JOINING OF 6061AL-15 WT.

% SICP COMPOSITE USING TRANSIENT

LIQUID PHASE DIFFUSION BONDING TECHNIQUE WITH MIXED AG-
CU INTERLAYER

Pallab Roy, Tapan Kumar Pal and Joydeep Maity

____________________________________________________________________________

Pallab Roy (presenting author) is Ph.D. Research Scholar, Welding Technology Center,
Department of Metallurgical and Material Engineering, Jadavpur University, Kolkata- 700032,
West Bengal, INDIA. E-Mail: prsec1@gmail.com

Tapan Kumar Pal is Professor & Coordinator, Welding Technology Center, Department of
Metallurgical and Material Engineering, Jadavpur University, Kolkata- 700032, West Bengal,
INDIA. E-mail: tkpal.ju@gmail.com

Joydeep Maity is Associate Professor, Department of Metallurgical and Materials Engineering,

National Institute of Technology, Durgapur-713209, West Bengal, INDIA. E-mail:
joydeep_maity@yahoo.co.in
____________________________________________________________________________

Abstract

In the present study Microstructure and shear strength of transient liquid phase diffusion bonded
6061Al-15 wt.% SiCp extruded composite using a 50 µm thick mixed Ag-Cu powder interlayer
have been investigated. The bonding is carried out in commercial argon environment at 560 °C
and 0.2MPa pressure using 50μm thick mixed Ag-Cu powder interlayer. The bonding
temperature (560°C) was kept above the eutectic temperature (500.6°C) of Al-Cu-Ag ternary
system and below the solidus temperature (582°C) of 6061 matrix alloy. During isothermal
solidification that took 2 h for completion, due to diffusion of Ag and Cu in Al, a ternary liquid
phase evolved. Subsequent cooling formed a ternary phase mixture (α-Al+CuAl2+Ag2Al) upon
eutectic solidification. The kinetics of isothermal solidification was found to be much faster than
that observed for joining pure Al by 50 µm thick Cu foil interlayer (pure monolithic system) as
well as for joining same composite with 50 µm thick pure Cu foil/powder interlayer under similar
temperature and pressure. Presence of brittle eutectic phase mixture (CuAl2 + Ag2Al) led to
poor joint strength at short TLP bonding times. Increased holding time (6 h) erased shrinkage
via solid state diffusion and yielded the highest joint strength (87 MPa) and fair joint efficiency
(83%).

Keywords: 6061-SiCp composite; transient liquid phase diffusion bonding; mixed Cu-Ag
powder interlayer; isothermal solidification; eutectic phase mixture; joint strength.

