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Journal of Alloys and Compounds 715 (2017) 91e104

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Journal of Alloys and Compounds


journal homepage: http://www.elsevier.com/locate/jalcom

Review

Aluminium based in-situ composite fabrication through friction stir


processing: A review
Namrata Gangil a, *, Arshad Noor Siddiquee b, Sachin Maheshwari a
a
Department of Manufacturing Processes and Automation Engineering, Netaji Subhas Institute of Technology, New Delhi, 110078, India
b
Department of Mechanical Engineering, Jamia Millia Islamia, New Delhi, 110025, India

a r t i c l e i n f o a b s t r a c t

Article history: Aluminium metal matrix composites (AMMCs) are the fastest developing materials for structural ap-
Received 19 March 2017 plications due to their high specific weight, modulus, resistance to corrosion and wear, and high tem-
Received in revised form perature strength. In-situ processing is preferred over ex-situ processing approach for producing fine and
19 April 2017
thermodynamically more stable reinforcements, but issues related to defects such as porosity, particle
Accepted 27 April 2017
Available online 29 April 2017
clustering etc. are always there in fabrication of AMMCs through conventional methods. Friction Stir
Processing (FSP) has evolved as a promising surface composite fabrication technique mainly because it is
an eco-friendly and solid-state process. Synthesizing reinforcing particles in aluminium matrix through
Keywords:
Metal matrix composites
FSP is more attractive than conventional AMMCs fabrication because intense plastic deformation during
Intermetallic compounds FSP not only synthesises the reinforcement phase in the matrix in-situ it also shears and diffuses the
Solid state reactions particles and progress the reaction between aluminium and added particles rapidly. This article ad-
Friction stir processing dresses the current status of in-situ AMMCs fabrication through FSP technique. The objective of this
Aluminium alloys article is to review and summarize various systems of in-situ AMMCs fabrication such as Al- Transition
metals (TM), Al- Metal oxides (MO), and Al-Salt reaction systems, at various operating conditions and FSP
parameters and their effects on resultant microstructure and final properties. This review article will be
useful to academicians, researchers and practitioners as it comprises significant knowledge pertaining to
AMMCs using FSP.
© 2017 Elsevier B.V. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
2. Al-transition metal (TM) system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
2.1. Al-Ti AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
2.2. Al-Ni AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
2.3. Al-Cu AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
2.4. Al-Fe AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
2.5. Al-Mo AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
3. Al-metal oxide (MO) system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
3.1. Al-TiO2 AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
3.2. Al-NiO AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
3.3. Al-SiO2 AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
3.4. Al-CuO AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
3.5. Al-CeO2 AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
3.6. Al-Cr2O3 AMMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
4. Al-salt reaction system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
4.1. Al-TiC AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
4.2. Al-TiB2 AMMCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

* Corresponding author.
E-mail address: namrata.gangil@gmail.com (N. Gangil).

http://dx.doi.org/10.1016/j.jallcom.2017.04.309
0925-8388/© 2017 Elsevier B.V. All rights reserved.
92 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

