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The Strength, Fracture Toughness, and Low

Cycle Fatigue Behavior of 17-4 PH


Stainless Steel
H. J. RACK AND DAVID KALISH

The influence of m i c r o s t r u c t u r e on the strength, f r a c t u r e toughness and low cycle fatigue


behavior of 17-4 PH s t a i n l e s s s t e e l has been examined. Aging hardening involves initial
f o r m a t i o n of coherent c o p p e r - r i c h c l u s t e r s which t r a n s f o r m to incoherent fcc E-copper
p r e c i p i t a t e s upon f u r t h e r aging. The changes in strength level and s t r a i n hardening r a t e s
o b s e r v e d during aging a r e consistent with p r e v i o u s l y suggested models for p r e c i p i t a t i o n
hardening b a s e d on differing e l a s t i c moduli. The f r a c t u r e toughness and fatigue c r a c k
growth r a t e s were shown to be a function of m i c r o s t r u c t u r e and environment. At equiva-
lent strength l e v e l s overaging r e s u l t e d in a higher f r a c t u r e toughness than did underaging.
The fatigue c r a c k growth r a t e s i n c r e a s e d with i n c r e a s i n g strength level and humidity but
were not a function of toughness level. Attempts to c o r r e l a t e the fatigue c r a c k growth
r a t e s with monotonic t e n s i l e p r o p e r t i e s were unsuccessful. However when final f a i l u r e
obeyed a c r i t i c a l s t r a i n c r i t e r i a , the f r a c t u r e toughness behavior could be r e a s o n a b l y d e -
s c r i b e d and r e l a t e d to p r e f e r e n t i a l void nucleation and growth at 5 - f e r r i t e - m a t r i x i n t e r -
faces.

K.~ENERALLY, p r e c i p i t a t i o n hardening m a r t e n s i t i c e n e r g y was taken as the sum of the c r a c k initiation


s t a i n l e s s s t e e l s have higher s t r e s s - c o r r o s i o n r e s i s - e n e r g y d e r i v e d f r o m the V-notch t e s t and the c r a c k
tance and f r a c t u r e toughness than do s e m i - a u s t e n i t i c propagation e n e r g y d e r i v e d f r o m the p r e c r a c k e d t e s t s .
p r e c i p i t a t i o n hardening s t a i n l e s s s t e e l s . 1 Of the f o r - Ronald 5 has shown that this p r o c e d u r e e l i m i n a t e s the
m e r 17-4 PH is p r e s e n t l y one of the most widely used i n e r t i a l effects n o r m a l l y a s s o c i a t e d with Charpy t e s t -
a l l o y s . Although previous investigations of this m a t e - ing. The c h a r a c t e r i s t i c dimensions of the compact t e n -
r i a l have examined the g e n e r a l age hardening r e - sion s p e c i m e n s , in a c c o r d a n c e with ASTM E399-72,
sponse, 2'3 no d i r e c t r e l a t i o n s h i p s between the m i c r o - were B = 1.125 in. (2.858 cm) and W = 2.0 in. (5.08 cm).
s t r u c t u r e and the strength, f r a c t u r e toughness, or f a - The slow bend Charpy and compact tension t e s t s e m -
tigue r e s i s t a n c e have been r e p o r t e d . The p r e s e n t in- ployed a e r o s s h e a d speed of 0.04 t n . / m i n (0.1 em/mtn)
vestigation was undertaken to e s t a b l i s h these r e l a t i o n - while tenstle t e s t s involved an Initial s t r a i n r a t e of 2.9
ships. • 10-2/min; a l l t e s t s were at room t e m p e r a t u r e .
Fatigue c r a c k growth r a t e s were m e a s u r e d with c o m -
EXPERIMENTAL PROCEDURES pact tension s p e c i m e n s with a T - L orientation, a The
e h a r a e t e r i s t l e dimensions were B = 0.35 in. (0.89 era)
The 17-4 PH s t a i n l e s s s t e e l used in this study was and W = 4.0 in. (10.16 cm). The t e s t s involved stnu-
m i l l - p r o c e s s e d and annealed plate, Table I. All heat soidal t e n s i o n - t e n s i o n loading (R = 0.1) at 10 c y c l e s
t r e a t m e n t s were p e r f o r m e d in ultrahigh p u r i t y argon. p e r second. The t e s t s were p e r f o r m e d in d r y argon
Solution annealing at 1900~ (1038~ was followed by (99.999 pet pure) and water s a t u r a t e d argon. The d r y
subcooling to 32~ (0~ to a s s u r e complete f o r m a t i o n a t m o s p h e r e was obtained by p a s s i n g ultrahigh p u r i t y
of m a r t e n s i t e . argon (dew point - 100~ through a d r y i n g agent just
The t e n s i l e and f r a c t u r e toughness p r o p e r t i e s were p r i o r to entering the specimen chamber, while water
e s t a b l i s h e d using a) 0.250 in. (0.635 cm) diam smooth s a t u r a t e d argon was obtained by slowly bubbling the
b a r t e n s i l e s p e c i m e n s f r o m the long t r a n s v e r s e d i r e c - gas through boiling water. A complete d e s c r i p t i o n of
tion, b) Charpy V-notch s p e c i m e n s with an L-S o r i e n - the data collection and a n a l y s i s techniques ts given
tation 4 and c) compact tension s p e c i m e n s with a T - L elsewherefl
orientation 4 machined in a c c o r d a n c e with ASTM Stan- Standard techniques were used to p r e p a r e s p e c i m e n s
d a r d E399-72. The Charpy s p e c i m e n s were t e s t e d at for light and 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 . 7 The
r o o m t e m p e r a t u r e in impact in the s t a n d a r d V-notch f r a c t u r e s u r f a c e s of v a r i o u s t e s t s p e c i m e n s were a l s o
configuration and with a fatigue p r e c a r c k at the root examined by scanning e l e c t r o n m i c r o s c o p y .
of the notch. Charpy V-notch and p r e c r a c k e d s p e c i -
mens were also t e s t e d in 3-point slow bending in o r -
d e r to s e p a r a t e the initiation and propagation s t a g e s Table I. Chemical Compositions
of f r a c t u r e . The slow bend c o r r e c t e d total f r a c t u r e
Element (wt. pct)
Form Cr Ni Cu C kin P S Si Cb Ta
H. J. RACKis Member of Technical Staff, Sandia Laboratories,
Albuquerque, N. Mex. 87115. DAVIDKALISHis Member of Techni- 5/8in. plate 15.8 4.25 3.46 0.037 0.24 0.015 0.015 0.60 0.29 0.01
cal Staff, BellTelephone Laboratories, Norcross,Ga. 30071. 188 plate 15.55 4.52 3.440.040 0.30 0.016 0.015 0.60 0.26 0.01
Manuscript submitted October 31, 1973.

METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1974- 1595


RESULTS Aging below 900~ (482~ does not p e r c e p t i v e l y a l -
Microstructure t e r the m i c r o s t r u c t u r e although some p r e c i p i t a t i o n was
o b s e r v e d after aging for 1 h at 900~ (482~ Fig. 2(a).
Unaged 17-4 PH s t a i n l e s s steel is a mixture of a - The e x t r e m e fineness of the p r e c i p i t a t e p r e c l u d e d its
m a r t e n s i t e and 6 - f e r r i t e , Fig. l(a). The m a r t e n s i t e identification by s e l e c t e d a r e a diffraction. Slight o v e r -
m a t r i x is equiaxed while the 6 - f e r r i t e phase is elon- aging, at 950~ (510~ for 1 h, r e v e a l e d an fcc c o p p e r -
gated in the p r i o r working d i r e c t i o n (Point At. Large rich e-phase, Fig. 2(b). Overaging at l l 0 0 ~ (593~
s i l i c a t e s t r i n g e r s were also noted (Point B). The m a r - confirmed this identification, Fig. 2(c). In a l l c a s e s ,
t e n s i t e m a t r i x in a i r cooled 17-4 PH is s i m i l a r to that the e-phase was s p h e r i c a l .
in 18 Ni m a r a g i n g steel. 8 It is a p r e c i p i t a t e - f r e e lath 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 r e v e a l e d that 5-
m a r t e n s i t e o c c a s i o n a l l y containing m i c r o - t w i n s , Fig. f e r r i t e contained a p r e c i p i t a t e which was unaffected
lib). The globular inclusions, which tend to lie on by aging, Fig. 3. These p a r t i c l e s a r e NbC, which
p r i o r austenite or a u s t e n i t e - 6 f e r r i t e boundaries, a r e f o r m e d during solidification and p r i o r hotworking.
p r o b a b l y M23C6 c a r b i d e s . 9 Finally, the 5-5 and 5 - m a t r i x b o u n d a r i e s exhibit p r e -
cipitate f r e e zones, with M2sC6 lying at the b o u n d a r i e s . 9

Mechanical P r o p e r t i e s
Aging 17-4 PH s t a i n l e s s s t e e l for 1 h between 800~
(428~ and l l 0 0 ~ (593~ r e s u l t s in a m a r k e d strength
i n c r e a s e above that o b s e r v e d in the solution heat t r e a t e d
condition, Fig. 4. This strength i n c r e a s e is not a c c o m -
panied by any significant d e c r e a s e in the t e n s i l e d u c t i l -
ity (elongation and r e d u c t i o n - i n - a r e a ) , although a slight
d e c r e a s e in r e d u c t i o n - i n - a r e a o c c u r s at the highest
strength. The s t r a i n hardening exponent is a l s o a func-
tion of aging t r e a t m e n t , d e c r e a s i n g from 0.099 to 0.082
to 0.014 as the aging t e m p e r a t u r e is i n c r e a s e d from
800~ (427~ to 900~ (482~ to l l 0 0 ~ (593~ re-
spectively.
The r e s u l t s of the f r a c t u r e toughness t e s t s a r e s u m -
m a r i z e d in Tables II and III. The f r a c t u r e toughness
of 17-4 PH, as m e a s u r e d by e i t h e r a s t a n d a r d Charpy
or fatigue p r e c r a c k e d impact test, indicates a b r o a d
minimum upon aging at 800~ (428~ to 900~ (482~
The c o r r e c t e d Charpy slow bend f r a c t u r e energy shows
a distinct minimum after aging at 900~ (482~ i.e.,
at the maximum strength. This minimum is due p r i -
m a r i l y to a minimum in the c r a c k propagation energy;
the c r a c k initiation e n e r g y is l e s s s e n s i t i v e to aging,
Table III.
Finally, the c o r r e c t e d slow bend e n e r g y and KIC
(KQ for the l l 0 0 ~ (593~ aging) both indicate that, at
an equivalent strength, overaging y i e l d s higher f r a c -
t u r e toughness than does underaging.
Over a l i m i t e d c r a c k growth range, the fatigue data,
Fig. 5, can be d e s c r i b e d in t e r m s of a power r e l a t i o n -
ship:
,~t / ,~Y = A (Me) rn [1]
The values for A and m a r e given in Table IV. Only
the growth region between 10-7to 10-Sin./cycle (2.54 • -9
to 2.54 • 10 -7 m / c y c l e ) was c o n s i d e r e d since a) non-plane
s t r a i n propagation o c c u r s above this r a t e tn s p e c i m e n s

Table II. Charpy Impact Energei$

V-Notched Precracked
AgingTemp in-lb/in2 (103 m'N/m2) in-lb/in2 (103 m'N/m 2)
As-solutionized 2710(475) 2000(350)
800~ (428~ 813(142) 184(32)
900~ (482~ 834(146) 576(101)
Fig. 1--Unaged 17-4 PH s t a i n l e s s steel. (a) Light m i c r o g r a p h 950~ (510~ 2110(370) 1550(271)
of section n o r m a l to long t r a n s v e r s e grain direction. Point A-- 1000~F (538~ 3090(541) 1790(314)
delta f e r r i t e , Point B - - s i l i c a t e s t r i n g e r . (b) T r a n s m i s s i o n e l e c - 1100~ (593~ 3070(532) 2470(433)
tron micrograph.

