Beruflich Dokumente
Kultur Dokumente
AND
R. P. REED
R. E. SCHRAMM is Physicist, and R. P. REED is Supervisory Metallurgist, Cryogenics Division, Institute for Basic Standards, Boulder,
Colorado 80302.
Manuscript submitted November4, 1974.
METALLURGICAL TRANSACTIONS A
O Previous Measurements
i~90
(Table I)
9 This Report
}h/ AAAso
Fe
]O
20
30
40
50
60
70
80
90
Ni
Reference
Composition, Pet
Cr
Ni
Method, Variables
Others
I5-20
18-20
8-11
Internal stresses
Whelan (1959)
30*
18-20
8-11
Swann(1963)
14"
16"
30*
36*
44*
17.9
17,6
18,1
17.6
17.8
7.1
7.9
12.8
12.7
17.8
0.06C,
0.06C,
0.02C,
0.02C,
0.03C,
Extended nodes
Breedis (1964)
29.2*
40.7*
51.1"
76.1"
98.0*
19.3
17.3
16.0
13.0
10.4
11.2
11.0
t2.1
14.2
16.2
28-41 .cxl
58*
131"
18.74
20
20
9.43
20
40
8.5
18.3
22
18
16
18
22.0
11.84
10.28
9.87
9.87
9.87
8
34.0
Twin frequency
Extended nodes, a0 = 3.6
G = 7.4 101~
2
53 *d
64 *d
15.3
15.8
15.9
23.0
48 *c'd
15.9
15.8
70.2 *c'd
t5.4
24.7
19
16.6
9.5
53 c
17,8
Vingsbro (1967)
~8
23 a
32 a
40 a'b
38
34
53 a'b
40 a
45 a
57 a
23 b
34 b
38
38
34
~ 5 0 c'd
23-28 *c'a
28-32 *c'd
23-28*
20-25*
30*
>46*
0,11N
0.04N
0.12N
0.004N
0.004N
0.028C
Extended nodes
14.1
18
13
0.02C
Tetrahedra
10
15
20
25
30
20
20
20
20
10
15
20
25
30
20
20
20
20
30
0.006C 0.005N
0.018C. 0 . 0 0 3 N
0.015C, 0.006N
0.009C. 0,006N
0.011C~ 0.006N
0.012C, 0.004N
0.019C, 0.005N
0.022C. 0.O05N
0.036C. 0.005N
0.012C. 0.044N
O.O10C 0.035N
0.018C. 0.05 IN
0.009C 0.033N
0.010C, 0.029N
0.012C, 0.013N
0.012C, 0.011N
0.017C, 0.047N
0.027C, 0.003N
0.050C, 0.010N
44 b
47
43 a
47
20
20
20
20
20
10
15
25
30
20
20
20
20
20
10
15
25
20
20
Latanision, Ruff(1969)
23.1 1.7
18.7
15.9
Murr (1969)
21 c'a
18.43
48 b
9.52
*The reported value has been multiplied by 2.3 (cf. Brown (t964), G allagher (1970)).
a'b'C'dThese points were used in computing the respective lines in Figs. 2 and 3.