5. Concluding remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101


References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

1. Introduction improvement of arc welded joints [56e58], fabrication of metal


foam [59,60], fabrication of ex-situ [3,4,31,61e68] and in-situ
Aluminium and its alloys are most widely used in many in- composites [70e73,75e80,83e96,102e104].
dustries like aerospace, transportation and several structural ap- The aluminium alloys are fast subsuming other materials such as
plications because of their high specific strength, good formability steels mainly due to their superior mechanical properties such as
and good corrosion resistance [1,2]. The strive to further enhance high strength to weight ratio and corrosion resistance etc. The
mechanical properties of aluminium alloys initiated constant ef- recent developments in the FSP allow considerable scope in further
forts by various means and popularized metal matrix composite enhancing the properties. But, the situation is complex as it in-
technology in past three decades [3,4]. Al-based Metal Matrix volves a large number of process parameters and their effects on
Composites (AMMC) develop high strength, high young's modulus, various important properties that are often contradictory in nature.
improved resistance to corrosion, fatigue, creep and wear; which Moreover, the response of variety of processing systems and their
make them favourable structural materials for many industrial conditions to these process parameters themselves is embarrass-
sectors [5,6]. AMMCs fabricated through traditional ex-situ ingly varied. Furthermore, the properties of aluminium matrix
approach in which externally prepared reinforcements added into composites depend on type, size, volume fraction, bonding and
the matrix material often accompany porosity, larger grain size, distribution of evolved compounds in the matrix. There is, thus, a
clustering of particles, poor bonding, improper wetting and unde- need to unveil the state of the art so that the status is reported to
sirable interfacial reaction product [7e9]. In-situ approach of the researchers in a holistic manner. This paper is written with this
AMMC fabrication involves synthesizing desirable reinforcements objective and focuses on the current status of FSP process in
during processing itself. This approach has distinct advantages over aluminium based in-situ composite fabrication. In this paper the
the traditional ex-situ approach due to its capability to produce state of the art of in-situ composite fabrication through FSP is
finer grain size with excellent thermodynamic stability economi- presented in broadly three systems namely- Al-Transition Metal
cally [10e27]. This approach is also adopted in various conventional (Al-TM) system, Al-Metal Oxide (Al-MO) system, and Al-salt reac-
processes including powder metallurgy (PM) [10], liquid metal- tion systems.
lurgy (LM) [11e24], and mechanical alloying (MA) [25e29] for
fabrication of AMMCs. PM route is often associated with porosity 2. Al-transition metal (TM) system
which affects tensile properties significantly [10]. In LM practices
unavoidable casting defects and particle clustering [15] are the In this approach various transition metal powders are intro-
major drawbacks which results in poor mechanical properties. A duced in the Aluminum alloys substrate through FSP. In-situ
significant loss of ductility of AMMCs is often associated with MA AMMCs are largely fabricated by adding variety of metal powders
method [28,29]. Inhomogeneous microstructure and introduction such as Ti, Ni, Fe, Cu, Mo and various aluminide particles Al3Ti
of contaminants are most often the possible reasons of this loss of [70e73], Al3Ni [75e77], Al2Cu [72,73,78], Al3Fe [79], Al12Mo [80]
ductility [28]. This method also increases the production cost and etc. are produced during friction stir processing itself. The reac-
its duration. Moreover, the ex-situ has a major limitation in which tion between Al and TMs is exothermic in nature which releases
the there exists considerable lack of homogeneity in reinforcement heat and further increases reaction. The friction stir processing of
particle's spreading, mixing and dispersion by the FSP. The prob- tool promotes mixing and breaking of particles and produces
lems associated with above mentioned methods for MMC fabrica- enough heat for reaction to facilitate formation of intermetallic
tion has been successfully overcome by friction stir processing compounds and fabricate fully dense composites. The fabrication of
(FSP) during the last decade. FSP was first developed by Mishra in-situ composites through Al-TM system is summarized in Table 1.
et al. to impart high strain rate superplasticity to 7075 aluminium
alloy [30]. They were successful in fabrication of ex-situ surface
2.1. Al-Ti AMMCs
composite and their work led to numerous researches on com-
posite fabrication using friction stir processing (FSP) [31].
Al3Ti is a very popular reinforcing phase in aluminium due to its
FSP is based on the principles of FSW developed at “The Welding
low density (3.3 g/cm3), high melting point (1350  C), high elastic
Institute (TWI), UK” in 1991 [32]. In FSW/FSP a rotating cylindrical
modulus (217 GPa) and excellent mechanical properties at both
tool with a shoulder and probe (pin) is first plunged in to a metallic
ambient and elevated temperature [10]. The heat of formation for
plate and then traversed along the surface of workpiece. The rub-
Al3Ti is 35.6 kJ/g atom at 298 K and during the formation of Al3Ti
bing action of tool shoulder with the plate's surface generates
the temperature rises adiabatically to nearly 1400 K (with the heat
frictional heat and softens material under the shoulder which also
capacity as ~25 J/K mol) [69]. The temperature rise further accel-
undergoes severe plastic deformation at high strain rate by the
erates the reaction between Al and Ti particles and causes local
rotating pin (called stirring). During FSW/FSP, material is subjected
melting of Al at Al-Ti interface which, in turn, further enhances the
to a combination of metal working processes e.g. friction, extrusion
reaction. The large plastic strain induced by stirring shears the
and forging [32e37]. Compared with other metalworking tech-
particles and creates direct contact between Al and Ti by removing
niques FSP has many advantages such as it is a green, energy effi-
Al3Ti particles rapidly resulting in ultrafine-grained Al3Ti
cient, short-route and a solid-state processing technique [38,39].
(<100 nm). The compressive yield strength higher than tensile
Main applications of FSP for microstructural modification in
strength has been reported which is mainly attributed to different
metallic materials include superplasticity [30,40e45], homogeni-
coefficient of thermal expansion (CTE) of Al and Al3Ti. The fine grain
zation of aluminium alloys [46e48] and AMMCs [49e51], micro-
matrix in Al-Al3Ti composites and Orowan strengthening is re-
structural refinement of cast aluminium alloys [52e55], fatigue life
ported to be the main factors causing increase in yield strength [70].
N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104 93

Table 1
Al-Transition Metal composites fabricated through FSP.

Starting Materials/Workpiece Tool Material and Geometry Processing Parameters Prominent Results Reference
preparation