1596-VOLUME 5, JULY 1974 METALLURGICAL TRANSACTIONS


aged at 800~ (428~ and II00~ (593~ and b) fast mental conditions. This AK level, (~xKICF), the cor-
fracture occurred above this range in specimens aged rosion fatigue limit, is given by: I~
at 900~ (482~
AKIc F ~- (1.7 =L0.2) 10-4E (ivTm.) [2]
At low AK, i.e., propagation rates less than 10-7
in./cycle (2.54• 10-9 m/cycle), the fatigue crack growth Applying Eq. [2] to the fatigue crack growth behavior
rates are independent of environment. Speidel et al. ~~ of 17-4 PH stainless steel with E = 29.3 x 106 psi (202
have suggested that below a certain AK level, which xl03 MN/me) predicts that AKIc F ~ 5.0 ksi i~-n-~. (5.5
depends only on the elastic modulus (E), the fatigue MNm-3/z). This is in excellent agreement with the
crack growth rate should be insensitive to environ- present experimental results, Fig. 5.

Fig. 2--Transmission electron micrographs of 17-4 PH stain-


less steel aged 1 h at (a) 900~ (482~ (b) 950~ (510~ and
(c) I100~ (593~

METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1 9 7 4 - 1597


Table III. Charpy Slow Bend and Plane-Strain Fracture Toughness

Crack Initiation Energy Crack Propagation Energy Corrected Total Fracture Energy KIC
Aging Temp in.lb/in 2 (10 a N-m/m2) in-lb/in2 (103 N.m/m 2) in-lb/in2 (103 N.m/m 2) ksi ~/~ (MNm"3/2)

As-solutionized 689 (121) 1669 (292) 2358 (413) - -


800~ (428~ 946 (166) 1800 (315) 2746 (481) 79.5 (87.4)
900~ (482~ 570 (100) 286 (50) 856 (150 43.9 (48.2)
1100~ (593~ 571 (100) 2053 (360) 2624 (460) 108.2 (119)*
*Test did not meet ASTM requirements for valid KICdetermination.

AGING TEMPERATURE(~
Table IV. Fatigue Crack Growth Rate Law Constants _~ 425 4/5 525 5/5 625
-- 250 I 1 i i I 15
Relative AGING TIME: 1 HR
Aging Temp Humidity, pct log A m REDUCTION IN AREA
(READ RIGHT)
0 -17.2 2.7 ].50(]-
800~ (428~ 100 -20.3 3.5
0 -20.7 3.6 21111 50
900~ (482~ 100 -22.5 4.1 ~,~-'~T,,,,~r ULTIMATE STRENGTH
0 -18.2 2.9
1100~ (593~ 100 -21.5 3.8
eL.
t~

i000 150 f# - 0.2~ YIELD STRENGTH


(READ LEFT)

ELONGATION
(READ RIGHT)
I I I I 0
800 900 i000 II00 1200
AGING TEMPERATURE(~
Fig. 4 - - I n f l u e n c e of aging t e m p e r a t u r e on t e n s i l e p r o p e r t i e s
of 17-4 PH s t a i n l e s s s t e e l .

i.e., 900~ (428~ and ll00~ (593~ where Carter


et al z showed that KISCC > 0 . 8 5 KIC. Thus, the effects
of s t r e s s corrosion cracking and of fatigue crack
growth in an inert environment z~-~s cannot be s u p e r -
imposed in 17-4 PI-I stainless steel and a high s t r e s s
corrosion resistance does not presuppose an environ-
mentally insensitive fatigue crack growth behavior.
At high ~ levels, the rate of change of the crack
growth rates in specimens aged at 800~ (428~ and
ll00~ (593~ decreased. This transition occurs in
either inert or corrosive atmospheres. If no environ-
ment effects are involved and if this transition is due
to a gradual deviation from plane strain crack propa-
gation, then the s t r e s s intensity, K m a x , associated
with the initial departure from plane strain conditions
can be estimated from: 14
Fig. 3 - - T r a n s m i s s i o n e l e c t r o n m i e r o g r a p h of (5 p h a s e in 17-4
PH aged for 1 h at 950~ (510~
ayB z/2
Kmax - 1.58 [3]

The principal influence of the humid environment where B is the specimen thickness and ay is the yield
on the fatigue crack growth involves plane strain crack strength. Application of Eq. [3] indicates that Kma x
propagation. Increasing the humidity increases the ~ 57 ksi i~]~:-. (62.5 MNm -s/2) for test specimens aged
growth rate. Table IV does indicate that the environ- at 800~ (428~ and ll00~ (593~ Experimentally
mental effects appear to be more pronounced after the ~ levels associated with the initial decrease in
aging at either 800~ (428~ or ll00~ (593~ than slope of the fatigue crack growth rate curve when the
after aging at 900~ (482~ However, the absolute fatigue tests were c a r r i e d out in an inert atmosphere
crack growth rate, at any given ~ level, is always are far below these calculated values. Indeed, when
greater following the latter aging treatment. It should the tests were performed in 100 pct humidity, this de-
be noted also that the influence of environment on the c r e a s e in slope occurred at still lower ~ levels. This
fatigue crack growth rate includes aging treatments, indicates that the decrease in crack growth rate at high