(Table I continued on following page)
1346-VOLUME
METALLURGICAL TRANSACTIONS A
Table I (Contd)
Stacking
Fault
Energy
(mJ/m 2)
Reference
Composition, Pct
Cr
Ni
Others
Method, Variables
LeCroisey, Thomas
(1970)
45
24
17.8
15.9
14. l
12.5
0.01C
<0.01C
Latanision, Ruff(1971)
16.4 1.1
23.6 0.9
18.3
t8.7
10.7
15.9
0.005C
0.005C
60
30
20
16
5
10
15
18
20
I5
10
8
0.04C
0.04C
0.04C
0.04C
X-ray diffraction
Cr
Mn
Me
Si
8.28
18.31
0.82
0.02
0.025
0.30
0.010
0.007
AISI 305
1 t.85
18.02
1.64
0.10
0.074
0.32
0.013
0.002
AISI 310 S
18.8
24.7
1.73
0.44
0.047
0.56
0.022
0.005
AISI 316
21-6-9(melt 1)
21-6-9(melt 2)
22-13-5
Hadfield
13.01
7.11
6.48
12.34
4.1
17.15
21.00
20.30
21.57
1.40
8.75
9.55
5.17
15.7
2.09
0.03
0.055
0.027
0.034
0.04t
0.91
0.53
0.43
0.t3
0.40
1.29
0.027
0.011
0.022
0.020
0.009
0.008
0.003
0.012
0.004
0.017
AISI 304L
Ni
2.20
METALLURGICAL TRANSACTIONS A
Others
A1 < 0.001, Co = 0.03, Cu = 0.01 Nb < 0,005,
Pb < 0.004, Sn < 0.005, Ti < 0.002, V = 0.0t 5,
Zn < 0.01, H ~ 10-4, O = 0.0130, N = 0.0183
A1 = 0.001, Co = 0.01, Cu = 0.09, Nb < 0.01,
Pb < 0.001, Sn = 0.002, Ti = 0.066, V = 0.04,
Zn < 0.005
A1 = 0.005, Co = 0.15, Cu = 0.015, Nb = 0.015,
Pb < 0.004, Sn < 0.005, Ti = 0.003, V = 0.05,
Zn < 0.01
Co = 0.08, Cu = 0.067, N = 0.31
N = 0.26
Co = 0.11,Cu = 0.15
X-RAY METHOD
The s h o r t - r a n g e m i c r o s t r a i n s r e s u l t i n g from any
dislocation configuration contribute to X - r a y diffraction
line profile broadening. Using the W a r r e n - A v e r b a c h
technique, ~'27 it is p o s s i b l e to m e a s u r e this and the
additional broadening caused by s m a l l p a r t i c l e s i z e
by c o m p a r i n g the F o u r i e r cosine coefficients for the
( l l l ) and (222) p r o f i l e s . I n s t r u m e n t a l broadening is
eliminated by c o m p a r i n g the diffraction p a t t e r n of an
annealed s p e c i m e n with that of a d e f o r m e d s p e c i m e n
of the s a m e m a t e r i a l . The r m s m i c r o s t r a i n m e a s u r e d
, 2 ~I/2
h e r e , ~%o;111, is a v e r a g e d o v e r a column 50~ long in
the [111] d i r e c t i o n , which is the c u s t o m a r y p r a c t i c e .
Compared to p u r e e l e m e n t s , za m i c r o s t r a i n m e a s u r e ment v a r i a b i l i t y was usually g r e a t e r ; this p r o b a b l y
r e s u l t e d from i n c r e a s e d f l u o r e s c e n c e due to the p r e s ence of Cr. It was expected that the AISI 304L alloy
would exhibit l e s s s c a t t e r , since the solid s p e c i m e n
was p l a s t i c a l l y s t r a i n e d c o n s i d e r a b l y l e s s than the
powdered s p e c i m e n s .
Stacking faults o c c u r on the (111) c l o s e - p a c k e d
planes in an fee c r y s t a l and r e s u l t in a shift in the
position of the diffraction l i n e s . Comparison between
an annealed s t a n d a r d and a d e f o r m e d s p e c i m e n is the
e a s i e s t approach to m e a s u r e the stacking fault p r o b a bility. To avoid d i f f r a c t o m e t e r z e r o e r r o r s and to inc r e a s e s e n s i t i v i t y , it is b e s t to obtain the p r o f i l e a n gular s e p a r a t i o n of (111) and (200) r e f l e c t i o n s r a t h e r
than absolute 20 positions. As the density of stacking
V O L U M E 6A, J U L Y 1 9 7 5 - 1 3 4 7
f a u l t s i n c r e a s e s , L e . , a s the s t a c k i n g fault p r o b a b i l i t y ,
a , i n c r e a s e s , the d e g r e e of line shifting i n c r e a s e s .
This can be c a l c u l a t e d f r o m : 2~
h20 = (20zo o - 2 0 ~ ) C W -
(20~oo - 2Ore)AN N
Om]a ,
[1]
g m wo G (m) ao A-~
( C~o) 111
[2]
where
Km r
6.6 = p r o p o r t i o n a l i t y constant,
G ( u ~ s h e a r m o d u l u s in the (111) fault p l a n e ,
=
+ cll -
the unit c e l l d i m e n s i o n . V e r y l i t t l e of t h i s t y p e of d a t a
e x i s t s in the l i t e r a t u r e for t h e s e a l l o y s , but it is enough
to p r o c e e d if s o m e a s s u m p t i o n s a r e m a d e . E l a s t i c d a t a
on t h r e e a l l o y s with c o m p o s i t i o n s s i m i l a r to t h e s t e e l s
s t u d i e d h e r e a r e l i s t e d in T a b l e IIL 3z'33 While c l l and
c 12 v a r y with c o m p o s i t i o n , the s h e a r m o d u l u s and a n i s o tropy are relatively constant. Therefore, average values of t h e s e p a r a m e t e r s w e r e u s e d f o r a l l of the s t e e l s
r e p o r t e d on h e r e , i . e . ,
G(111) = 0.65 1011 N / m 2.
and
A = 3.43.
