Scripta METALLURGICA

et MATERIALIA

Vol. 24, pp. 873-878, 1990

Printed in the U.S.A.

MICROSTRUCTURE-PROPERTY

CORRELATION

IN AI/TiB2(XD*)

Pergamon Press plc

All rights reserved

COMPOSITES

A.K.Kuruvilla, K.S.Prasad, V.V.Bhanuprasad and Y.R.Mahajan

Defence Metallurgical Research Laboratory
Hyderabad - 500 258, INDIA
(Received October
(Revised February

16, 1989)
22, 1990)

Introduction
Aluminium
alloys
discontinuously
reinforced with
ceramic
particulates,
whiskers
or fibres are currently being developed for various
high performance
applications.
SiC appears to be the most popular choice by virtue of its good
compatibility with aluminium and influence on the strength and stiffness of the
composite. However, other materials like B.C(1), TIC(2), TiB2(3,4) and AI20 ~ (5)
have
been examined for potential reinforcement applications in aluminium m~trix
composites. In a previous study (6), a comparison of the tensile properties
and
the moduli of AI/B4C, AI/TiC, AI/SiC and AI/TiB 2 composites showed that TiC was
the most
potent
reinforcement.
Recently
Roebuck
and Forno
(4) have
systematically
carried out a comparative study of 2014-AI alloy reinforced with
either
SiC or TiB 9 particulates. It was found that TiB~ is a more
effective
reinforcement
as ~ompared
to SiC as far as the
srengthening
effect
is
concerned.
The
size
of the reinforcement particles would have an influence
on the
properties
of the composites. It is expected that a reduction in the particle
size of the reinforcement would lead to improvements in strength, assuming
all
other
things
(shape,
chemistry
and
distribution)
are equal.
The matrix
reinforcement
bond also plays a significant role in influencing the properties
of the
composite. A strong mechanical bond without the presence of a chemical
reaction product would be expected to show the best properties in composites.
In light
of the forgoing discussion, the possibility
of forming
TiB_
z
in-situ
in an aluminium matrix by XD process (7) appears to be very attractlve,
as it opens
up a new avenue for producing metal matrix
composites.
In this
process,
Ti and B are elementall~ blended with A1 and the resultant
blend
is
compacted
and heated to about 800 C. In the presence of a liquid phase, the Ti
and
B react exothermically to produce submicron size TiB 9 dispersoids.
These
dispersoids
would have a considerable effect on the strength of the composite.
The matrix-reinforcement
interface
could also be sound considering
that the
reinforcement is formed in-situ in the matrix (8,9).
The present study compared two types of AI/TiB 2 composites. In one
case,
the AI/TiB 9 composite was prepared by blending TiB 2 particulates with AI, while
in the ot~er
case,
Ti and B were added in the elemental
form to A1 and
subsequently
processed
so as to form AI/TiB~ composite. Such a comparison
is
unavailable
in the literature; it is also timely since this process appears
to
be attractive and clear understanding of the process and nature of the interface
is lacking.
Experimental

Procedure

The composites were fabricated using powder metallurgical techniques.

The
atomised aluminium powder (0.023% Fe, 0.15% Si) was supplied by the Metal Powder
Co., Madurai, India, and had an average particle size of 45um. In one case,
the
* P r o p r , e t o r y process o f M a r t i n M a r i e t t a L a b o r a t o r i e s

873
0036-978/90 $3.00 + .00
Copyright (c) 1990 Pergamon Press plc

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MICROSTRUCTURE CORRELATION

Vol.