1598 -VOLUME 5, JULY 1974 METALLURGICAL TRANSACTIONS


AK levels cannot be due to a simple departure from ture. Following aging, the fracture surface was even
plane strain crack propagation. more complex, the dimple sizes being smaller and
highly nonuniform, Fig. 6(b).
Tensile and impact loading of notched and p r e -
Fractography cracked 17-4 PH resulted in some quasi-cleavage
The fracture appearance depends upon heat t r e a t - failure, the amount depending upon the prior heat
ment and s t r e s s state. Tensile failure of smooth spec- treatment, Fig. 7. Although microvoid coalescence
imens occurred by transgranular dimple rupture inde- predominated when specimens were aged at 800~
pendent of heat treatment, Fig. 6(a). However, heat (428~ and ll00~ (593~ large amounts of quasi-
treatment did influence the dimple sizes and distribu- cleavage failure (Point A) were observed in speci-
tion. The as-solutionized condition was characterized mens aged at 900~ (482~ Parting plane cracks
by relatively uniform dimples, the l a r g e r dimples be- (Point C) which appeared to be related to the p r e s -
ing associated with bulk particles, presumably silicates, ence of 6-ferrite and presumably a r o s e when an ad-
while the smaller dimples had a dispersoid free s t r u c - vancing crack front encountered a 5-~ interface were

K (MN -m3/2) A K (MN m-3/2)


10 20 40 70 100 70 100
10-3 10-3 10 20 40
{ I I I
{~] i0-5
I I I i IN_ 10-5
9 DRY ARGON { [" DRY ARGON ]
[] I00~ HUMIDITY I {'- [~ 100~ HUMIDITY J]
i0 -4
:.
L7 9
__ 10-6 10-6
} 9
-~ i0"5 d 10-5 d
d
i0-7 10-7
W-
10-6
lO-s ~ 10-8

104 f 10-7 { - ~
t.0

R = 0. i {- 10-9 II R =0.1
~a: i0 cps
1-- i0 -9
w = i0 cps I
10-8 ,,,[ ,,,l , ,,l, ,,,I,,,,,I 10-8 l l ,l I I ,,I , , , I ,,,Jl,,,,,l, ,
96 I0 20 40 70 i00 6 I0 20 40 lO i00
A K (ksi-in. I12) d K (ksi - in. 1/2)
(a) (b)

AK(MN m-312)
10 20 40 70 100
i0-3

DRY ARGON
i00~ HUMIDITY
IO -4 - - D~'.~:

10-6
d
10-5 6
10-7 Fig. 5 - - F a t i g u e c r a c k g r o w t h r a t e d e p e n d e n c e on s t r e s s i n -
t e n s i t y r a n g e f o r 17-4 PH s t a i n l e s s s t e e l aged f o r 1 h at (a)
800~ (428~ (b) 900~ (482~ (c) l l 0 0 ~ (593~
i0 -6
O
10-8
r

10-7
FD
-9
I R=0.1 -- 10
I (A 10 cps
10-8 1 ,,,1 ,,I]{ I ,]lll, I,,,,,I , L
10 20 40 70 100
K (ksi-in. I12)
(:)

METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1974-1599


also o b s e r v e d in unaged, underage and o v e r a g e d 17-4 gon environment were c h a r a c t e r i z e d by ductile fatigue
PH, Fig. 7(a). s t r i a t i o n s , Fig. 9. However some s e c o n d a r y c r a c k i n g
The influence of heat t r e a t m e n t on fatigue c r a c k was o b s e r v e d at high AK l e v e l s when these heat t r e a t -
propagation is evident on both a m a c r o s c o p i c and m i - ments were t e s t e d in 100 pct humidity, Fig. 10.
c r o s c o p i c s c a l e . Macroscopic examination showed While ductile fatigue s t r i a t i o n s were o b s e r v e d at
that at high AK l e v e l s a deviation from p l a n e - s t r a i n low ZkK l e v e l s in s p e c i m e n s aged at 900~ (482~ in-
c r a c k propagation o c c u r r e d in those s p e c i m e n s aged c r e a s i n g amounts of q u a s i - c l e a v a g e f a i l u r e were ob-
at 800~ (428~ and l l 0 0 ~ (593~ Fig. 8. This d e - s e r v e d with i n c r e a s i n g 5Jr level, Fig. 11. F u r t h e r m o r e
p a r t u r e f r o m c r a c k growth n o r m a l to the applied t e n - at equivalent 5K l e v e l s t e s t i n g in 100 pct humidity r e -
s i l e axis is thought to have manifested itself in the sulted in s t i l l f u r t h e r i n c r e a s e s in the amounts of q u a s i -
d e c r e a s e in the r a t e of change of the c r a c k growth cleavage c r a c k propagation, Fig. 12.
r a t e s p r e v i o u s l y alluded to, i.e., the calculation of K
is invalid when c r a c k growth is not n o r m a l to the a p - DISCUSSION
plied t e n s i l e load. Aging at 900~ (482~ r e s u l t e d in
Age Hardening
plane s t r a i n c r a c k propagation throughout. All fatigue
c r a c k growth on a m i c r o s c o p i c s c a l e was t r a n s g r a n u - The p r e c i p i t a t i o n sequence o b s e r v e d in 17-4 PI-I
l a r . Growth in s p e c i m e n s aged at 800~ (428~ and s t a i n l e s s s t e e l is e s s e n t i a l l y that p r e v i o u s l y o b s e r v e d
l l 0 0 ~ (593~ and t e s t e d in e i t h e r the d r y or wet a r - in F e - C u and F e - C u - X a l l o y s . 15-22 Briefly, this in-

Fig. 6--Scanning electron fractographs of 17-4 PH stainless Fig. 7--Scanning electron fractographs of 17-4 PH stainless
steel tested in tension following aging at (a) 75~ (25~ and steel tested in impact following aging at (a) 75~ (25~ and
(b) 900~ (482~ (b) 900~ (482~