Al (325 mesh), Ti (325 mesh)/PM Threaded pin profile, PD- 6 mm R-700, 1400 rpm (CCW), T- (1) The size of Al3Ti increases with [70]
route 45 mm/min, TT-3 , FSP Passes- increasing R and Passes. Higher R
2, 4, Ti content- 5, 10, 15 at. % resulted in lower yield strength.
(2) At higher R, Ti content, and passes
Al3Ti particle volume fraction and
hardness increased to 0.49 and
192 ± 12 HV, respectively.
(3) Significant increase in Young's
modulus (114 GPa) and strength
with higher fraction of Al3Ti.
Al (13 mm), Ti (45 mm)/PM route H-13, Concave shoulder, R-1000-2000 rpm, T-25 mm/ (1) For VHP at 640  C and 180 min, all [71]
threaded conical pin, SD - min, FSP Passes-4, VHP at 500, Ti reacted with Al to form Al3Ti 0.5
20 mm, PD- root- 8 mm, tip- 600, 640  C for 5, 120, 180 min, e3 mm in size.
5.5 mm, PL- 5.8 mm. respectively. (2) Complete AleTi reaction during
VHP and then processing at R-
1000 rpm exhibited an optimum
combination of strength and
ductility.
Al (13 mm), Ti (45 mm), Cu (75 mm)/ Steel tool, Concave shoulder R-1000 rpm, T-25 mm/min for (1) Al3Ti/Ale5.5Cu composites [72]
PM route SD - 20 mm, Threaded conical FSP-air, 200 mm/min for FSP- fabricated.
pin, root dia- 8 mm, tip-5.5 mm, water, FSP Passes-4 in air, 2 in (2) The ultrafine matrix grains with a
PL- 4 mm water, Some FSP- water high density of dislocations were
samples aged at 175  C for 4 h. obtained with resulted in
significant increase in strengths and
reduction in ductility.
Al (13 mm), Ti (45 mm), Cu (18 mm), H-13, Concave shoulder, R-2000 rpm, T-25 mm/min, FSP (1) In the Al-Ti-Cu sample Cu enhanced [73]
Mg (32 mm)/PM route threaded conical pin, SD - Passes- 4 the Al3Ti reaction.
20 mm, PD- root- 8 mm, tip- (2) For the Al-Ti-Mg sample, along with
5.5 mm, PL- 5.8 mm Al3Ti, some Ti2Mg3Al18 particles
were also formed.
Al1060 Plate (5 mm thick), Ni Columnar shoulder, Threaded R-1500 rpm, T-23.5 mm/min, (1) Al3Ni and Al3Ni2 exist in the [75]
(2.3 mm)/2 rank holes on 2 pin profile, SD - 28 mm, PD- TT-3 , PD-0.4e0.5 mm, Passes- processing zone.
plates-2.5 mm dia, 3 mm depth 10 mm, PL- 8.5 mm, Pitch- 3, HT-550  C for 6 h after FSP (2) The microhardness of the Al3Ni2
with 3 mm interval 1 mm and Al3Ni were measured as 1283
and 841 HV, respectively.
(3) The 0.2% YS and UTS of composite
was 110 and 144 MPa.
Al1100-H14 plate (8 mm thick), Ni W18Cr4V HSS, columnar R-1180 rpm, T-60 mm/min, PD- (1) Al3Ni exits in processing zone. [76]
(25e38 mm)/Groove- W- 3 mm, shoulder, SD - 25 mm, threaded 0.3 mm, FSP Passes-6 (2) UTS and microhardness increased
D- 5 mm tapered pin, PD-root-9.6 mm with increasing number of FSP
tip- 5 mm, PL- 6 mm passes and found 209 MPa, and 92
Hv, respectively, when processed
with 6 passes.
Al1100 plate (8 mm thick), Ni H-13, columnar shoulder, SD - R-1600, 2000 rpm, T-12, (1) Al3Ni exits in processing zone. [77]
(<10 mm) 20 mm, tapered pin, PD-root-6 25 mm/min, FSP Passes- 2, 4, 6, (2) Composite exhibited 60%
mm tip- 5 mm, PL- 4 mm Variable AS & RS technique improvement in microhardness
(47 Hv) at higher R/T ratio and
passes.
Al and Cu powder/PM route Threaded pin profile, PD- 6 mm, R-700 rpm (CCW), T-45 mm/ (1) The fabricated AleAl2Cu composite [78]
pitch-1.2 mm min, TT-3 , FSP Passes- 2 was fully dense, pore free, fine
grained and the Al2Cu particles
distributed homogeneously.
(2) The composite showed enhanced
modulus (88 ± 8 GPa), good
compressive strength (450 MPa
yield strength and 650 MPa
ultimate strength) with reasonable
good compressive ductility.
Al (325 mesh) & 10% Fe (325 mesh) Threaded pin profile, M1.2  6 R- 1400 rpm (CCW), T-45 mm/ (1) Fine Al13Fe4 produced (100 nm) as a [79]
pin min, TT-3 , FSP Passes- 2, 4 second phase particles. Distribution
improved with passes.
(2) Composite exhibited enhanced
modulus 91 MPa and Tensile
Strength 217 MPa.
Al (~325mesh), Mo (4 mm)/PM route M1.2  6 pin, SD-18mm R-1400 rpm, T-30-45 mm/min, (1) Reinforcing phases are Al12Mo [80]
TT-0.052 rad, FSP passes-4, (large amount) and Al5Mo (very
Various Mo content, Post-FSP small amout).
HT-1 and 10 h at 873 K (2) Maximum hardness achieved when
sample processed with 1400-
30 þ 873-10 h.

Note: mm-micro meter, nm-nano meter, SD-shoulder diameter, PD-pin diameter, PL-pin length, R-rotational speed, T-traversing speed, TT-tool tilt angle, PD-plunge depth, HT-
heat treatment, CCW-counter clock-wise, W- Width, D- Depth.
94 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

The Al-Ti systems have also been processed by combination of 2.2. Al-Ni AMMCs
vacuum hot pressing (VHP) and FSP [71]. During VHP-FSP hybrid
processing VHP was performed at 650  C and it was inferred that The binary phase diagram of Al-Ni system as shown in Fig. 2
formation of Al3Ti was facilitated by reactive diffusion which, in reveals that the temperature and Al/Ni atom ratio required for
turn, resulted in improvement of mechanical properties as YS (yield formation Al3Ni is lower than that for Al3Ni2 [74]. When FSP is
strength), UTS (ultimate tensile strength) and elongation (364 MPa, performed on Al-alloys using Ni powder the Al3Ni2 along with
413 MPa and 14%, respectively) [71]. Further, addition of Cu powder Al3Ni intermetallics reinforcements are formed in-situ. In such
accelerates formation of Al3Ti particles but also results in coars- FSPed samples Al3Ni2 has been detected along with Al3Ni with
ening of matrix and formation of coarse Al3Ti clusters with Al2Cu complete Al-Ni reaction (as shown in Fig. 3). In this figure gray
particles. Coarse grains and clusters can be subdivided by multi- phase is identified as Al3Ni, light gray phase as Al3Ni2, and dark gray
pass FSP resulting in refinement and redistribution of Al3Ti clus- phase as Al matrix [75]. The sequence of chemical reactions is as
ters coupled with dissolution and reprecipitation of Al2Cu particles. follows:
This also enhances strength significantly but causes ductility to
reduce. If the multi-pass FSP is performed with water-cooling the 3Al þ Ni/NiAl3 þ 258Kcal=mol (3)
dissolution of Al2Cu, ultra fine-grained matrix with high density of
dislocation can be obtained. VHP-FSP hybrid processed Al matrix- NiAl3 þ Ni/Ni2 Al3 þ 90Kcal=mol (4)
Ti þ Cu composites also exhibit precipitation of metastable phases
A similar kind of structure was also found by Farber et al. [7]. The
due to aging which leads to strengthening (YS-417 MPa and UTS-
thermodynamics and diffusion kinetics involved with the forma-
582 MPa) and slight increase in ductility (9%) due to reduction of
tion of these in-situ reinforcement particles has been explained by
dislocation density [72]. In case Mg is mixed with Ti instead of Cu
researchers in the light of effective Gibbs free energy change model
then intermetallic compound of Ti2Mg3Al18 (23.8 vol %) are formed
[76]. It is reported that heat input produced at R/T ratio (ratio of
with fine twin lamellas of Al3Ti (17.2 vol %) as shown in Fig. 1. This
rotational to traversing speed) of lower than 80 is insufficient to
may, in turn, increase total volume fraction of reinforcement and
support Al-Ni reaction. Literature also report that the amount and
consequently UTS is greatly improved (702 MPa) but at the same
distribution of Al3Ni particles and microhardness of composite
time elongation dropped significantly. The chemical reactions for
improves with increasing number of passes at higher R/T ratio [77].
Al-Ti and Al-Ti-Mg system may take place as follows [73]:

