Sie sind auf Seite 1von 9

H O S T E D BY Available online at www.sciencedirect.

com

ScienceDirect
Journal of Magnesium and Alloys 3 (2015) 1e9
www.elsevier.com/journals/journal-of-magnesium-and-alloys/2213-9567

Full length article

Improved mechanical proprieties of “magnesium based composites” with


titaniumealuminum hybrids
Muhammad Rashad a,b,*, Fusheng Pan a,b,c, Muhammad Asif d, Jia She a,b, Ahsan Ullah e
a
College of Materials Science and Engineering, Chongqing University, Chongqing 400044, China
b
National Engineering Research Center for Magnesium Alloys, Chongqing University, Chongqing 400044, China
c
Chongqing Academy of Science and Technology, Chongqing, Chongqing 401123, China
d
School of Materials Science and Engineering, Dalian University of Technology, Dalian 116024, China
e
Department of Physics, Quaid-i-Azam University, Islamabad 46000, Pakistan
Received 25 November 2014; revised 19 December 2014; accepted 25 December 2014
Available online 25 March 2015

Abstract

In this study, the effect of micron-sized titanium and aluminum addition on the microstructural, mechanical and work-hardening behavior of
pure Mg is investigated. Pure Mg reinforced with 10%Ti and 10%Tie1%Al particulates were synthesized through semi-powder metallurgy route
followed by hot extrusion. Semi-powder metallurgy appears to be promising approach for the synthesis of Mg based composite, as it is free of
ball milling. Tensile results indicate that the direct addition of micron-sized 10wt.% titanium particulates to pure Mg, caused an improvement in
elastic modulus, 0.2% yield strength, ultimate tensile strength, and failure strain (þ72%; þ41%; þ29%; and þ79% respectively). The addition
of micron-sized 10wt.% titanium particles along with 1.0wt.% Al particles to pure Mg, resulted in an enhancement in elastic modulus, 0.2%
yield strength, ultimate tensile strength, and failure strain (þ74%; þ56%; þ45%; and þ241% respectively). Besides tensile test, Vickers
hardness and work-hardening behavior of prepared composites were also examined. Impressive failure strain of Mge10Tie1Al composite can
be attributed to the better compatibility of Ti particulates with Mg due to presence of alloying element Al.
Copyright 2015, National Engineering Research Center for Magnesium Alloys of China, Chongqing University. Production and hosting by
Elsevier B.V. All rights reserved.

Keywords: Mechanical properties; Microstructure; Powder metallurgy method; Metal matrix composite

1. Introduction ductility and toughness [2]. The problem of low ductility and
tensile strength of Mg can be overcome by incorporation of
Magnesium alloys are a class of structural materials with different kind of reinforcements in the form of particles or
increasing industrial interest in automobile service due to their fibers. Literature study reveals that ceramic and intermetallic
good strength to weight ratio and low density [1]. Mg has (SiC, TiC, TiB2, Al2O3, Y2O3, TiO2, Mg2Si etc) re-
hexagonal closed-packed (HCP) structure which leads to low inforcements have been extensively used to increase the
strength of monolithic Mg [3e14]. But brittle nature of re-
inforcements leads to limited ductility of Mg composites.
During past decade, carbon nanotubes (CNTs) have been
* Corresponding author. College of Materials Science and Engineering, extensively used as reinforcement for magnesium composites.
Chongqing University, Chongqing 400044, China. Even though CNT/Mg composites have been extensively
E-mail address: rashadphy87@gmail.com (M. Rashad). investigated, but uniform dispersion of CNTs in the matrix is
Peer review under responsibility of National Engineering Research Center big challenge for researchers which limit its use for practical
for Magnesium Alloys of China, Chongqing University.