1
1. Introduction
Extensive industrial applications of
aluminium based metal matrix composites
(AlMMCs) is restricted by the intricacy
encountered in joining them by
conventional processes (fusion welding,
solid state diffusion bonding etc.) in spite
of possessing better properties to
monolithic aluminium alloys [1-9]. The
transient liquid phase (TLP) diffusion
bonding process which involves four
stages; namely: (I) dissolution of interlayer
(II) homogenization of the liquid (III)
isothermal solidification and (IV)
homogenization of bond region at solid
state [9-26] has been found to be efficient
for joining AlMMCs. In most of the
investigations reported on TLP diffusion
bonding of AlMMCs, joint shear strength
and joint efficiency were investigated
keeping low bonding time (maximum of 2
h) without illustrating a relationship with
the fundamental process mechanism [9-
12, 22-24]. A comprehensive study in view
of achieving reasonable joint efficiency in
correlation with fundamental process
mechanism (particularly the isothermal
solidification stage) was first carried out by
Maity [27,28] and Maity et al. [29-33] for
joining 6061Al-15 wt.% SiCp composite by
TLP diffusion bonding process at 560°C
under 0.2 MPa pressure using 50 µm thick
pure copper interlayer (both in foil and
powder form). As compared to monolithic
pure system improved isothermal
solidification kinetics was observed in
composite system. With pure Cu interlayer
TLP diffusion bonding of AlMMC involves
Al-Cu binary system possessing a eutectic
temperature of 548°C [34]. If mixed Ag-Cu
is used as an interlayer, the resultant Al-
Ag-Cu ternary system possesses much
lower eutectic temperature (500.6°C) [35].
Moreover, the diffusion coefficient of Ag is
higher than Cu in Al [15, 36]. Thus, at a
particular bonding temperature (above
eutectic temperature) higher atomic
mobility of Al-Cu-Ag system as compared
to Al-Cu system would further improve the
kinetics of isothermal solidification.
Bushby and Scott [23] achieved a bond
strength of 54 MPa (60% joint efficiency),
in an early study on SiC fibre/Al
composite, using 50 µm thick Ag-29 wt%
Cu foil interlayer, for 30 minutes of holding
2
at 550°C under 20 MPa pressure in air
environment. The joint efficiency was poor
due to existence of oxides since the
bonding was not carried out in inert
environment or vacuum. Also, application
of high pressure caused a great deal of
undesired material deformation. Huang et
al. [37] in a current study, ascertained the
viability of joining 2618Al-17 vol.% SiCp
composite by TLP diffusion bonding using
mixed Al-Cu-Ag interlayer. But, neither
detailed mechanism along with kinetics
was studied nor the joint shear strength
was correlated with base material shear
strength in terms of joint efficiency.
Moreover, their approach was more
towards ‘Brazing’ and not ‘TLP diffusion
bonding’. The use of Al powder mixed with
Cu and Ag as an interlayer would instantly
form eutectic liquid irrespective of diffusion
of Cu and Ag in Al based matrix of the
composite. In true TLP diffusion bonding
process atomic diffusion of mixed Cu and
Ag powder interlayer into Al based matrix
of the composite should form transient
liquid phase. Accordingly, in the present
research work an investigation is carried
out on joining 6061 Al-15 wt.% SiCp
composite by TLP diffusion bonding
process at 560°C, 0.2 MPa, using a 50 µm
thick mixed Cu-Ag powder interlayer in
argon environment. The microstructure
development with bonding time has been
meticulously investigated with regard to
process mechanism correlating with joint
shear strength and mode of failure.
2. Experimental procedure
2.1 Material
The as-received material was an extruded
AlMMC rod consisting of 6061Al matrix
alloy (1.0 wt.% Mg, 0.6 wt.% Si, 0.3 wt.%
Cu, 0.2 wt.% Cr, 0.6 wt.% Fe and balance
Al) and 15 wt.% (13 vol.%) silicon carbide
(SiC) particulate reinforcement.
2.2 TLP diffusion bonding
The extruded rod was machined to
produce discs of 15 mm diameter and 10
mm in height. The faying surfaces of were
polished with grades of emery papers
soaked in kerosene & liquid paraffin (1:1)
up to 1000 grit, and finally with 1 μm
diamond paste. Then, the surfaces were
cleaned in acetone and dried by hot air
blast. To retain a mixed copper and silver
powder interlayer (1:2.1 by weight) of 50
μm thickness, initially 30 mg of copper
powder and 63 mg of silver powder was
taken and mixed thoroughly by manual
stirring. The proportion of copper powder
and silver powder was chosen on the
basis of eutectic composition of Al-Cu-Ag
ternary eutectic system (40 wt.% Al, 19.3
wt.% Cu and 40.7 wt.% Ag) [35]. After
manual mixing, a few drops of ethanol
were applied to the powder mixture to
make a paste. After applying the paste
between the discs, the assembly was
pressed from both sides and set by an
adhesive tape. The tape was then locally
dislodged at the joint region and thickness
of the powder interlayer was measured