1600-VOLUME 5, JULY 1974 METALLURGICALTRANSACTIONS


v o l v e s the i n i t i a l f o r m a t i o n of c o h e r e n t c o p p e r - r i c h c o h e r e n c y s t r a i n s a s s o c i a t e d with p r e c i p i t a t i o n a r e
c l u s t e r s which t r a n s f o r m to i n c o h e r e n t fcc e - c o p p e r m i n i m a l . In e i t h e r c a s e , the age h a r d e n i n g of 17-4 PH,
p r e c i p i t a t e s upon f u r t h e r aging. Youle and Ralph TM F e - C u , and F e - C u - X a l l o y s m u s t depend on s o m e t h i n g
showed that c o h e r e n t c o p p e r - r i c h c l u s t e r s ( ~ 204) o t h e r than e l a s t i c s t r a i n s a s s o c i a t e d with the p r e c i p i -
r e s u l t in m a x i m u m h a r d n e s s in F e - C u a l l o y s . T h e s e t a t e . This fact is r e e m p h a s i z e d when the influence of
p a r t i c l e s cannot be o b s e r v e d using s t a n d a r d t r a n s m i s - a g i n g on the w o r k h a r d e n i n g r a t e is c o n s i d e r e d . The
s i o n e l e c t r o n m i c r o s c o p y t e c h n i q u e s . This d i f f i c u l t y u s u a l r a p i d i n c r e a s e in w o r k h a r d e n i n g r a t e n o r m a l l y
s u g g e s t s that t h e s e c o p p e r - r i c h c l u s t e r s have the s a m e a s s o c i a t e d with o v e r a g i n g is a b s e n t in t h e s e s y s t e m s .
c r y s t a l s t r u c t u r e a s the m a t r i x (i.e., b c c ) o r that the Knowles and K e l l y 23 and R u s s e l l and Brown u r e c e n t l y
p r o p o s e d t h a t the age h a r d e n i n g b e h a v i o r of F e - C u a l -
l o y s can be e x p l a i n e d b y the i n t e r a c t i o n b e t w e e n a m a -
t r i x d i s l o c a t i o n and a s e c o n d p h a s e p a r t i c l e with a d i f -
f e r e n t s h e a r modulus than the m a t r i x . Knowles and
K e l l y 2s noted that one t e s t of this h y p o t h e s i s r e q u i r e s
that the p a r t i c l e s have the s a m e c r y s t a l s t r u c t u r e a s
the m a t r i x . This c r i t e r i o n m a y have b e e n v i o l a t e d in
the two s t u d i e s c i t e d . T h e y both c o n s i d e r e d F e - C u a l -
l o y s a g e d to a s t a g e w h e r e p r e c i p i t a t e p a r t i c l e m e a -

Fig. 9--Scanning electron fractographs of fatigue crack prop-


agation in 17-4 PH stainless steel tested in 100 pct humidity
following aging at 1100~ (593~ Arrow denotes macroscopic
fatigue crack growth directions.

Fig. 8 - - M a e r o g r a p h s of 17-4 PH s t a i n l e s s steel fatigue c r a c k Fig. 10--Secondary c r a c k i n g in 17-4 PH s t a i n l e s s steel t e s t e d


growth s p e c i m e n s t e s t e d in dry argon following aging at (a) in 100 pct humidity following aging at l l 0 0 ~ (593~ Arrow
800~ (428~ and (b) l l 0 0 ~ (593~ denotes m a c r o s c o p i c fatigue c r a c k growth directions.

METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1974-1601


s u r e m e n t s b y T E M could be o b t a i n e d . Our r e s u l t s
i n d i c a t e that when the p r e c i p i t a t e p a r t i c l e s a r e v i s i b l e ,
t h e y a r e fcc e - c o p p e r p r e c i p i t a t e s in the b c c m a t r i x .
P e r h a p s the r e q u i r e m e n t of i d e n t i c a l m a t r i x and p a r -
t i c l e c r y s t a l s t r u c t u r e is of s e c o n d a r y i m p o r t a n c e in
F e - C u s y s t e m w h e r e c o m p l i c a t i o n s due to l o c a l o r d e r -
ing within the p r e c i p i t a t e p a r t i c l e a r e not e x p e c t e d .
The o t h e r c r i t e r i a f o r s h e a r m o d u l u s h a r d e n i n g , d i f -
f e r e n t s h e a r m o d u l i i b e t w e e n m a t r i x and p a r t i c l e and
a s m a l l s i z e d i f f e r e n c e b e t w e e n p a r t i c l e and m a t r i x
a t o m , m a y b e of o v e r r i d i n g i m p o r t a n c e in F e - C u t y p e
alloys.
Knowles and K e l l y 23 i n d i c a t e d that A~, the s t r e s s
n e c e s s a r y to f o r c e a d i s l o c a t i o n p a s s e d the p r e c i p i -
t a t e p a r t i c l e s , is given b y :
(6
- --T~\0x / m a x \ ~r ! [4]
w h e r e A g = ~ m a t r i x - ~particle, f is the p r e c i p i t a t e
v o l u m e f r a c t i o n , b is the B u r g e r s v e c t o r of the d i s l o -
c a t i o n and (OE/Ox)max i s the m a x i m u m v a l u e of the
s l o p e of the e n e r g y / d i s t a n c e c u r v e for s p h e r i c a l p a r -
t i c l e s of r a d i u s R . It should b e noted that the r e l a t i o n -
s h i p b e t w e e n b (0E/Ox)ma x and (R/b) a l s o d e p e n d s upon
the e f f e c t i v e c o r e r a d i u s , ro, of the d i s l o c a t i o n c u t t i n g
the p a r t i c l e , s e e F i g . 1 of Ref. 23. Since the m a x i m u m
s t r e n g t h e n i n g m u s t c o r r e s p o n d to a m a x i m u m in a
b (aE/aX_)ma x v s (R/b) c u r v e , Eq. [4] m a y b e i n v e r t e d
and b (OE/Ox)max e v a l u a t e d if we a s s u m e that a l l of the
c o p p e r not in s o l i d s o l u t i o n at the a g i n g t e m p e r a t u r e
is a s s o c i a t e d with c o p p e r c l u s t e r s , and that A~ is the
d i f f e r e n c e b e t w e e n the unaged and a g e d s t r e n g t h . A p -
p l i c a t i o n of t h i s s t r e n g t h e n i n g m o d e l to 17-4 PH s t a i n -
l e s s s t e e l a g e d at 900~ (482~ p r e d i c t s that R / b u 6
when r o = 2b. This v a l u e of R a g r e e s quite well with
the r e c e n t r e s u l t s of Youle and Ralph. 19 Eq. [4] can
now b e a p p l i e d to the 1100~ (593~ a g i n g condition
b y u s i n g the s a m e c o r e r a d i u s and the c a l c u l a t e d v a l u e
Fig. ll--Scanning electron micrograph of fatigue crack propa- of b (• 9 This r e s u l t s in a p r e d i c t e d (R/b)
gation in 17-4 PH stainless steel tested in dry argon following --- 60, a g a i n in good a g r e e m e n t with p a r t i c l e s i z e m e a -
aging at 900~ (482~ (a) A/f 2. 19 ksi i~/~n. (20 9 MNm -3/2) s u r e m e n t s on o v e r a g e d 17-4 PH, s e e Fig. 2(c). T h e s e
(b) ZkK ~ 25 ksi'l~n. (27.5 MNm -3 2). Arrows denote macro- r e s u l t s s u p p o r t the c o n c l u s i o n that p a r t i c l e cutting is
scopic crack growth directions. the p r e d o m i n a t e d e f o r m a t i o n m e c h a n i s m in 17-4 PH
s t a i n l e s s s t e e l and that at l e a s t within the a g i n g r e -
g i m e i n v e s t i g a t e d , the s l i p mode i s i n d e p e n d e n t of h e a t
treatment.