http://dx.doi.org/10.1016/j.jma.2014.12.010.
2213-9567/Copyright 2015, National Engineering Research Center for Magnesium Alloys of China, Chongqing University. Production and hosting by Elsevier B.V. All rights reserved.
2 M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9

applications. This is caused by agglomerates formation due to the Mg composites [18,19]. In 2011, Sankaranarayanan et al.
its one dimensional structure and strong van der Waal attrac- [20] investigated the mechanical behavior of Mg-5.6wt.%Ti-
tions between carbon atoms [15,16]. 2.5wt.%Al2O3 composite. The evaluation of mechanical
Metallic reinforcement such as titanium has good ductility, properties indicated a significant enhancement in tensile
strength, hardness and Young's modulus. The main advantage strength however failure stain was no more than 6.8%. Similar
of Ti based Mg alloys it that there is no formation of any behavior in strength properties were observed when Cu par-
brittle inter-metallic compounds between Ti and Mg as shown ticulates were added to Mg-5.6wt.%Ti alloy [21]. Recently,
in TieMg binary phase diagram [17]. The research on hybrid Sankaranarayanan et al. Ref. [22] examined the effect of nano-
reinforcement is gaining importance in recent years because SiC particles on mechanical behavior of Mg-5.6wt.%Ti com-
they have positive influence on the mechanical properties of posites. Room temperature tensile results revealed an

Fig. 1. Flowchart of semi-powder metallurgy method.


M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9 3

2. Experimental procedures

2.1. Materials

Raw materials, magnesium, aluminum and titanium pow-


ders (having particle size of 74, 3 and 25 mm respectively)
with 99.5% purity were purchased from Shanghai Customs
Golden Powder Material Co. Ltd. China.

2.2. Processing

Ball milling is an incompatible technique as it produces


heat which can burn Mg powder easily. Therefore, a simple
solution based strategy named as semi-powder metallurgy
method was adopted to mix the composite powders (Fig. 1).
Pure Mg powder was mixed in ethanol using a mechanical
agitator at the speed of 2000RPM. At the same time rein-
forcement particles 10wt.%Ti and 1.0wt.% Al were mixed in
ethanol using magnetic stirring. Reinforcement particle solu-
tion was then added drop wise into the above Mg slurry in
ethanol. Mixing process was continued for an hour to obtain
the homogeneous mixture. Mechanically agitated mixture was
filtered and vacuum dried at 80  C for 12 h to obtain the
mixture powder. Samples of pure Mg and Mg-10wt.%Ti
composite were prepared using same procedure. Pure Mg,
Mg-10wt.%Ti and Mg-10wt.%Ti-1.0wt.%Al composite pow-
ders were compacted under 620 MPa pressure to obtain the
green billets of 75 mm in diameter and 40 mm in height. The
compacted billets were sintered in the box furnace at 630  C
for 110 min under argon atmosphere. The sintered billets were
preheated to 350  C for an hour and extruded at 1 m/min
extrusion speed. Final diameter of the rods obtained after
extrusion was 16 mm. Samples from extruded rods were used
for further characterization.

2.3. Materials characterization


Fig. 2. X-ray diffraction spectra of pure Mg and its composites conducted on:
(a) powder samples; and (b) extruded samples.
X-ray diffraction (XRD) analysis on powder mixtures and
polished samples from extruded bars were carried out by X-
ray diffraction (D/MAX-1200, China), using Cu Ka radiation
in the range 10e90 . Raw XRD data were refined and
analyzed via MDI Jade 6.0 program (Materials Data Incor-
improvement in tensile strength and failure strain (i.e Failure
porated: Livermore, CA, USA). Samples for microstructural
strain was 9.6%). In another report, effect of 9.6wt.%Ti par-
characterization were machined from the extruded bars. Op-
ticulates addition on mechanical properties of pure Mg was
tical microscopy was used to investigate the grain size of pure
investigated. Tensile results indicated improvement in tensile
Mg and Mg-10wt.%Ti, Mg-10wt.%Ti-1.0wt.%Al composites.
strength and ductility (ductility was 9.5%) [23].
Scanning electron microscopy (SEM) equipped with energy-
In current work, an attempt have been made to increase the
dispersive spectrometer (EDS) was used to analyze the sur-
ductility of pure Mg by adding micron-sized Ti (10wt.%) and
face morphology and dispersion of reinforcement particles in
Al (1.0wt.%) particulates through semi-powder metallurgy
the matrix. Automatic digital micro hardness tester
technique. Room temperature mechanical testing revealed a
(SHANGHAI HX-1000TM) was used to measure the Vickers
significant enhancement in tensile strength and failure strain.
Hardness of monolithic Mg and Mg-10wt.%Ti, Mg-10wt.%Ti-
The failure strain value was higher than that of earlier reports
1.0wt.%Al composites. Micro hardness test was carried out on
[20e23]. Besides tensile strength, microstructure and work-
polished samples under a load of 100 g and 15 s dwell time in
hardening behavior of Pure Mg and its composites were also
accordance with the ASTM standard E384-99. For tensile test,
analyzed.
4 M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9