2.3. Al-Cu AMMC


3Al þ Ti/Al3 Ti (1)
Cu dissolves in Al in liquid state and forms AA2xxx series of
Alloys. In solid state FSP the reaction between Al and Cu produces
Al2Cu compound. During sintering in air, Cu reacts with oxygen and
18Al þ 2Ti þ 3Mg/Ti2 Mg3 Al18 (2)
forms Cu oxides CuO and Cu2O as shown in Fig. 4. During FSP, Al
reacts with Cu oxides and form Al2Cu and Al2O3. Al2Cu compound

Fig. 1. TEM images of FSP samples: (a) Al3Ti, (b) Al-Ti-Cu, (c) Al-Ti-Mg and (d) Ti2Mg3Al18 in Al-Ti-Mg sample [73].
N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104 95

Fig. 2. Al-Ni phase diagram [74].

Fig. 3. The SEM micrograph of heat treated specimen [75].

with <1e2 mm size some of which finer than 100 nm has been Fig. 4. XRD patterns for as-sintered and FSPed specimens.
reported in literature. Al2Cu particles volume fraction and com-
posite density were found 0.42 ± 0.03 and 3.4 g/cm3, respectively
[78]. 2.5. Al-Mo AMMC

Mo powder has been tried for making in-situ Al-based com-


2.4. Al-Fe AMMC posites and it is reported that the reinforcement phases are formed
as a result of Al-Mo reaction and this reaction significantly depends
Al-Fe reactions form fine elliptical shaped Al13Fe4 (also deno- on the at% of Mo in the fabricated composites [80]. At higher Mo
ted as Al3Fe) phase (100e200 nm long and 50e100 nm wide) content coarse intermetallic particles are produced and the coars-
along with small amount of Al5Fe2 (Fig. 5). Vast difference in ening is mainly attributed to coalescence of neighbouring particles.
Young's modulii of Al Matrix (70 GPa) and constituent interme- This is reported to be manifested in scattering of peak hardness
tallic compound (i.e. Al3Fe) particles (130 GPa) increases the values. Researchers have varied FSP process parameter and per-
modulus of the resultant composite. With increasing number of formed post FSP sintering and investigated effects of these pro-
FSP passes the hardness of SZ is reported to be greatly enhanced cessing conditions on responses such as microstructure,
from 40 HV of as received specimen to 104 HV of 4-pass com- microhardness and other characteristics. Table 2 shows the volume
posites [79]. fraction and hardness of Al-5Mo composite at various processing
96 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

Hot pressing (HP), FSP process parameters and effect of water


cooling during FSP significantly affect composite properties [84].
The chemical reactions between Al and TiO2 [25] may consist of
following two parts:

3TiO2 þ 4Al/2Al2 O3 þ 3½Ti (7)

½Ti þ 3Al/Al3 Ti (8)


The reaction products of Al-Mg alloy and TiO2 are Al3Ti and
MgO. During multi-pass FSP higher number of FSP passes and TiO2
content facilitates more refinement which results in nano-sized
phases in the matrix. It is reported that onion ring pattern and
increased high angle grain boundaries (HAGBs) are observed with
higher TiO2 contents. Moreover, agglomeration in advancing side
Fig. 5. TEM image showing uniform distribution of fine Al13Fe4 particles in matrix [79]. (AS) of specimen at higher TiO2 content results in non-uniformity
in hardness profile in AS. It was reported that the TiO2 vol. % of
up to 3.1 gives improvement in mechanical strength of composite
conditions. The chemical reactions in Al-Mo system may take place
[85]. Investigation of the role of deformation temperature reveals
as follows:
that the composite possesses higher temperature strength, defor-
12Al þ Mo/Al12 Mo þ DH1 (5) mation resistance, flow stress and stress exponent. Dynamic
recrystallization (DRX) during hot deformation is the main resto-
ration mechanism which results in flow softening at elevated
5 7
Al Mo þ Mo/Al5 Mo þ DH2 (6) temperatures [86]. Wrought Al-Mg alloys exhibit strain rate
12 12 12
strengthening during stirring and the strengthening effect found to
where DH1 (298 K) ¼ 200 kJ/mol and DH2 (298 K) ¼ 107 kJ/mol. be diminished for annealed condition (as shown in Fig. 6) [87]. Al-
Mg Alloy-TiO2 composite shows 28% and 32% improvement in fa-
tigue strength at 2 and 3.5 vol % of TiO2 respectively (as shown in
3. Al-metal oxide (MO) system
Fig. 7) as compared to annealed sample [88].

