Field 1978
Field 1978
Field 1978
The
f r o m the o p p o s i t e f r a c t u r e f a c e s e s t a b l i s h e d that the w o r k was s u p p o r t e d by the U.S. E n e r g y R e s e a r c h and
s u r f a c e s t e p s w e r e m a t c h i n g and i n t e r l o c k i n g in a l l Development Administration, Contract EY-76-C-02-
c a s e s . The f a c e t s b e t w e e n the s t e p s w e r e flat and 1198.
a p p e a r e d to be p a r a l l e l with n e i g h b o r i n g f a c e t s . A thin
l a y e r of/3 e x i s t e d b e t w e e n the c~ p l a t e s and this p h a s e
f r a c t u r e d in a d u c t i l e f a s h i o n , f r e q u e n t l y p r o d u c i n g I. T. R. Beckand E. A. Grens,II: J. Electrochem. Soc., 1969, vol. i66, p. 177.
k n i f e - e d g e r i d g e s which m a t c h e d p e a k - t o - p e a k on the 2. J. C. SculIyand D. T. PowelI:Corros. ScL, 1970,vol. t0, p. 719.
opposite fracture faces. 3. G. H. Koch:Ph.D. Thesis,Universityof Illinoisat Urbana-Champaign,i976.
T h e f r a c t o g r a p h i c c h a r a c t e r i s t i c s a r e fully c o n s i s t - 4. D. N. Williams:J. Iron SteellnsL, 1962-63,voL91, p. 147.
ent with f r a c t u r e of the o~ p h a s e o c c u r r i n g b y c l e a v a g e .
T h e f a n - l i k e m o r p h o l o g y of the s u r f a c e s t e p s within
e a c h a p l a t e , r e p o r t e d by many w o r k e r s , can be a c -
counted f o r in t e r m s of c l e a v a g e b y a s s u m i n g that the
c r a c k m a i n t a i n s a c o n s t a n t s e m i c i r c u l a r p r o f i l e within Microstructural Observations of Metal
e a c h p l a t e and p r o p a g a t e s longitudinally along the
p l a t e a s i l l u s t r a t e d in F i g . 2, and that the s t e p s a r e Powders Using Analytical Electron
p e r p e n d i c u l a r to the c r a c k f r o n t a s in conventional M icroscopy
c l e a v a g e . The s h a p e of the c l e a v a g e s t e p s can then be
r e p r e s e n t e d by equations of the f o r m
RO/3ERT D. F I E L D AND HAMISH L. F R A S E R
P o w d e r m e t a l l u r g y is one a r e a of p r o c e s s i n g which
p r o m i s e s s i g n i f i c a n t i m p r o v e m e n t s in m a t e r i a l s p r o p -
w h e r e a is the r a d i u s of the c r a c k , and this is d i s - e r t i e s beyond c u r r e n t l y known l i m i t s . T h e r e is now
p l a y e d g r a p h i c a l l y in F i g . 2. C o m p a r i s o n with F i g . 1 c o n s i d e r a b l e e m p h a s i s b e i n g p l a c e d on the d e v e l o p m e n t
i n d i c a t e s that a g r e e m e n t i s good, although it is p r o b a - of r a p i d s o l i d i f i c a t i o n t e c h n i q u e s to p r o d u c e c o m p l e x
b l e that the c r a c k f r o n t s a r e not p r e c i s e l y s e m i c i r c u - a l l o y p o w d e r s p o s s e s s i n g the a p p r o p r i a t e s t r u c t u r e
l a r in p r a c t i c e . The a p p r o x i m a t e l y s e m i c i r c u l a r and p h a s e d i s t r i b u t i o n . T h e r e a l i z a t i o n of the " a p p r o -
c r a c k p r o f i l e p r e s u m a b l y r e s u l t s f r o m the pinning ef- p r i a t e " s t r u c t u r e and p h a s e d i s t r i b u t i o n in a powder is
fect of the thin l a y e r s of d u c t i l e / 3 p h a s e which s e p a r a t e an i m p o r t a n t p r o b l e m . C l e a r l y , the p r o p e r t i e s of the
the o~ p l a t e s . The c l e a v a g e s t e p s a r e c o n t i n u a l l y c r e - r e s u l t a n t m a t e r i a l will i n e v i t a b l y be a f f e c t e d by the
a t e d at the c r a c k front and t e r m i n a t e at the a-/3 i n t e r - s t r u c t u r e of the p o w d e r s u s e d in its f a b r i c a t i o n ; f o r
f a c e . T h e o r i g i n of the s t e p s is not u n d e r s t o o d , a l - e x a m p l e , it is often d e s i r a b l e for the p o w d e r s to p o s -
though it i s p o s s i b l e that they a r e g e n e r a t e d when the sess nonequilibrium structures. Thus, microstruc-
crack intersects dislocations. t u r e , p h a s e d i s t r i b u t i o n and c h e m i c a l s e g r e g a t i o n of
B a s e d on this model, the f r a c t o g r a p h y within an a g - the e l e m e n t a l c o m p o n e n t s a r e a l l e x t r e m e l y i m p o r t a n t
g r e g a t e of t~ p l a t e s can be i n t e r p r e t e d . F o r e x a m p l e , p a r a m e t e r s in p o w d e r m e t a l l u r g y .