Fig. 3. Optical microscopic images showing the grain characteristic of: (a) Pure Mg; (b) Mge10Ti; and (c) Mge10Tie1Al composites.

the Al were absent which can be attributed to the low volume


fraction of Al in the Mge10Tie1Al composite. Fig. 2(b)
Table 1
Grain size characteristics of pure Mg and its composites.
shows the x-ray diffraction patterns of extruded samples. It is
clear from the figure that only peaks corresponding to pure Mg
Materials Grain size (mm) Aspect ratio
and Ti are observed in Mge10Ti and Mge10Tie1Al extruded
Pure Mg 29 ± 3.5 1.62 ± 0.32 composites. This witness that no phase formation occurs be-
Mge10Ti 20 ± 4.1 1.58 ± 0.40
Mge10Tie1Al 10 ± 3.2 1.60 ± 0.25
tween Mg and Ti which is consistent with their binary phase
diagram [17]. According to phase diagrams of MgeAl and
TieAl, the Al can react with both Mg and Ti to form inter
metallic phases however in Mge10Tie1Al composite its
round samples with 3 mm diameter and 15 mm gauge length content is too low to form intermetallic phase and was not
were machined from the extruded rods (Fig. 1). Tensile test detected by XRD. For both Mge10Ti and Mge10Tie1Al
was carried out at ambient temperature with initial strain speed composites, the intensity of Mg diffraction patterns becomes
of 1  10-3 s1 and the tensile direction was parallel to stronger which may be attributed to the recrystallization and
extrusion direction (ED). Three samples were made for each grain refinement during sintering and extrusion process.
composition to minimize the error. Images of tensile fracture The grain characteristics (grain size and morphology) of
surfaces were taken using SEM. pure Mg and its composites are depicted in Fig. 3(aec) and
Table 1. The pure Mg exhibits largest grain size (29 mm).
3. Results and discussion However, addition of Ti particulates to the pure Mg (Mge10Ti
composite) leads to the refined grain structure. The combined
3.1. Microstructure additions of micron-sized Ti and Al particulates to the pure
Mg, lead to the effective reduction in grain size which reveals
The results of x-ray diffraction analysis conducted on pure the smallest grain size (about 10 mm) among all the materials.
Mg, Mge10Ti and Mge10Tie1Al composite powders are The microstructure of pure Mg and synthesized composites
depicted in Fig. 2(a). In addition to the Mg peaks, Ti peaks is depicted in Fig. 4(aed). It can be seen that pure Mg exhibits
were observed in the powder samples. Peaks corresponding to large grain size and a lot of micro pores on its surface. On the
M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9 5

Fig. 4. SEM micrographs showing the surface morphology: (a) Pure Mg; (b) Mge10Ti; (c) Mge10Tie1Al; and (d) micrograph showing the insoluble Ti par-
ticulates in the Mg matrix.

Table 2
Room temperature mechanical properties of Pure Mg, Mge10Ti and Mge10Tie1Al composites.
Materials E (GPa) 0.2%YS (MPa) UTS (MPa) d (%) Vickers hardness (HV)
Pure Mg ~7.0 ~104 ~164 ~6.2 ~40
Mge10Ti ~12.1 ~147 ~212 ~11.1 ~46
Mge10Tie1Al ~12.2 ~163 ~238 ~21.2 ~55
E: Elastic modulus; YS: yield stress; UTS: ultimate tensile stress; d: strain to failure.

