Materia& Science and Engineering, A 147 ( 1991) 229-237 229

Reaction rates during mechanical alloying

B. J. M. Aikin, T. H. Courtney and D. R. Maurice
Department of Materials Science, University of Virginia, Charlottesville, VA 22901 (U.S.A.)

(ReceivedFebruary 20, 1991; in revised form April 22, 1991)

Abstract

This paper presents a simple kinetic model of the coalescence and fracturing events that occur during
mechanical alloying (MA). The model is based on reaction kinetics based on times between powder par-
ticle collisions and particle specific probabilities of welding and fracture. The model is combined with
experimental studies and previous models of the MA process to provide information relative to the
welding and fracturing probabilities of the various particle species involved. We find that, during MA of
Cu-Nb alloys in an attritor, the probability of welding for copper particles is approximately one in 2000
for a ball-to-powder charge ratio of 50 to one. Decreasing the charge ratio decreases the probability of
particle welding and lengthens the milling time necessary for alloying.

1. Introduction consolidation by cold pressing and subsequent

Mechanical alloying (MA) is a solid state pro-
cess used for generating powders manifesting
novel and/or unique microstructures. Amor-
phous powders [1-6], intermetallic materials [7,
8], solid solution alloys [9], and metal matrix
composites of fine microstructural scale [10-12]
can be made through this process. State of the art
dispersion-strengthened materials are produced
commercially via M A [13-19] and novel uses of
mechanically alloyed materials are currently
being developed [20-23].
MA is the high energy ball milling of powdered
materials in a dry environment and is sometimes
termed reaction milling. Spex shaker mills, attri-
tors, planetary mills and ball or rod mills of large
diameter are used to produce M A powders for
research and commercial applications. The rela-
tive tendencies for particle welding and fracturing
in the mill can be optimized by altering the atmos-
phere, temperature, process control agents, ball-
to-powder charge ratio, and impellor or mill
rotation rate. The resulting mechanically alloyed
powders are then consolidated using conven-
tional powder metallurgy techniques (e.g. extru-
sion, hot isostatic pressing). However, the high
hardness of most M A powder often precludes
sintering.
What occurs during MA is known in a qualita-
tive sense [24-36]. For example, metal powders
generally become flake-shaped particles. If a
metallic charge is composed of two elemental
powders of comparable hardness, a lamellar-like
structure is developed. This lamellar structure
becomes progressively finer with continued
alloying, often giving rise to a very fine crystalline
structure or an amorphous material due to the
extensive cold work attendant to MA. If particles
of a relatively hard material are milled with parti-
cles of a soft material, the harder particles are
fractured and distributed between the welds of
the softer particles. The dispersion of the hard
particles becomes more uniform as milling pro-
ceeds. The milling process is often considered
complete if the lamellar structure can no longer
be resolved by optical microscopy or if a prop-
erty, such as hardness, attains an asymptotic level.
Quantitative descriptions of MA have been
slower in coming. This is undoubtedly a result of
the complex nature of the process. We, and
others, have recently attempted descriptions of
M A in terms of the mechanics and geometry of
the process [37-41]. In this paper we report on a