under optical microscope with graduated
eye piece. Thickness of 50 μm was fixed
on several trials. Then the weight gain
was measured in a digital microbalance
(PRECISA-205A-SCS, Switzerland) to
determine actual mass of powder
interlayer. Considering all specimens, the
mass of mixed powder interlayer (mean ±
standard deviation) was found to be 87 ±
2 mg. Next, the assembly was inserted
inside the diffusion bonding unit
(programmable electric furnace), where
the bonding was carried out at 560°C
under 0.2 MPa pressure in argon
environment. The bonding temperature
was kept above the eutectic temperature
(500.6°C) of Al-Cu-Ag ternary system [35]
and below the solidus temperature
(582°C) of 6061 matrix alloy [38]. The
specimens were heated to the bonding
temperature at a rate of 9°C min–1, held at
that temperature for six different lengths of
bonding time, viz. 20 min, 1 h, 2 h, 3 h, 6 h
and 9 h; and cooled down to 480°C (below
eutectic temperature) at a rate of 5°C min–
1
inside the furnace. Then the specimens
were taken out of the furnace and cooled
in still air to the room temperature.
2.3 Bonded composite characterization
Bonded cylindrical samples were sliced
perpendicular to the bonding plane; then
polished, etched (using Keller’s reagent)
and studied under optical microscope with
digital photomicrography and image
analysis facility (ZEISS, Imager.A1m,
Germany) as well as under a scanning
3
electron microscope (JEOL, JSM-5800)
with energy dispersive X-ray spectroscopy
(EDS) detector (Oxford INCA EDS
System, UK). The grain size measurement
of the matrix was carried out following
ASTM E112 standard [39]. To assess the
joint shear strength, bonded samples were
machined to 10 mm diameter to eliminate
edge effects. These specimens of about
20 mm length and 10 mm diameter and
the as-received composite of similar
dimension were loaded in a specially
prepared jig (Fig. 1) and the grips were
pulled in tension in a 100 KN capacity
universal testing machine (INSTRON-
8862) at 0.5 mm min–1 cross head speed
in position control mode to subject the
specimen to pure shear stress across the
bond interface. The fractured surfaces of
the shear tested specimens were studied
under scanning electron microscope. Thin
specimens machined out from around the
fractured surface of the shear tested
specimens were subjected to XRD
analysis at slow scan rate (0.5° min−1) in a
high resolution X-ray diffractometer (X'
Pert Pro, PANalytical Instruments,
Netherlands).
Fig. 1: Jig for joint strength determination.
3. Results and Discussion
3.1 Microstructure evolution and
process mechanism
3.1.1 As-received Composite
In Fig. 2(a)-(c) the microstructure of as-
received extruded AlMMC is shown. SEM
back scattered electron (BSE) image (Fig.
2(a)) shows randomly dispersed Silicon
carbide (SiC) particles in 6061Al matrix.
Presence of SiC and an intermetallic
compound of iron and aluminium (FeAl3)
are further confirmed by respective SEM
based EDS spectra (Fig. 2(b) and (c)).
The presence of iron as an impurity in
6061 Al alloy in the form of FeAl3 is also
supported by literature [22] and justified
with the little solubility of iron in aluminium
as foreseen in Fe-Al phase diagram [34].
3.1.2 TLP diffusion bonded composites
The SEM BSE image at bond centerline
and EDS elemental mapping of the
specimen with 20 min holding are shown
respectively in Fig. 3 and 4.
Fig. 3: SEM back scattered electron image
around bond centerline of the specimen
with 20 min holding.
Fig. 2: Microstructure of as-received 6061-SiCp composite:
(a) SEM Back scattered electron image (b) EDS spectra of SiC (c) EDS spectra of FeAl3.
4
Segregated SiC particles with very fine
phase mixture of bright appearance are
identified at bond centerline (Fig. 3). EDS
elemental mapping specifies a high
concentration of Cu and Ag around bond
centerline along with Si and C. At higher
magnification this finely mixed region can
be resolved by SEM back scattered
electron image (Fig. 5(a)) where presence
of two phases, viz. Ag2Al and CuAl2 are
identified in a matrix of aluminium based
α-solid solution as seen in respective EDS
spectra (Fig. 5(b)-(d)), signifying existence
of a liquid phase at 560°C even after
holding for 20 min. This liquid is evolved
through interdiffusion and mixing of Ag
and Cu powders with Al based matrix
since the holding temperature (560°C) is
higher than the eutectic temperature of Al-
Cu-Ag ternary system (500.6°C). The
average width of the region containing
bright eutectic phase mixture (i.e. the
width of prior liquid zone) on 20 min
holding is measured as 69 µm. The first
two stages (melting of interlayer and
widening of liquid) of TLP diffusion
bonding occurs within a few seconds
[14,15]. In the present study, heating from
the eutectic temperature (500.6°C) to the
bonding temperature (560°C) at a rate of
9°Cmin−1 takes about 7 minutes. Thus, the
first two stages are completed during
heating to the bonding temperature.

