nanomaterials Article
Effects of Carbon Source on TiC Particles’ Distribution, Tensile, and Abrasive Wear Properties of In Situ TiC/Al-Cu Nanocomposites Prepared in the Al-Ti-C System Yu-Yang Gao 1,2 , Feng Qiu 1,2,3, * Qi-Chuan Jiang 1,2, * 1
2 3
*
ID
, Tian-Shu Liu 1,2 , Jian-Ge Chu 1,2 , Qing-Long Zhao 1,2
ID
and
State Key Laboratory of Automotive Simulation and Control, Jilin University, No. 5988, Renmin Street, Changchun 130025, China;
[email protected] (Y.-Y.G.);
[email protected] (T.-S.L.);
[email protected] (J.-G.C.);
[email protected] (Q.-L.Z.) Key Laboratory of Automobile Materials, Ministry of Education and Department of Materials Science and Engineering, Jilin University, No. 5988, Renmin Street, Changchun 130025, China Qingdao Automotive Research Institute of Jilin University, No. 1, Loushan Road, Qingdao 266000, China Correspondence:
[email protected] (F.Q.);
[email protected] (Q.-C.J.); Tel.: +86-431-8509-5592 (F.Q.); +86-431-8509-4699 (Q.-C.J.)
Received: 15 July 2018; Accepted: 3 August 2018; Published: 10 August 2018
Abstract: The in situ TiC/Al-Cu nanocomposites were fabricated in the Al-Ti-C reaction systems with various carbon sources by the combined method of combustion synthesis, hot pressing, and hot extrusion. The carbon sources used in this paper were the pure C black, hybrid carbon source (50 wt.% C black + 50 wt.% CNTs) and pure CNTs. The average sizes of nano-TiC particles range from 67 nm to 239 nm. The TiC/Al-Cu nanocomposites fabricated by the hybrid carbon source showed more homogenously distributed nano-TiC particles, higher tensile strength and hardness, and better abrasive wear resistance than those of the nanocomposites fabricated by pure C black and pure CNTs. As the nano-TiC particles content increased, the tensile strength, hardness, and the abrasive wear resistance of the nanocomposites increased. The 30 vol.% TiC/Al-Cu nanocomposite fabricated by the hybrid carbon source showed the highest yield strength (531 MPa), tensile strength (656 MPa), hardness (331.2 HV), and the best abrasive wear resistance. Keywords: in situ nano-TiC; Al matrix nanocomposites; tensile properties; abrasive wear behaviors
1. Introduction The demands for energy saving and low fuel consumption in the structural fields and heat sink applications have inspired the developments of the lightweight Al alloys and corresponding Al matrix composites [1–6]. The Al matrix composites with ceramic particles reinforcements show more excellent thermal stability, mechanical performance and wear resistance than the Al alloys [7–12]. The commonly used ceramic particle enhancers for Al matrix composites are TiC, TiB2 , SiC, and B4 C ceramic particles [13–19]. The TiC particles showed low mismatch with Al matrix and obtained excellent Al-TiC interface bonding without the generation of interfacial reaction products [20–25]. The superior Al-TiC interface provided good adhesion between the TiC particles and Al matrix, which contributed to decrease the thermal boundary resistance, resist the plastic deformation and increased the strength and hardness of the Al matrix [4,26,27]. It is necessary to mention that, the Al-Cu composites reinforced with nano-sized ceramic particles showed finer α-Al grains, higher tensile strength and ductility, higher creep resistance, and better sliding wear resistance than those of the
Nanomaterials 2018, 8, 610; doi:10.3390/nano8080610
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composites reinforced with the micron-sized particles [7,28,29]. As reported, the in situ TiC/Al-Cu nanocomposites obtained simultaneous increases in tensile strength and ductility at high temperatures (ranging from 298 K to 573 K) compared to the Al-Cu matrix alloys [23,25]. Tian et al. found that, the 0.5 wt.% TiC/Al-Cu nanocomposite showed much better sliding wear resistance than the Al-Cu alloy, with the highest increase of 83.5% in relative wear resistance at 453 K and applied load of 20 N [7]. The nano-TiC particles are very effective and promising enhancers for the Al-Cu alloys. The most challenge work for the Al matrix nanocomposite is how to obtain homogenous distribution of the nanoparticles, which greatly affect the thermal, electrical, and mechanical properties of the nanocomposites [8,19,27]. Currently, the TiC/Al nanocomposites are prepared by the ex and in situ processing routes, such as mechanical alloying, stir casting, powder metallurgy, spark plasma sintering, combustion synthesis, etc. [30–36]. However, these ex situ methods possess some drawbacks, such as poor interface bonding, uneven distributions, and interface contamination [34,37]. Zhou et al. modified TiC nanoparticles by deposition Ni coating on the TiC surface to improve the wetting between TiC and Al matrix, and the 0.8 wt.% TiC/Al–Cu nanocomposite prepared by stir casting obtained the highest tensile strength (573 MPa) [34]. The distribution of the TiC nanoparticles in the Al matrix composites prepared by methods of mechanical alloying, powder metallurgy and spark plasma sintering were largely depended on the ball milling parameters, such as milling times, speed and the weight ratio of ball to powders [4,5,31,35]. Nemati et al. prepared the Al-4.5 wt.% Cu-TiC nanocomposites by fabrication route of high energy attritor ball milling and hot sintering to obtain uniformly-dispersed TiC nanoparticles [31]. When the TiC nanoparticles content is higher than the critical level (5 wt.%), the TiC nanoparticles agglomerations increased, which lowered the strengthening effects [31]. The in situ TiC/Al nanocomposites, which were synthesized in Al-Ti-CNTs systems by the method of combustion synthesis and hot pressing, have obtained a relatively ideal distribution of nano-TiC particles and excellent Al-TiC interface bonding [25,38]. The combined method of combustion synthesis, hot pressing, and hot extrusion can further improve the nanoparticles distribution in the synthesized nanocomposites and densify the nanocomposites. The in situ TiC/Al-Cu-Mg nanocomposites synthesized by this combined method showed superior room temperature tensile properties with superior yield strength (404 MPa), tensile strength (601 MPa), and fracture strain (10.8%) [25]. However, the CNTs shows strong tendency to form agglomerations due to the strong van der Waals force. In the ball-milling process, the CNTs can be easily tangled and twisted together. As reported, the CNTs’ clusters in the raw reaction powders led to the uneven distribution of precipitated nano-TiC particles in the synthesized nanocomposites [25]. Chen et al. took the combined methods of the high energy ball milling and the solution ball milling to obtain the homogenously distributed CNTs on the Al powders [39]. Najimi et al. took a mixed ball-milling mode (200 rpm, 2 h + 1000 rpm, 1 h) to improve the CNTs distribution in the mixed powders, which successfully improved the mechanical properties of prepared composites [40]. It is well known to us that the high-speed ball-milling device is usually very expensive and the cost of CNTs is also high. Carbon black (C black) is another commonly used and easily dispersed carbon source with fine size and low cost. It is reported that the TiC particles synthesized by carbon source of C black show larger average sizes compared to that synthesized by CNTs [41,42]. The increase in TiC particles sizes might weaken the van der Walls force between the nanoparticles and impair the tendency of the nano-TiC particles to form clusters in the synthesized nanocomposites. Therefore, we chose the hybrid carbon source (C black + CNTs) to improve the nano-TiC particle distribution in the synthesized TiC/Al-Cu nanocomposites. In this study, in situ TiC/Al-Cu nanocomposites were synthesized in Al-Ti-C systems with various carbon sources (C black, hybrid C/CNTs and CNTs) by the combined method of combustion synthesis, hot pressing and hot extrusion. The effects of carbon source on the nano-TiC particles distribution, tensile, and abrasive wear properties of the TiC/Al-Cu nanocomposites were studied. This work aims at providing a simple and low-cost way to obtain the in situ TiC/Al-Cu nanocomposites with high strength and abrasive wear resistance.
