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Acta mom-. Vol. 45, No. 10, pp.

42834296, 1997
0 1997 Acta Metallurgica Inc.
Pergamon Published by Elsevier Science Ltd. All rights reserved
Printed in Great Britain
PII: s1359-6454(97)ooo73-6 1359-6454197 $17.00 + 0.00

EFFECT OF CYCLIC PRESSURE ON THE LOW


TEMPERATURE CONSOLIDATION OF SEVERAL
COMPOSITE POWDER SYSTEMS

CHING-YAO HUANG and GLENN S. DAEHN


Department of Materials Science and Engineering, The Ohio State University, 2041 College Road,
Columbus, Ohio 43210, U.S.A.

(Received 2 October 1996; acrepted 23 December 1996)

Abstract-The effect of cyclic pressure on the room temperature composite powder consolidation has been
studied. Mixed metal and ceramic powders were consolidated under static and cyclic pressure at room
temperature in constrained “uniaxial” consolidation. In this paper, five composite powder systems,
Pb/TiOz, Pb/SiC, Al/AbO,, Al/Sic, and Zn/AbO,, have been studied at 40% ceramic by volume. This
complements an extensive study of Pb/AhOj in static and cyclic consolidation that was reported earlier
[l]. The experiments show that pressure cycling greatly enhances densification relative to static compaction
at the same maximum pressures. The proposed reason for improved densification in cyclic pressure is that
the pressure changes (AP) may directly induce plastic deformation due to elastic mismatch strains that
develop between the metal and ceramic phases. These are induced owing to the compressibility difference
(A/Y)between the two phases. The six powder systems studied to date (at many pressure cycle amplitudes)
show that all the data for density change nearly collapse to one trend line when plotted against the
dimensionless strain ratio, ABAP/c,, where the numerator represents the linear elastic mismatch strain and
to is the matrix yield strain. This term must exceed a value near 3 in order to significantly improve
consolidation by pressure cycling. This effect is expected to have practical importance as the pressures
required to improve consolidation are often accessible and the strengths of the compacts formed by
pressure cycling are significantly greater than those produced in static consolidation. 0 1997 Acta
Metallurgica Inc.

INTRODUCTION produced with each pressure cycle, incremental


consolidation could take place over many cycles.
Powder metallurgy techniques hold much promise Previous work from the Pb/ ALO3 system supported
for the creation of metal-ceramic composites, as has this hypothesis. In the experiments, simple con-
been shown in many studies [2-h]. The ability to use strained die compaction performed in static com-
relatively low consolidation temperatures offers the paction was compared to that done with a sinusoidal
ability to retain metastable phases that might be pressure-time variation. Figure 1 is reproduced from
formed by rapid solidification, for example. How- that work. This shows that for lead reinforced with
ever, when the ceramic fraction becomes large, large amounts of alumina, compaction is greatly
it becomes difficult to densify the metal-ceramic aided by pressure cycling. However for pure lead,
aggregate [ 1, 7-l l] and often the compacts produced compaction is not aided by pressure cycling. The
have significant density gradients [12]. The most effect is shown to be so strong that by the imposition
common methods used to mitigate such problems are of 100,000 l-Hz pressure cycles between 414 MPa
the applications of higher compaction pressures and 0 MPa pressure, Pb-40% AlzOs will become
or temperatures. While this may be effective for more dense than unreinforced lead compacted at
consolidation, higher pressures require larger pro- 414 MPa for 100,000 s. Related work [13] also
cessing equipment and higher temperatures can cause demonstrated that the density is more uniformly
the loss of metastable phases or produce undesirable distributed in these cyclically processed composite
matrix-reinforcement reactions, or both. compacts.
In a previous paper [l], we suggested that the The previous work considered several possible
application of cyclic, instead of static, pressure may mechanisms by which density might be improved and
aid the densification of metal-ceramic powder argued that elastic strain mismatch is responsible.
metallurgy compacts. We argued that upon a change Experiments show that there is generally a critical
in pressure, deviatoric stresses would be generated at pressure cycle amplitude that is required to initiate
matrix-reinforcement interfaces and those stresses the enhancement in densification and beyond this,
in turn can produce plastic deformation which can for a given number of cycles, the density increases
aid the filling of voids. As small strains may be almost linearly with increasing pressure cycle

