-7AIN
STRAIN AGING AND
FAILURE IN
"DELAYED
0 AHIGH-STRENGTH STEELS
TECHNICAL DOCUMENTARY REPORT No. ASD-TDR-62-968
NOVEMBER 1962
NOTICES
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that may in any way be related thereto.
Qualified requesters may obtain copies of this report from the Armed
Services Technical Information Agency, (ASTIA), Arlington Hall Station,
Arlington 12, Virginia.
This report has been released to The Offi~e of Technical Services, U.S.
Department of Commerce, Washington 25, D.C., for sale to the general public.
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FOREWORD
This report was prepared by TAPCO, a division of Thompson Ramo
Wooldridge Inc., under USAF Contrast No. AF 33(657)-7512. The contract
was initiated under Project No. 2(8-7351) and Task No. 73521. The project
was administered under the direction of the Directorate cf Materials and
Processes, Deputy for Technology, Aeronautical Systems Division, with
Lt. Robert T. Ault acting as project engineer.
This report covers the period from Octobar 15, 1961, to October 14, 1962,
II.
ABSTRACT
Spontaneous strain aging which occurs during tensile testing was
examined for several high-strength steels. The results of smooth and
notch tensile tests indicated that significant strain aging effects
occurred in most high-strength steels in the 300*F to 800*F temperature
range and this behavior was analogous to "blue brittleness" in mild steels.
Constant load, stress rupture tests were conducted on the steels to
determine the possible relationship between strain-aging embrittlement and
delayed failure. Only the 300 M steel tested at 400"F exhibited an
appreciable degree of delayed failure. This embrittlement, was extremely
sensitive to test environment and was elimainated when tests were conducted
in argon. Although strain aging was not a sufficient condition to initiate
delayed failure, it appeared to increase the severity of the environmental
effects in the particular range where sufficient interstitial mobility
existed.
:-
'.4
W. J. TRAPP
iii
*=
TABLE OF CONTENTS
Page
I
INTRODUCTION
II
MATERIALS EVALUATED
III
TEST PROCEDURE
IV
8
8
30
41
vI
BIBITOGRAPHY
42
45
A,
"B.
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iv
20
IN
21
LIST OF FIGURES
age
Fig2ure
I
Atmosphere.
Tensile Properties of 300 M Steel (600*F Temper) CrossHead Speed of 0.050 in/miii,
10
11
-4
8
9
12
13
14
15
16
11
17
12
19
13
21
22
10
14
15
Notch Specimens in an
23
~Pag
16
-17
18
19
20
21
22
23
24
26
27
28
29
32
33
34
36
Kvi
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24
26
'27
S211
:-1
37
39
40
48
Q.1
p,'-v
INTRODUCTION
The r3ed for airborne ccmponents with very high strength-to-weipnht ratios
has generated many xinique problems for the materials engineer. These problem
areas involve not only the selection of meaningful design stren th parameters,
but also the consideration of certain types of embrittlements which may limit
".."
*
The irreversible
the performance capaciV of these high-strength materials.
600F
temperature range
the
500*F
to
tempering
in
embrittlement produced .f-tcr
(1)* and the time dependent failures due to hydrogen (2) or mildly corrosive
environments (3, 4, 5) are well-known examples where the load-carrying ability
of a structure can be significantl.y reduced by embrittlewents.
The embrittlement due to strain aging in mild steels is well recognized
and has been frequently studied (6, 7, 8).
In the case of high-strength steel,
however, this phenomenon has only recently received attention and relatively
little
data exist on the decrease in notch strength which is produced by this
factor.
Strain aging is generally defined as a time-dependent change in
properties that results from a sequence of plastic strain and aging. Under
certain conditions of strain rate and test temperature, strain aging can
occur spontaneously during a normal tensile cest and result in ductility
minima and in most cases strength maxima. In mild steels this strain aging
process, which occurs during conventional tensile testing, is often referred
to as "blue brittleness" (8).
In high-strength steels the sequence of tensile straining followed by
aging below the original tempering temperature htas been investigated as a
method for increasing the smooth strength properties of a material. Recent
work with the low alloy martensitic steels (W340) and the hot-work die steels
(11-11) has indicated that a significant increase in tensile and yield strength
can be produced by this mechanical-thermal treatment (9, 10, 11),
The property variations which have been observed as a result of the
straining plus aging sequence have been attributed to a change in the carbide
morphology during the aging treatment.