other hand, Mge10Ti composite exhibits very smooth surface and extrusion process. Therefore, restricts the grain growth, so
with few micro pores on its surface. Therefore reveals higher resulting in refined structure [24].
tensile strength as compare to pure Mg (Table 2). The Fig. 5(aed) shows x-ray mapping results of the
microstructure of Mge10Tie1Al composite reveals unclear Mge10Tie1Al composite. It can be seen that reinforcements
grain boundaries which may be due to diffusion of Al par- Ti and Al are uniformly distributed in the matrix. The
ticulates at grain boundaries. The diffused Al particulates reasonably uniform distribution of reinforcement particles can
induce the better compatibility between Mg and Ti particles be attributed to the efficient strategy adopted while fabrication
thus resulting in higher tensile strength as compared to the of the composites.
pure Mg and Mge10Ti composite (Table 2). Moreover it can
be seen from Fig. 4(d) that Ti particles are insoluble in the Mg 3.2. Mechanical characterization
matrix. Therefore Mg matrix and Ti particles interface are free
of intermetallic phase, as evident from the XRD analysis The room temperature mechanical properties are depicted
(Fig. 2(b)) and phase diagram [17]. The insoluble Ti particles in Fig. 6 and Table 2. It can be seen that pure Mg reveals very
act as site for the grain nucleation center during the sintering low hardness, tensile strength and failure strain. However
6 M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9

Fig. 5. X-ray mapping of Mge10Tie1Al composite: (a) Mge10Tie1Al composite; (b) Magnesium matrix; (c) Titanium; and (d) Aluminum.

addition of micron-sized Ti particulates to pure Mg dispersion of Ti particulates in the matrix, the ductile Ti
(Mge10Ti) leads to significant enhancement in hardness, particles can more easily assist the geometrical changes of
elastic modulus, yield strength, ultimate tensile strength and Mg during tensile loading without rupture. In addition, the
failure strain. The improvement in mechanical properties of absence of intermetallic phases is also advantageous. Thus
Mge10Ti composite can be attributed to the strengthening leads to the higher failure strain (11.1%) of Mge10Ti com-
effects arisen from the (1) Hall-Petch relationship due to posite. The failure strain of the synthesized Mge10Ti com-
refined grains (Fig. 2 and Table 1), (2) mismatch in co- posite is limited up to 11.1% which maybe attribute to the
efficient of thermal expansion (CTE), elastic modulus and insolubility of Ti in the Mg matrix. Thus leads to poor
hardness between Mg matrix and Ti particulates, and (c) op- bonding between matrix Mg and Ti particles. The common
position offered by Ti particulates against the dislocation alloying element Al has good solubility and bonding with the
motion [25e28]. matrix Mg and Ti particulates. Therefore, synergetic effect of
The synergetic effect of 10wt% Ti and 1wt%Al Ti and small fraction of Al is effective to improve the boding
(Mge10Tie1Al composite) particulates in the Mg matrix between Ti particles and Mg matrix. Thus lead to impressive
revealed the impressive increase in the hardness, tensile increase in the failure strain of the Mge10Tie1Al composite
strength and failure strain values. The Mge10Tie1Al com- (Fig. 6 and Table 2). The small fraction of alloying element
posite displayed the higher mechanical properties than pure Al was used to prevent the formation of intermetallic phases
Mg and Mge10Ti composite as shown in Fig. 6 and Table 2. between Ti/Mg and Al which have adverse effect on the
The enhancement in the tensile strength is due to the effects failure strain.
similar to that observed with addition of individual micro- Besides tensile test, work-hardening behavior of the sam-
sized Ti particulates, as explained in above paragraph. ples was also examined as shown in Fig. 6(c). The work-
It can be seen from Table 2 that an impressive enhance- hardening rate, q (q ¼ ds/dε; where s and ε are macro-
ment in failure strain (21.2%) was achieved by the combined scopic stress and strain) [29] verses strain ε curves are shown
addition of Ti and Al particulates. Interestingly such failure in Fig. 6(c). It can be seen that work-hardening rate q for pure
stain improvement occurred along with significant positive Mg, Mge10Ti and Mge10Tie1Al composites are 9689,
effect on the tensile properties. Since the Ti is more ductile 14,069, and 13,827 MPa respectively. It can be observed from
as compare to the Mg, therefore during homogeneous the graph that Mge10Ti and Mge10Tie1Al composites
M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9 7

Fig. 6. Mechanical behavior of pure Mg, Mge10Ti and Mge10Tie1Al composites: (a) True stressestrain curves; (b) Engineering stressestrain curves; (c) work-
hardening rate vs strain plots; and (d) Hardening capacities.