Fig. 4: EDS elemental mapping around
bond centerline of the specimen with 20
min holding. SZ: segregation zone; ISZ:
Isothermally Solidified Zone.
The liquid widening completes and
isothermal solidification starts much
before 20 min of holding. Isothermal
solidification is not completed on 20
minutes holding, and some amount of
liquid is left out around bond centerline
adjacent to isothermally solidified zone
(ISZ). This residual liquid, undergoes
ternary eutectic reaction [35] during
cooling from bonding temperature to room
temperature,: Liquid → α + Ag2Al + CuAl2.
At 560°C, this liquid phase (eutectic
mixture of α, Ag2Al and CuAl2 at room
temperature) together with SiC particles
form the ‘segregation zone’. During
isothermal solidification, relatively smaller
SiC particles are pushed by the moving
solidification front and segregate around
the bond centerline; while coarser
5
particles are engulfed in the ISZ [29-33].
The region between segregation zone and
base metal solidifies isothermally at
bonding temperature (560°C), forming
‘ISZ’, where the presence of CuAl2 apart
from engulfed SiC and FeAl3, is identified
by SEM back scattered electron image
and EDS spectra (Fig. 6(a)-(d)). CuAl2
phase is found to preferably precipitate on
SiC particle. In bonded composites, the
CuAl2 phase is precipitated out in the ISZ
during cooling from the bonding
temperature as the solubility of Cu in
primary α decreases with decreasing
temperature following the solvus curve
[39], though the as-received unbounded
AlMMC does not contain any CuAl2 phase.
Fig. 7 and 8 shows the SEM micrographs
of the bond region for 1 h holding. The
overall SEM BSE image (Fig. 7) around
bond centerline reveals the presence of
fine bright eutectic mixture of Ag2Al and
CuAl2 in α-matrix, along with segregated
SiC particles. The average width of the
bright eutectic phase mixture region on 1
h holding is measured as 46 µm, lower
than that with 20 min holding (69 µm). The
reduction in the width indicates progress
of isothermal solidification. Besides, high
magnification BSE image of segregation
zone separately identifies relatively
brighter Ag2Al and less bright CuAl2 (Fig.
8(a)). In ISZ (Fig. 8(b)) presence of
engulfed SiC, CuAl2 precipitate and FeAl3
in α-Al matrix is observed. As a
remarkable feature, several grains are
observed around the SiC particle (Fig.
8(b)). However, many SiC particles (in the
form of cluster/segregation) are not
present at the triple point junction of the
grains. This signifies that the SiC particle
is not pushed and subsequently entrapped
by the converging solidification fronts.
During engulfment, solidification front
splits to generate many grains around a
particle. Solidification fronts recombine
away from the particle. In literature similar
phenomenon is reported [31,40].
For 2 hours of holding, bond centerline is
devoid of any eutectic mixture (Fig. 9(a)),
indicating nonexistence of any liquid
phase at 560°C that would have
transformed to eutectic mixture during
cooling.
 Fig. 5: SEM analysis of SZ at high magnification in the specimen with 20 min holding: (a)
SEM BSE image; and EDS spectra of (b) CuAl2, (c) Ag2Al, and (d) α-solid solution.