24,

No. 5

A1 powder was blended with TiB9 particulates (99.5% pure and average size of
4
um from CERAC) to form A1 / 20 v/o TiB 9 composite. The uniform
dispersion
of
TiB 9 p a r t i c u l a t e s in A1 matrix was achieved by following the wet blending route
usiHg polar solvent (i0). In the other case, Ti powder (ii00 ppm 09, 200 ppm N~
from Micron
Metals,
Inc.) with an average size of 36 um was
bl~nded
with
B
powder (99.9% pure from CERAC) having an average size of 1 um, and this mixture
was
further blended with the A1 powder. In elemental blending, 17 wt% of Ti and
8 wt%
of B powders were taken so as to form 20 volume percent of TiBin the
composite
if all the Ti reacted
with
B. Those
two powder
blinds were
cold-isostatica~ly pressed at a pressure of 200 MPa and subsequently degassed in
vacuum
at
450 C for lh. The AI-Ti-B compact was heated to 800 C in an argon
atmosphere
and held at that temperature for 15 mins. The AI/TiB 2 compact
thus
obtained
(henceforth
referred to as AI/TiB 2 (XD)) was porous
in nature.
One
sample 8f pure A1 powder was also cold-isostatically pressed, degassed in vacuum
at
450 C and
sintered
at
600C for lh. This was done
for the purpose
of
comparison with the composites.
Both the compacts were rolled into rods of 6mm dia at a temperature
of
600C.
Rolling
of these compacts into round sections was accomplished
by a
special
canning
process which helped to consolidate the material
and prevent
breakage
while
rolling. The processing sequence for the AI/TiB 2 composite
is
schematically shown in Fig.l(a), and that for AI/TiB 2 (XD) is shown in Fig.l(b).
Samples were taken from the composite rods and polished for metallographic
examination.
The microstructure was observed both under an o p t i c a l microscope
and
SEM.
Thin foils for TEM were prepared by a twin jet polishing
technique,
using an electrolyte of methanol, butanol, and perchloride acid. The foils were
observed in a Philips EM430T electron microscope at 300 kV. X-ray diffractometer
scan was made on AI/TiB 2 (XD) specimen using Cu Ku radiation.
Elastic moduli of these samples were measured on machined rods of 5mm dia
and
100mm
length
using a resonance technique (by analysing
the vibrational
behaviour
of the sample following an impulse excitation). Tensile test
samples
having
a gauge diameter of 4 mm and a gauge length of 25mm were machined
from
the rods and tested at a strain rate of 6.6 x i0 /s. The fracture surfaces
of
the tensile tested samples were examined in the SEM.
Results and Discussion
The microstructure
of the AI/TiB9 composite is shown in Fig.2.
The TiB 2
particulates
appear well dispersed in he matrix, though they are irregular
in
shape.
In comparison,
the
AI/TiB 2
(XD)
composite
reveals
a different
microstructure
as shown in Fig.3. THere are some coarse particles
which
have
been found to be an intermetallic phase of unknown composition A1 Ti. Apart from
these coarse precipitates, micrometer -sized TiB 2 precipitates ar~ also present,
and adhere well to the matrix.
Table
1 shows the tensile properties of the two composites.
The tensile
property values of pure A1 are also shown for comparison. The elastic modulus of
the AI/TiB 9 composite (96 GPa) is substantially higher than that of pure A1
(70
GPa)
althSugh
the value is much lower than the value of 143 GPa predicted
by
application of the rule of mixture. However, the AI/TiB 9 (XD) composite shows
a
value
of 131 GPa, which is substantially high and is almost double the modulus
of pure AI. Considering the strength values, the AI/TiB 2 composite
displays
a
yield strength of 121 MPa compared to the 64 MPa of pure A1 and a UTS of 166 MPa
compared
to the
90 MPa of a pure A1. The AI/TiB 2
(XD)
composite
displays
dramatic improvements in strength. The YS and UTS of this composite are 235 MPa
and
334 MPa, respectively. These strength values are significantly higher
than
that of a conventionally processed A1/TiB 2 composite. The major contribution
to
stengthening
is most likely due to the flne dispersion of the high-modulus TiB 2
particles which are well bonded to the matrix(8).
The XD route followed in the present case probably involves the solution of

~l.~uaTRu~uR~

C ~ A , I O N

875

Ti and B in liquid A1, and the solute assisted reaction leading to the
in-situ
formation
of
submicrometer
size
TiB9
dispersion(7).
Eventhough
the exact
mechanism
is not clear at this time, ~uch a process as described
above
would
result
in the formation of TiB^ in the liquid phase, thus forming an excellent
matrix/reinforcement
bond.
Th~ experimental results of XRD (Fig.4)
show the
presence
of TiB~ along with A1 peak in AI/TiBo (XD) composite.
The calculated
'd' values of TiB 9 are very close to the theor~tica! values. This observation is
further
confirmea with TEM of the same composite specimen. It may be noted that
the X-ray
diffraction
peaks corresponding to the A1 Ti phase
could
not be
observed
as its volume
fraction
was below the deection
limits o f
x-ray
analysis.
The microstructure
of the AI/TiB~ (XD) composite is shown in Fig.5.
The TiB~
particles
a.e present in ~he =orm of hexagonal and block-llke crystals (Fig.5=7
and the corresponding SADP is shown in Figure 5b. These TiB~ particles
are of
sizes
ranging
from a sub-micrometer to a micrometer level ~nd are distributed
uniformly in the matrix. A high dislocation density is observed at the particle
matrix interface (Fig.6). The presence of a high dislocation density observed at
the interface is probably due to (i) semi-coherent AI-TiB 2 interface produced by
in-situ
formation
of TiB~ crystals and (ii) thermal shock associated with
the
exothermic
reaction. The presence of extremely fine size TiB~ particles in the
matrix along with the dense interfacial dislocation sub-strucEure results in the
increased strength level in the AI/TiB~ (XD) composite. It may be noted that the
conventionally
produced
composite
~ontains
coarser
and
incoherent
TiB 2
particles, which are probably responsible for the lower strength.
The fracture surface of the tensile samples show the presence
of micron-sized
TiB^ in the case of the AI/TiB 2 (XD), as seen in Fig.7. Essentially the fracture
surface
displays
dimples
which
are
small
as compared
to that
of the
conventionally
processed
AI/TiBo
composite (Fig.8). Since
the size of the
dimples
indicate
matrix
controlled
fracture
defined
by the
interparticle
spacing, the smaller dimples suggest the fineness and closenes of the dispersion
of TiB 2 in the AI/TiB 2 (XD) composite.
Conclusion
The XD process(7)
shows great promise for the fabrication
of metal matrix
composites
for high performance applications. The AI-20 v/o TiB9 (XD) composite
shows a modulus of 131 GPa, which is higher than that of conventionally produced
composite. This process also results in MMCs with superior strength
properties,
as compared
to conventionally processed 5~Cs. These
results
are attributed
primarily
to the presence of extremely fine size TiB~
particles,
excellent
matrix reinforcement bonding, and dense interfacial disl~cation sub-structure.
Acknowledgements
The authors
thank
Dr.P.Rama
Rao, Director,
Defence
Metallurgical
Laboratory, for his encouragement and permission to publish this paper.

