
w i t h c o m p o s i t i o n s a p p r o x i m a t i n g t h a t of I N C O N E L 718,
p r o d u c e s i n c r e a s e d 7 ' (Llz) p r e c i p i t a t i o n c o m p a r e d
w i t h 7 " (DO22) f o r m a t i o n .
II) T h e t i m e s e q u e n c e of the p r e c i p i t a t i o n r e a c t i o n
h a s b e e n d e t e r m i n e d . A t low a g i n g t e m p e r a t u r e s 7 "
particles are always associated with 7' precipitates.
F o r a c e r t a i n r a n g e of a g i n g t e m p e r a t u r e s , d e p e n d i n g
upon the T i , A1, and Nb c o n t e n t s it has b e e n s h o w n that
7' precipitates first. The TTT curves corresponding
to the s t a r t of the 7 " p r e c i p i t a t i o n h a v e b e e n d e t e r m i n e d .
tII) A p e c u l i a r p r e c i p i t a t i o n m i c r o s t r u c t u r e h a s b e e n
identified: cube-shaped 7' particles coated with a 7"
METALLURGICAL TRANSACTIONS
(1,)
cl,
, ",,%/
E ...... -7 TI+AI+Nb#U
Aging Time
Fig. 18--Schematic drawing of TTT curves for the appearance
of y ' and 3'" phases showing the existence of a critical t e m -
perature Tc bound to the critical size L c , temperature below
which the compact morphology cannot be obtained. The a r -
rows indicate respectively that the distance between 7 ' and
7 " curves is an increasing function of Ti + A1/Nb and that all
the curves are translated towards the upper temperatures
when (Ti + A1 + Nb) is increased.
shell over their six faces. This "compact morphology"
h a s p r o v e d to h a v e a v e r y s l o w r a t e of c o a r s e n i n g . An
i m p r o v e m e n t in t h e r m a l s t a b i l i t y i s t h e r e f o r e a s s o c i -
ated with this microstructure.
IV) R e q u i s i t e c o n d i t i o n s to a c h i e v e t h i s m o r p h o l o g y
have been investigated. A minimum Ti + A1/Nb ratio
b e t w e e n 0.9 and 1 h a s b e e n o b s e r v e d to b e n e c e s s a r y .
M o r e o v e r the a g i n g t e m p e r a t u r e h a s to be c h o s e n in
s u c h a w a y t h a t i n i t i a l l y i s o l a t e d V' p r e c i p i t a t e s r e a c h
a s i z e of a b o u t 200A b e f o r e p r o d u c t i o n of 7 " p r e c i p i -
tates.
ACKNOWLEDGEMENTS
T h e a u t h o r s a r e g r a t e f u l to M r . Y. H o n n o r a t ( L e
C r e u s o t L o i r e , I m p h y ) f o r p r o v i d i n g the f o u r s t u d i e d
a l l o y s . T h e y thank a l s o M r . A . Hue f o r the a s s i s t a n c e
in v a r i o u s p o r t i o n s of t h i s w o r k , and M r . Y. I m b e r t
( S N E C M A - C o r b e i l E s s o n n e s ) and D r . F . L e c r o i s e y f o r
stimulating discussions,
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1I. G. Faivre:Phys. Status Solidi, 1969, vol. 35, p. 249.
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VOLUME 4, JANUARY 1973-59