the d i r e c t i o n of the c l e a v a g e s t e p s in F i g . 3 i n d i c a t e s It is, then, e s s e n t i a l to be a b l e to c h a r a c t e r i z e a s i n -
that a c r a c k t r a v e l l i n g f r o m r i g h t to left in c~-plate A gle m e t a l p o w d e r on a s fine a s c a l e a s p o s s i b l e . H e r e ,
e n t e r e d a d j a c e n t p l a t e 13 at C, w h e r e it s p r e a d in op- c h a r a c t e r i z a t i o n is taken to m e a n m o r p h o l o g y and m i -
p o s i t e d i r e c t i o n s within that p l a t e . It follows that r e - c r o s t r u c t u r e , p h a s e d i s t r i b u t i o n and c r y s t a l s t r u c t u r e ,
gions of plate A f r a c t u r e d b e f o r e n e i g h b o r i n g r e g i o n s and m i c r o c h e m i s t r y . In p r i n c i p l e , such c h a r a c t e r i z a -
on the o t h e r s i d e of the/3 f i l m in p l a t e B, r e q u i r i n g tion can be c a r r i e d out using the r e c e n t l y d e v e l o p e d
that the c r a c k - t i p o p e n i n g d i s p l a c e m e n t f o r c l e a v a g e techniques of a n a l y t i c a l e l e c t r o n m i c r o s c o p y (AEM);
of the a be l e s s than the s t r a i n n e c e s s a r y to r u p t u r e a specimen suitable for transmission electron mi-
the i3. S p r e a d i n g of c r a c k s into n e i g h b o r i n g p l a t e s was c r o s c o p y is p r e p a r e d , and s t u d i e s a r e u n d e r t a k e n u s -
c o m m o n l y o b s e r v e d , and o c c u r r e d at r e g i o n s w h e r e i n g both conventional and s c a n n i n g t r a n s m i s s i o n e l e c -
the ~3 f i l m was a b s e n t . Thus it a p p e a r s that, in our e x - t r o n m i c r o s c o p y , d e n o t e d C T E M and STEM, r e s p e c -
p e r i m e n t s , c r a c k s w e r e confined to s i n g l e ~ p l a t e s t i v e l y , coupled with an e n e r g y d i s p e r s i v e X - r a y
by the e n v e l o p e of d u c t i l e /3, a c c o u n t i n g for the g e n e r a l a n a l y z e r . T h e i m p o r t a n t s t e p is the thinning and
f a n - l i k e m o r p h o l o g y of the c l e a v a g e s t e p s , and s p r e a d p o l i s h i n g of a s i n g l e p o w d e r , so that t h e r e a r e s o m e
into n e i g h b o r i n g p l a t e s at b r e a k s in the d u c t i l e en- a r e a s in the p o w d e r of a p p r o x i m a t e l y 50 to 100 nm in
v e l o p e . It i s c l e a r f r o m F i g . 3 and f r o m the study of t h i c k n e s s . T h i s is not a t r i v i a l p r o b l e m s i n c e t y p i c a l l y
many s p e c i m e n s that the c r a c k f r o n t is f r e q u e n t l y i r - p o w d e r s have d i a m e t e r s r a n g i n g b e t w e e n 20 to 200
r e g u l a r on a m i c r o s c o p i c s c a l e . /an. K o t v a l , D i c k e y and L e w i s 1 have a t t e m p t e d to
It is concluded that the s i m i l a r i t i e s b e t w e e n the p o l i s h s i n g l e p o w d e r s , but a p p a r e n t l y m e t with l i m i t e d
f r a c t u r e s u r f a c e s p r o d u c e d b y SCC and SSRHE and the s u c c e s s . T h i s p a p e r r e p o r t s on the s u c c e s s f u l d e v e l o p -
r e a d y i n t e r p r e t a t i o n of t h e s e s u r f a c e s by the c l e a v a g e m e n t of a thinning technique f o r N i - b a s e s u p e r a l l o y
m o d e l l e a v e s l i t t l e doubt that the p r o p a g a t i o n of SCC p o w d e r s , and p r e s e n t s s o m e p r e l i m i n a r y e x a m p l e s of
in this a l l o y is m e c h a n i c a l . F u r t h e r , the c o m p a r i s o n
p r o v i d e s s t r o n g i n d i r e c t e v i d e n c e that SCC a l s o in-
R. D. FIELD and H. L. FRASER are Research Assistant and Assist-
v o l v e s h y d r o g e n , g e n e r a t e d in this c a s e by the aqueous ant Professor, respectively, in the Department of Metallurgy and Min-
solution. ing Engineering, University of Illinois at Urbana-Champaign, Urbana,
The a u t h o r s wish to acknowledge U. / 3 e r t o c c i f o r IL 61801.
helpful d i s c u s s i o n , and R. Dewit f o r his a s s i s t a n c e in Manuscript submitted March 2, 1977.