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2. Experimental Procedure The raw powders were Al-Cu (Al-4.7 wt.% Cu-0.32 wt.% Mg-0.65 wt.% Mn-0.44 wt.% Si) alloy 2. Experimental Procedure powders (~13 μm, 99% purity), Ti powders (~25 μm, 99.5% purity), C black (~40 nm, 99% purity), and raw powders were Al-Cu (Al-4.7 Cu-0.3295.0% wt.% purity). Mg-0.65The wt.% Mn-0.44 wt.% Si) alloy CNTsThe (~20–100 μm in length and 10–20 nmwt.% in diameter, nominal compositions of powders (~13 µm, 99% purity), Ti powders (~25 µm, 99.5% purity), C black (~40 nm, 99% and TiC/Al-Cu nanocomposites were presented in Table 1. Figure 1 shows the processpurity), schematic CNTs (~20–100 µm in length 10–20 nm in diameter, 95.0% purity). nominal compositions of diagrams for preparation theand in situ TiC/Al-Cu nanocomposites. The The mixed Al alloy powders, Ti TiC/Al-Cu nanocomposites were presented in Table 1. Figure 1 shows the process schematic diagrams powders, and carbon powders (C black/CNTs) were ball milling at a speed of 50 rpm for 18 h. The for preparation the was in situ nanocomposites. Thecold mixed Al alloy Ti powders, and molar ratio of Ti/C 1:1.TiC/Al-Cu The ball-milled powders were pressed intopowders, the cylindrical compacts carbon powders (C black/CNTs) were ballTiC/Al-Cu milling at nanocomposites a speed of 50 rpm for 18 h. The molar ratio of (ϕ 45 mm × 36 mm). The fabrication of the were performed in a vacuum Ti/C was 1:1. The ball-milled powders were cold pressed into the cylindrical compacts (φ 45 mmthe × furnace at a heating speed of about 30 K/min. When a sudden jump in temperature observed, 36 mm). The fabrication of the TiC/Al-Cu nanocomposites were performed in a vacuum furnace at combustion synthesis reaction proceeded and the compact was densified by applying an axial pressa heating 30 K/min. When sudden jumpby in the temperature combustion (~50 MPaspeed for 20ofs).about The Al-Cu matrix alloyawas prepared method ofobserved, hot press the sintering at 873 synthesis reaction proceeded and the compact was densified by applying an axial press (~50 MPa for K for 60 min. The hot extrusion was performed on the sintered Al-Cu alloy and TiC/Al-Cu 20 s). The Al-Cu with matrix was prepared by the of hot press sintering at 873 K for 60tomin. nanocomposites analloy extrusion ratio of 19:1 at method 833 K. The extruded sheets were subjected T6 The hot extrusion was performed on the sintered Al-Cu alloy and TiC/Al-Cu nanocomposites with heat treatment, which included solution treatment (778 K for 2 h), quenching in water, and artificial an extrusion ratio aging (433 K for 18of h).19:1 at 833 K. The extruded sheets were subjected to T6 heat treatment, which included solution treatment (778 K for 2 h), quenching in water, and artificial aging (433 K for 18 h). Table 1. Characteristics of the in situ TiC/Al-Cu nanocomposites synthesized in Al-Ti-C systems. Table 1. Characteristics of the in situ TiC/Al-Cu nanocomposites synthesized in Al-Ti-C systems.
Designed Composition Designed Samples 10 vol.% TiC/Al-Cu 10B Composition 10H 10 vol.% TiC/Al-Cu 10B 10 vol.% TiC/Al-Cu 10C 10 vol.% TiC/Al-Cu 10H 10 vol.% TiC/Al-Cu 10 vol.% TiC/Al-Cu 20B10C 20 vol.% TiC/Al-Cu 20B 20 vol.% TiC/Al-Cu 20H 20 vol.% TiC/Al-Cu 20H 20 vol.% TiC/Al-Cu 20C 20 vol.% TiC/Al-Cu 20C 20 vol.% TiC/Al-Cu 30B30B 30 vol.% TiC/Al-Cu 30 vol.% TiC/Al-Cu 30H 30 vol.% TiC/Al-Cu 30H 30 vol.% TiC/Al-Cu 30C 30 vol.% TiC/Al-Cu 30C 30 vol.% TiC/Al-Cu
Samples
Actual TiC Carbon Source Used Powders (wt.%) Content Actual TiC Powders (wt.%) 8.9 vol.% C Carbon black Source 83.1% Al Used + 13.5% Ti + 3.4% C black Content 9.0 vol.% Hybrid C/CNTs 83.1% Al + 13.5% Ti + 1.7% C black + black 1.7% CNTs 8.9 vol.% C black 83.1% Al + 13.5% Ti + 3.4% C 9.2 vol.% CNTs 83.1% + 13.5% Ti + C3.4% 9.0 vol.% Hybrid C/CNTs 83.1% Al + Al 13.5% Ti + 1.7% blackCNTs + 1.7% CNTs 9.2 vol.% CNTs 83.1% + 13.5% + 3.4% 19.8 vol.% C black 68.7% Al +Al 25.0% Ti +Ti6.3% C CNTs black 19.8 vol.% Hybrid C/CNTs C black 68.7% Al 6.3% C 19.9 vol.% 68.7% Al + 25.0% Ti ++ 25.0% 3.15%TiC+black + black 3.15% CNTs 19.9 vol.% Hybrid C/CNTs 68.7% Al + 25.0% Ti + 3.15% C black + 3.15% CNTs 19.9 vol.% CNTs 68.7% Al + 25.0% Ti + 6.3% CNTs 19.9 vol.% CNTs 68.7% Al + 25.0% Ti + 6.3% CNTs 29.8 vol.% C black 56.1% Al Al + 35.1% TiTi+ +8.8% 29.8 vol.% C black 56.1% + 35.1% 8.8%CCblack black 29.9 vol.% Hybrid Hybrid C/CNTs 56.1% 56.1% + 35.1% + 4.4% black++4.4% 4.4% CNTs CNTs 29.9 vol.% C/CNTs Al +Al35.1% Ti Ti + 4.4% C Cblack 29.9 vol.% 56.1% + 35.1% 8.8%CNTs CNTs 29.9 vol.% CNTsCNTs 56.1% Al Al + 35.1% TiTi+ +8.8%
Figure 1. The process schematic diagrams for preparation the in situ TiC/Al-Cu nanocomposites, (a) Figure 1. The process schematic diagrams for preparation the in situ TiC/Al-Cu nanocomposites, (a) ball milling ball milling process process of of the the raw raw powders, powders, (b) (b) cold cold pressing pressing into into the the cylindrical cylindrical compacts, compacts, (c) (c) fabrication fabrication the TiC/Al-Cu nanocomposites T6 the TiC/Al-Cu nanocompositesby bycombustion combustionsynthesis synthesisand andhot hot pressing, pressing, (d) (d) hot hot extrusion, extrusion, (e) (e) T6 heat treatment, and (f) TiC/Al-Cu nanocomposites. heat treatment, and (f) TiC/Al-Cu nanocomposites.