4283
HUANG and DAEHN: EFFECT OF CY’C’LI(‘PRESSURE

- Cyclic
^___ Static

_+_-"----
85 - ___-_--- ___-- -o------
*c ____----
_G%

hhnber of Cycles or Time (see)


Fk 1. ComParison of compact consolidation under steady pressure (open symbols) and cyc[ic compaction
in Pb-AhQ powder compacts with O%, IO%, 20%, and 40% (by volume) alumina. In the static case,
the horizontal axis corresponds to time and the applied pressure was held at 414 MPa. In the cyclic case,
Pressure cycled between 414 and 0 MPa and 1 Hz cycles were used. Note that in pressure cycling large
changes in density take Place for the highly reinforced compacts, but there is little change for those dilute
in reinforcement.

amplitude. The interpretation of this is that beneath we find that all the systems appear to follow a
a critical pressure change, the metal at the matrix- common trend that can be expressed in terms of
reinforcement interface is not loaded to its yield stress A/?AP/G,~ and similar to our previous work [l], the
at the extreme pressures and densification is not mechanical properties of the compact improved
aided. Following this argument, one would expect beyond those seen in static compaction by a much
that a good figure of merit in analyzing such larger factor than density, suggesting that inter-
experiments would be the ratio of the Eshelby particle adhesion is also greatly improved. These
mismatch strain [14-161 to the yield strain of the results can be applied to the design of processes that
matrix. This can be expressed as A/I API&,, where AjI may improve the consolidation of composites from
is the difference in compressibility between the matrix mixed metal and ceramic powders.
and reinforcement, AF represents the pressure change
imposed, and 60 represents the matrix yield strain.
EXPERIMENTAL PROCEDURE
If this term is above some value, the consolidation of
a given green composite could be aided by pressure The experimental work foIlows that of our
cycling. previous studies [ 1, 171. Five composite powder
The present work seeks to find whether the effect systems based upon three metal powders (Pb, Al, Zn)
of pressure cycling aids consolidation in other and three ceramic reinforcements (A1203, TiOz, Sic)
Powder Metallurgy (P/M) composite systems. and were studied. Several scanning electron images were
whether the term, A/3 APIt,, is a good characterizing used to roughly estimate average particle size and
figure of merit. Here we examine combinations of assess shape. Representative images of the initial
three different particulate matrix metals and three metal and ceramic powders are shown in Figs 2
ceramic reinforcements under pressure cycling and and 3, respectively. Note that images of Pb and
static compaction at room temperature. In summary, Alz03 particles are available in Ref. [I]. The average
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4285

Fig. 2. Scanning electron micrographs of the metal powders: (a) Al, (b) Zn

particle size of Pb powder is about 10 pm and the length on average and also tends to agglomerate.
shape tends to be globular. The Al and Zn powders The properties of the components [18, 191 and
have average particle sizes of about 7 and 5 pm, combinations studied are summarized in Tables 1
respectively, and are nearly spherical in shape. In and 2, respectively.
contrast, the ceramic reinforcements tend to be more To compare with the previous study, we chose to
irregular in shape. AlzOs is 6 pm in average particle use 40% (by volume) loading of ceramic as our
diameter and rather plate-like in shape. TiOz is standard condition, and the relationship between
0.2 pm in average particle size and spherical in shape, pressure cycle amplitude and density is of primary
and agglomerates rather strongly. The SIC has a interest. The five composite powder systems were
whisker morphology 1 pm in diameter 20 pm in mixed in a twin shell mechanical dry blender for
4286 HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE

Fig. 3. Scanning electron micrographs of the ceramic reinforcements: (a) SIC whiskers, (b) TiOz powders