ISSN0360-2133/78/0110-0131$00.75]0
METALLURGICAL TRANSACTIONS A 9 1978 AMERICANSOCIETYFOR METALSAND VOLUME 9A, JANUARY 1978-131
THE METALLURGICALSOCIETYOF AIME
Fig. 1--Secondaryelectron image of a thinnedpowder in a
nickel binder. Area of analysis is designated with an " X " .
m o r p h o l o g i c a l and m i c r o c h e m i c a l c h a r a c t e r i z a t i o n of
a powder possessing a dendritic m i c r o s t r u c t u r e .
E x p e r i m e n t a l P r o c e d u r e . IN 100 (a N i - b a s e s u p e r -
a l l o y containing a p p r o x i m a t e l y 0.18 pct C, 10 pct C r ,
15 p c t Co, 3 pct Mo, 4.7 pct Ti, 5.5 pct AI, 0.014 pct Fig. 2--Transmission electron micrograph taken at low mag-
B, 0.06 pct Z r , 1.0 pct V) p o w d e r s w e r e used.* The nification to allow a survey view of the dendritic structure of
*Thepowderswerekindly supplied by Pratt and WitneyAircraftGroup, the powder in Fig. 1. The central portion of the mierograph
United TechnologiesCo~poraticn,WestPalm Beach,Florida;the powderswere is oriented for diffraction by {200}; g as shown; beam direc-
made as part of a programsponsored by the AdvancedResearchProjects Agency. tion close to [001]; accelerating voltage 200 kV.
B 84
,,_A::)
250nm
(b)
F i g . 4 - - S c a n n i n g 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 of s e c -
o n d a r y d e n d r i t e s and b o u n d a r i e s . T h i s a r e a w a s u s e d for m i -
c r o c h e m i e a l a n a l y s i s , the r e s u l t s of w h i c h a r e s h o w n in the
s u b s e q u e n t f i g u r e s . T h e foil has been d e l i b e r a t e l y o r i e n t e d
to avoid diffraction c o n t r a s t e f f e c t s w h i c h m a y lead to a n o m -
alous X - r a y e m i s s i o n .
8
a)
8 Ni
0
ID
0
0o
O
Z
Coo
~/ Cr P~o o
i --, II ~ i] ~ o
(c)
Fig. 3-Continued.
"T' 1 I I ~ I I
0,00 2.00 4.00 6.00 8,00 10.00
ENERGY (KEV)
shows a r e l a t i v e l y low m a g n i f i c a t i o n m i c r o g r a p h of
this area. The m i c r o g r a p h c o n s i s t s of i m a g e s of a
p r i m a r y dendrite with a s s o c i a t e d s e c o n d a r y dendrite oo
a r m s . At the e x t r e m i t i e s of the s e c o n d a r y d e n d r i t e s ,
there are boundaries between these and other s e c o n d -
ary a r m s o r i g i n a t i n g f r o m other p r i m a r y dendrites. A 0
number of o b s e r v a t i o n s of the m i c r o s t r u c t u r e can be d
O
b)
Discussion of "Application of
8 Heterogeneous Nucleation Theory to
Precipitate Nucleation at GP Zones"*
ERHARD HORNBOGEN
In a r e c e n t p a p e r Marth, A a r o n s o n , L o r i m e r , B a r t e l ,
o
and R u s s e l l (MALBR) p r e s e n t a t h e o r y of n u c l e a t i o n at
o ~ ~0 o oo 0
GP z o n e s in which c l a s s i c a l t h e o r y of h e t e r o g e n e o u s
n u c l e a t i o n is applied.1 A m o d e l is used in which it is
a s s u m e d that the c o n t r i b u t i o n of the i n t e r r a c i a l e n e r g y
4.15 41.29 41.49 4t.,56 4170 41.84
ENERGY (KEV)
Fig. 6--Processed data for the TiKc~ peaks. (a) Taken from * P. E. MARTH, H. I. AARONSON, G. W. LORIMER, T. L. BARTEL,
point A (Fig. 4), (b) taken from point B (Fig. 4). The squares and K. C. RUSSELL: Met. Trans. A., 1976, voi. 7A, pp. 1519-28.
correspond to the data points with background and system ERHARD HORNBOGEN is Professor, Materials Science Depart-
counts subtracted 9 The solid lines are computer generated ment, Mechanical Engineering, Ruhr-Universit~t Bochum, D-4630
profiles (see text). Note change in vertical scale between (a) Bochum 1, Germany.
and (b). Discussion submitted June 16, 1977.
ISSN0360-2133/78/0110-0134500.75/0
134-VOLUME 9A, JANUARY 1978 9 1978 AMERICANSOCIETYFOR METALSAND METALLURGICAL TRANSACTIONS A
THE METALLURGICALSOCIETYOF AIME