Fig. 6: SEM analysis of ISZ in the specimen with 20 min holding: (a) SEM back scattered
electron image; and EDS spectra of (b) SiC, (c) CuAl2, and (d) FeAl3.

This confirms the completion of isothermal
solidification with 2 hours of holding at
560°C for joining 6061Al-15 wt.% SiCp
composite using mixed Cu-Ag powder
interlayer. According to Natsume et al.
[15] and further analysis by Maity [27], for
joining pure aluminium by 50 μm Cu
interlayer at 570°C, isothermal
solidification takes about 9 hours 46
minutes for completion. This is much
longer duration of isothermal solidification
proportionate to much slower diffusion
coefficient of Cu in pure aluminium,
attributed to short-circuit diffusion in
composite through defect-rich particle-
matrix interfacial region of high dislocation
density unlike monolithic aluminium [38,
41-43]. While joining 6061 Al-15 wt. % SiC
by TLP diffusion bonding technique using
50 μm thick Cu powder interlayer under
0.2 MPa pressure at 560°C, Maity et al.
[31] experienced 3 hours holding time for
isothermal solidification completion.
Hence, kinetics of TLP diffusion bonding is
further accelerated at 560°C with the use
of mixed Cu-Ag powder interlayer instead
of pure Cu powder interlayer. On
completion of isothermal solidification the
entire bond region is basically the ISZ