30 min to provide a uniform distribution. However, average sizes of remaining Sic whisker agglomerates
for Pb/TiO*, PbjSiC, and Al/SIC powder systems, in the PbjSiC and Al/Sic systems are about 150
it was difficult to obtain a uniform distribution and 600 pm, respectively. This is probably due to the
because of agglomeration in the original ceramic larger particle size and much higher density of Pb
powders. But during powder mixing, significant relative to Al, which provides a greater force to break
de-agglomeration took place as was observed by the Sic whisker agglomerates in mixing. Hence, we
examining the mixed powders with the scanning expect somewhat greater matrix-reinforcement con-
electron microscope (SEM). Further detail on this is tact in the PbjSiC system than in the Al/Sic system.
provided in Ref. [17]. In the Pb/TiOl system, significant de-agglomeration
More complete de-agglomeration occurred in also occurred. The average final size of Ti02 powder
the PbjSiC system than in the Al/Sic system. The agglomerates is about 40 pm. However, there are still
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4287

Table I. The values of compressibility and the average particle size inthe studied metal and
ceramic powders
Properties Pb Zn Al A1201 TiOz Sic
b x 1O-6 (MPam’) 22.37t 13.32t 13.147 4.17t 4.54t 3.85t
Average particle size (pm) 10 5 7 6 0.2 I:20 (d:l)
tData from Ref. [18].
fData calculated using b = 3(1 - 2v)iE from Ref. [19].

a few large agglomerates existing after mixing, which center of the samples using a diamond saw and
are about 200 km in size. In this system, the TiOt subjected to three-point bend testing. In each case,
particles tend to essentially coat the Pb particles. the bar’s axis is normal to the compaction direction.
Compaction was carried out in a standard right The testing conditions were the same as the earlier
cylindrical die 12.7 mm in diameter. For each system, study in the Pb/A1203 system [l]. No replicate
the same mass of powder was used to produce a experiments were run to assess the reproducibility of
compact about 9 mm in height. Static compaction this procedure. However, from examination of the
was carried out at 414 MPa for 10,000 s. Cyclic deviation of similarly developed data (trend-line in
compaction was conducted by simply imposing Fig. 10 of ref. [l]), a variance of 20% of the value
sinusoidal force cycles to 100,000 cycles at 10 Hz. or less is expected. After testing, the fracture surfaces
This provided the same time at pressure for both of composite powder compacts were examined by
static and cyclic compaction. In all cases, except when SEM.
AP was 483 MPa, the maximum pressure in the cycle
was held at 414 MPa, and the minimum pressure was RESULTS
varied to control the cycle amplitude. In the case
Effect of pressure cycle amplitude
where AP was 483 MPa, the low pressure was set
to zero. In all cases, loading was performed on a PbIA1203, ZniALO,, and Al/AlzO, systems. The
servo-hydraulic test frame in closed-loop load composite powder compacts consisting of 40% AhO3
controlled mode. The accuracy and precision of the ceramic powders and various metal powders were
extreme loads are within 1% of their nominal values. consolidated under static and cyclic pressure con-
After compaction, the composite green density of ditions with the maximum pressure held at 414 MPa
the cylindrical samples was determined by simply and variable low pressures. Fractional density as
measuring the mass (to within $0.001 g) and the a function of pressure cycle amplitude is shown in
volume (by measurements of the right cylinder to Fig. 4. All three systems exhibit a region at low
+O.Ol mm precision). The fractional density is the pressure cycle amplitudes where density varies
ratio of the bulk density of the specimen to the little with pressure amplitude, and beyond a critical
theoretical density of the powder composite which pressure amplitude there is another region where
is determined by the simple rule of mixtures. In all density increases nearly linearly with pressure
cases, the compacts took the shape of the die cavity amplitude. The critical pressure change, APctit, is
after extraction and showed a diameter about 0.3% 140 MPa for the Pb/A1203 system, 210 MPa for the
greater than that of the die cavity owing to elastic Zn/AhO, system, and 320 MPa for the Al/Al,O,
spring back. To test the reproducibility of the density system.
measurements, nominally identical replication of 12 There is one small unusual feature in these data,
compaction conditions of the Pb/A1203 systems were i.e. for the Zn-AlzOj system, the density actually
run 2-3 times each. In all cases, the variance in decreases slightly with increasing pressure cycle
measured density between identical conditions was amplitude in a small pressure amplitude region.
0.6% or less. The average standard deviation of these It appears that this is due to a significant time
experiments is 0.17%. dependence of the zinc powder at room temperature
In order to estimate the green tensile strength and because as the pressure cycle amplitude increases,
of many composite systems that contain a the time-averaged stress in the compact decreases.
lead matrix, small rectangular parallelepiped bars Thus, the consolidation rate decreases with increasing
12.7 mm x 3.2 mm x 2.0 mm were cut from the AP. Also, zinc is interesting from the point of view