exhibit steeper curves than pure Mg of stage III. The differ- 4. Conclusions
ence in slopes of stage III may be attributed to the difference
of the dislocations density. The hardening capacity, Hc of the The pure Mg and its composites were successfully syn-
materials can be defined as Hc¼(sUTS  s0.2)/s0.2 [30] where thesized through semi-powder metallurgy method followed by
sUTS and s0.2 are the ultimate tensile stress and 0.2% yield hot extrusion technique. Based on microstructural and me-
stress. Fig. 6(d) revealed that pure Mg exhibit highest hard- chanical characterization following conclusions can be drawn.
ening capacity (0.58). One the other hand Mge10Ti and
Mge10Tie1Al composites revealed hardening capacities of 1- Semi-powder metallurgy method is an efficient technique
0.44 and 0.46 respectively. The variation of Hc is related to the to fabricate Mg based composite by excluding the ball
grain size and dislocation density of as extruded samples. milling process.
2- Compare to monolithic Mg, the synthesized composites
3.3. Fractography (Mge10Ti & Mge10Tie1Al) exhibited improved hard-
ness, elastic modulus, 0.2% yield strength, ultimate
The fractographic evidences of pure Mg and its composites strength and failure strain (%).
under tensile loading are depicted in Fig. 7(aec). The frac- 3- The impressive increase in failure strain of the
tograph of pure Mg exhibits brittle fracture as shown in Mge10Tie1Al composite is due to the better compatibility
Fig. 7(a). Generally, micro-cracks are generated in the com- of Mg matrix with Ti particulates due to presence of small
posites due to the interfacial stresses between matrix and re- fraction of alloying element Al.
inforcements [31]. The tensile fracture image of Mge10Ti 4- Increased hardness and tensile strength of the composites
composite reveals cleavage planes and tear ridges as shown in can be attributed to the (a) mismatch in CTE and Elastic
Fig. 7(b). The fracture image of Mge10Tie1Al composite modulus; (b) Orowan strengthening; and (c) load transfer
(Fig. 7(c)) composed of dimples which witness the high mechanism, between Mg matrix and reinforcement.
elasticity (21.2%) [32e39].
8 M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9

Fig. 7. Tensile fracture images of: (a) Pure Mg; (b) Mge10Ti; and (c) Mge10Tie1Al composite.