Aluminium on combining with less reactive metal oxides pro-


3.2. Al-NiO AMMC
duces thermit reaction and forms Al2O3. The kind of Al2O3 phases
(amorphous, g, d, q, a) formed by this reaction depends on
Use of NiO in the Al matrix produces in-situ Al2O3 and Al3Ni as
displacement reactions. The g-Al2O3 metastable phase exists at
reinforcements. In the first reaction of Al-NiO system, NiO is
temperature below ~723 K, while at ~1473 K the stable phase a-
reduced by Al to form Al2O3 as follows:
Al2O3 is formed [81,82]. AMCs reinforced with Al2O3 particles have
been produced through in-situ route by utilizing oxide aluminium 2Al þ 3NiO/Al2 O3 þ 3Ni (9)
displacement reactions. The Al-Al2O3 in-situ composites have been
produced in many Al-oxide systems [83,84,89e91,93] through FSP. The displaced Ni then reacts with Al to form Al3Ni according to
Al-MO systems release much higher heat than Al-TM system, and Eqn (3). AA6061-T6 alloy and NiO reaction produces Al3Ni (100 nm)
hence higher reaction rate is obtained. Aluminium based in-situ and Al2O3 (80 nm) phases of hexagonal and facet morphologies,
MMCs are synthesized largely through FSP by utilizing the hot respectively, which significantly enhanced the wear resistance of
working nature of FSP and displacement reactions between nanocomposite as shown in Fig. 8 [89].
aluminium and suitable metal oxides such as TiO2 [83e88], NiO
[89], SiO2 [90], CuO [91,92], CeO2 [93], and Cr2O3 [94]. A summary of 3.3. Al-SiO2 AMMC
this system is given in Table 3.
Al present in the matrix can also reduce SiO2 during FSP. The
3.1. Al-TiO2 AMMCs chemical reaction of Al-SiO2 system is as follows:

3 3
Al-TiO2 reaction produces Al3Ti and Al2O3 phases. TiO2 powder 2Al þ SiO2 / Si þ Al2 O3 þ DH (10)
smaller in size forms higher Al3Ti and a-Al2O3 through what is 2 2
reported as deformation assisted solution precipitation and defor- The reaction products of Al and SiO2 are a-Al2O3 of ultra fine-
mation assisted interfacial reaction mechanisms, respectively. The grained structure with average size of 1.5 mm. If FSP parameters
significant enhancement in yield strength of composite is reported are adequately optimized then composite with better properties
to be mainly attributed to Orowan strengthening mechanism [83]. can be fabricated. Tool RPM, traverse speed and other parameters,

Table 2
Amount of Al-Mo intermetallic compounds (in volume fraction) formed determined by quantitative XRD analysis [80].

VAl12Mo VAl5Mo VMo 4 Hardness (MPa)

As-sintered (823 K-20 min) e e 0.035 0 353 ± 10


FSP-1400-45 0.112 e 0.034 0.27 597 ± 39
FSP-1400-30 0.254 e 0.027 0.39 715 ± 29
FSP-1400-30 þ 873 K-1 h 0.579 0.01 0.005 0.90 960 ± 39
FSP-1400-30 þ 873-10 h 0.642 e e e 1833 ± 196

Note: 4 is fraction of Mo reacted.


N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104 97

Table 3
Al-Metal Oxide (MO) composite fabrication through FSP.

Starting Material and Tool Material and Geometry Processing Parameters Prominent Results Reference
workpiece Preparation