Table 2. Experiments performed in pressure cycling and static consolidation


Reinforcement/Metal Pb Zn Al
ALO, Several Vr 40% 40%
(see Ref. [l])
TiOz 40% Not studied Not studied
Sic 40% Not studied 40%
None Isotropic- Hexagonal- Not studied
no mismatch produces mismatch
4288 HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE

Fig. 4.Effect of pressure cycle amplitude on the fractional density for P&40% ALO,, Zn40% A1201,
and A140% AhO, powder systems. All of the data tested in the cyclic pressure conditions were measured
after 100,000 cycles at 10 Hz.

that it is an h.c.p. metal and the imposition of The difference in compressibility between the
pressure on an aggregate of h.c.p. grains will produce ceramic and metal phases is very similar in these three
deviatoric stresses that can, in principle, induce cases. Therefore, the data in Fig. 5 give insight as
plasticity. This effect was also studied by consolidat- to how changes in particle shape (and possibly
ing pure Zn powder in static and pressure cycling agglomeration) affect densification in pressure
conditions [17]. In the static pressure conditions, Zn cycling. It is interesting to note that in each case, the
powders were compacted at 414 MPa for 30, 1000, values of APall are similar as are the slopes of the lines
and 10,000 s. Also compaction was run for the same at large pressure cycle amplitudes. The different
amount of time with 1 and 10 Hz sinusoidal pressure reinforcements mostly affect the absolute values of
cycles between 0 and 414 MPa. For zinc, the time fractional density in a way that might be intuitively
dependence was much stronger than the pressure expected.
cycle dependence. Increasing the dwell time during AIIAlzO, and Al/Sic systems. Part of the
static compaction from 30 to 10,000 s raised the motivation to study aluminum/alumina and alumi-
density from 93% to 96%. Pressure cycling only num/silicon carbide comes about because both
added about 1% to the density and the 1 Hz cycles systems have been extensively studied as potential
gave higher densities than the 10 Hz ones despite the structural materials. The results on densification as a
imposition of fewer cycles. This shows that there is function of pressure cycle amplitude are presented in
a complicated time dependence in the zinc system, the usual way in Fig. 6. The critical pressure cycle
but consolidation is not strongly enhanced by the amplitude in the Al/SC system is significantly lower
level of pressure cycles that are imposed. These results than that in the Al/A1203 system. To first order, we
were quite different from the Pb and Al cases expect that the similar compressibility mismatch
which show fairly rate-insensitive but cycle-number between matrix and reinforcement should produce a
dependent behavior in these experiments. similar critical pressure change. The relative differ-
Pb/AlzOs, PblTi02, and PbjSiC systems. Figure 5 ence between the AP,,, values might be attributed
shows results from all three reinforcements with a to the varied morphologies of the reinforcements.
lead matrix. There is a clear AP,,, in the Pb/A120j Whisker-like reinforcements may be expected to give
and PbjSiC systems, but the transition between low reduced critical mismatch strains owing to greater
and high pressure cycle amplitude behavior is more geometric constraint [20], but a rigorous analysis that
obscure in the Pb/TiOz system (but the slope of the would directly apply to this case is difficult. Note that
lines does increase at large AP values, which we can a very similar trend is seen in the lead system with the
use to suggest a AP,,,,). In this case, the increase in SIC and AllO reinforcements, although the trend is
densification at low cycle amplitudes is likely due not as strong. Also, the SIC system tends to
to the break-up of significant Ti02 aggregates in agglomerate much more significantly. This may also
something like compression fatigue affect the absolute values of density. It might also be
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4289

0 loo 200 300 400 500

AP UtdPa)
Fig. 5. Effect of pressure cycle amplitude on the fractional density for Pb40% AhOjpr Ph40%TiO+
and P&IO% Sic, powder systems. All of the data tested in the cyclic pressure conditions were measured
after 100,000 cycles at 10 Hz.