[4]
7 = 17.8 l0 s (%o)1,1 ( m j / m Z ) .
[5]
Cg
c1 ),
a o = unit c e l l edge d i m e n s i o n
A = Z e n e r a n i s o t r o p y = 2c,,,,/(c~ - c~2) , and
cij = e l a s t i c s t i f f n e s s c o e f f i c i e n t s .
[3]
E X P E R I M E N T A L PROCEDURE
The e q u i p m e n t and a p p r o a c h u s e d h e r e w e r e b a s i c a l l y the s a m e a s r e p o r t e d p r e v i o u s l y , z4 F i x e d - t i m e
point d a t a w e r e c o l l e c t e d f o r the (111) and (222) p r o f i l e s and the (111) and (200) p e a k p o s i t i o n s with a c o m m e r c i a l X - r a y d i f f r a c t o m e t e r and m o n o c h r o m a t e d
CoK(~ r a d i a t i o n (~ = 1.79021A). In this i n s t a n c e , Eq.
[1] r e d u c e s to A20 = -- 6.5 (~. P u b l i s h e d p r o c e d u r e s
and c o m p u t e r p r o g r a m s z8-31 p r o v i d e d the n e e d e d c o r r e c t i o n s and a n a l y s e s .
F o r the p r e s e n t m e a s u r e m e n t s , a s t e p p e r m o t o r r e p l a c e d the s y n c h r o n o u s e l e c t r i c m o t o r to d r i v e the d i f fractometer X-ray detector for strip-chart recording.
This change and the d i g i t a l output a l r e a d y a v a i l a b l e
f r o m the s c a l e r m a d e it p o s s i b l e to a u t o m a t e the d a t a
c o l l e c t i o n p r o c e s s with a m i n i c o m p u t e r having an 8K
m e m o r y . The s o f t w a r e p r o g r a m (in BASIC) r e q u i r e d
the i n i t i a l and final a n g u l a r l i m i t s , a n g u l a r s t e p i n c r e m e n t , and t i m e of count for each p r o f i l e . With the e n t r y of t h e s e p a r a m e t e r s , no f u r t h e r i n t e r v e n t i o n was
n e c e s s a r y and the c o m p u t e r r e c o r d e d a l l d a t a on m a g netic tape for subsequent processing at a central computation f a c i l i t y . S e v e r a l a d v a n t a g e s to t h i s a u t o m a t i o n
a r e o b v i o u s , but one is f o r e m o s t h e r e - - f o r the f i r s t
t i m e , it b e c a m e p r a c t i c a l to obtain m u l t i p l e m e a s u r e m e n t s on e a c h s p e c i m e n . C o l l e c t i n g t h r e e s e p a r a t e
s e t s of d a t a for each a l l o y a l l o w e d b e t t e r p r e c i s i o n
estimations.