Research

References
l.H.K.Slater,
P.M.Coon,
Proc. 4th Int. A1 Extrusion Tech.
Seminar,
Chicago,
(1988), 2, p.525.
2.Baturinskaya et al., Izv. Akad. Nauk SSSR Met., (1983), 3, p.166.
3.J.W.Mccoy. C.Jones and F.E.Wawner, SAMPE Quarterly, (1988), 19 (2), p.37.
4.B.Roebuck
and A.EJ.Forno, "TiB 9 and SiC Particulate
Reinforced
Aluminium
Alloy Metal Matrix Composites", i~ Modern Developments in Powder
Metallurgy,
Voi.20,
p.451, Proc. 1988 International Powder Metallurgy Conf., June
5-10,
1988.
5.David
M.Schuster,
Michael D.Skibo and William R.Hoover,
Light
Metal
Age,
(1989), Feb., Voi.47, p.15.
6.A.K.Kuruvilla,
V.V.Bhanuprasad, K.S.Prasad and Y.R.Mahajan (To be published
in Bulletin of Materials Science, 1989).
7.L.Christodoulou, D.C.Nagle and Brupbacher (1986) Int. Pat. No. WO86/06366.

876

MICROSTRUCTURE CORRELATION

VoL. 24, No. S

7.L.Christodoulou, D.C.Nagle and Brupbacher (1986) Int. Pat. No. WO86/06366.

8.T,M.F.Ronald, Advanced Materials and Processes, (1989), 135 (5), p.29.
9.AR.C.Westwood, Met. Trans. A, (1988), !gA, p.749.
10."Method of Making SiC Whisker Sheet Composites", U.S.Patent No.4 634 608,
January 1987.
Table
Material

E
(GPa)

Pure A1
A1/20 V/O TiB2
AI/20 V/O TiB2(XD)

TiB2

AI

70
96
131

At

WET
BLENDING

/
I

=-

PRESSING

I
]

REACTION
SINTERING

,,

37
85
110

SINT~RING

450"C/1h

800"Cllh

CANNING

SECTION
ROLLING

I COMPOSITE
L
ROD

21
16
7

COLD I505TATIC
DEGASSING

SEC;ION
ROLLING

Hardness
VHN

DRY

% E1

90
166
334

L
J DEGASSING }
450C/lh .

1
CANNING

UTS
(MPa)

BLENDING

COLD ISOSTATIC]
PRESSING

I 6oo'c/,.

64
121
235

Ti.B

YS
(MPa)

I COMPOSITE
ROD

(a)

(b)

Fig. I: Schematic representation of processing sequence

Fig.2: SEM micrograph showing TiB 2

particulates in conventionally
processed A!/TiB 2 composite

(a) AI/TiB 2 conventional

processing
(b) AI/TiB 2 XO process

o=

Fig.3:SF24 micrograph

showing

blocky AlxTi intermeta!!ics and

T i ~ particles in AI/TiB 2 (XD)

composite

Voi.

24,

No.

NICROSTRUCTURE CORRELATION

877

11

!
E
I

~L ___jL_"

j k_. ......
20

Fig.4: X-ray diffractogram

TiB 2 peaks

showing

Fig.6: TEM mlcrograph showing

interracial dislocation substructure

Fig.5:

(a) TEJ~ micrograph showing the TiB 2 c r y s t a l ~ in AI/TiB2(~)

composite
(b) SADP of TiB9 - [O00I] Zone Axis

878

MICROSTRUCTURE CORRELATION

Fig.7: SEM fractograph of A!/TiB 2 (XD) composite

Fig.8: S ~ fractograph of AI/Ti82 composite

Vol. 24, No. 5