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The microstructure of the synthesized TiC/Al-Cu nanocomposites was observed by scanning electron microscopy ((SEM, Evo18, Carl Zeiss, Oberkochen, Germany) and TEM (JEM 2100F, JEOL, Tokyo, Japan). The morphology of the nano-TiC particles was observed by FESEM (JSM-6700F, JEOL, Tokyo, Japan). The bulk nanocomposites were dissolved in 18 vol.% HCl aqueous solution to remove the Al matrix. About one thousand nano-TiC particles were randomly selected to count the average sizes. The preparation of TEM foils were firstly ground to 60 µm by mechanical polishing and then thinned by twin-jet electrical polishing in a mixed solution (10% perchloric acid + 90% ethanol) at 15 V and 243 K. The specimens for the tensile and the abrasive wear tests were machined from the nanocomposites along the extrusion direction. The dog-bone shaped tensile samples had a gauge length, gauge width, and gauge thickness of 10 mm, 4 mm, and 2 mm, respectively. The room tensile tests were performed using a servo hydraulic materials testing system (MTS 810, MTS Systems Corporation, Minneapolis, MN, USA) at a strain rate of 3 × 10−4 s−1 . The abrasive wear tests were conducted on a ML-30 wheeled abrasion tester with the sliding distance of 120 m and the applied load of 5 N, 15 N, and 25 N. The abrasive test was carried on the surface of extruded samples parallel to the extrusion direction with dimensions of 40 mm × 5 mm. The abrasive Al2 O3 papers with the abrasive particle sizes of 6.5 µm, 13 µm, and 23 µm were selected as the counter face. The actual density of the extruded samples was tested by the Archimedes method. The synthesized Al-Cu matrix alloy and nanocomposites obtained a high relative density (>100%), which meant that the nanocomposites were fully densified by the hot extrusion process. The volume loss during abrasive wear testing was determined by using mass loss divided by actual density. The abrasive wear resistance was defined by the ratio of the wear rate of the Al-Cu matrix alloy to that of the TiC/Al-Cu nanocomposites. The abrasive wear resistance of the Al-Cu alloy was set to the 1.00. The tensile and abrasive wear tests were repeated three times to characterize the tensile and abrasive wear properties of the samples. The micro-hardness of the specimens was characterized by a Vickers hardness tester (1600-5122VD, Buehler, Feasterville, PA, USA), using a dwell time of 10 s and an applied load of 5 N for 10 times. 3. Results and Discussion 3.1. Microstructure and Mchanical Properties Figure 2 shows the XRD detection results of TiC/Al-Cu nanocomposites prepared in the Al-Ti-C system by various carbon sources. It can be observed that the phase compositions of prepared TiC/Al-Cu nanocomposites are mainly composed of Al, TiC, CuAl2 , and Al3 Ti. When a lower content of reactants of Ti and C in the Al-Ti-C system occurs, the reaction could not proceed sufficiently and intermediate products remains. As shown in Figure 2a–c, the residual Al3 Ti phase could be observed in the 10 vol.% TiC/Al-Cu nanocomposites prepared by different carbon sources. The actual volume fractions of nano-TiC particles in the nanocomposites 10B (8.9 vol.%), 10H (9.0 vol.%), and 10C (9.2 vol.%) were lower than the designed content (10 vol.%). With the reactants increasing, pure reaction products were obtained in the fabricated 20 vol.% and 30 vol.% TiC/Al-Cu nanocomposites, and the actual volume fractions of the nano-TiC particles were very close to the target values. Figure 3 shows the SEM micrographs of the extruded TiC/Al-Cu nanocomposites fabricated by carbon sources of C black, hybrid C/CNTs, and CNTs. As the nano-TiC particles content increased, non-homogenous distribution regions of nano-TiC particles (labeled by the red circles) were obviously reduced, which means that the distribution of the nano-TiC particles was improved in the nanocomposites. The nanocomposites 30B, 30H, and 30C obtained relatively uniform distribution of nano-TiC particles, as shown in Figure 3g–i. On the other hand, the nanocomposites fabricated by the hybrid C/CNTs (nanocomposites 20H and 30H) showed more homogenous distributions than those of the nanocomposites fabricated by the pure C black (nanocomposites 20B and 30B) and the pure CNTs (nanocomposites 20C and 30C).
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Figure XRD patterns of the synthesized TiC/Al-Cu nanocomposites fabricated by carbon sources Figure2.2.2.The The XRD patterns of the the synthesized synthesized TiC/Al-Cu nanocomposites fabricated by carbon carbon Figure The XRD patterns of TiC/Al-Cu nanocomposites fabricated by of (a) pure C black, (b) hybrid C/CNTs, and (c) pure CNTs. sourcesof of(a) (a)pure pureCCblack, black,(b) (b)hybrid hybridC/CNTs, C/CNTs,and and(c) (c)pure pureCNTs. CNTs. sources
Figure3.3.3.SEM SEMmicrographs micrographsof ofthe theextruded extrudedTiC/Al-Cu TiC/Al-Cunanocomposites nanocomposites fabricated by carbon sources Figure SEM micrographs of the extruded Figure TiC/Al-Cu nanocompositesfabricated fabricatedby bycarbon carbonsources sources of pure C black, hybrid C/CNTs, and pure CNTs. (a) nanocomposite 10B, (b) nanocomposite 10H, (c) of pure pure C C black, black, hybrid pure CNTs. (a)(a) nanocomposite 10B,10B, (b) nanocomposite 10H,10H, (c) of hybridC/CNTs, C/CNTs,and and pure CNTs. nanocomposite (b) nanocomposite nanocomposite 10C, (d) nanocomposite 20B, (e) nanocomposite 20H, (f) nanocomposite 20C, (g) nanocomposite 10C,10C, (d) (d) nanocomposite 20B,20B, (e) nanocomposite 20H,20H, (f) nanocomposite 20C, 20C, (g) (c) nanocomposite nanocomposite (e) nanocomposite (f) nanocomposite nanocomposite 30B, (h) nanocomposite 30H and (i) nanocomposite 30C. nanocomposite 30B, (h) nanocomposite 30H and (i) nanocomposite 30C. (g) nanocomposite 30B, (h) nanocomposite 30H and (i) nanocomposite 30C.