Al (13 mm), TiO2 (450, Cermet tool, Concave shoulder, SD - R-1000 rpm, T-25 mm/min, FSP (1) Al3Ti, and a-Al2O3 exist in the processing [83]
150 nm)/PM route 20 mm, threaded cylindrical pin, PD- Passes- 4 zone.
6 mm, PL- 5 mm (2) Smaller TiO2 (150 nm) form more Al3Ti and
Al2O3.
(3) The microhardness, Young's modulus, YS,
UTS, and % elongation for 150 nm TiO2
processed FSPed samples was 107 Hv,
95 GPa, 314 MPa, 415 MPa, 15.5%,
respectively.
Al (13 mm), TiO2 Cermet tool, Concave shoulder, SD - HP parameters-Temp.-500, 550, (1) Al3Ti and Al2O3 volume fraction increased [84]
(150 nm)/PM route 20 mm, threaded cylindrical pin, PD- 630  C, holding time-5, 50, with decreased T with no effect on matrix
6 mm, PL- 5 mm 240 min. FSP parameters- R- grain size.
1000, 2000 rpm, T-25, 50, (2) Lower T with high R had little influence on
100 mm/min, FSP passes-4, in microstructure and properties.
last sample 4 passes carried out (3) FSP in water refines matrix grains and
at 25 mm/min, 2 passes at increases TS significantly.
50 mm/min in flowing water
Al-Mg alloy plate, TiO2 H-13 steel tool, SD-18, PD-5, PL- 4 mm, R-1200 rpm, T-100 mm/min, (1) Al3Ti and MgO (50 nm) particles were [85]
(30 nm)/Groove: D- threaded pin with 0.5 mm depth and FSP Passes- 4, 8, 12, TiO2 Vol. identified in the matrix which results in
3.5 mm, W- 0.8, 30 angle fraction-2.3, 3.1, 5, 6.1% significant enhancement of Tensile
1.2 mm Strength.
(2) Hardness profile through the thickness of
samples containing 2.3 and 3.1 vol % TiO2
was uniform and smooth.
AA5052-H32 (Al-Mg) H-13 steel tool, SD-18 mm, PD-5mm, R-1200 rpm, T-100 mm/min, (1) Al3Ti and MgO (50 nm) particles were [86]
plate, Solution PL- 4 mm, threaded pin with 0.5 mm FSP Passes- 4, TT-2.5 , identified.
Treated plate, TiO2 depth and 30 angle Deformation temp. in Tensile (2) Composite exhibited 2 mm grain size and
(~30 nm)/Groove: Testing-300,350,400,450 ~90% HAGB's.
W-1.2 mm, D- (3) Deformation activation energy of
3.5 mm composite was found 456 kJ/mol at higher
test temperatures.
AA5052-H32 plate, TiO2 H-13 steel, SD-18 mm, PD-5mm, PL- R-1200 rpm, T-100 mm/min, (1) Al3Ti, MgO particles exists in processing [87]
(~30 nm) some 4 mm, threaded pin with 0.5 mm depth FSP Passes- 4 zone.
samples annealed at and 30 angle (2) Pretreatment reduced the strain rate
500  C for 2 h/ sensitivity and strain hardening.
Groove- W-1.2 mm, (3) Microhardness of annealed and wrought
D- 3.5 mm FSPed samples were 87.9 ± 2 and
82.4 ± 1.6 Hv respectively.
AA5052-H32 plate, TiO2 H-13 steel, SD-18 mm, PD-5mm, PL- R-1200 rpm, T-100 mm/min, (1) Nano-sized Al3Ti, MgO phases exist in [88]
(~30 nm), some 4 mm, threaded pin with 0.5 mm depth FSP Passes- 4, 6 ~2 mm fine-grained matrix.
samples annealed at and 30 angle (2) Higher YS (158 MPa), UTS (252 MPa), and
500  C for 2 h/ elastic modulus (85 GPa) observed at
Groove- W- 0.8, higher TiO2 Content (3.5 vol %) and 6 FSP
1.2 mm, D-4 mm passes.
(3) Endurance limit of 154 and 148 MPa
observed at 2 and 3.5% of TiO2 volume
fraction with 6 FSP passes.
Al6061-T6 plate, NiO H-13 steel, threaded tapered tapered R-630 rpm, T-100 mm/min, TT- (1) Nano Al3Ni, and Al2O3 particles identified in [89]
(<1 mm)/Groove- W- pin, SD - 18 mm, PL- 4, PD- root-6mm, 3 matrix.
2 mm, D- 2 mm tip-4 mm (2) Microhardness and strength decreased due
to dissolution of precipitates but wear
resistance improved.
Al (325 mesh), SiO2 SD - 18 mm, PD- 6 mm, Pitch- 1.2 mm, R- 500e2000 rpm, T- 15 (1) Reinforcement phase was identified as a- [90]
(325 mesh)/PM route PL- 6 mm e90 mm/min, TT-3 , FSP Al2O3 (20 nm). The matrix has an ultra
Passes-Varied fine-grained structure (1.5 mm).
(2) Reaction increased with increasing R,
Passes and decreasing T.
(3) At 500 rpm, 15 mm/min and 4 passes, the
composite possessed enhanced modulus
(80 GPa), TS (319 MPa), and ductility ~13%.
Al (325 mesh), CuO SD - 18 mm, PD- 6 mm, Pitch- 1.2 mm R-500 rpm, T- 15 mm/min, FSP (1) Reinforcement phases identified as Al2Cu [91]
(200 mesh)/PM route Passes-4 (100 nm) and g-Al2O3 (in the form of
cluster) in nanometer sizes in matrix with
avg. grain size of 1 mm.
(2) Composite exhibited superior modulus
(86 GPa), YS (284 MPa) with good ductility
(value is not given).
Al (40 mm), Mg SD - 18 mm, PD- 6 mm, Pitch- 1.2 mm R-500 rpm, T- 15 mm/min, FSP (1) Nanometer-sized particles Al2Cu [92]
(100 mm), CuO Passes-4 (~200 nm), and MgO (10 nm in the form
(10 mm)/PM route of cluster) identified. Al grain size was
found ~600 nm.
(continued on next page)
98 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

Table 3 (continued )

Starting Material and Tool Material and Geometry Processing Parameters Prominent Results Reference
workpiece Preparation

(2) E88 GPa, YS (tension-350 MPa,


compression-436 MPa)
Al (40 mm), CeO2 M6 tool pin R-500 rpm, T-30-120 mm/min, (1) Reinforcing phases identified as Al11Ce3 (1.4 [93]
(7 mm)/MA route, TT-3 , FSP Passes-4 e3.5 mm) and d*-Al2O3 (10 nm).
sintering (2) At 30 mm/min traverse rate and 833 K
temperature 813 and sintering temperature the composite
833 K produced possesses enhanced
microhardness (165 ± 4 Hv), modulus
(109 GPa) and UTS (488 MPa) as well as a
ductility of ~3%.
AA6061- T6 plate, Cr2O3 H-13 steel, Threaded tapered pin, SD - R-630 rpm, T-100 mm/min, TT- (1) Al13Cr2, and Al11Cr2 identified in matrix. [94]
Powder/Preplaced 18 mm, PL- 4, PD- root-6mm, tip-4 mm 3 , FSP Passes-6 (2) Improvement in wear resistance and
composite layer by homogeneous distribution of reinforcing
APS technique phases achieved.