0921-5093/91/S3.50 © Elsevier Sequoia/Printed in The Netherlands

230
first attempt to determine "time constants" of the
MA process. This is done through some straight-
forward (albeit tedious) metallographic observa-
tions on the extent of powder alloying of two ele-
mental and insoluble (copper and niobium) metal
powders. Experimental observations are com-
bined with a rate analysis developed in the fol-
lowing section. As described there, this analysis
can be coupled with our previous studies to
determine factors such as the probability of weld-
ing or fracturing events taking place during MA.
2. Process kinetics
The kinetics of the MA process bear similarity
to those described by first-order chemical reac-
tions. However, there are some important differ-
ences as indicated in Fig. 1. Figure 1 is a
schematic of the welding (coalescence) pheno-
mena that can take place during the alloying of
two elemental powders A and B, to form alloy
particles C. Three of these occurrences (2A-" A,
2B --"B, and 2C --, C) correspond to two like parti-
cles combining to form a single particle of the
same species. One event (A+ B--, C) corresponds
to the removal of an elemental particle of each
species and the production of an alloy particle.
Two events (A+ C ~ C and B + C ~ C) remove an
elemental particle from the distribution while
leaving the number of alloyed particles
unchanged. The evolution of the powder distribu-
tion during fracturing is easier to describe. When
a particle of any type fractures, it breaks into two
particles (A-" 2A, B -+ 2B, and C --' 2C).
The following terminology is used in the
description and equations that follow. The time
between collisions for a powder particle is taken
as 3; the probability of a coalescence event
between two particles in any one collision is aij
8 -.o
2A- ~ g 2 B --~ a
--~ ~ ~--~ ~ ~
A+B-+C A+C-+C
Fig. 1. Welding events in a b a l l - p o w d e r - b a l l collision that
can occur during MA.
(e.g. aAA is the probability per collision of two A
particles welding); and ai is the probability of a
particle of species i fracturing in a single collision.
The change in the number N A of particles of A
per unit time t is
dNg_ 1
d ~ - - ~ ( - NgfgCtgg--2NAfBCtAB
- 2NAfCaAC + NAn g ) ( 1)
where f~ is the fraction of species i in the powder
mixture. The factor of 2 in the second and third
terms arises from considering both A-B (and
B-A) or A-C (and C-A) welding events. An
equation similar to eqn. (1) can be written for par-
ticles of species B. The corresponding equation
for the alloy particles is
dNc = 1 (
-- - N c f c a c c + 2NAfBaAB + N c a c ) (2)
dt r
Division of eqns. (1) and (2) by the total number
of particles N( = NA+ Na + Nc) leads to
1 dNg 1
- (--fA2CtAA- 2fAfat~gB
N dt r
- 2fgfcaAc +fAnA) (3)
with a comparable expression for dNB/dt , and
1 dNc 1
N - dt
- - ( - f c r2 a c c + 2 f A f s a A s + f c a c ) (4)
The above equations are general. That is, they
can be used to describe the evolution of particle
numbers with time during MA for each species in
the mill. However, there are three coefficients
describing the fracturing processes and six
describing the welding events. In principle, the
number of independent coefficients can be
reduced to seven by measuring the evolution of
particle numbers during the milling of elemental
powders. Such a procedure would yield the dif-
eren e etweeo, eorexampe, oAAan o
with this simplification, the equations would have
ven
2C-+C limited value due to the large number of indepen-
dent coefficients. The analysis can be made more
~ ~ useful, albeit less general and precise, through
some simplifying assumptions.
B +C--) C
We assume the various coalescence and frac-
turing probabilities are independent of particle
species to a first approximation. Thus a~ is desig-