Figures444 and and 555 show show the the FESEM images and average sizes ofnano-TiC nano-TiC particles fabricated in Figures average sizes of particles fabricated in Figures show theFESEM FESEMimages imagesand and average sizes of nano-TiC particles fabricated Al-Ti-C systems with carbon sources of pure C black, hybrid C/CNTs, and pure CNTs. The Al-Ti-C systems with carbon sources of pure C black, hybrid C/CNTs, and pure The in Al-Ti-C systems with carbon sources of pure C black, hybrid C/CNTs, and CNTs. pure CNTs. nanocomposite 10Cobtained obtained thesmallest smallest sizednano-TiC nano-TiC particles (67nm). nm).(67 With theincrease increase in nanonanocomposite 10C the sized particles (67 With the nanoThe nanocomposite 10C obtained the smallest sized nano-TiC particles nm). With thein increase TiC particlesparticles content,the the average sizes ofnano-TiC nano-TiC particles increased fromincreased 67nm nmin innanocomposite nanocomposite TiC particles content, average sizes of increased from 67 in nano-TiC content, the average sizes particles of nano-TiC particles from 67 nm in 10C, 97 nm in nanocomposite 20C to 116 nm in nanocomposite 30C. When the carbon sources in AlAl10C, 97 nm in nanocomposite 20C to 116 nm in nanocomposite 30C. When the carbon sources nanocomposite 10C, 97 nm in nanocomposite 20C to 116 nm in nanocomposite 30C. When the in carbon Ti-C systems transferred from C black, hybrid C/CNTs to CNTs, the average sizes of generated nanoTi-C systems transferred from C black, hybrid CNTs,C/CNTs the average of the generated nanosources in Al-Ti-C systems transferred from C/CNTs C black,tohybrid to sizes CNTs, average sizes TiC particles decreased obviously. By using the hybrid carbon black/CNTs, the nanocomposite 30H TiC particles decreased obviously. By using the hybrid carbon black/CNTs, the nanocomposite 30H of generated nano-TiC particles decreased obviously. By using the hybrid carbon black/CNTs, the showed moderate moderate nano-TiC nano-TiC particles particles size size of of 176 176 nm nm between between the the nanocomposite nanocomposite 30B 30B (239 (239 nm) nm) and and showed nanocomposite 30H showed moderate nano-TiC particles size of 176 nm between the nanocomposite the nanocomposite 30C (116 nm). the (239 nanocomposite (116 nm). 30B nm) and the30C nanocomposite 30C (116 nm).
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Figure 4.FESEM FESEMimages imagesof ofextracted extractednano-TiC nano-TiCparticles particlesfrom fromTiC/Al-Cu TiC/Al-Cunanocomposites nanocomposites fabricated Figure4.4. FESEM images of extracted nano-TiC particles from TiC/Al-Cu nanocompositesfabricated fabricated Figure by carbon sources of pure C black, hybrid C/CNTs, and pure CNTs. (a) nanocomposite 10B,10B, (b) by carbon carbonsources sourcesofofpure pureCCblack, black,hybrid hybrid C/CNTs, pure CNTs. (a) nanocomposite by C/CNTs, andand pure CNTs. (a) nanocomposite 10B, (b) nanocomposite 10H, (c) nanocomposite 10C, (d) nanocomposite 20B, (e) nanocomposite 20H, (f) (b) nanocomposite (c) nanocomposite (d) nanocomposite (e) nanocomposite nanocomposite 10H,10H, (c) nanocomposite 10C, 10C, (d) nanocomposite 20B, 20B, (e) nanocomposite 20H,20H, (f) nanocomposite 20C, (g)nanocomposite nanocomposite 30B, (h)(h) nanocomposite 30H and (i)(i) nanocomposite 30C. (f) nanocomposite 20C, (g) nanocomposite 30B, nanocomposite 30H and nanocomposite 30C. nanocomposite 20C, (g) 30B, (h) nanocomposite 30H and (i) nanocomposite 30C.
Figure 5. of nano-TiC particles in TiC/Al-Cu nanocomposites fabricated by carbon Figure Theaverage averagesizes sizesof ofnano-TiC nano-TiCparticles particlesin inTiC/Al-Cu TiC/Al-Cunanocomposites nanocomposites Figure 5.5.The fabricated by carbon sources of pure C black, hybrid C/CNTs, and pure CNTs. sources of pure C black, hybrid C/CNTs, and pure CNTs. sources of pure C black, hybrid C/CNTs, and pure CNTs.
In the the Al-Ti-C Al-Ti-C reaction system, Al powders in the original reactants firstly melted and then Al Ti In reactionsystem, system,Al Alpowders powdersin inthe theoriginal original reactantsfirstly firstlymelted meltedand andthen thenAl Al33Ti 3Ti In the Al-Ti-C reaction reactants phase formed by Al-Ti reaction. As the temperature increased, Al Ti phase dissolved and Al-Ti binary phaseformed formedby byAl-Ti Al-Tireaction. reaction.As Asthe thetemperature temperatureincreased, increased,Al Al333Ti Tiphase phasedissolved dissolvedand andAl-Ti Al-Tibinary binary phase liquid formed. With the heating temperature further increasing, Al-Ti-C ternary liquid phase formed liquidformed. formed.With Withthe theheating heatingtemperature temperaturefurther furtherincreasing, increasing,Al-Ti-C Al-Ti-Cternary ternaryliquid liquidphase phaseformed formed liquid with the decomposition and dissolve of carbon source. WithWith the concentration of [C] of reached the critical with the decomposition and dissolve of carbon source. the concentration [C] reached the with the decomposition andignited dissolve carbon source. With the concentration of [C] reached the point, the [Ti]-[C] reaction andof nano-TiC particles precipitated. The carbon decomposition critical point, the [Ti]-[C] reaction ignited and nano-TiC particles precipitated. The carbon critical point, [Ti]-[C] reaction ignited and sufficiently nano-TiC by particles precipitated. Thegenerated carbon accelerated andthe the combustion reaction proceeded thesufficiently great amount of heat decomposition accelerated andthe thecombustion combustion reactionproceeded proceeded bythe the great amount decomposition accelerated and reaction sufficiently by great amount by heat the [Ti]-[C] reaction. Considering the higher chemistrythe activity and higher specific CNTs, of generated by the the [Ti]-[C] reaction. reaction. Considering higher chemistry activityarea andofhigher higher of heat generated by [Ti]-[C] Considering the higher chemistry activity and the Al-Ti-C liquid phase could occur at a lower temperature with the carbon source of CNTs than specificarea areaof ofCNTs, CNTs,the theAl-Ti-C Al-Ti-Cliquid liquidphase phasecould couldoccur occurat ataalower lowertemperature temperaturewith withthe thecarbon carbon specific those ofofCCNTs black than and hybrid C/CNTs. the Al-Ti-C Therefore, system with the carbonsystem source with of CNTs source those of of blackTherefore, andhybrid hybrid C/CNTs. the Al-Ti-C the source of CNTs than those CCblack and C/CNTs. Therefore, the Al-Ti-C system with the carbon source of CNTs reacted at a lower temperature. Furthermore, the rapid decomposition of the carbon source of CNTs reacted at a lower temperature. Furthermore, the rapid decomposition of the
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reacted at a lower temperature. Furthermore, the rapid decomposition of the CNTs guaranteed the shorter combustion reaction time of Al-Ti-C system when compared to the carbon sources of C black and hybrid C/CNTs. According to the index functional relation between the ceramic particles growth and the combustion temperature, the lower combustion temperature assured the smaller sizes of precipitated nano-TiC particles [26,41]. As a consequence, the sizes of generated nano-TiC particles decreased gradually with the carbon sources transferring from CNTs, hybrid C/CNTs to C black. However, the twisting and tangling of CNTs would cause the non-homogenous distribution of the rich regions of dissolved [C] and, subsequently, nano-TiC particles’ precipitation in the Al matrix. Moreover, the van der Waals forces between in the nano-TiC particles became more favorable with the nano-TiC particles sizes decreasing when carbon sources transferring from C black, hybrid C/CNTs, to CNTs. As a consequence, the nano-TiC/Al-Cu nanocomposites synthesized by a carbon source of CNTs exhibited terrible dispersions of nano-TiC particles, as shown in Figure 3c–i. In contrast to the CNTs, the C black with lower chemistry activity and decomposition rate would lead to the uneven distribution of [C] regions. These uneven [Ti]-[C] reactions occurred which resulted in the abnormal growth and non-ideal dispersion of precipitated nano-TiC particles. Additionally, the great amount of heat released by uneven reaction regions might cause the formation of voids, which is reflected by the lower actual density of TiC/Al-Cu nanocomposites synthesized by a carbon source of C black, as observed in Table 2. In this paper, we took the hybrid C/CNTs to weaken the twisting and tangling of CNTs and obtain relative uniform distribution of carbon source in the Al-Ti-C system. Finally, the TiC/Al-Cu nanocomposites fabricated by the carbon source of hybrid C/CNTs exhibited a more homogenous distribution of nano-TiC particles. Table 2. Room tensile properties and hardness of the Al-Cu matrix alloy and the TiC/Al-Cu nanocomposites. Samples