Acknowledgment [12] C. Mayencourt, R. Schaller, Mater. Mater. Sci. Eng. A 325 (2002) 286e291.
[13] Y. Park, K. Terasaki, K. Igarashi, T. Shimizu, Adv. Comp. Mater. 10
(2001) 17e28.
The present work was supported by the National Natural [14] S. Vaucher, O. Beffort, J. Kübler, F. Lehner, Adv. Eng. Mater. 5 (2003)
Science Funds of China (No. 50725413), the Ministry of 669e672.
Science and Technology of China (MOST) (No. [15] T. Hertel, R.E. Walkup, P. Avouris, Phy. Rev. B 58 (1998) 13870e13873.
2010DFR50010 and 2011FU125Z07), and Chongqing Science [16] L.Y. Jiang, Y. Huang, H. Jiang, G. Ravichandran, H. Gao, K.C. Hwang,
and Technology Commission (CSTC2013JCYJC60001). B. Liu, J. Mech. Phys. Solids 54 (2006) 2436e2452.
[17] J.L. Murray, ASM Int. (1998).
[18] M. Rashad, F. Pan, H. Hu, M. Asif, S. Hussain, J. She, Mater Sci Eng A
References 630 (2015) 36e44.
[19] M.K. Habibi, S.P. Joshi, M. Gupta, Acta Mater. 58 (2010) 6104e6114.
[1] F.H. Froes, Mater. Sci. Eng. A 184 (1994) 119e133. [20] S. Sankaranarayanan, S. Jayalakshmi, M. Gupta, J. Alloys Compd. 509
[2] M. Rashad, F. Pan, M. Asif, in: M. S. A. Tiwari (Eds.), Graphene ma- (2011) 7229e7237.
terials: fundamentals and emerging applications, Wiley-Scrivener Pub- [21] S. Sankaranarayanan, S. Jayalakshmi, M. Gupta, Mater. Des. 37 (2012)
lishing LLC, Beverly, MA, 2015, pp. 153e189. 274e284.
[3] J. Lan, Y. Yang, X. Li, Mater. Sci. Eng. A 386 (2004) 284e290. [22] S. Sankaranarayanan, R.K. Sabat, S. Jayalakshmi, S. Suwas, M. Gupta, J.
[4] H. Ferkel, B.L. Mordike, Mater. Sci. Eng. A 298 (2001) 193e199. Alloys Compd. 575 (2013) 207e217.
[5] R.A. Saravanan, M.K. Surappa, Mater. Mater. Sci. Eng. A 276 (2000) [23] S.F. Hassan, M. Gupta, J. Alloys Compd. 345 (2002) 246e251.
108e116. [24] M. Gupta, T.S. Srivatsan, J. Mater. Eng. Perform. 8 (1999) 473e478.
[6] M. Gupta, M.O. Lai, D. Saravanaranganathan, J. Mater. Sci. 35 (2000) [25] D.J. Lloyd, Int. Mater. Rev. 39 (1994) 1e23.
2155e2165. [26] S. Colin, Metals Reference Book, fifth ed., Butterworth's & Co. Ltd,
[7] Z. Xiuqing, W. Haowei, L. Lihua, T. Xinying, M. Naiheng, Mater. Lett. London, 1976.
59 (2005) 2105e2109. [27] G. Meijer, F. Ellyin, Z. Xia, Comp. Part B: Eng. 31 (2000) 29e37.
[8] G. Garces, M. Rodríguez, P. Perez, P. Adeva, Mater. Mater. Sci. Eng. A [28] G.E. Dieter, Mechanical Metallurgy, McGraw-Hill, USA, 1986.
419 (2006) 357e364. [29] U.F. Kocks, H. Mecking, Prog. Mater. Sci. 48 (2003) 171e173.
[9] S.F. Hassan, M. Gupta, Mater. Mater. Sci. Eng. A 392 (2005) 163e168. [30] N. Afrin, D.L. Chen, X. Cao, M. Jahazi, Scr. Mater. 57 (2007)
[10] L. Lu, K.K. Thong, M. Gupta, Comp. Sci. Technol. 63 (2003) 627e632. 1004e1007.
[11] V. Sklenicka, M. Svoboda, M. Pahutova, K. Kucharova, T.G. Langdon, [31] N.M.L. S., M. Gupta, Magn. Magn. Alloys Magn. Composit. (2011).
Mater. Sci. Eng. A 319e321 (2001) 741e745. Wiley.com.
M. Rashad et al. / Journal of Magnesium and Alloys 3 (2015) 1e9 9

[32] M. Rashad, F. Pan, A. Tang, Y. Lu, M. Asif, S. Hussain, J. She, J. Gou, [36] M. Rashad, F. Pan, A. Tang, M. Asif, M. Aamir, J. Alloys Compd. 603
J. Mao, J. Magn. Alloys 1 (2013) 242e248. (2014) 111e118.
[33] M. Rashad, F. Pan, M. Asif, A. Tang, J. Indust. Eng. Chem. 20 (2014) [37] M. Rashad, F. Pan, M. Asif, S. Hussain, M. Saleem, Mater. Charact. 95
4250e4255. (2014) 140e147.
[34] M. Rashad, F. Pan, A. Tang, M. Asif, J. She, J. Gou, J. Mao, H. Hu, J [38] M. Rashad, F. Pan, A. Tang, M. Asif, Prog. Nat. Sci. 24 (2014) 101e108.
Com Mater 49 (3) (2015) 285e293. [39] M. Rashad, F. Pan, M. Asif, A. Ullah, Mater. Sci. Technol. (2014), http://
[35] M. Rashad, F. Pan, A. Tang, M. Asif, S. Hussain, J. Gou, J. Mao, J. Ind. dx.doi.org/10.1179/1743284714Y.0000000726.
Eng. Chem. (2014). http://dx.doi.org/10.1016/j.jiec.2014.08.024.

Das könnte Ihnen auch gefallen