E X P E R I M E N T A L RESULTS
To c a l c u l a t e the s t a c k i n g fault e n e r g y f r o m Eq. [2],
it i s n e c e s s a r y not o n l y to m e a s u r e t h e X - r a y p a r a m e t e r s but to know the e l a s t i c s t i f f n e s s c o e f f i c i e n t s and
1 3 4 8 - V O L U M E 6A, JULY 1975
c1~
G(t ll)
Shear Modulus
A
Anisotropy
c,2
c~
1.626
1.235
0.647
3.50
1.25
1.19
1.22
t.24
0.650
0-653
3.34
3.44
Alloy
AISI 304L
AIS1305
AtSI 310 S
AISI 316
21-6-9(melt 1)
21-6-9(melt 2)
22-13-5
Hadfield
106(e~o>lll
l03
103 (eso)ut
a
6.1 (1.4)
28.6 (7.7)
66.9 (11.6)
27.9 (15.0)
112.1 (5t.7)
68.1 (13.8)
49.7(26.I)
38.9 (5.1)
7 (2)
15 (5)
13 (2)
6 (3)
31 (9)
29 (4)
14(3)
34 (0)
1.0 (0.1)
t.9 (0.4)
5.3 (0.8)
4.4 (0.2)
3.6 (0.6)
2.3 (1 A)
3.6(1.1)
t.2 (0.1)
Stacking Fault
Energy,
7, (mJ/m:)
18 (2)
34 (7)
94 (14)
78 (6)
65 (t2)
41 (20)
64(20)
21 (2)
As noted above, the AISI 304L, AISI 305, and Hadfield s t e e l p a r t i a l l y t r a n s f o r m e d m a r t e n s i t i c a l l y ; this
could p o s s i b l y be a s o u r c e of s y s t e m a t i c e r r o r due to
s o m e line overlap. Since the AISI 304L bulk s p e c i m e n
was lightly cold worked r a t h e r than a powder, the exi s t e n c e of r e s i d u a l s t r e s s e s (not p r e s e n t in the r a n d o m l y o r i e n t e d powders) could introduce shifts in the
line positions, Assuming a r a t h e r high r e s i d u a l s t r e s s
of 30,000 psi (2.1 108 N / m 2) and a Young's modulus of
30 10~ psi (2,1 101~ N/m~), one d i m e n s i o n a l r e s i d u a l
s t r e s s calculations r e s u l t in a =e 3 10"s p o s s i b l e change
of ~, leading to an e s t i m a t e d 50 pct e r r o r of the s t a c k ing fault probability.
DISCUSSION
It has been demonstrated (Table I) that Ni raises the
stacking fault energy of F e - C r ' N i alloys and this has
been associated with its influence on dislocation cross
slip. High Ni alloys display a cellular structure of dis
locations in the austenite phase, {.e., cross slip is
easy.a'35 Several workers have examined quantitatively
the dependence of T on Ni concentration in Fe-Cr-Ni
austenitic alloys. Swarm,8 Douglass, et al, I~ and Dulieu
and Nutting,11holding the Cr concentration at 18 to 20
pct, reported an almost linear dependence on Ni concentration in the range 8 to 27 pct Ni,
[6]
[7]
[Sa]
[8b]
[8c]
[8d]
Only data f r o m d i r e c t m e a s u r e m e n t s w e r e used to o b tain Eq. [8a] to [Sd] and these a r e identified in Table I,
using [a], [b], [c], and [d] s u p e r s c r i p t s . F o r the N i - C r - C
line of Eq. [8a] Ca in Fig. 2 and Table I), only data w e r e
100 --
90
80
70
c~
"~ 60
0
50
~ 40
,<
30
20
0
O
10
I .......
.......... l
20
40
60
80
100
120
WEIGHT PERCENT COMPOSITION EQUIVALENT
a: [4+I,8(%~i)-0.2(%Cr)
b:[34+I.4(%N~)-I.O(%Cr)-76(%N)]
I
140
I00
90
80
70 - E
60 - u~
z
OQ
~- 50 - -
40 m
~o
30 --
20
I0
o
0
/
l
20
,,
40
t
60
WEIGHT PERCs
I ........
80
t
I00
....... I
120
COMPOSITION EQUIVALENT
140
c: [34
d: [32+2.4(gMi)-l.3(%Cr)-1.3(%Mn)]
and Fe-Ni-Cr-Mn.
[9]
100
90
80
REFERENCES
70
c~
e
0
~0
50
0
0
~ 40
0 ~
%o
30
0
20
I0
0 V,
20
II
Our Work
Electron Microscopy,
L i t e r a t u r e Data.
.....I........... I
40
60
80
I00
120
WEIGHT PRECENT COMPOSITION EQUIVALENT
1
140
[-53+6.2(%Ni )+0.7(%Cr)+3.2(%Mn)+9.3(%Mo)]
Fig. 4--Relationship between stacldng fault energy and FeNi-Cr-Mn-Mo composition in austenitic stainless steels.
METALLURGICAL TRANSACTIONS A
1, S. Bamartt, R, Stickler, and D. van Rooyen: Corros. Sci., 1963, voL 13,
pp. 9-16.
2, M. L Holzwor~h: Corrosion-NACE, 1969, vol. 25, pp. t07-15.
3. R. B. Benson, R. K. Dann, and L. W. Roberts: Trans. TMS-AIME, 1968, voI.
242, pp. 2199-2205.
4. P. C. J. Gallagher: Met. Trans., 1970, rot. 1, pp. 2429-61.
5. R. P. Reed and R. E. Schramm: National Bureau of Standards, Boulder,
Colorado, unpublished research, 1975.