σ 0.2 (MPa)
σ UTS (MPa)
εf (%)
Hardness (HV)
Actual Density (g/cm−3 )
Al alloy 10B 10H 10C 20B 20H 20C 30B 30H 30C
320 ± 6 394 ± 8 441 ± 6 415 ± 7 426 ± 5 503 ± 8 471 ± 9 470 ± 10 531 ± 9 508 ± 7
468 ± 13 493 ± 12 570 ± 16 553 ± 12 522 ± 10 636 ± 13 591 ± 8 551 ± 9 656 ± 12 616 ± 14
17.6 ± 2.8 2.5 ± 1.4 2.4 ± 0.8 3.9 ± 2.0 2.3 ± 0.5 3.2 ± 0.6 3.0 ± 1.3 2.3 ± 0.2 3.0 ± 0.8 2.5 ± 0.8
135.7 ± 3 213.8 ± 5 228.5 ± 8 199.3 ± 5 270.0 ± 4 295.6 ± 9 269.9 ± 11 303.3 ± 5 331.2 ± 5 285.1 ± 6
2.997 ± 0.001 2.814 ± 0.003 3.249 ± 0.002 3.085 ± 0.002 3.293 ± 0.004 3.575 ± 0.002 3.320 ± 0.003 3.538 ± 0.004 3.555 ± 0.003 3.599 ± 0.003
Figure 6 shows the yield strength (σ0.2 ), tensile strength (σUTS ), and hardness (HV) of the Al-Cu alloy and the TiC/Al-Cu nanocomposites. The room tensile properties (σ0.2 , σUTS , and fracture strain (εf )) and hardness are presented in Table 2. As observed in Figure 6, the TiC/Al-Cu nanocomposites showed much better σ0.2 , σUTS and HV compared to the Al-Cu alloy. As the nano-TiC particles content increased, the σ0.2 , σUTS , and HV of the nanocomposites increased significantly. The nanocomposites 30B, 30H, and 30C showed the superior σUTS and hardness of 551 MPa and 303.3 HV, 656 MPa, and 331.2 HV, and 616 MPa and 285.1 HV, respectively. On the other hand, the nanocomposites fabricated by carbon source of the hybrid C/CNTs (nanocomposites 20H and 30H) showed better σ0.2 , σUTS , HV, and actual density than those of the nanocomposites fabricated by C black (nanocomposites 20B and 30B) and CNTs (nanocomposites 20C and 30C). It can be inferred that the number of nano-TiC particles in nanocomposite 30B is less than that in the nanocomposites 30H and 30C due to the larger nano-TiC particle sizes. Compared to the nanocomposite 30C, the nanocomposite 30H obtained a more homogenous distribution of nano-TiC particles. The nanocomposite 30H might obtain better Orowan strengthening effects than those of nanocomposites 30B and 30C attributed to the higher number and more homogenous distribution of nano-TiC particles. The nanocomposite 30H obtained the best comprehensive tensile properties and hardness with σ0.2 , σUTS , εf , and HV of 531 MPa, 656 MPa, 3.0%, and 331.2 HV, respectively.
particles in nanocomposite 30B is less than that in the nanocomposites 30H and 30C due to the larger nano-TiC particle sizes. Compared to the nanocomposite 30C, the nanocomposite 30H obtained a more homogenous distribution of nano-TiC particles. The nanocomposite 30H might obtain better Orowan strengthening effects than those of nanocomposites 30B and 30C attributed to the higher number and more homogenous distribution of nano-TiC particles. The nanocomposite 30H obtained the best2018, comprehensive tensile properties and hardness with σ0.2, σUTS, εf, and HV of 531 MPa, 656 8 of 21 Nanomaterials 8, 610 MPa, 3.0%, and 331.2 HV, respectively.
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Figure 6. The (a) yield strength, and(c) (c)hardness hardness TiC/Al-Cu nanocomposites Figure 6. The (a) yield strength,(b) (b)tensile tensilestrength, strength, and ofof TiC/Al-Cu nanocomposites fabricated by carbon sources pureCCblack, black, hybrid hybrid C/CNTs, and pure CNTs. fabricated by carbon sources ofofpure C/CNTs, and pure CNTs.
Figure 7 Room shows the TEM micrographs nanocomposite 20H hot extrusion and T6 heat Table 2. tensile properties and hardnessofofthe the Al-Cu matrix alloy and theafter TiC/Al-Cu nanocomposites. treatments. Figure 7a shows the σfine sized α-Al εgrains of the nanocomposite 20H. Density Figure(g/cm 7b,c−3)show the Samples σ0.2 (MPa) UTS (MPa) f (%) Hardness (HV) Actual Al alloy 320 ± 6 ± 13 135.7 ±3 2.997 ± 0.001 Figure 7d,e nano-TiC particles distributed in468 the interior 17.6 and± 2.8 at the grain boundaries of α-Al grains. 394 ± 8 493 ± 12 2.5 ± 1.4 213.8 ± 5 2.814 ± 0.003 show the10B morphology and corresponded selected-area electron diffraction (SAED) of the generated 10H 441 ± 6 570 ± 16 2.4 ± 0.8 228.5 ± 8 3.249 ± 0.002 nano-TiC10C particles. 415 As± 7shown in553Figure 7f, the a low mismatch ± 12 3.9 ±in 2.0 situ nano-TiC 199.3 ± 5particles showed 3.085 ± 0.002 20B 426 Attributed ±5 522 10 good wetting 2.3 ± 0.5 ability 270.0 ± 0.004 with molten with Al matrix (3.7%). to±the of in± 4situ nano-TiC3.293 particles 20H 503 ± 8 636 ± 13 3.2 ± 0.6 295.6 ± 9 3.575 ± 0.002 Al, some20C nano-TiC particles were591 captured by3.0the growing 269.9 α-Al± 11 grains, which3.320 were observed in the 471 ± 9 ±8 ± 1.3 ± 0.003 30Bα-Al grains, 470 ± 10 9 ± 0.2 303.3 5 3.538 ± 0.004 interior of as shown551 in±Figure 7b.2.3Additionally, the±nano-TiC particles, which were not 531 ± 9 656 ± 12 3.0 ± 0.8 331.2 ± 5 3.555 ± 0.003 captured30H by the rapidly advancing liquid-solid interface, were eventually distributed at the grain 30C 508 ± 7 616 ± 14 2.5 ± 0.8 285.1 ± 6 3.599 ± 0.003 boundaries, as shown in Figure 7c. The nano-TiC particles, distributed at grain boundaries and within the α-Al Figure grains,7 shows impeded the dislocation The dislocation networks and dislocation the TEM micrographsmotions. of the nanocomposite 20H after hot extrusion and T6 heat walls formed, as seen in Figure 7a,b. As a result, the nano-TiC particles increased the plastic deformation treatments. Figure 7a shows the fine sized α-Al grains of the nanocomposite 20H. Figure 7b,c show the nano-TiC distributedwhich in the interior and at boundaries of α-Al grains. Figureof the resistance of the particles nanocomposites, is reflected bythe thegrain improved strength and hardness 7d,e show the morphology and corresponded selected-area electron diffraction (SAED) of the generated nano-TiC particles. As shown in Figure 7f, the in situ nano-TiC particles showed a low mismatch with Al matrix (3.7%). Attributed to the good wetting ability of in situ nano-TiC particles with molten Al, some nano-TiC particles were captured by the growing α-Al grains, which were observed in the interior of α-Al grains, as shown in Figure 7b. Additionally, the nano-TiC particles,
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and dislocation walls formed, as seen in Figure 7a,b. As a result, the nano-TiC particles increased the plastic deformation resistance of the nanocomposites, which is reflected by the improved strength nanocomposites. to the most homogeneous distribution of nano-TiC particles and high and hardness of Attributed the nanocomposites. Attributed to the most homogeneous distribution of nano-TiC nano-TiC particles content (30 vol.%), the nanocomposite 30H exhibited the best Orowan strengthening particles and high nano-TiC particles content (30 vol.%), the nanocomposite 30H exhibited the best effects andstrengthening highest tensile strength hardness. Orowan effects and and highest tensile strength and hardness.