nated as aw and ai as af. With this approxima-
tion, the sum of the rates of change for the total
number of particles can be obtained as
1 d N _ 1 ( a f - aw) (5)
N dt v
If N o is the initial number of particles in the
ensemble, then
N (a~- aw)t
N 0 - exp T (6)
That is, when af> t/w, the number of particles
increases with time and vice versa as intuitively
expected.
Particle numbers can be measured through
surface-to-volume (i.e. particle size) analysis for
the entire batch. However, information relative to
welding probabilities can be obtained by measur-
ing the fraction of particles of each species. As we
show next, the measurement of particle fractions
for each species is relatively straightforward
experimentally.
The fraction of particles of species A is defined
by fA = NA/N and since both N g and N vary with
time
dfA_ 1 dNA NA d N
dt N dt N 2 dt
l dNA fA d N
- N dt N dt (7)
Substituting expressions from eqns. (3) and (5)
into eqn. (7) leads to
dfA_dt awfA(lr --fg) (8)
On integrating this expression between the origi-
hal particle volume fraction fA0 of A and fg, and
between t = 0 and t = t, we obtain
fA _ f A , ~ e x p ( ~--) (9)
1--fA 1--fA0
There is a corresponding expression for the frac-
tion of B particles. Thus these simplifying
assumptions allow the determination of the weld-
ing probability if the time between powder par-
ticle collisions is known. The latter can be
estimated using previously developed descrip-
231
tions of MA. This simplified analysis has been
applied to the model system Cu-Nb as described
in the following section.
3. E x p e r i m e n t a l p r o c e d u r e a n d r e s u l t s
Commercially pure - 3 2 5 mesh copper and
niobium powders were used as starting materials
in the experiments. Elemental powders were
mounted in epoxy and polished for microscopic
analysis and hardness determinations. The start-
ing copper powder particles were small spheres
containing significant porosity (Fig. 2(a)) and
had a Vickers microhardness of 54 V H N
(approximately 180 MN m-2 = 26 000 lbf in-2).
The niobium particles were angular in shape (Fig.
2(b)) having a VHN of 153 (approximately 510
M N m - 2 = 7 4 0 0 0 lbfin-2).
Blends of elemental powders were milled for
various times in a heavy duty laboratory attritor
with a water-cooled jacket using an impeller rota-
tion of approximately 280 rev min- 1. The grind-
ing media were hardened stainless steel balls
0.48 cm in diameter. A dynamic atmosphere
of 90% Ar and 10% 02 was maintained in the
attritor. Several different compositional blends
were used: Cu-11vol.%Nb, Cu-15vol.%Nb and
Cu-50vol.%Nb. The Cu-llvol.%Nb blend was
milled with a ball-to-powder charge weight ratio
CR of 50:1 for times between 1 and 10 h. The
CR for the other two blends was 10:1, and mil-
ling times varied between 1 and 20 h.
As expected, the degree of alloying increased
with milling time. The backscattered electron
micrographs of Fig. 3 illustrate a series of
Cu-15vol.%Nb alloys milled for various times.
The "white" areas in the micrographs correspond
to areas of high niobium content, the gray to cop-
per, and the black area is background. In alloys
milled for only 1 h (Fig. 3(a)) many pure copper
and niobium particles remain. Moreover, the
shapes of these elemental powders closely re-
semble their initial morphologies, suggesting
they have been involved in a minimal number of
impacts during milling. A few flake-shaped alloy
particles, containing layers of both copper and
niobium, can also be seen in Fig. 3(a). After 5 h of
milling (Fig. 3(b)) the fraction of alloy particles
has increased substantially and almost all of the
particles are alloyed after milling for 15 h (Fig.
3(c)).
Determination of the fraction of alloyed and
unalloyed particles was done in two different
232

f ways. Optical microscopy was used for the

Cu-llvol.%Nb samples. Point counting was
employed on mounted and polished powder par-
ticles. For relatively short milling times a reason-
ably high accuracy can be attained by this
technique due to the different colors of metallic
niobium and copper. The sensitivity of the tech-
nique becomes less as alloying progresses. In
particular, niobium layer thicknesses become
comparable to the resolution available with opti-
cal microscopy. Thus data obtained by this proce-
dure are most accurate for relatively short milling
times.
The Cu-15vol.%Nb and Cu-50vol.%Nb alloys
were, subsequent to alloying for various times,
mounted, polished and carbon coated for ex-
amination with a JEOL 35C scanning electron
microscope equipped with a Tracor Northern
energy dispersive X-ray analysis system. This sys-
tem was used to determine the chemical composi-
tion and size of each powder particle via scanning
; ~: of the electron beam. At least 500 particles for
....................... each sample were analyzed in this manner. A par-
ticle was classified as copper if the composition as
determined exceeded 95 at.% Cu and a particle
was classified as niobium if its composition was
less than 10 at.% Cu. (Some measure of experi-
mental (and arbitrary) judgement was required to
stipulate these limits. High background counts
corresponding to copper (from the sample hol-
der) were present in the spectra and could not be
removed before analysis. Therefore, in order to
obtain niobium particle fractions comparable to
those obtained by an optical analysis of mixed
copper and niobium powders, the criterion for a
"pure" niobium particle was set as a composition
less than 10% Cu.) All other particles were classi-
fied as alloy particles. Several Cu-llvol.%Nb
milled samples were "spot checked" using the
scanning electron microscope to determine if the
two types of analysis yielded comparable results,
which they did.
Particle fractions as a function of milling time
for the three alloys are provided in Fig. 4. The
Cu-1 lvol.%Nb alloy (milled with a CR of 50) is
essentially completely alloyed in 10 h of milling
(Fig. 4(a)). We note that the definition of complete
alloying given here is the absence of pure copper
• , :~, and niobium particles. The data indicate that
........... while the copper particle fraction decreases con-
[] tinuously with milling time, and the alloy fraction
Fig. 2. Secondary electron micrographs of starting powders: concurrently increases, a significant fraction of
(a) copper particles; (b) niobium particles, niobium elemental particles remain at longer