F a t i g u e C r a c k Growth
Although Hahn et al ~5 have s u g g e s t e d t h a t fatigue
c r a c k growth r a t e s in s t e e l s a r e i n s e n s i t i v e to y i e l d
s t r e n g t h , c o m p o s i t i o n , and d u c t i l i t y , t h e y do s u g g e s t
that t h e s e f a c t o r s a r e i m p o r t a n t in a l u m i n u m b a s e
a l l o y s . 26 The p r e s e n t r e s u l t s , Fig. 5 and T a b l e IV,
show that the growth r a t e s in 17-4 PH s t a i n l e s s s t e e l
b e t w e e n 10 -7 and 10 -5 i n . / c y c l e (2.54 x 10 -9 and 2.54
• 10 -7 m / c y c l e ) are a function of y i e l d s t r e n g t h . Indeed
the y i e l d s t r e n g t h effect on growth r a t e is m o r e p r o -
nounced in d r y a r g o n than in 100 pct h u m i d i t y . How-
e v e r , when 17-4 PH is a g e d at 800~ (427~ o r
l l 0 0 ~ (593~ to a c o n s t a n t s t r e n g t h l e v e l , ~ 150 k s i
(1032 MN/m2), but not to a c o n s t a n t KIC l e v e l , the
Fig. 12--Scanning electron micrograph of fatigue crack prop- fatigue c r a c k growth r a t e s a r e c o m p a r a b l e . It should
agation in 17-4 PH stainless steel tested in 100 pct humidity b e noted that the c o m p a r i s o n s in 17-4 PH a r e b a s e d
following aging at 900~ (482~ Arrow denotes macroscopic on a s y s t e m w h e r e the s l i p mode, a s noted above, is
crack growth direction. unaffected b y h e a t t r e a t m e n t . T h i s e l i m i n a t e s the
1602-VOLUME 5, JULY 1974 METALLURGICAL TRANSACTIONS
c o m p l i c a t i n g f a c t o r of r e l a t i n g s l i p c h a r a c t e r a s w e l l AGING TEMPERATURE(o C)
a s y i e l d s t r e n g t h and f r a c t u r e t o u g h n e s s to the growth 450 500 550 600
I I i I

rate. o 100%HUMIDITY
V a r i o u s o t h e r i n v e s t i g a t o r s have s u g g e s t e d t h a t i10-7
9 DRY ARGON
the c o e f f i c i e n t A in Eq. [1] m a y be r e l a t e d to such
m e c h a n i c a l b e h a v i o r p a r a m e t e r s a s the y i e l d 10-4
s t r e n g t h , f r a c t u r e t o u g h n e s s , t e n s i l e d u c t i l i t y , Young's
10-8
m o d u l u s , and s t r a i n h a r d e n i n g c o e f f i c i e n t . 1x'27-s5 A

A
T a b l e V s u m m a r i z e s the r e l e v a n t p r o p e r t i e s d e t e r - o~

m i n e d d u r i n g t h i s i n v e s t i g a t i o n which can be u t i l i z e d 10-5 E


.E
to e v a l u a t e fatigue c r a c k growth m o d e l s . Young's
10-9 ~
m o d u l u s is i n d e p e n d e n t of h e a t t r e a t m e n t (within e x -
p e r i m e n t a l a c c u r a c y ) so that a m o d e l which a t t r i b u t e s
m
AK = 10.0ksi iVr~n
. 1 0 -6
d i f f e r e n c e s in growth r a t e to d i f f e r e n c e s in m o d u l i
a l o n e is not a p p l i c a b l e . F u r t h e r m o r e , m o d e l s which 10-10
s u g g e s t an i n v e r s e r e l a t i o n s h i p b e t w e e n y i e l d o r u l t i -
m a t e t e n s i l e s t r e n g t h and growth r a t e a r e a l s o not AK = 6.0 ksi iVq'n'n
c o n s i s t e n t with the e x p e r i m e n t a l r e s u l t s . T h e s e c r i - 10-/
t e r i a e l i m i n a t e the m o d e l s p r o p o s e d b y P e a r s o n , 3z 10-11
McClintock, s~ and M c E v i l y and Wei. zl
T h r o o p and M i l l e r ~ have shown t h a t the o t h e r m o d - 10-8 , , , /
e l s c a n be e x a m i n e d b y c o n s i d e r i n g the influence of 800 900 1000 1100
a g i n g t e m p e r a t u r e on the g r o w t h c o e f f i c i e n t , A. F i g . AGINGTEMPERATURE(oF)
13 i s a r e p l o t of o u r p r e s e n t r e s u l t s and shows that
Fig. 1 3 - - F a t i g u e c r a c k g r o w t h r a t e s at c o n s t a n t zkK a s a f u n c -
a t c o n s t a n t AK, the c r a c k growth r a t e s go t h r o u g h a tion of a g i n g t e m p e r a t u r e .
m a x i m a upon a g i n g at 900~ (482~ If at f i r s t we
a s s u m e t h a t m in Eq. [1] is i n d e p e n d e n t of h e a t t r e a t -
AGING TEMPERATURE(~
ment, then an e v a l u a t i o n of A a s a function of a g i n g
t e m p e r a t u r e should e x h i b i t a d e p e n d e n c e s i m i l a r to 450 500 550 600
I I I I