6. M. J. Whelan, P. B. Hirsch, R. W. Home, and W. Bollmann: Proc. Roy. Soc. A,
1957, vol. 240, pp. 524-38.
7. M. J. Whelan: Proc. Roy. Soc. A, 1959, vol. 249, pp. 114-37.
8. P. R. Swarm: Corrosion, 1963, vol. 19, pp. 102t-112t.
9. J. F. Breedis: Trans. TMS-AIME, 1964, vol. 230, pp. 1583-96.
10. D, L. Douglass, G. Thomas, and W. R. Roser: Corrosion, 1964, vol. 20, pp.
15t-28t.
11. D. Dulieu and J. Nutting: Metallurgical Developments in tfigh-Alloy Steels,
pp, 140-45, Special Report 86, The Iron and Steel Institute, 1964.
t2. J. M. Silcock, R. W. Rookes, and J. Barford: J. Iron SteetlnsL, 1966, vol. 204,
pp. 623-27.
13. A. Clement, N. Clement, and P. Coulomb: Phys. Status. Solidi, 1967, voL 2l,
pp. K97-K98.
14. B. Thomas and G. Henry: Mere. Sci. Rev. Met., 1967, vol. 64, pp. 625-36.
15. B. J. Thomas: Metaux, Corrosion, lndustrie, 1969, no. 532, pp. 405-38.
16. O. Vingsbro: A cta Met., 1967, vol. 15, pp. 615-21.
17. R. Fawley, M. A. Quader, and R. A. Dodd: Trans, TMS-AtME, 1968, voL 242,
pp. 771-76.
18. R. M. Latanision and A. W. Ruff, Jr.: Jr. Appl. Phys., 1969, vol. 40, pp.
2716-20.
19, L. E. Murr: Thin Solid Films, 1969, vol. 4, pp, 389-412.
20. F. LeCroisey and B, Thomas: Phys. Status. Solidi (a), 1970, vol. 2, pp.
K217-K20.
21. R, M. Latanision and A. W. Ruff, Jr.: Met. Trans., 1971, vol. 2, pp. 505-09.
22. E, D. Butakova, K. A. Malyshev, and N. 1. Noskova: Fiz. Metal. Metalloved.,
1973, vol. 35, no. 3, pp. 662-64.
23. L. M. Brown: Phil Mag., 1964, vol. 10, pp. 441-66,
24. R. P. Reed and R. E. Schramm: J. AppL Phys., 1974, vol. 45, pp. 4705-1 h
25. R. R. Vandervoort: Metals Eng. Quart., 1972, voL 12, pp. 10-16.
26. C. J. Newton and A. W. Ruff, Jr.: J. AppL Phys., 1966, vol. 37, pp. 3860-68.
27. B. E. Warren: Prog. MetalPhys., 1959, vol. 8, pp. 14%202.
28. R. E. Schramm: National Bureau of Standards Tech. Note 600, t971.
29. C. P. Gazzara, J. J. Stiglich, Jr., F. P. Meyer, and A. M. Hansen: Advances in
X-Ray Analysis, vol. 12, pp. 257, Plenum Press, New York, 1969.
30. R. L. Rothman and J, B. Cohen: Advances in X-Ray Analysis, vol. 12, p. 208,
Plenum Press, New York, 1969.
31. Residual Stress Measurement by X-Ray Diffraction, SAE J 784a, p. 51, Society
of Automotive Engineers, New York, 1971,
32. K, Salmutter and F. Stangler: Z. Metallk., 1960, vol. 51, pp. 544-48.
33. M~ C. Mangalick and F. Fiore: Trans. TMS-AIME, 1968, vol. 242, pp. 2363-64.
34. R. P. Reed: Acta Met., 1962, vol. 10, pp. 865-77.
35. G. Thomas: Acta Met., 1963, vol. 11, pp. 1369-71.
36. R. P. Reed and J. F. Breedis: Behavior of Materials at Cryogenic Temperatures,
ASTM/STP 387, p. 60, Am. Soc. Testing Mats., 1966.
37. D. V. Neff, T. E. Mitchell, and A. R. Troiano: Trans. A&M, 1969, vol. 62,
pp. 858-68.
38. P. G. Hod: Introduction to Mathematical Statistics, p. 172, John Wiley and
Sons, Inc., New York, 1962.
39. P. G. Hoel: ibid., p. 244.
V O L U M E 6A, JULY 1 9 7 5 - 1 3 5 1