The phenomenon of spontaneous strain
aging during a tensile test (blue brittleness) has not been systematically
evaluated in the high-strength steels. In these materials The major interest
has been in the improvement of the transition tcmperature as measured by a
sharply-not'hed specimen, and relatively little
data. are available on properties in the super-transition temperature regions where strain aging may be
presento In addition, the high-strength steels do not generally exhibit
-ield point effects and therefore the simple interactions between dislocations
and interstitial atoms (8) which are employed to describe strain aging in
mild steels are not believed to play a dominant role in the mechanical properties of the ultra-high-strength steels.
___
Recent daba by Srawley and Beachem (12) and Preston and Morrison (13)
have indicated that a milnimum in the notch tensile strength occurs in the
low alloy martensitic high-strength steels when they are tested in the
super-transition temperztlre range. Since the temperature at which this
decrease in notch properties takes place is comparable to the region where
"blue brittleness" occurs in mild steels, the question arises as to whether
spontaneous strain aging effects are present to a significant degree in highstrength steels. There is considerable current interest in the nechanical
properties of materials in this super-transition temperature region since
this is the temperature spectrum under consideration for the supersonic
transport. Certain pressure vessel applications may also involve temperatures up to 5OO*F and any decrease in load-carrying capacity may be a
critical consideration at these temperatures which are above the conventional
sharp-notch transition temperature.
Since strain aging is a time dependernt phenomenon, there is the possibility that this embrittlement will also be operative in constant load
Troiano (2) has recently proposed
tests where the test time is a maxirmu.
a mechanism for strain aging embrittlement which predicts this effect and
which involves the clustering of interstitial aton3 at the tip of a crack
or dislocation pile-up. The interstitial grouping is believed to lower
the cohesive strength of the material and cause crack extension. Although
his res'ilts are based on work with hydrogenated steels, the possibility
exists that carbon and/or nitrogen strain aging can also lead to delayed
failure in temperature regions where these interstitials have a mobility
similar to hydrogen at room temperature. The high-strength steels with
their marginal crack propagation resistance represent materials which may
be particularly susceptible to a non-hydrogen induced type of static fatiguee
The purpose of this investigation was to evaluate the magnitude and
kinetics of spontaneous strain aging in high-strength steels and determine
its possible association with delayed failure under static loads.
- .
II
MATERIALS EVALUATED
Four basic types of high-strength steel (see Table I) were selected for
the experimental program. All the materials, with the exception of the Ni-
Nf
III
TEST PROCEDURE
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24. as
for a thermally activated process., such as strain aging., the temperature where
embrittlement occurred decreased as the testing time increased (i.e. at decreasing strain rates). Figu,nre 6 illustrates a comparable type of notch
embrittlement which occurred in the 300 M tempered at 1025*F. In this case
the region of maximum embrittlement occurred at a slightly higher test
temperature than when the steel was tempered at 600"F.
The results of smooth and notch tensile tests of 4340 steel tempered
at 750"F are shown in Figures 7 and 8. Although the results are similar
to those obtained with the 300 M, the degree of notch embrittlement in the
4340 steel at this strength level was more severe.
The smooth and notch tensile properties of the H-11 die steel are
presented as a function of test temperature in Figure 9. This material,
which was double tempered at 1O000F, exhibited no anomalies in properties
which could suggest significant strain aging effects. It is interesting
to note however, that the notch tensile strength as determined by the
precracked specimens was below the yield strength over the entire range of
test temperatures.
The 17-7 PH stainless steel (see Figure 10) also exhibited no noticeable
maxima or minima in mechanical properties that would be indicative of spontaneous strain aging during the test. As shown in Figure I1, the AM 355
precipitation-hardening stainless steel, in agreement with previously
pablished data (17), exhibited a maxima in tensile strength in the 600*F
to 800OF test temperature range. The peak tensile strength values were
shifted to lower temperatures with decreasing strain rate, indicating that
a strain aging phenomenon was operative. Although the notch tensile tests
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The results obtained from stress rupture tests conducted at 300'F, 400*F,
and 550"F with 300 M high-strength steel tempered at 600*F are shown in
Figure 13. In order to compare the results for different temperatures, the
applied stress was normalized by dividing it by the conventional notch tensile
strength obtained at the particular test temperature and with a crosshead
speed of 0.050"/min. (see Figure 5). The specimens tested at 400"F, which
is in the temperature region where strain aging was prominent in the tensile
test, failed in relatively short times at applied stress values as low as
0.6 the normal notch tensile strength. This rather large rarge of delayed
failure was not present in tests conducted at 300*F and 550'F. The fact
that failures did not occur at 550OF indicates that the fractures at 400"F
could not be attributed to conventional creep processes. It is also very
improbable that the failures could be due to hydrogen since the steel was
i- -n unhydrogenated condition, and hydrogen-induced delayed failures are
nL present at temperatures above 300*F (20).