Figure 7. TEM micrographs of 20 vol.% TiC/Al-Cu nanocomposites fabricated by the hybrid carbon Figure 7. TEM micrographs of 20 vol.% TiC/Al-Cu nanocomposites fabricated by the hybrid carbon source. (a–c) microstructure images, (d) nano-TiC particles, and (e,f) corresponded selected-area source. (a–c) microstructure images, (d) nano-TiC particles, and (e,f) corresponded selected-area electron electron diffraction (SAED) patterns and HRTEM image of area A. diffraction (SAED) patterns and HRTEM image of area A.
3.2. Abrasive Wear Behaviors 3.2. Abrasive Wear Behaviors Figure 8 shows the variations of wear rate with applied load (5 N, 15 N, and 25 N) for the Al-Cu Figure 8 shows variations of nanocomposites wear rate with applied load (5 N,10H, 15 N,20H, and and 25 N) for the Al-Cu matrix alloy and inthe situ TiC/Al-Cu (nanocomposites 30H) against matrix alloy and in situ TiC/Al-Cu nanocomposites (nanocomposites 10H, 20H, and 30H) against various Al2O3 particle sizes. As the applied load increased, the wear rates (WR) of the Al-Cu matrix various Al2 O sizes. As increased. the applied increased, the8a, wear (WR) ofload the Al-Cu matrix alloy and the nanocomposites Asload shown in Figure withrates the applied increasing 3 particle −11 3 alloy and the As/m) shown Figurematrix 8a, with the applied from load 7.72, increasing from from 5 N, tonanocomposites 15 N, to 25 N, theincreased. WR (10 m of theinAl-Cu alloy increased to 15.48, −11 m 3 /m) of the Al-Cu matrix alloy increased from 7.72, to 15.48, 5 N, to 15 N, to 25the N, abrasive the WR (10 to 22.27 against particle size of 23 μm. The TiC/Al-Cu nanocomposites showed much thanthe those of the Al-Cu matrix The WR the nanocomposites decreased obviously to lower 22.27 WR against abrasive particle size alloy. of 23 µm. TheofTiC/Al-Cu nanocomposites showed much withWR the increase in the nano-TiC content. theof nano-TiC particles content increased from lower than those of the Al-Cuparticles matrix alloy. TheAs WR the nanocomposites decreased obviously 10 vol.%, 20 vol.%, to 30 vol.%, the hardness of the As nanocomposites 228.5 HV in the with the increase in the nano-TiC particles content. the nano-TiCincreased particles from content increased from nanocomposite 10H, 295.6 HV in the nanocomposite 20H to 331.2 HV in the nanocomposite 30H, 10 vol.%, 20 vol.%, to 30 vol.%, the hardness of the nanocomposites increased from 228.5 HV in the −11 m 3/m) decreased from 15.57 in the nanocomposite 10H, 9.19 in the nanocomposite while the WR (10 nanocomposite 10H, 295.6 HV in the nanocomposite 20H to 331.2 HV in the nanocomposite 30H, while 20H to 7.93 in the nanocomposite 30H with load of 25 N and abrasive 2O3 particle the WR (10−11 m3 /m) decreased from 15.57the in applied the nanocomposite 10H,the 9.19 in the Al nanocomposite size 23 μm. Thenanocomposite abrasive wear resistance theapplied nanocomposite 30H higher that 20H toof7.93 in the 30H withofthe load of 25 Nwas and1.81 the times abrasive Al2than O3 particle of Al-Cu alloy under the applied load of 25 N and abrasive Al2O3 particle size of 23 μm. On the other size of 23 µm. The abrasive wear resistance of the nanocomposite 30H was 1.81 times higher than hand, the WR of the Al-Cu matrix alloy and the nanocomposites decreased when the abrasive Al2O3 that of Al-Cu alloy under the applied load of 25 N and abrasive Al2 O3 particle size of 23 µm. On the particle sizes decreased. The WR of the nanocomposite 30H decreased from 7.93, to 3.01, to 1.64 with other hand, the WR of the Al-Cu matrix alloy and the nanocomposites decreased when the abrasive the decreases in the abrasive Al2O3 particle sizes from 23 μm, to 13 μm, to 6.5 μm under the applied Al2 O3 particle sizes decreased. The WR of the nanocomposite 30H decreased from 7.93, to 3.01, to load of 25 N. With the applied load of 5 N and abrasive Al2O3 particle size of 6.5 μm, the WR of 1.64 with the decreases in the abrasive Al2 O3and particle sizes from 23 µm, to 13 µm, to 6.5 µm under the nanocomposite 30H was 0.78 (10−11 m3/m), the abrasive wear resistance was 2.54 times higher applied load of 25 N. With the applied load of 5 N and abrasive Al2 O3 particle size of 6.5 µm, the WR than that of the Al-Cu alloy. of nanocomposite 30H was 0.78 (10−11 m3 /m), and the abrasive wear resistance was 2.54 times higher than that of the Al-Cu alloy.
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Figure Variationsofofwear wearrate ratewith withapplied applied load load for nanocomposites Figure 8. 8. Variations for the the Al-Cu Al-Cualloy alloyand andTiC/Al-Cu TiC/Al-Cu nanocomposites (fabricated by the hybrid C/CNTs) under the abrasive Al 2O3 particle sizes of (a) 23 μm, (b) 13 μm, and (fabricated by the hybrid C/CNTs) under the abrasive Al2 O3 particle sizes of (a) 23 µm, (b) 13 µm, and (c) 6.5 μm. (c) 6.5 µm.