when set for higher R/T ratio, may result in reduced matrix flow and compressive strengths due to larger grain size and lower
stress and provide better reinforcement particle flow in the matrix; amount of reinforcements which was attributed to shorter reaction
this in turn, may lead to better particle distribution [90]. time and lower reaction temperature. By applying sintering at
833 K and subsequently FSP the resultant composite reported to
3.4. Al-CuO AMMCs possess enhanced modulus and strength mainly due to Orowan
strengthening [93].
This system produces Al2Cu particles and clusters of g-Al2O3
nanometer-sized particles (Fig. 9a). These composites reported to 3.6. Al-Cr2O3 AMMC
possess superior strength and ductility both mainly due to Orowan
strengthening and dislocation pinning (Fig. 9b) between intra- When Cr2O3 is used in Al matrix to fabricate surface composites
granular particles. But, reaction product g-Al2O3 acts as a barrier very hard multiple intermetallic compounds (IMCs) such as Al13Cr2
and retards Al and CuO reaction further, resulting incomplete re-
action [91]. To enhance Al-CuO reaction magnesium is added to
utilize Mg-MO displacement reaction. The Al2Cu to Al wt.% ratio
reported to be increased to 0.54 as compared to 0.36 for Al-CuO
system on adding magnesium [92].

3.5. Al-CeO2 AMMC

When CeO2 is used in FSP the Al-CeO2 system reactions pro-


duces two different in-situ strengthening phases:

3 3
2Al þ CeO2 /Al2 O3 þ Ce þ DH1 (11)
2 2

11Al þ 3Ce/Al11 Ce3 þ DH2 (12)

where DH1 ¼ 44 kJ/mol and DH2 ¼ 574 kJ/mol. Ultrafine grained
AMMC (average grain size 350e550 nm) can be developed. In a
typical investigation higher traverse speed resulted in lower tensile Fig. 7. S-N Curve showing fatigue response of the materials at R ¼ 0.1 [88].

Fig. 6. Effect of strain rate on the engineering stress-strain curves of (a) annealed and (b) wrought nanocomposites at strain rates of 0.001, 0.01, and 0.1 s1 [87].
N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104 99

Fig. 8. Friction coefficient vs. sliding distance for (a) Al6061 alloy, (b) 5-pass FSPed Al6061 alloy, and (c) 5-pass FSPed Al6061/Al2O3-Al3Ni composite at 350  C [89].

Fig. 9. TEM/BFI showing the (a) nanometer-sized particles in matrix (b) Dislocations that were pinned by particles [91].

and Al11Cr2 are formed during FSP. These IMCs are hard and greatly and salt combination commonly used are shown in Table 4 and
improve the wear resistance of composites. For this investigation these salts disintegrate to yield in-situ strengthening phases such
the performance chart for wear rate (mg/m) of samples vs sliding as TiC [95,96] and TiB2 [102e104]. These salt based composites have
distance (m) is depicted in Fig. 10. In this study the authors been fabricated by utilizing Al-Salt reaction system and the same is
compared the friction coefficients of BM, simple FSPed samples and summarized in Table 4. FSP, in fact, was basically applied on these
Cr2O3 in-situ surface composites and reported the coefficient values fabricated composites as a secondary processing method to elimi-
as 0.28, 0.45, and 0.17, respectively [94]. nate casting defects and to achieve complete homogenized fine-
grained microstructure.
4. Al-salt reaction system
4.1. Al-TiC AMMCs
Even complex salts can also be used which, during FSP, disin-
tegrate and produce in-situ strengthening phases. Typical Al matrix In-situ Al-TiC composite can be fabricated using reactions
100 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

composites high rotational speed (greater than 800 rpm) is rec-


ommended [95]. The cast structure of the bulk composite so pro-
duced is homogenized through multiple pass FSP, which also
results in grain refinement and high dislocation density etc. Dy-
namic recovery due to high stacking-fault energy (SFE) of
aluminium results in arrangement of dislocations into LAGBs (low-
angle sub-grain boundary) configuration (Fig. 11) [96].

4.2. Al-TiB2 AMMCs

TiB2 (Titanium diboride) reinforcing phase also emerged as a


beneficial product as it has high hardness (3400 Hv), melting point
(3225  C), elastic modulus (534 GPa) with good thermal stability
and excellent wear resistance [18,97]. Various processing methods
derived from conventional liquid and powder metallurgy route
have been developed to fabricate Al-TiB2 composites as reviewed
Fig. 10. Wear rates of samples [94].
by Tjong and Ma [98]. The stir casting is widely used method to
synthesize TiB2 in-situ in which K2TiF6 salt rich in Ti and KBF4 salt
between K2TiF6 salt (rich in Ti) and graphite powder (rich in C) in rich in B are added in to aluminium melt [19e22]. The sequence of
aluminium melt [95,96]. For defect free fabrication of these synthesis of TiB2 can be summarized as follows [23,24]:

Table 4
Al-Salt reaction system for in situ composite fabrication and its homogenization through FSP.