milling times. This behavior, also observed with
the other alloy combinations, could result from
either a high niobium particle fracturing rate (due
to the initial hardness and subsequent work har-
dening of the niobium during milling) or a reluc-
tance of niobium to cold weld to copper and/or
alloy particles,
As shown in Figs. 4(b) and 4(c), decreases in
charge ratio require longer milling times to effect
complete alloying. The data in Fig. 4 can be
replotted in terms of the parameters of the analy-
sis described in Section 2. This is done in Fig. 5
where the parameter fA/(1 --fA ), divided by the
value of this parameter for the starting blend, is
plotted vs. milling time for both the copper and
niobium species. The copper particles behave in a
manner consistent with that predicted by the
analysis of Section 2; i.e. the data lie approxi-
mately on a straight line on the semilogarithmic
coordinates employed in Fig. 5(a). The time con-
stant r/aw for the coalescence reaction is the
time at which the parameter fA/(1-fA ) is equal
to 1/e of the initial value. This time is approxi-
mately 1.8 h for the material alloyed with a CR of
50 and is about 7.8 h for the materials alloyed
with a C R o f 10.
As shown in Fig. 5(b), the effective time con-
stant for the niobium particles is much higher
than it is for copper. Moreover, the agreement
between the simplified model developed in Sec-
tion 2 and the experimental data for niobium is
[]
Fig. 3. Backscattere~ectron micrographs of Cu-15vol.%Nb alloy powders milled for various times: (a) 1 h; (b) 5 h; (c) 15 h.
1"hewhite areas in the micrographs represent niobium, the gray areas are copper and the black regions are background.
233
not obvious. Since the geometry of alloying is
not dependent on particle species, we must con-
clude that niobium particles, as suggested earlier,
display a much greater reluctance to cold welding
than do the copper particles.
The time required to alloy copper varies
approximately in the ratio of the charge ratios
employed (7.8 h for CR = 10, and 1.8 h for
CR = 50). This is further illustrated in Fig. 6
where the time coordinate is now the milling time
multiplied by the charge ratio. Within experi-
mental accuracy, the kinetics of alloying are the
same for both conditions when this measure of
milling time is employed. Previous analyses of the
MA process [41] indicate that alloying times,
when defined on the basis of a critical accumu-
lated process strain, correlate with CR in this
simple and direct way. However, it is not clear
that reaction times as defined in the manner they
are in this paper should manifest this same kind
of correlation. Further discussion of this is pre-
sented in the next section.
4. Discussion
The experimental results indicate that the
kinetic analysis developed in Section 2 reasonably
describes the evolution of copper particles during
MA of C u - N b materials. It is also clear that the
assumptions made in the simplified analysis relat-
ing to the species independence of fracturing and
!
234