Sustained load tests conducted on 300 M specimens tempered at I025*F
did not show any failure in 200 hours at temperatures below 800*F and at
applied stress levels which were 90% of the normal notch tensile strength.
The static fatigue curves obtained from notch tests at 800"F and 900*F are
shown in Figure 14. In this series of tests the failures appear to be due
to conventional creep behavior,
Stress rupture tests conducted on notch specimens of the 18% nickelmaraging steel are shown in Figure 15. Once again no appreciable region
of delayed failure was present which could be attributed to non-creep type
processes. Sustained load tests on 4340 steel tempered at 750*F, and AM 355,
showed no delayed failure in 200 hours at an applied stress of 0.9 times the
conventional notch strength and in temperature regions where strain aging
was experienced.
Since the association between strain aging and delayed failure was only
apparent to any appreciable extent in the 300 M steel tempered at 600*F,
this material was selected for further evaluation of the delayed failure
mechanism.
The which
macroscopic
the fracture
a specimen
of 300 M steel
failed appearance
under staticof load
is shown surface
in Figureof 16.
The
failure pattern consisted of the following segmentst
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24
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a)
b)
c)
d)
The heat tinting which occurred during the test allowed each mode of crack
propagation to be readily distinguished. The appearance of the slow crack
was considerably more fibrous than either the crack extension that occurred
on initial loading or the fatigue precrack. In an effort to further study
the kinetics of the slow crack growth, resistance measurements were employed daring the sustained load tests on the 300 kl high-strength steel
The variation of resistance with time is presented in Figures 17 and 18
for test temperatures of 300"F and 00*F. At 300"F, an incubation time
was observed before slow crack growth was initiated and this incubation
time was extremely sensitive to applied stress (see Figure 19). At the
t00*F test temperature, ao incubation was observed at any applied stress
level where delayed failure occurred and slow crack growth was initiated
as soon as the load was applied.
The lack of an incubation period is typical of environmentally-induces
delayed failure in high-strength steels (4).
To evaluate this possibility,
sustained load tests were conducted on notch specimens of 300 M at 400F in
an argon atmosphere. The results presented in Figure 20 indicate that the
delayed failure at 400OF was completely eliminated when an argon atmn sphere
was used. The static fatigue in 300 M steel was therefore induced oy
environmental effects and was presumably due to stress corrosion by the
air atmosphere. The strain aging effects previously described with reference
to tensile testing were re-'valuated by conducting notch tensile tests on
300 Y, (600*F temper) in an ai gon atmosphere. A minimum in notch tensile
strength was present at the same test temperatures in both test environments,
indicating that the tensile test data were associated with a material phenomenon and not with the external test conditions.
Although the delayed failure is environmentally induced, it is still
significant that the temperatu.- region where delayed failure occurred
corresponded to the range where strain aging effects were observed. As
the crack slowly grows in a constant load test, because of environmental
effects, the applied stress is increasing due to the decrease in load
carrying area, On this basis, the sustained load test is comparablc to a
slow 3train rate tensile test provided a mechanism, such as stress corrosion,
is available to continually produce a slow crack propagation. Strain-aging
effects should therefore influence the failure properties in this temperature
range just as they decrease the notch tensile strength in conventional tensile
tests. The lack of delayed failure in the other materials investigated is in
general agreement with their decreased susceptibility for the initiation of
slow crack growth and stress corrosion effects (h)*. Additional work is still
needed to determine the mechanism whereby mild environments such as air can
produce such a rapid deterioration in load carrying ability of a high-strength
steel.
*
600
FRACTURE
500
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400
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300
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3)
S.for!iation
22),
24),
The short range ordering of solute atoms about dislocations has been
described in some detail by Schcedc and Seeger (21) and Wilson and Russell
(22).
