S c r i p t a M E T A L L U R G I C A V o l . 2 3 , p p .

3 3 9 - 3 4 4 , 1 9 8 9 P e r g a m o n P r e s s p l c
P r i n t e d i n t h e U . S . A . A l l r l g h t s r e s e r v e d
TRANSIENT AND INTERMITTENT CRACK GROWTH DURING
EMBRITTLEMENT OF 7075-T651 ALUMINUM BY MERCURY
Y. Liu and R. G. Hoagland
Department of Mechanical & Materials Engineering
Washington State University
Pullman, WA 99164
( R e c e i v e d De c e mb e r 20, 1988)
Introduction
The interaction of atoms of liquid mercury with the atoms at the tip of a crack in solid aluminum greatly
reduces the stress intensity required to propagate that crack, and like hydrogen embrittlement (HE) and stress
corrosion cracking (SCC) in aqueous environments, this example of liquid metal embrittlement (LME) is generally
regarded as a type of environmentally-induced fracture (1-5). Al so like these other forms of embrittlement, the
way in which this interaction diminishes crack tip deformation or promotes crack extension, or both, is not clear
although a number of postulates have been advanced. Some mechanisms which have been suggested, such as
those i nvol vi ng the weakeni ng of interatomic bonds at the solid surface at the crack tip due to the presence of
embrittling species or a shift in bias either toward or away from crack-tip dislocation nucleation (5-8), may be
common to all three types of brittle fractures. Whatever the mechanism(s), it is also cl ear that there are other
factors operating. For example, most of the work reported on mercury embrittlement of aluminum concerns only
high strength alloys, as low strength, or pure aluminum, is not severely embrittled. In addition, certain species in
the mercury may be important, and, in this regard, Wheel er and Hoagland (9) have suggested that oxygen dis-
solved in the mercury is available to form protective aluminum oxide, a reaction that competes with the embnttle-
ment. This suggestion was an attempt to explain the non-unique v-K curves they observed. Thus, structure of the
v-K curve can reveal some features of the cracking mechanisms.
This paper presents some results which show intermittent and transient crack growth behavior of a high
strength aluminum al l oy embrittled by liquid mercury. Run-arrest-run type of cracking behavior resulted in "n"
and "m" -shaped curves on the crack velocity (da/dt) vs. stress intensity (K) diagram. While variations in oxygen
activity in the crack tip environment (9) may pl ay a role in producing non-unique v-K behavior, the results re-
ported here suggest that formation and rupture of ligaments during crack extension may also be at work in a way
that causes the stress intensity associated with the field local to the crack tip (Ktip) to vary stochastically as the
crack extends.
Exoerimental Details
Double cantilever beam specimens used in crack growth tests were machined out of a 12.5 mm thick clad
7075-T651 plate supplied by Kaiser Aluminum. The plate came with a hardness of Rockwell B 91.5 The geome-
tries of the DCB specimens are shown in Figure 1. Specimens were machined such that crack propagation oc-
curred in the long transverse orientation with the crack plane perpendicular to the rolling direction (the L-T
orientation). Specimens were side-grooved to a net thickness of 4.6 mm.
O n e d r o p o f concentrated H F w a s placed at the m a c h i n e d slot tip to r e m o v e the oxide a n d then a p p m x ~
mately 2 m l o f liquid m e r c u r y w a s applied to the crack tip. After 5 rain. the specimens w e r e loaded at a crosshead
speed o f 0.152 m m / s c c . E a c h s p e c i m e n w a s loaded until a significant departure f r o m linearity occurred in the
load-displacement curve w a s noticed indicating onset o f crack extension. After crack extension c o m m e n c e d the
loading c o m m a n d w a s either switched to fixed l o a d (increasing stress intensity with crack growth) or to fixed
crosshead (decreasing stress intensity). A s noted below, crack g r o w t h w o u l d occasionally stop, momentarily,
then r e c o m m e n c e . Eventually, u n d e r fixed grip conditions, crack g r o w t h w o u l d stop, permanently, a n d the
applied K at that arrest is referred to as a threshold. T h e s p e c i m e n could then b e reloaded a n d another te~t
conducted. Generally five or six run-arrest events could b e conducted o n a single specimen. H o w e v e r , if the nine
3 3 9
0 0 3 6 - 9 7 4 8 / 8 9 $ 3 . 0 0 + . 0 0
C o p y r i g h t ( c ) 1 9 8 9 P e r g a m o n P r e s s p l c
340 E M B R I T T L E H E N T OF AL BY Hg Vol. 23, No. 3
between tests was too long (> 20 min.), the mercury would crawl out of the crack and embrittlement would no
longer occur.