welding tendencies are not supported by the As noted, the effective time constants f l a w for
results we have obtained. Nonetheless, the simpli- the welding of copper powder are 1.8 h (6.48 ×
fied analysis "works" for copper, and the simpli- 103 s) and 7.8 h (2.81 x 104 s) for charge ratios
fied model can be considered a useful first of 50 and 10 respectively. T h e welding probabil-
approximation for describing M A kinetics. Using ity factor aw can be estimated as follows.
the analysis in this spirit allows it to be placed in T h e time r in eqn. (1) and those following is the
the context of our previous model dealing with time between impacts of a given powder particle.
the geometry and mechanics of M A [40, 41]. Thus r is obtained by first multiplying the time
between ball collisions r B by the ratio of the total
powder volume to the volume per impact and
then dividing this time by the number of powder
1.o particles in the impacted volume. The stipulated
multiplication takes into account that only a (rela-
0.0 tively small) fraction of the powder in the mill is
g 0.6'
involved in a given impact. The second factor,
that pertaining to the number of powder particles
0.4 in the impact volume, allows normalization to the
time between impacts of a given particle.
0.2 The above parameters can be estimated on the
basis of the simple model for M A developed by
0.0. . . . . . . . . . . Maurice and Courtney. The time between ball
5 10 15 20
T~r~,h collisions is the distance between collision sur-
(a)

1.0-

10

0.2" • .01

00 "'*" 9
0 5 10 15 20 .001
Time, h 5 10 is 20
Time, h
(b) (a)
lO
1.0.

0.8" 1 rT ~

i 0.6'

0.4'

0.2
%
" I

.01

.0OI . . . . ~ . . . . , . . . . , . . . .
0.0 . . . . , . . . . , . . . . , - - . .. , 0 5 10 15 20
5 10 lS 20 Time, h

~m,
(e)
Fig. 4. Particle fraction vs. time for mechanically alloyed
copper and niobium (u, copper; e, niobium; zx, alloy): (a)
Cu-1 lvol.%Nb, CR= 50:1; (b) Cu-15vol.%Nb, CR = 10:1;
(c) Cu-50vol.%Nb, CR = 10:1.
h (b)
Fig. 5. Normalized particle fractions of (a) copper and (b)
niobiumdecrease as a function of milling lime at different
rates depending on the charge ratio used during milling: m,
Cu-1 lvol.%Nb, CR=50:I; e, Cu-15vol.%Nb, CR = 10:1;
o, Cu-50vol.%Nb, CR = 10:1.
 235

faces divided by the relative impact velocity of the
balls in the mill. For an attritor of the type used in
this investigation, the relative velocity is about
0.53 m s-~ and the mean path between ball colli-
sions is estimated as 0.8 times the ball radius (i.e.
0.8 × 2.4 x 10-3 m). Thus rB = 3.6 × 10-3 S.
In determining the ratio of the powder volume
to the impact volume it is convenient to work
with a "unit cell" volume. For an attritor this
volume is that associated with a single ball, and
has a value about twice that of the volume of the
spherical ball. Since the charge ratio is defined as
the ratio of the tool mass to the powder mass, we
find that the powder volume Vpin this unit cell is
Vp- VBpB
CRpp
where VB is the ball volume, PB represents the
ball density, and pp is the powder density. The
analysis of Maurice and Courtney yields the
impact (collision)volume Vc as
0.8~RrhZpB
Vc -
3CRpp
where R is the ball radius and r h is the radius of
the impacted volume (the Hertz radius, see refs.
40 and 41 ). Equations (10) and ( 11 ) yield
VP = 5 (R]2
-- (12)
Vc \rh I
With R = 2 . 4 x 1 0 -3 m and r h = 5 . 9 × 1 0 -5 m
(from the analysis of Maurice and Courtney), Vp/
Vc = 8.3 × 103. When rB is multiplied by this
term, an effective time between volume impacts
of 30 s is obtained. This time must be divided by
the number of particles in the impacted volume to
determine the time between collisions for a given
particle. The particle sizes, as estimated via image
(10) analyses with the scanning electron microscope,
are given in Fig. 7. While there is a slight variation
among alloy systems as well as with milling time,
for the most part the powder particle volumes are
in the range of 1.4 x 10 -14 m 3 throughout the
milling process. Using the above equation for Vc
with PB = 8.80 g c m -3 and pp= 8.85 g c m -3, w e
obtain
(11)
700 x 10- i4
Vc (13)
CR