Figure 9 showsthe theworn wornsurface surfaceof of the the Al-Cu Al-Cu alloy 10H, 20H, and 30H. Figure 9 shows alloyand andthe thenanocomposites nanocomposites 10H, 20H, and 30H. As observed, the nanocomposites showed much smoother worn surface compared to the Al-Cu alloy. As observed, the nanocomposites showed much smoother worn surface compared to the Al-Cu alloy. As mentioned above, the nanocomposites with higher nano-TiC particles content obtained higher As mentioned above, the nanocomposites with higher nano-TiC particles content obtained higher HV, HV, which decreased the contacting area between the abrasive Al2O3 particles and the samples. On which decreased the contacting area between the abrasive Al2 O3 particles and the samples. On the the other hand, the nano-TiC particles helped to constrain the plastic deformation of Al matrix, other hand, the nano-TiC particles helped to constrain the plastic deformation of Al matrix, impeded impeded the penetrating of abrasive particles and reduced the cutting efficiency of abrasive particles, the penetrating of abrasive particles and reduced the cutting efficiency of abrasive particles, which which helped to increase the abrasive wear resistance of the nanocomposites [26]. As the nano-TiC helped to increase abrasive wear of the to nanocomposites As the nano-TiC particles particles content the increased from 10 resistance vol.%, 20 vol.%, 30 vol.% in the[26]. nanocomposites, the microcontent increased from 10 vol.%, 20 vol.%, to 30 vol.% in the nanocomposites, the micro-ploughing ploughing efficiency of the abrasive Al2O3 particles decreased and the abrasive wear mechanism efficiency of the abrasive Al2 O3 particles decreased and the abrasive wear mechanism transferred from
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Nanomaterials 2018, 8, xto FOR REVIEW 11 of 20 the micro-ploughing thePEER micro-cutting. As shown in Figure 9a–l, the abrasive wear grooves on the worn surface of the nanocomposites became shallower and narrower with the increase in nano-TiC transferred from the micro-ploughing to the micro-cutting. As shown in Figure 9a–l, the abrasive particles content. The penetrating ability of the abrasive Al2 O3 particles increased with the applied load wear grooves on the worn surface of the nanocomposites became shallower and narrower with the increasing, which contributed to increasing the depth and width of the grooves [43,44]. As the applied increase in nano-TiC particles content. The penetrating ability of the abrasive Al 2O3 particles load increased increasedwith fromthe 5 N, to 15load N, to 25 N, thewhich amount of abrasive debris and plastic deformation applied increasing, contributed to increasing thethe depth and width of regions the grooves onapplied the worn of the increased as the along grooves [43,44]. As the loadsurface increased fromAl-Cu 5 N, toalloy 15 N,and to 25nanocomposites N, the amount of abrasive shown in Figure The penetration depth andthe thegrooves micro-cutting efficiency abrasive Al2 O3 debris and the9a–l. plastic deformation regions along on the worn surface of of the the Al-Cu alloy anddecreased nanocomposites as shown Figure The penetration depth and thethe micro-cutting particle with increased the decrease in theinsizes of9a–l. abrasive Al2 O3 particle, while abrasive wear efficiency of samples the abrasive Al2O3 particle decreased with the decrease sizes ofAl abrasive Al 2O3 sizes resistance of the increased. As observed in Figure 9l,p,t, with in thethe abrasive 2 O3 particle particle, while abrasive wear of the samples increased. As grooves observeddecreased in Figure 9l,p,t, decreasing from 23the µm, to 13 µm, toresistance 6.5 µm, the width and depth of the obviously with the abrasive Al 2O3 particle sizes decreasing from 23 μm, to 13 μm, to 6.5 μm, the width and and the shallow and narrow grooves occupied the main parts. The micro-cutting was the abrasive depth of the grooves decreased obviously and the shallow and narrow grooves occupied the main wear mechanism for the Al-Cu alloy and the nanocomposites tested under the abrasive Al2 O3 particle parts. The micro-cutting was the abrasive wear mechanism for the Al-Cu alloy and the sizes of 13 µm and 6.5 µm.
nanocomposites tested under the abrasive Al2O3 particle sizes of 13 μm and 6.5 μm.
Figure 9. The SEM micrographs of worn surface of the Al-Cu alloy and TiC/Al-Cu nanocomposites
Figure 9. The SEM micrographs of worn surface of the Al-Cu alloy and TiC/Al-Cu nanocomposites (fabricated by the hybrid C/CNTs) under various abrasive Al2O3 particle sizes and applied loads. (a) (fabricated by the(b) hybrid C/CNTs) abrasive particle sizes applied loads. (a) Al-Cu alloy, 10H, (c) 20H and under (d) 30Hvarious under tested load Al of 25O N3 and abrasive Aland 2O3 particle size of Al-Cu23alloy, (b) 10H, (c) 20H and (d) 30H under tested load of 5 N and abrasive Al O particleAlsize of 23 2 3abrasive μm; (e) Al-Cu alloy, (f) 10H, (g) 20H and (h) 30H under tested load of 15 N and 2O3 µm; (e) Al-Cusize alloy, (f)μm; 10H, 20Halloy, and (h) tested load ofunder 15 N and abrasive O3and particle particle of 23 (i)(g) Al-Cu (j) 30H 10H, under (k) 20H and (l) 30H tested load of Al 252N size of 23 µm;Al (i)2OAl-Cu alloy, (k)(m) 20H andalloy, (l) 30H tested load(p) of30H 25 Nunder and tested abrasive Al2 O3 abrasive 3 particle size(j) of 10H, 23 μm; Al-Cu (n)under 10H, (o) 20H and load of 25 N and abrasive Al2O 3 particle size(n) of 13 μm;(o) (q)20H Al-Cu alloy, 10H, (s) 20H and (t) 30Hofunder particle size of 23 µm; (m) Al-Cu alloy, 10H, and (p) (r) 30H under tested load 25 N and tested of 25 N and abrasive Al2O3 particle size of 6.5 μm. abrasive Alload 2 O3 particle size of 13 µm; (q) Al-Cu alloy, (r) 10H, (s) 20H and (t) 30H under tested load of 25 N and abrasive Al2 O3 particle size of 6.5 µm.
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Figure 10 shows the variations of wear rate with applied load (5 N, 15 N, and 25 N) for the Figurealloy 10 shows thesitu variations of wear rate with applied load (5 and N, 1530B) N, and 25 N) for theabrasive AlAl-Cu matrix and in TiC/Al-Cu nanocomposites (10B, 20B, under various Cu matrix alloy and in situ TiC/Al-Cu nanocomposites (10B, 20B, and 30B) under various abrasive Al2 O3 particle sizes. The WR of the nanocomposites increased with the increases in the applied load 2O3 particle sizes. The WR of the nanocomposites increased with the increases in the applied load andAlabrasive Al2 O3 particle size, while decreased with the nano-TiC particles’ content increasing. and abrasiveload Al2Oincreased 3 particle size, while decreased with the nano-TiC particles’ content increasing. As As the applied from 5 N, to 15 N, to 25 N, the WR of the nanocomposite 30B increased the applied load increased from 5 N, to 15 N, to 25 N, the WR of the nanocomposite 30B increased − 11 from 5.06, 6.58 to 8.22 (10 m3 /m) against the abrasive Al2 O3 particle size of 23 µm. When the from 5.06, 6.58 to 8.22 (10−11 m3/m) against the abrasive Al2O3 particle size of 23 μm. When the applied applied load increasing up to 25N, the abrasive wear resistance of the nanocomposite 30B was 1.71, load increasing up to 25N, the abrasive wear resistance of the nanocomposite 30B was 1.71, 0.56, and 0.56, and 0.48 times higher than those of the Al-Cu alloy with the abrasive Al2 O3 particle size 23 µm, 0.48 times higher than those of the Al-Cu alloy with the abrasive Al2O3 particle size 23 μm, 13 μm, 13 µm, 6.5 µm, respectively. 11 shows the worn of the alloy Al-Cuand alloy and and 6.5 μm, respectively. FigureFigure 11 shows the worn surfacesurface imagesimages of the Al-Cu theand the nanocomposites nanocomposites10B, 10B, 20B and 30B. It can be observed in Figure 11 that the worn surface of the 20B and 30B. It can be observed in Figure 11 that the worn surface of the nanocomposites 10B, 20B, variationtendencies tendencies with nanocomposites nanocomposites 10B, 20B,and and30B 30Bdisplayed displayed similar similar variation with thethe nanocomposites 10H, 20H, and 30H, as a function of the applied load and abrasive particle size. 10H, 20H, and 30H, as a function of the applied load and abrasive particle size.