4.60 mm
50.8 mm ~
Io
! ~ 2 5 4 mm
12.7 mm
19.1 mm
FIG. 1. Double cantilever beam specimen used in the crack growth
tests
During the tests, load and
di spl acement were recorded
simultaneously at a rate of 5 Hz on a
12bit digital recorder A five-point
weighted running average of the
recorded data points was calculated to
reduce high frequency noise. The
smoothed data were used to calculate
the crack length and the applied stress
intensity (K) using Kanninen' s
equation for this geometry(10). Crack
velocity (da/dt) was calculated by
four-point, central differences The
accuracy of crack length calculated by
this method is on the order of 1.0
rnm, but the sensitivity in determining
da/dt is about +5.0 x 10 -5 m/sec.
Resul~
Examples of load time records in which the crosshead was stopped after the crack began to extend are
shown in Figures 2 and 3. They are the results of two events of fLxed crosshead run-arrest from a single DCB
specimen. Shown in Fig. 4 is the corresponding da/dt-K curve. The crack velocity accelerates from a low level,
reaches its maximum value and decreases as a result of decreased K and finally arrests at the K threshold The
crack acceleration produced an inflexion on the load-time curves, and correspondingly, a "n" shaped transient rise
on the v-K diagram. During the crack propagation, occasionally intermittent crack growth was detected as
indicated by the flat step on the load-time curve and the valley-like "m" shaped structure on the v-K plot,
indicating that, momentarily, crack growth stopped then re, commenced.
o
t=
0
1100
1000
900
800
700
~ , ~ GRIP RXED
a
o
600
. . . . I
500 , , , t . . . .
150 200 250 300 350 400
TIME (Seconds)
FIG. 2. Plot of load vs. time from a run-arrest event
with constant displacement control. Steps on the
curve represent intermittent crack growth behavior.
0
t=
0
. J
600
500
400
300
200
u - , i n " I I l
- - - 3 G.,..ix 0
| i l l i I I I ~ I I
320 340 360 380 400 420 440 460
TIME (Seconds)
FIG. 3. Plot of load vs. time from a run-arrest
event with constant displacement control.
Inflection on the curve represents a momentary
slowing of crack growth.
With constant-load control the stress intensity increases with crack extension. An example of results
from a fixed load test is shown in Figure 5 in which a loop in the K-v curve was generated that signals the
failure of the machine to maintain a constant load due to the speed of the crack. Figure. 6 is the K-v diagram of
five run-arrest events which were obtainedfrom one DCB spegimen. The variation suggests that the thresholds
are never the same but fall in a range generally from 4 to 9 Mpa',/m. The maximum crack velocity detected in these
tests was 0.02 m/s.
Vol. 23, No. 3 E M B R I T T L E M E N T OF AL BY Hg 341
001
,0001 ' -
4 5 6 0 7 . 5 9 . 0 10
, ; . . . , . . . ; . . . , o , , ' 1
1 2 0 1 3 5 K ( MP a ~ / m)
K ( Mp a ~ / m)
FIG.4. K-v results from fixed-grip tests showing
"m" and "n"-shaped curves representing transient
and intermittent crack growth.
FIG. 5. K-v plot from a fi xed-l oad test
(increasing K with crack growth).The loop
occurred due to a combination of a transient
crack accel erat i on and the failure of the
loading system to maintain constant load
control during the transient.
i
001
0001
45
i I i i i
! ! ' !
- ~ 7 1 .
50 55 6.0 - ' 65 5
K ( MP a ~ m )
FIG. 6. Results of 5 run-arrest events in a single specimen showing non-unique K-v.
The ductile dimple fracture appearance, characteristic of in-air fracture surface topography of aluminum,
changes dramatically when in contact with mercury, as has been reported elsewhere (9). Some of the fractographic
features are readi l y recognizable as both cleavage and intergranular as well as very small ductile dimples after
fracture in mercury. Some additional features are worth noting. Figure 7 and a part of Figure 8 show the fracture
as a set of fiat, roughly parallel, but non-coplanar steps. Running diagonally across Figure 8 from the top right to
the bottom left is a feature that marks an arrested crack front. The crack had been propagating in contact with
mercury from fight to left, arrested, the mercury removed, and the sample was then broken in air, producing, in
Figure 8, cleavage-like appearance on the fight and ductile dimple on the left. Higher magnification in Figure 9
shows a fi ver pattern suggest i ve of cl eavage as well as evidence of l ocal i zed ductile rupture. (The crack
propagation direction is fight-to-left in all cases). Frequently, with mercury, delamination of the sample also
occurred by one or more cracks propagating, onl.y intergranularly, on planes roughly parallel to the rolling plane
as shown in Figure 10. Indeed, in some cases grmns were completely encircled by these intergranular cracks and
became detached from the surface. Figure 10 also clearly shows the non-coplanar steps on the main fracture
surface (arrowed right edge). Some examples of detached grains are shown in Figure 11 which also provides a
fairly cl ear indication of the typical grain shape and size. A commonly observed feature on the surface was shear
walls which are the nearly vertical rises in the stepped surface and which di spl ay evidence of ductile rupture
342 E M B R I T T L E M E N T OF AL BY Hg Vol. 23, No. 3
(Figure 12). As discussed below, we believe the fracture of these walls lags behind the embrittled crack and
consequently these walls act as ligaments.