argued that the lower AP,,,, is affected by the break-up enhanced with increasing numbers of applied cycles
of Sic aggregates. and pressure cycle amplitude. This is in accord with
the fractional density results. However, the relative
Green strength in bending
strength changes are much greater than the relative
The mechanical properties of the three composite changes in density. For example, while density may
systems with a lead matrix were examined by increase lo%, strength can increase by a factor
measuring the bend strength of small machined bars. of 4-6. This shows that interparticle bonding is also
The results are shown in Fig. 7. In each case studied, strongly improved by pressure cycling. Also, the
cyclic compaction greatly improves the strength of relative strengths of the three systems seem to show
the green composite and strength is generally a rather consistent pattern where the AlzOi and

Fig. 6. Effect of pressure cycle amplitude on the fractional density for AlMO% A1~01~ and A140% Sic,
powder systems. All of the data were measured after 100,000 cycles at 10 Hz.
4290 HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE

El Pb/AW,p
120 ?? PblSiCw
?? Pb/TiO,p

StrtiC
P.414 MPa
10,000 set
!l!
Cyclic
AP414 MPa
10,000 cycles
Cyclic
AP-414 MPa
100,000 cycles
Cyclic
AP=483 MPa
100,000 cycles
Fig. 7. Comparison of green strength between static and cyclic compaction for Pkeramics composite
systems. Cyclic data were obtained at 10 Hz. In the case of AP = 483 MPa, the peak pressure was also
483 MPa. In the other cases, the peak pressure was 414 MPa.

SIC reinforced systems show similar strengths after sample is much more homogeneous and less granular,
the same processing route, while the TiOl system suggesting much better interparticle bonding.
is significantly weaker than the A&Or or SIC The fracture surfaces of Al/SIC and Al/A120r
reinforced composites after identical processing. We composite powder compacts obtained under static
expect that because the TiOl particles are so much and cyclic pressure conditions are shown in Figs 10
smaller than the lead particles, they tend to coat the and 11, respectively. Pressure cycling produces
initial particle surfaces and this inhibits interparticle significantly improved densification relative to the
bonding. static condition as well as more extensive particle
deformation and apparent interparticle bonding.
Microstructural observations
Many of the Al powders in the static case retain much
Comparisons of the fracture surfaces of PbjSiC of their original particle shape even though plastic
and Pb/TiOz composite powder compacts obtained deformation occurs on the Al particle surface. In
under static and cyclic pressure conditions are shown contrast, the original particle shape of Al powders in
in Figs 8 and 9, respectively. All the images presented the cyclic case can no longer be detected, with the
here were taken near the center of all specimens from exception of a few of the smaller Al powders.
machined bars that were broken in bending. In the
PbjSiC system, the images show that a larger number DISCUSSION AND ANALYSIS
of elliptically shaped cavities exist in the static case
than in the cyclic case. The size of these cavities These results show that the five composite systems
is similar to that of the Sic whisker agglomerates with relatively different combinations of material
after mixing. The cavities presumably develop their characteristics and morphology behave very similarly
elliptical shape owing to axial compaction. The in pressure cycling. Repeated pressure changes
existence of the fewer and smaller cavities in the cyclic consistently significantly improve compact density,
case suggests that Pb particles have become heavily green strength, and appear to produce more
deformed and appear to be somewhat able to homogeneous microstructure with improved inter-
penetrate the Sic whisker agglomerates and might particle bonding. We have proposed that this effect is
possibly bond with whiskers. Also note that in the due to compressibility mismatch between the matrix
high magnification images, particles appear to be and reinforcing phases inducing plastic deformation.
discrete after static compaction, but the material A significant amount of support for this idea
is much more homogeneous and continuous after was presented in a previous publication [l]. For
cyclic compaction. example, the observation that pressure cycling does
In the Pb/Ti02 system, the image in the static case not significantly improve the densification of
shows little evidence of either gross plastic defor- single-phase powders of cubic crystals is in support of
mation of the lead or particle-particle bonding. In this idea. Also, other possible mechanisms for
contrast, the surface of the cyclically compacted enhanced densification were considered [l]. Possibly,
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4291