Starting Material/Billet Tool Material and Geometry Processing Parameters Prominent Results Reference
Preparation Method

K2TiF6 salt, 1.3 times Gr M2 tool steel, SD-12mm, PD- R-640,800,1000 rpm, T- 60, (1) Al-TiC composite fabricated. [95]
(50 mm), Pure Al/LM 4 mm, PL-3.5 mm 120, 150 mm/min, AF-5 KN, (2) The optimum parameter combination
route Target depth-4.2 mm found to be R-1000 rpm, and T-60 mm/m.
(3) At optimum condition grain size was 9 mm
hardness-48Hv, 0.2% proof stress-103 MPa,
UTS-163 MPa, elongation- 16%.
K2TiF6 salt, 1.3 times Gr M2 tool steel, SD-12mm, PD- R-1000 rpm, T-60 mm/min, AF- FSP results in complete homogenization, casting [96]
(50 mm), pure Al/LM 4 mm, PL-3.5 mm 5 KN, FSP Passes-2 defects elimination and grain refinement to
route 4 mm, led to significant improvement in the
Hardness (58 Hv), 0.2% proof stress (123 MPa),
UTS (172 MPa) and %E (19%).
Pure Al, salt mixture M2 steel, SD-15 mm, PD- 5 mm, R-1000 rpm, T-30 mm/min, FSP (1) Al-TiB2 composite fabricated in-situ. [102]
(K2TiF6þKBF4)/LM PL-4 mm Passes-2 (2) Casting defects and agglomeration
route prevented after second pass.
(3) Microhardness, UTS and ductility of 2 pass
FSP sample were 52 Hv, 170 MPa and 19%
respectively.
AA7075-T6 rod, K2TiF6, HCHCr, Hexagonal pin, SD- R-1200 rpm, T-50 mm/min, AF- Grain Size-6.3 mm, Microhardness-160 VHN, [103]
KBF4/LM route 18mm, PD-6mm, PL-5.8 mm 10 KN, UTS-340 MPa, Elongation-2.5%, Wear rate-
98 mm3/m.
Al, Mg, Al-Si alloy, H-13, Screwed tapered pin, PL- R-600 rpm, T-200 mm/min, (1) AA6063/TiB2 composite fabricated with [104]
K2TiF6, KBF4/LM 6mm, PD-root-8mm, tip-6mm Four FSP passes with varied 4.2  1014 m2 average dislocation
route AS&RS technique, T6 heat density, 2 mm grain size, and 92 Hv
treatment hardness.
(2) Composite was thermally stable during
heat treatment.

Fig. 11. TEM micrographs showing (a) ultrafine grains, (b) high dislocation density, (c) recovery structure, in 2 pass sample [96].
N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104 101

Fig. 12. SEM image of fractured surface showing (a) TiB2 particle morphology and (b) particle top view [102].

during FSP rounds up the particles with intra-granular distribution


13 4 and results in change of morphology. Fractured surface, thus often
K2 TiF6 þ Al/Al3 Ti þ AlF3 þ 2KF (13)
3 3 reveal spherical morphology (Fig. 13) of TiB2 particles [103]. It was
observed that AA6063/TiB2 composite contains less recrystalliza-
2KBF4 þ 3Al/AlB2 þ 2AlF3 þ 2KF (14) tion component than sheared component due to the presence of
nano-sized TiB2 particles which blocked the grain boundaries
Al3 Ti þ AlB2 /TiB2 þ 4Al (15) movement [104].

Composites produced by metal casting techniques possess


several imperfections such as particle clustering and segregation 5. Concluding remarks
along grain boundaries [23], salt and oxide inclusions [20]. High
interfacial energy between aluminium and TiB2 causes trapping of FSP technique is energy efficient, environment friendly, versatile
TiB2 particles at the grain boundaries [17]. To eliminate these par- and successfully emerged as material processing technique for
ticle clusters several methods including mushy state rolling [99], producing the fine-grained structure, surface and bulk composites
isothermal holding [100], equal channel angular pressing [101], in various aluminium alloys and synthesizing the composite and
etc., as a secondary processing technique have been utilized but intermetallic compounds in situ. AMMC's fabricated through con-
these are found critical for complete homogenization. FSP can be ventional methods could not contribute to the strength by Orowan
used as an effective tool for fine and homogeneous distribution of mechanism because they contains reinforcements inter-granularly
particles in the matrix to a desirable range. FSP of Al-TiB2 cast in the matrix with particle size greater than 1 mm. Synthesizing
composite at its second pass have shown homogeneous particle intermetallic compounds in aluminium matrix in-situ through FSP
dispersion with elimination of all clustered particles and casting is more attractive than conventional AMMCs fabrication. The hot
defects. SEM image (Fig. 12) showing hexagonal pyramidal working nature of FSP effectively promotes exothermic reactions
morphology of TiB2 particle in fractured surface [102]. between aluminium and constituent elements and produces rein-
TiB2 exhibits various morphologies (Spherical, hexagonal, cubic) forcement phases (particles). Intense plastic deformation created
before FSP with inter-granular distribution. Abrading action of tool during FSP does not only distribute the particles in matrix it also
shears and diffuses the particles and proceeds the reaction between
aluminium and added particles rapidly. In addition the reaction
products get detached from un-reacted particles rapidly and from
the interface which results in limited growth of particles and pro-
duces fully dense fine grained and ultra fine-grained structure.
AMMCs in which large amount of nanometer-sized particles
distributed inter-granularly and intra-granularly, the major
strength contributors are Orowan and grain-size strengthening
mechanism. In these cases inter-particle spacing can be decreased
to 100 nm or less and the ultrafine-grained structure can be
restricted to sub micrometer range due to Zener pinning effect. In-
situ reaction produced by FSP completes within a very short
duration. High density of dislocations and exothermic reaction
promotes the diffusion of elements in matrix and it further depends
on the kind of fabrication system and FSP parameter used. In this
article particular emphasis has been given to the various reaction
system and friction stir processing parameters on resultant
microstructure and final mechanical properties of aluminium based
in-situ metal matrix composite. The higher ratio of tool rotation
speed to traverse speed and number of passes generates more heat
and promote the reaction but it should not be excessive as it cause
Fig. 13. Fracture morphology of friction stir processed AA7075/TiB2 AMC [103]. extreme melting in the material and may result in the large cavities
102 N. Gangil et al. / Journal of Alloys and Compounds 715 (2017) 91e104

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