FIG. 7. Typi cal fract ure surface of al umi num
embrittled by mercury showing non-coplanar steps and
cleavage-like features.
FIG. 8. A view of a region of transition from
mercury embfittled fracture (fight) to air fracture
(left).
FIG. 9. Cleavage fiver pattern and evidence of
localized ductile dimples.
FIG. 10. A transverse section (perpendicular to crack propagation direction) showing intergranular delamination
and non-coplanar steps on the main fracture surface (right edge).
Vol. 23, No. 3 E M B R I T T L E M E N T OF AL BY Hg 343
FIG. 11. Detached grains from the fracture surface
of intergranular delamination.
FIG. 12. (A): An example of a shear wall that appears as a nearly vertical step (art-owed). (B): High magnification
of the shear wall showing evidence of ductile rupture.
Discussion
The results of this study indicate that the response of the crack velocity is only "loosely" related to the
applied stress intensity, and, as a consequence, the K-v relation is not unique and displays a broad spectrum of
behavior due to transient and intermittent crack growth. Thus, instead of the typical three-stage relation often
associated with SCC (11,12), we find a variety of "m" and "n" shaped curves and loops.The size and shapes of
the individual steps observed on the mercury-embrittled fracture surfaces appear to be fiat, transgranular cross
sections of individual grains as the schematic on Figure 13 suggests. In addition, Figure 13 depicts intergranular
delamination fracture. Clearly, the intergranular fracture requires very little driving force (the nominal tensile stress
acting parallel to the crack front is sufficient), but transgranular fracture, when it occurs, is probably cleavage, as
the characteristic river marks suggest.
When crack extension occurs by cleavage in plain carbon steels, it is commonly observed that unbroken
ligaments are generated at the advancing crack front as a result of the crack plane becoming segmented at different
altitudes in a way suggested in Figure 13. It is thought that such ligaments play an important role in determining
the arrest and the propagation toughness as a result of a crack shielding effect (13-15). Similarly, Jones (16)
suggests that non-coplanar cracking behavior results in shear ridges running parallel to the crack growth direction.
Such shear ridges, like ligaments, shield the crack tip by exerting closure forces reducing the local K. We believe
that the fractographic evidence shown here indicates that such features are being generated during mercury-LME
and, further, that they can be responsible for the non unique K-v results.
3 4 4 E M B R I T T L E M E N T O F A L B Y H g V o l . 23, No. 3
FIG. 13. Schematic of the relation between the grain
morphology and the creation of fiat, non-coplanar steps
separated by shear walls and intergranular fracture
perpendicular to the main crack plane.
While we expect to publish a complete
analysis of the ligament effect in the near future,
as a qualitative explanation, we suggest that the
formation and subsequent rupture of ligaments,
shear-walls, etc, as the crack extends is a process
that produces a continually varying configuration
and therefore, a continually changing shielding
contribution. The result is that the shielding
contribution varies stochastically and, even if the
K-v relation were unique (where K here refers to
the local K), the decoupling from the applied K
produces an apparent non-uni que relation
between the applied K and the crack velocity.
Fract ographi c analysis shows that
LME cracks prefer the paths through grain
boundaries, if the specimen orientation favors it.
This is consistent with most frequent reports. If
the orientation of the specimen does not favor an
intergranular pat h, as for example in this work,
cleavage appears to occur. There remains some
question as to the crystallographic character of
this fracture, however, as cleavage in FCC
metals is quite unusual.
Conclusions
Crack propagation tests of 7075-T651 aluminum embritfled by liquid mercury display a spectrum of
transient and intermittent crack growth behavior suggesting the the crack velocity is, at best, weakly dependent
upon the applied stress intensity. While concurrent crack tip oxidation has been proposed as a contributing factor,
fractographic features indicate that ligament formation and rupture is also a potential explanation for the non-
unique K-v relation for this alloy. SEM fractographs show that mercury-LME fracture of this alloy occurred by
intergranular cracking, localized shearing and transgranular cleavage.
Aeknowledgment
The authors wish to thank Dr. J. H. Larsen, Mr. Brian Miller, Ms. Chris Davitt and Ms. Joyce Davis for
assistance. This work was supported by the Department of Energy under contract DE-FG06-87ER45287.
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