the most plausible other explanation is that pressure The main purpose of this paper is to examine if
cycling produces sample heating owing to plastic there is a first-order trend that runs through several
work, or punch-die friction (elastic deformation can data sets. By the logic presented briefly in the
also produce a temperature change, but these heat introduction and a little more thoroughly elsewhere
flows are reversible). Indeed, pressure cycling does [l, 13, 17,211, we believe that if mismatch strains are
cause moderate temperature rises. At 10 Hz at steady responsible for improved densification, the ratio
state (i.e. over 2 h of cycling), a temperature rise of AfiAP/c, should represent a rough, but predictive
5°C is measured on the die (upon removing the figure of merit for pressure cycling compaction,
compact, we also note the temperature rise of the so long as data sets are compared at the same
sample and die are quite similar). However, at 1 Hz, reinforcement fraction and number of cycles. Of
there is no detectable temperature rise on the die. As course, changes in relative sizes of the metal and
the change in measured density is the same in both reinforcement, differences in particle morphology,
cases, the effect of temperature rise can be discounted. differences in initial packing density, and compli-
Furthermore, similar temperature rises take place cations like agglomeration are fully expected to
in cyclic compaction of pure metals, and cyclic modify this first-order “model”.
compaction at 10 Hz only slightly increased the In order to assess this figure of merit, the yield
density of pure lead and zinc compacts relative to strain (or yield stress and Young’s modulus) of the
static compaction. matrix powder materials must be known. This was

Fig. 8(a,b). Caption overleaf.


4292 HUANG and DAEHN: EFFECT OF CYCLIC‘ PRESSURE

Fig. 8. Fracture surfaces of Pb-40% Sic, green composite powder compacts broken in three-point
bending; (a) and (b) show the material that was consolidated at 414 MPa static pressure for 10,000 s (c)
and (d) show material subjected to 100,000 cycles at IO Hz to a peak pressure of 414 MPa. These images
were taken near the center of specimens and the compaction direction is vertical.

estimated by simple uniaxial compression tests on 70 MPa may appear to overestimate the aluminum
unreinforced metal compacts. Pure metal powders flow stress based on the data shown in Fig. 12, this
were first compacted at 414 MPa for 10,000 s to may still underestimate the actual material flow
a final L/D ratio of 2.0 and the fractional stress.
density fortuitously turned out to be 93% for each of The data shown in Figs 4-6, as well as data from
the three metal compacts. The results of the the Pb-A1201 system published earlier [1], is replotted
compression tests on each of these compacts are in terms of the change in fractional density relative to
shown in Fig. 12. The exact yield point is difficult to static compaction vs the normalized mismatch strain,
precisely identify in each case, but estimates that are A jAP/c, in Fig. 13. The results show that despite
reasonable for this first-order analysis are available. differences in morphologies, relative sizes, and
We estimate the yield stresses of the Pb, Zn, and properties, all six data sets nearly collapse to
Al systems to be approximately 30 MPa, 90 MPa, one relatively narrow band. Specifically, density is
and 70 MPa, respectively. In the case of the Al increased by pressure cycling in each system when the
system, the compact began to peel apart long before mismatch strain becomes greater than approximately
peak load, suggesting the actual yield strength of three times the matrix yield strain, and very
the material was not reached. As a result while significant changes in density are observed after
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4293

Fig. 9. Fracture surfaces of P&40% Ti02, green composite powder compacts broken in three-point
bending; (a) shows the material that was consolidated at 414 MPa static pressure for 10,000 s; (b) shows
material subjected to 100,000 cycles at 10 Hz to a peak pressure of 414 MPa.

100,000 pressure cycles when the mismatch strain the same pressure, densities no higher than 98% of
becomes about six times the matrix yield strain. theoretical could be obtained. Thus, the proposed
These data can be compared with those on powder figure of merit of the normalized mismatch strain
consolidation of white cast iron powders subjected to seems to give insight. Many cycles with small
pressure through 10 cycles of ferrite-austenite phase mismatch strain can give similar effects to a few cycles
transformations induced by temperature cycling with very large mismatch strains.
performed by Ruano .et al. [22]. In this case, the Of course, the explanation presented here falls far
calculated normalized mismatch strain is about 140, short of a careful first-principles model. Factors such
but full densification was obtained in 10 phase as relative particle size, agglomeration, particle shape,
transition cycles. In isothermal deformation at and possibly the frictional or sticking conditions
4294 HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE

Fig. 10. Fracture surfaces of A140% Sic, green composite powder compacts broken in three-point
bending: (a) shows the material that was consolidated at 414 MPa static pressure for 10.000 s. (b) shows
material subjected to 100,000 cycles at IO Hr to a peak pressure of 414 MPa.

at the matrix-reinforcement interfaces are fully powder composites as many hot or cold compac Zion
expected to influence the results. Thus, one would not devices can simply be equipped to apply cyclic 1oads
necessarily expect the data shown in Fig. 13 to at rapid loading rates.
collapse to a single line, and more variation than is
shown may well be expected even within the confines
CONCLUDING REMARKS
of our explanation. While it would be desirable to
“model” this process from first principles, the authors Six composite powder systems with 40% reinfc Irce-
believe this would presently be a formidable task. ment have been studied both in static compaction and
Regardless of this, it appears that this mechanism can in pressure cycling compaction under val :ious
simply be used to improve the consolidation of pressure amplitudes. A very consistent trend ran
HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE 4295

Fig. 11. Fracture surfaces of AlAO% A120jp green composite powder compacts broken in three-point
bending; (a) shows the aterial that was consolidated at 414 MPa static pressure for 10,000 s, (b) shows
material subjected to 100,000 cycles at 10 Hz to a peak pressure of 414 MPa.

through all these data. At small pressure cycle can induce plastic deformation. As the entire
amplitudes, cycling did not improve consolidation; experiment takes place in compression, this plastic
however beyond a critical amplitude, density strain can aid in closing porosity [23]. This is similar
increases in a nearly linear manner with increasing to the manner in which the plastic deformation in
pressure cycle amplitude. We have proposed that this rolling or extrusion can close porosity in materials,
effect takes place because the elastic compressibility except that in this case plastic deformation accumu-
mismatch strain (APAP) can become large relative to lates over small plastic strain increments in each
the yield strain of the matrix (co). When the elastic cycle.
mismatch becomes much greater than the matrix When all six data sets were compared in terms of
yield strain, the imposed change in hydrostatic stress change in density vs A/SAP/c,, we find that despite
4296 HUANG and DAEHN: EFFECT OF CYCLIC PRESSURE

effect to be quite general and the effect can bc


extended to new systems through consideration ot
A/?AP/t, as a normalizing term. Also, even with only
this empirical understanding of this effect. it might
be used profitably in practical powder compaction
as cyclic loads are easy to apply rapidly and the
matrix yield strain can simply be reduced by heating
the powder compacts. This makes the effect useful in
a wide number of systems.

REFERENCES
1. Huang, C. Y. and Daehn, G. S.. Acta metall., 1996, 44,
1035.
-0.~00 0'01 0.‘02 0.03 0.04 0.05 2. Ramakrishnan, P., in Advances in Powder Metallurgy
and Particulate Materials, Vol. 9, ed. J. M. Capus and
R. M. German. Metal Powder Industries Federation.
Princeton, NJ, 1992, p. 237.
Fig. 12. Normalized load-displacement curves taken in
3. Hunt, W. H. Jr and Rodjom, T. J., Ibid. p, 21.
compression for compacts of pure Pb, Zn, and Al powders
4. Sagar, R., Madan, P. K., Kumar, M. and Sachdeva, S..
consolidated to 93% of theoretical density. The range of u0
Ibid. p. 45.
inferred is 2244 MPa for Pb, 655100 MPa for Zn, and
5. Mileiko, S. T.. in Fabrication of Composites, Vol. 4,
4658 MPa for Al.
of Handbook of Composites, ed. A. Kelly and S. T.
Mileiko. Elsevier Science Pub., New York, 1983. p. 221.
significant differences in the morphologies and 6. Rack, H. J.. in Metal Matrh Composites: Processing
properties of the systems, all the data for change in and Interfaces, ed. R. K. Everett and R. J. Arsenault.
Academic Press, San Diego, CA, 1991, p. 85.
density vs AjAP/t, collapse to one trend wherein
7. Singh, B. N., Powder Metall., 1971, 14, 277.
when the normalized strain mismatch is less than 3, 8. Lange, F. F., Atteraas, L., Zok, F. and Porter. J. R.,
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