t h a t of the growth r a t e . F i g . 14 p o r t r a y s the c a l c u l a - o KRAFFT(REF. 331


t i o n a l r e s u l t s of four m o d e l s p r o p o s e d b y M c E v i l y and + THROOPAND MILLER(REF.28) A
[] McCLINTOCK (REF. 29) ,/~
Johnston, 27 Krafft, 33 T h r o o p and M i l l e r , 28 and M c C l i n -
tock. 2e H e r e i n the q u a n t i t y C, which is p r o p o r t i o n a l to 10-16 O Mc EVILY AND JOHNSTON , /
(~EF. 271
A , the growth c o e f f i c i e n t , is p r e s e n t e d a s a function of
a g i n g t e m p e r a t u r e . M c E v i l y and J o h n s t o n ' s m o d e l was
e v a l u a t e d b y a s s u m i n g that the s t r a i n h a r d e n i n g b e h a v -
10-1/ E( ou + ay) a 2
u( u I0-23
i o r of 17-4 PH is d e s c r i b e d b y an e x p r e s s i o n of the
f o r m a = K E n , and that Eu, the e n g i n e e r i n g s t r a i n at I 1
n e c k i n g , is equal to e n - 1. C ~E2a2u( 2f
At low AK l e v e l s , M c C l i n t o c k ' s function a d e q u a t e l y
10-30 1 10-24
d e s c r i b e s the s h a p e of the c r a c k growth r a t e v e r s u s
a g i n g c u r v e while a t high AK l e v e l s t h a t of T h r o o p and
M i l l e r p r o v i d e s the b e s t d e s c r i p t i o n . H o w e v e r none of
t h e s e m o d e l s a g r e e s with o u r r e s u l t s o v e r the e n t i r e
10-31 1 10-1/
AK r a n g e i n v e s t i g a t i o n . In a d d i t i o n T a b l e IV shows
t h a t o u r a s s u m p t i o n of a c o n s t a n t m in Eq. [1] is i n - Ea KIC
31,34 35
c o r r e c t . Although T o m k i n s and c o - w o r k e r s '
have e x t e n d e d t h e s e a n a l y s i s b y t a k i n g into account 10-32 I = J = 10-18
the s t r a i n h a r d e n i n g c h a r a c t e r i s t i c s of m a t e r i a l s , 800 900 1000 1100
t h e i r a n a l y s i s a) is l i m i t e d to l a r g e s t r a i n a m p l i t u d e s AGI NG TEMPERATURE(~
and b) i n d i c a t e s that m is a s i n g l e d v a l u e d p a r a m e t e r F i g . 1 4 - - I n f l u e n c e of a g i n g t e m p e r a t u r e on C: [ d a / d N
-~ 2. Again the p r e s e n t i n v e s t i g a t i o n h a s shown that = A(ZkK)m]; A = (eonst)C.

Table V. Numerical Parameters for Growth Rate Evaluation

.y % F. K~c
Aging Temp ksi (MN/m2) ksi 0dN/m 2) n* psi (10 a MN/m2) ksi V ~ (bin m "312) e;

800~ (427~ 150 (1034) 176 (1214) 0.099 29.3 X 106 (202) 79.5 (87.4) 0.77
900~ (482~ 176 (1214) 200 (1379) 0.082 29.3 X 106 (202) 43.9 (48.2) 0.65
1100~ (593~ 156 (1076) 162 (1117) 0.014 29.3 X 106 (202) 108.2 (119.0) 0.83
*From o = Ke n over the plastic strain range 0.002 to 0.004.
re/- -~ ln(1/I-RA).

METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1 9 7 4 - 1603


m is a function of yield strength and environment. In
s u m m a r y , none of the models p r e s e n t e d to date can ex-
plain the influence of m i c r o s t r u c t u r e on the fatigue
ZCzc=/-- v- L e [8]
c r a c k growth behavior of 17-4 PH s t a i n l e s s s t e e l . Any
where the t e r m s a r e as defined above. Eq. [7] p r e d i c t s
i m p r o v e d model must c o n s i d e r the influence of m i c r o -
that d t equals 14.0 and 31.6 ~ for 17-4 PH s t a i n l e s s
s t r u c t u r e on both rn and A as defined in Eq. [1]. The
s t e e l aged at 800~ (428~ and l l 0 0 ~ (493~ re-
most p r o m i s i n g approach to date a p p e a r s to be that of
spectively. These values of d t a r e well within the
Tomkins, where the cyclic s t r a i n hardening behavior of
the m a t e r i a l just in advance of a propagating fatigue range of spacings o b s e r v e d for 5 - f e r r i t e p a r t i c l e s
c r a c k is c o n s i d e r e d . in 17-4 PH, s e e Fig. 5. F r a c t o g r a p h i c evidence, Fig.
7(a), a l s o suggest that 5 - ~ i n t e r f a c e s may be planes
of weakness and thus may s e r v e as void nucleation
F r a c t u r e Toughness s i t e s in 17-4 PH. Indeed it is well known that the f r a c -
t u r e toughness of this alloy is quite s e n s i t i v e to s p e c i -
Several models have been p r o p o s e d to explain the men orientation and section s i z e and this s e n s i t i v i t y
influence of m i c r o s t r u c t u r e , and in turn the t e n s i l e is d i r e c t l y r e l a t e d to the amount and d i s t r i b u t i o n of
p r o p e r t i e s , on the plane s t r a i n f r a c t u r e toughness of the r e t a i n e d 5 f e r r i t e . 39
high strength m a t e r i a l s . All of these models a s s u m e
that final f a i l u r e involves m i c r o v o i d c o a l e s c e n c e and
obey a c r i t i c a l s t r a i n c r i t e r i a . Although t e n s i l e f a i l - C ONC LUSIONS
ure of smooth s p e c i m e n s in 17-4 PH a p p e a r s to obey 1. Age hardening of 17-4 PH involves initial f o r m a -
these r e q u i r e m e n t s , t r a n s l a t i o n of this approach to tion of c o p p e r - r i c h c l u s t e r s which t r a n s f o r m i n - s i t u
f r a c t u r e toughness p r e d i c t i o n must be made with c a r e . to incoherent fcc 6 - c o p p e r p r e c i p i t a t e s upon f u r t h e r
Toughness s p e c i m e n s aged at 900~ (482~ a r e c h a r - aging.
a c t e r i z e d by q u a s l - c l e a v a g e c r a c k i n g and thus do not 2. While the t e n s i l e strength goes through a m a x i -
obey the above a s s u m p t i o n s . However, the r e s u l t s of mum after aging for 1 h at 900~ (482~ the work
s p e c i m e n s aged at 800~ (428~ and l l 0 0 ~ (593~ hardening r a t e g r a d u a l l y d e c r e a s e s with i n c r e a s i n g
can s t i l l f o r m a b a s i s for a valid evaluation of the aging t e m p e r a t u r e .
proposed models. 3. The f r a c t u r e toughness of 17-4 PH exhibits a
Hahn and Rosenfield 36 have suggested that: distinct minimum after aging at 900~ (482~ i.e.,
Kic ~- [~ECryef(O.O005 + n2)]~/2 [5] to the maximum strength. At an equivalent strength
level overaging r e s u l t s in a higher f r a c t u r e toughness
where E is Young's modulus, ay the tensile yield stress, than does underaging.
n is the strain hardening coefficient, and ~f the critical 4. At low ~ l e v e l s the fatigue c r a c k growth r a t e s
true strain for coalescing voids. The latter may be ap- a r e independent of environment while at i n t e r m e d i a t e
proximated in a tensile test by the true strain at frac- l e v e l s i n c r e a s i n g humidity and strength level i n c r e a s e
ture. An evaluation of Eq. [5] for 17-4 PH aged at the growth r a t e s . At high AK l e v e l s s p e c i m e n s aged
800~ (428~ and II00~ (593~ indicates that/~o at 800~ (428~ and l l 0 0 ~ (593~ exhibit a gradual
> K~~176 This is not consistent with the results of the d e c r e a s e in the slope of the c r a c k growth r a t e curve
present investigation although only our 800~ (428~ which cannot be attributed to a s i m p l e deviation from
measurement is actually a KIc value. Eq. [5] predicts plane s t r a i n c r a c k propagation.
that, other things being equal, increasing the strain 5. The p r e c i p i t a t i o n hardening b e h a v i o r of 17-4 PH
hardening coefficient should increase the fracture is consistent with p r o p o s e d models b a s e d on the i n t e r -
toughness. Clearly this does not agree with the re- action of a m a t r i x dislocation and a second phase p a r -
sults obtained on 17-4 PH stainless steel. ticle of lower s h e a r modulus than the m a t r i x .
The model proposed by Krafft37 suggests: 6. Attempts to c o r r e l a t e the fatigue c r a c k growth
K I c ~- [ 2 ~ E ~ 2 d t ] !/2 [6] r a t e s with monotonic t e n s i l e behavior were unsuc-
cessful. The most s e r i o u s defect of the p r e s e n t mod-
where d t is now the distance ahead of an advancing els a p p e a r s to lie in t h e i r complete neglect of m i c r o -
c r a c k tip where the c r i t i c a l s t r a i n for f r a c t u r e is s t r u c t u r a l effects on the cyclic s t r a i n hardening b e -
reached. havior of the m a t e r i a l just in advance of a propagative
Eq. [6] p r e d i c t s that d t equals 3.05 ~m, and 282 gm fatigue c r a c k .
for 17-4 PH s t a i n l e s s s t e e l aged at 800~ (428~ and 7. The f r a c t u r e toughness behavior, when obeying
l l 0 0 ~ (493~ r e s p e c t i v e l y . No c l e a r c o r r e l a t i o n b e - a c r i t i c a l s t r a i n c r i t e r i a , can be d e s c r i b e d using a
tween d t and any m i c r o s t r u c t u r a l feature, for example, model r e c e n t l y p r o p o s e d by Rice. 38
grain size, p r e c i p i t a t e spacing, or the spacing between
5 - f e r r i t e p a r t i c l e s , is a p p a r e n t . F u r t h e r m o r e , b a s e d ACKNOWLEDGMENTS
on this model, the f r a c t u r e toughness should again in-
c r e a s e with i n c r e a s i n g s t r a i n hardening coefficient, The authors a r e indebted to H. P e a r s o n , J. W. Elling,
again in contradiction with our r e s u l t s on 17-4 PH. K. D. Fike, D. Paschal, and C. Miglionico for t h e i r a s -
F i n a l l y Rice 38 has r e c e n t l y attempted to extend s i s t a n c e in the e x p e r i m e n t a l portion of this i n v e s t i g a -
these models. He suggested that tion. The c r i t i c a l comments of J. Munford and J.
Swearengen in reviewing the m a n u s c r i p t a r e g r e a t l y

dt =0.49-~yL ~-
%
E
l+n ln [7]
a p p r e c i a t e d . This work was supported in p a r t by the
U. S. Atomic E n e r g y Commission.

1604-VOLUME 5, JULY 1974 METALLURGICALTRANSACTIONS


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METALLURGICAL TRANSACTIONS VOLUME 5, JULY 1 9 7 4 - 1605

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