The interstitial atom produces a distortion with a symmetry which
is different from the symmetry of the lattice. On this basis, the interwill take up preferred positions within the lattice when a nonstitial
hydrostatic stress field is present. Under certain time-temperature conditions the ordering of the interstitials about the moving dislocation will
produce a restraining force because energy is dissipated during the ordering
which takes place.
This dragging force is not apparent at low dislocation
velocities or high-test temperatures where the ordering always reaches thermodynamic equilibrium. At high velocities or low temperatures the time is insufficient for redistribution to take place and the restraining force is also
absent. An ordering phenomenon of this type produces the well-known Snoek
peak in internal friction studies and is characterized by 'he relatively
short times involved, since redistribution only takes place over atomic
dimensions. A second type of dragging force which can occui is due to the
of a Cottrell cloud about a moving dislocation (8, 23).
The
times required for this strengthening to occur should be approximately
100 times greater than that involved in ordering since the interstitials
have to move over greater distances to form the cloud (25).
The role of strain-induced solution and precipitation of carbide particles
has been used in both mild (7) and high-strength steels (10, 11) to describe
strengthening effects produced by tensile straining, followed by suitable
aging. A simple application of precipitation as a mechanism for strain aging
which occurs during the test (blue brittleness) is difficult to visualize
since it would require the precipitation process to occur on a moving dislocation. Certain internal friction peaks, which involve oscillating dislocations however, have been attributed to very small coherent carbide precipitation (26).
In addition, the flow process may be fairly complex in the
high-strength steels and may involve intermittent moveme it of specific dislocations which would allow precipitation effects to become operative.
On
this basis, the possibility of solution and reprecipitation of carbides in
"blue brittle" behavior should not be disregarded.
___.
30
&Ae
~where:
N.
strain rate
constant
activation energy
gas constant
absolute temperature
To evaluate the activation energy Q, the logarithm of the crosshead speed was
plotted as a function of l/T. T was taken as the temperature where the tensile
btrength was a maximum, or the notch tensile strength was a minimum. The
results are presented in Figure 21 for the time-temperature dependency of the
notch strength minima and in Figure 22 for the smooth tensile strength maxima,
These data indicate that both parameters conform to the conventional rate
equation and have an activation energy of approximately 25,OOO cal/mole.
Due to the difficulty in selecting the exact maxima or minima from the
mechanical property data the activation energies can have a spread of
approximately +hOOO cal/mole.
The data which are available for the "blue
brittleness" of mild steels (27) have been plotted in Figure 23.
The
activation energy for this embrittlement in mild steel is essentially equal
to that which occurs in the high-strength steels and strongly suggests that
comparable mechanisms are operative.
Although stress-induced ordering of carbon or nitrogen and the drag of
Cottrell clouds of interstitials with dislocations are generally accepted as
contributing to the spontaneous strain-aging behavior in mild steels, the
following results must still
be explained before these mechanisms can be
applied to the present data on high-strength steels:
"
1.
2.
3.
31
0.
700 0 F
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6000 F
5000 F
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4000F
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5000 F
4000 F
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(6009 F TEMPER)
0.1
Q 26,200 cal/mole
w% .01
a::
0\
o
AM355
-_.-
Q 23,500 cl/0mole
.001
1.4
-_
1.6
1.8
2.0
INVERSE TEMPERATURE
2.2
2.4
- 10-3, K-I
2.6
700
10
Z'-
500
,10
4000 F
THIS INVESTIGATION
NOTCH TENSILE STRENGTH
MINIMA (4340 STEEL)
__,
___
690
I__
(REF. 27
MILD STEEL) "
:;
z"% I0-2
10
w
a--)
W
x
)(I.
0
,,
---
-'
THIS INVESTIGATION
300 M, i025-F TEMPER
-3
10--
(REF. 27
:MILD
1.2
STEEL)
1.4
1.6
1.8
2.0
2.2
INVERSE TEMPERATURE
2.4
2.6
2.8
- 10-0 K I
3.0
3.2
v4
35
P 10'0 LINE"i/CM2
=
""
I0 LINES/CM
rm 4
L)
II. 0
0 1&--
00-- -. L C
00
200
400
300
TEST TEMPERATURE -
500
600
36
700
22
C%
13.