6
containing engulfed SiC, CuAl2 precipitate
and FeAl3 in α-Al matrix (Fig. (9(a)).
Fig. 7: SEM back scattered electron image
around bond centerline of the specimen
with 1 h holding.
Analogous microstructural features are
observed for still higher bonding time viz.
3 h, 6 h and 9 h (Fig. 9(b)-(d)) where
entire bond region is isothermally
solidified. Shrinkage porosity appears
around bond centerline on completion of
isothermal solidification (2 h holding) (Fig.
9(a)) and persists for 3 h holding (Fig.
9(b)). Prolonged holding up to 6 h
eliminates these porosities (Fig. 9(c))
through solid state atomic diffusion under
pressure (0.2 MPa).
Fig. 8: SEM backscattered electron image
of the bond region at higher magnification
in the specimen with 1 h holding: (a)
Segregation zone; (b) Isothermally
Solidified Zone.
Another noteworthy feature observed is
the existence of SiC particle segregation
(Fig. 9(a)-(d)) even on completion of
isothermal solidification. In Fig. 10(a)-(b)
the selected EDS line scans representing
concentration variation of two main
diffusing species Ag and Cu across the
bond interface are shown. The
concentration gradient of Ag and Cu
existing initially (20 min holding) is
7
diminished through diffusion later on (6 h
holding), corroborating completion of
homogenization of bond region with 6 h
holding. Now, the diffusivity (D) of Cu in Al
and that of Ag in Al at the bonding
temperature (T = 833 K) can be calculated
based on the values of the frequency
factor (D0) and the activation energy (Q)
found from standard literature [15,36]
using the relationship: D = D0 e–Q/RT
(where, R = 8.314 J.mol–1.K–1, the molar
gas constant). D0 = 1.50 × 10–5 and 9 ×
10–4 m2 s–1; and Q = 1.26 × 105 and 1.10 ×
105 J mol–1 for diffusion of Cu in Al and
that of Ag in Al, respectively. Thus, it is
found that at 560°C (T = 833 K), the
diffusivity of Ag (1.14 × 10–10 m2 s–1) is
much higher than that of Cu (1.89 × 10–13
m2 s–1). Presence of Ag in the form of
Ag2Al precipitate is not found in the ISZ,
though CuAl2 precipitate is readily found,
attributed to the higher solubility of Ag in
Al than Cu in Al as observed in Ag-Al and
Cu-Al phase diagrams [34]. So, Ag mainly
remains in the primary α-solid solution
(aluminium based terminal solid solution)
in the ISZ; whereas in the segregation
zone it is present as eutectic Ag2Al. The
results of XRD study (Fig. 11) agree with
the peaks of Al, SiC and FeAl3 in as-
received composite. During isothermal
solidification (20 min and 1 h holding),
peaks of Al, SiC, Ag2Al, CuAl2 and FeAl3
are observed in bonded composites. On
completion of isothermal solidification (2 h
holding and onwards), peaks of all phases
except Ag2Al are obtained due to absence
of eutectic phases where bond region is
entirely ISZ and Ag mainly goes to solid
solution.
3.2 Bond strength and fractured
surface
In Fig. 12, shear strength of the joint for
various bonding time is graphically
presented. The as-received composite
possesses shear strength of 105±2 MPa
[27]. At lesser bonding time (20 min and 1
h) the bond strength is low and with
increasing holding time the bond strength
increases up to 6 h holding and then
decreases. The highest joint strength
(87±3 MPa) of the bonded composite is
achieved with 6 h holding, which is 83% of
the shear strength (105 MPa [27]) of the
as-received composite (representing 83%
joint efficiency). The fractured surface of
shear tested as-received composite
exhibits dimples and tear ridges (Fig.
13(a) and (b)), feature of distinctive ductile
fracture of Al/SiCp composite [44]. In Fig.
14(a)-(f) back-scattered electron images
of the fractured surfaces of bonded
composites are shown. For specimen with
20 min holding (Fig. 14(a)) flat brittle
fractured surface is observed.
Considerable existence of bright eutectic
phase mixture (CuAl2+Ag2Al) with a few
segregated SiC particles is visible. This
shows that the brittle intermetallic eutectic
particles (CuAl2+Ag2Al) are accountable
for failure with poor joint strength. The
failure occurs primarily through
decohesion at eutectic particle-matrix
interface in the segregation zone. In case
of the specimen with 1 h holding, fractured
surface (Fig. 14(b)) reveals the presence
of a large SiC cluster along with bright
eutectic phase mixture (CuAl2+Ag2Al). As
isothermal solidification advances,
proportion of eutectic phase mixture is
reduced (since amount of liquid phase is
reduced) and proportion of segregated
SiC particles is increased (due to more
particle pushing by solidification front),
resulting in improved joint strength. In this
case, both SiC cluster and brittle eutectic
Fig. 9: SEM back scattered electron images of the bond region for higher bonding time:
(a) 2 h; (b) 3 h; (c) 6 h; and (d) 9 h.
8
particles are the failure initiation sites. On
completion of isothermal solidification (2 h
holding), joint strength is further improved
due to elimination of eutectic phase
mixture from joint region. Here, fractured
surface mainly contains SiC particle
segregation, which is primarily responsible
for failure (Fig. 14(c)). Also, solidification
shrinkage porosity is observed on
fractured surface (Fig. 14(c)) in
accordance with that identified in SEM
metallography at the joint region (Fig.
9(a)). Therefore, solidification shrinkage
porosities are the secondary sites for
failure. Fractured surface for 3 h holding
(Fig. 14(d)) exhibits features similar to that
for 2 h holding, but the proportion of
shrinkage porosity appears to be reduced
(Fig. 14(d) and 9(b)). Further holding at
solid state up to 6 h eliminates
solidification shrinkage porosity through
solid state diffusion as observed in
fractured surface (Fig. 14(e)) and SEM
metallography at the joint region (Fig.
9(c)). Accordingly, highest joint strength
(87 MPa) and joint efficiency (83%) are
achieved for 6 h bonding time. Here,
segregated SiC particles are the main
failure initiation sites ((Fig. 14(e)).
Fractured surface for 9 h holding (Fig.
14(f)) appears similar to that of 6 h
holding.
However, the joint strength is reduced on
9 h holding as compared to 6 h holding.
This is attributed to grain coarsening of
the isothermally solidified joint region on
prolong holding at solid state.
Fig. 10: Selected EDS line scans
representing the concentration variation of
Ag and Cu across the bond centerline:
(a) 20 min; (b) 6 h.
Fig. 11: Results of X-ray diffraction
analysis.
The grain boundaries are clearly
delineated in optical metallography. The
grain sizes of the aluminium based matrix
at bond region measured (in terms of
average grain diameter) from optical
micrographs (Fig. 15(a) and (b)) of the
specimens with 6 h and 9 h holdings are
73±7 µm and 148±9 µm, respectively. This
indicates substantial grain coarsening
effect reducing the joint strength on
prolong holding (9 h) at solid state.
Compared to other investigations, the
maximum joint efficiency achieved (83%)
9
in the present investigation appears to be
a reasonable one. However, the presence
of particle segregation even after
completion of isothermal solidification is
responsible for not obtaining still higher
(above 90%) joint efficiency.
Fig. 12: Variation of mean shear strength
of the bond region with bonding time.
4. Conclusion
(i) TLP bonding of extruded 6061 Al-15
wt.% SiCp composite (560°C, 0.2 MPa)
using 50 µm thick mixed Ag-Cu powder
interlayer formed a ternary phase mixture
(α-Al+CuAl2+Ag2Al) upon eutectic
solidification that was completed in 2 h.
(ii) Compared to pure Cu interlayer, the
mixed Ag-Cu powder interlayer
accelerated the TLP bonding though
during isothermal solidification SiC
segregated.
(iii) Because of the brittle eutectic phase
mixture (CuAl2+Ag2Al) short TLP bonding
times led to low joint strength. With 2 h
long isothermal solidification, the brittle
mixture vanished leading to improved joint
strength though peak strength was not
achieved due to solidification shrinkage.
(iv) Through solid state diffusion, longer (6
h) hold eliminated shrinkage porosity and
led to highest strength (87 MPa) with 83%
joint efficiency. The failure occurred via
decohesion at SiC cluster-matrix interface.
(v) Due to significant grain coarsening,
prolong hold (up to 9 h) reduced the joint
strength.
 Fig. 13: SEM micrographs of the fractured surface of as-received composite:
(a) Secondary electron image; (b) Back-scattered electron image.

Fig. 14: SEM back-scattered electron images of the fractured surfaces of bonded
composites: (a) 20 min; (b) 1 h; (c) 2 h; (d) 3 h; (e) 6 h; and (f) 9 h.

Fig. 15: Matrix grain size for holding times of (a) 6 h and (b) 9 h.

10
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