, 0 ~ Thus the average number of particles per colli-

,~ o sion ranges from 50 for a charge ratio of 10 to 10
~ for a charge ratio of 50. (These are relatively
" • small numbers of particles per collision. It has
,-" ~ " ] ~,,...~ . been stated that somewhere on the order of 1000
1 * . powder particles can be involved in a single colli-
'°' l . , i ~ sion. Indeed this can be the case for low charge
ratios (e.g. C R = 3 ) and relatively fine powder
.~1 • , particles (e.g. particle radii on the order of 10
0 100 200 300 400 500

MIIIIngTIme* Charge Ratio, h ~m). The small numbers found here result from
(a)
10.

60'

o •° o . -- h.-
@

c
o
.01 " .-~ 20

,001 , , , , 10 •
100 200 300 400 500
MilllngTIme * Charge Ratio, h
0 . . . . i . . . . i . . . . i . . . . i
(b) 5 10 15 20
Time, h

Fig. 6. Normalized particle fractions are independent of

charge ratio when plotted against the milling time multiplied Fig. 7. Equivalent spherical diameter of powder particles
by the charge ratio for (a) copper and (b) niobium (symbols as that have been mechanically alloyed for various times: e,
in Fig. 5). Cu-15vol.%Nb, CR = 10:1; o, Cu-50vol.%Nb, CR = 10:1.
236
the relatively large charge ratios used in this
study, and the relatively large particle sizes
(volume equivalent diameter, approximately 30
~m) generated.) On this basis, the time between
collisions for an individual particle is
30 s
r=--=0.6 s (14)
50
for CR = 10 and
30 s
r= =3s
10
for CR = 50.
As noted when the parameter fA/(1--fa )
reaches 1/e of its initial value, a w t / r i s unity. The
corresponding milling times were found in Sec-
tion 3 to be 2.81 x 104 s for a charge ratio of 10
and 6.48 x 103 s for a charge ratio of 50. There-
fore the welding probabilities are
0.6
a w - 2.81 x 1 0 4 - 2.1 x 1 O-5
for CR = 10 and
3 4 L. Schultz, Mater. Sci. Eng., 97(1988) 15.
a w - 6.48 x 103 =4.6 x 10-4
for CR = 50. Note that the welding probabilities
increase with the charge ratio, at least on the basis
of the model used. This is reasonable since the
energy expended per particle is greater when the
impact volume contains fewer particles. In a
philosophical sense, this result is consistent with
ideas related to microstructural refinement
during MA. Refinement is promoted by high
charge ratios which lead to a greater process
strain per collision and a corresponding reduc-
tion in the time required for alloying,
5. Summary
A kinetic model based on coalescence and
fracturing events that occur during M A has been
d e v e l o p e d . T h e m o d e l is b a s e d o n the c h a n g e in
particle species numbers which is reflected by
probabilities for welding and fracturing of each
particle species. The assumption that the welding
and fracturing probabilities were independent of
particle type is not fully supported by the experi-
mental data. On the other hand, the model does
reasonably mimic the extent of alloying depen-
dence on milling time. In addition, the variation in
copper particle fractions in mechanically alloyed
C u - N b materials is consistent with the model.
Using a model of M A derived by Maurice and
Courtney, it was found that the welding probabil-
ity increases with charge ratio (giving rise to
shorter milling times). This is likely due to a
smaller number of particles and a larger amount
of energy absorbed per particle during a collision.
This work is being continued in order to deter-
mine the species-dependent welding and fractur-
(15)
ing probabilities.
Acknowledgment
This work was supported by the Army
Research Office with Dr. Andrew Crowson as
grant monitor.
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