(A)
-.
co
NORMAL STRENGTH
W
U)
I.-
*,
DECREASE()
(13
C3
Woo
ISTRENGTH
200
OURVES(4,. 4;
400
600
TEST TEMPERATURE
V
I___
(C)__
f)
800
10
-'F
38
.*..,.
,.
. ,
.-
-*
- *
- .o -
--
S-,
',
0836
300 M SPECIMEN, STRESSED IN STRAIN
MICROSTRUCTURE OF NECKED REGION
<!
AGING REGION,
S
.-
0839
'J
00S M
26" ELECTRON
FIG.
'-
"AT
PECIMEN -UNSTRESSED
600* F, MAG.
10,000 X.
39
-ZN)
01
w
0
a-
S160
--
0
w
120
w
IIC-)
w
L-J
I--
100 0
00
I0
20
30
40
50
60
AT 4000 F ""MINUTES
Mz
ROOM
TEMPERATURE
V CONCLUSIONS
High-strength steels can exhibit significant strain aging effects during
tensile testing, when tested in the temperature range 300*F to 800*F. The
strain aging phenomena are characterized by an increase in smooth tensile
strength and a decrease in notch tensile strength. The strain-aging behavior
is dependent on strain rate in a manner which is analogous to "blue brittleness" in mild steels. The activation energy for the phenomena is comparable
to that shown by "blue brittleness" and is approximately 25,000 cal/mole.
The strain aging effects were observed in the low alloy martensitic steels
(300 M and 4340), the precipitation-hardening stainless steel (AM 355), and
the maraging steel (18% nickel, 7% cobalt, 5% molybdenum),
No strain aging
was noted in the H-11 hot-work die steel or the 17-7 PH precipitationhardening stainless steel.
Constant load tests were conducted to determine a possible correlation
between the strain aging effects noted in the tensile tests and the susceptibility for delayed failure. An appreciable region of delayed failure
was present only in the high-strength 300 M steel tested at hOO"F This
delayed failure phenomenon was extremely sensitive to environmental effects
and was completely eliminated by testing in an argon atmosphere. Although
the strain aging did not initiate failure under sustained load, it was
tested at hOO4F.
The spontaneous strain aging in high-strength steels which occurred
during tensile testing was attributed to an interaction between interstitials
and moving dislocations rather than precipitate formation.
LL
~41
VI
1.
BIBLIOGRAPHY
(1954).
5.
E. H. Phelps and A. W. Logii- w, "Stress Corrosion of Steels for Aircraft and Missiles", Corrosion, 16, No. 7, 97, (July, 1960).
6o
9.
12,
J. E. Srawley and C. D. Beachem, "Crack Propagation Tests of Some HighStrength Sheet Steels", NRL Report 5263, (January 10, 1959).
13.
14.
-~
42
BIBLIOGRAPHY (Continued)
15.
16.
E. A. Steigerwald and Go L. Hanna, "Initiation of Slow Crack Propagation in High-Strength Materials", ASTM, Preprint 74, (1962).
17.
18.
19.
20.
21,
G. Schoeck and A. Seeger, "The Flow Stress of Iron and Its Dependence
on Impurities", Acta Mete, 7, No. 7, 409, (July, 1959).
22.
23.
24.
25.
27.
H.
S. Gurev and W. M. Baldwin, "Research on Strain Aging Effects in
Titanium",
WADC TR 59-223, (September,
Etl
1959).
43
BIBLIOGRAPHY (Continued)
28.
(1958)o
29.
*.
-,"
.-.
N
APPENDIX I
Calculation of Ordering Effects Due to Interstitials
Schoeck and Seeger (21) present a functional relationship between the
force exerted on a dislocation by interstitial ordering and a dimensionless
parameter which involves the relaxation frequency for the interstitial and
the speed of the moving dislocation. This relationship which can be
expressed as:
where:
Li
frequency factor.
0.5 bff-
strain rate
Burgers' vector
f'
where:
(2)
dislocation density
c(
-
1.52 V~
where:
Burgers' vector
2.47
5.2 x I 0
5
-8
10
cm
"9000/T cm2/sec.
1.84 x I0"20
Rcm
the value
fA
(ref, 8)
(ref. 21)
10 /cm
44
46
--
000
0N
0H
c'coZ
p)
0
H
ON
IHj
zII
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0
H
0 0-
co
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Ho
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HI
A
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oc
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co
CC
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to
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000
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