Figure 10. Variations of rate wear rate with load applied load for alloy the Al-Cu alloy andnanocomposites TiC/Al-Cu Figure 10. Variations of wear with applied for the Al-Cu and TiC/Al-Cu nanocomposites (fabricated by the pure C black) under the abrasive Al 2O3 particle sizes of (a) 23 μm, (fabricated by the pure C black) under the abrasive Al2 O3 particle sizes of (a) 23 µm, (b) 13 µm, and (c) (b) 13 μm, and (c) 6.5 μm. 6.5 µm.
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Figure The SEMmicrographs micrographsofofworn wornsurface surface of of the the Al-Cu Al-Cu alloy Figure 11.11. The SEM alloy and andTiC/Al-Cu TiC/Al-Cunanocomposites nanocomposites (fabricated by the pure C black) under various abrasive Al2O3 particle sizes and applied loads. (a) Al(fabricated by the pure C black) under various abrasive Al2 O3 particle sizes and applied loads. (a) Cu alloy, (b) 10B, (c) 20B and (d) 30B under tested load of 5 N and abrasive Al2O3 particle size of 23 Al-Cu alloy, (b) 10B, (c) 20B and (d) 30B under tested load of 5 N and abrasive Al2 O3 particle size μm; (e) Al-Cu alloy, (f) 10B, (g) 20B and (h) 30B under tested load of 15 N and abrasive Al2O3 particle of 23 µm; (e) Al-Cu alloy, (f) 10B, (g) 20B and (h) 30B under tested load of 15 N and abrasive Al2 O3 size of 23 μm; (i) Al-Cu alloy, (j) 10B, (k) 20B and (l) 30B under tested load of 25 N and abrasive Al2O3 particle size of 23 µm; (i) Al-Cu alloy, (j) 10B, (k) 20B and (l) 30B under tested load of 25 N and abrasive particle size of 23 μm; (m) Al-Cu alloy, (n) 10B, (o) 20B and (p) 30B under tested load of 25 N and Al2 O3 particle size of 23 µm; (m) Al-Cu alloy, (n) 10B, (o) 20B and (p) 30B under tested load of 25 N abrasive Al2O3 particle size of 13 μm; (q) Al-Cu alloy, (r) 10B, (s) 20B and (t) 30B under tested load of and abrasive Al2 O3 particle size of 13 µm; (q) Al-Cu alloy, (r) 10B, (s) 20B and (t) 30B under tested load 25 N and abrasive Al2O3 particle size of 6.5 μm. of 25 N and abrasive Al2 O3 particle size of 6.5 µm.
Figure 12 shows the variations of wear rate with applied load (5 N, 15 N, and 25 N) for the AlFigure 12 shows the variations of wear rate with applied load (5 N, 15 N, and 25 N) for the Al-Cu Cu matrix alloy and in situ TiC/Al-Cu nanocomposites (nanocomposites 10C, 20C, and 30C) under matrix alloy and in situ TiC/Al-Cu nanocomposites (nanocomposites 10C, 20C, and 30C) under various various abrasive Al2O3 particle sizes. Figure 13 shows the worn surface of the Al-Cu alloy and abrasive Al2 O3 particle Figure showsvarious the worn surface of the Al-Cu alloyAland nanocomposites nanocomposites 10C, sizes. 20C, and 30C13against applied loads and abrasive 2O3 particle sizes. 10C, 30C against various loads and abrasive Allower As seen in Figures 2 O3 particle As20C, seenand in Figures 12 and 13, theapplied nanocomposite 30C showed WR andsizes. smoother worn surface 12 and 13, the nanocomposite 30C showed lower WR and smoother worn surface at the tested conditions. at the tested conditions. With the applied load increasing from 5 N, 15 N to 25 N, the WR of the With the applied load increasingfrom from5.55, 5 N,9.78 15 N 25 N, themWR the nanocomposite increased 3/m)of nanocomposite 30C increased to to 10.17 (10−11 against the abrasive Al30C 2O3 particle − 11 3 from 10.17the (10applied m /m) thethe abrasive Alwear size of 23 µm. When the 2 O3 particle size5.55, of 239.78 μm.toWhen load against was 25 N, abrasive resistance of the nanocomposite applied load was 25 N, the abrasive wear resistance of the nanocomposite 30C was 1.19, 0.85 30C was 1.19, 0.85 and 1.08 times higher than that of the Al-Cu base alloy with the abrasive Al2Oand 3
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1.08 times higher than that of the Al-Cu base alloy with the abrasive Al2 O3 particle size 23 µm, 13 µm, particle size 23 μm, 13 μm, and 6.5 μm, respectively. It can be inferred that abrasive wear of the and 6.5 µm, respectively. It can be30C inferred thataabrasive wear of the nanocomposites 10C, 20C, and 30C nanocomposites 10C, 20C, and showed similar variation tendency with the nanocomposites showed a similar variation tendency with 10B, the nanocomposites 10H, 20H, andof30H and nanocomposites 10H, 20H, and 30H and nanocomposites 20B, and 30B under the effects different applied load 10B, 20B, and 30B under the effects of different applied load and abrasive Al O particle size. 2 3 and abrasive Al2O3 particle size.
Figure Variations of rate wearwith rateapplied with load applied load for alloy the Al-Cu alloy and TiC/Al-Cu Figure 12. 12. Variations of wear for the Al-Cu and TiC/Al-Cu nanocomposites nanocomposites (fabricated the pure CNTs) under abrasive Al2O3 particle sizes of (a) 23 μm, (fabricated by the pure CNTs)by under the abrasive Al2 Othe 3 particle sizes of (a) 23 µm, (b) 13 µm, and (c) 13 μm, and (c) 6.5 μm. 6.5(b) µm.
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Figure 13. The SEM micrographs of worn surface of the Al-Cu alloy and TiC/Al-Cu nanocomposites Figure 13. The SEM micrographs of worn surface of the Al-Cu alloy and TiC/Al-Cu nanocomposites (fabricated by the pure CNTs) under various abrasive Al2O3 particle sizes and applied loads. (a) Al(fabricated by the pure CNTs) under various abrasive Al2 O3 particle sizes and applied loads. (a) Al-Cu Cu alloy, (b) 10C, (c) 20C and (d) 30C under tested load of 5 N and abrasive Al2O3 particle size of 23 alloy, (b) 10C, (c) 20C and (d) 30C under tested load of 5 N and abrasive Al2 O3 particle size of 23 µm; μm; (e) Al-Cu alloy, (f) 10C, (g) 20C and (h) 30C under tested load of 15 N and abrasive Al2O3 particle (e) Al-Cu alloy, (f) 10C, (g) 20C and (h) 30C under tested load of 15 N and abrasive Al2 O3 particle size size of 23 μm; (i) Al-Cu alloy, (j) 10C, (k) 20C and (l) 30C under tested load of 25 N and abrasive Al2O3 of 23 µm; (i) Al-Cu alloy, (j) 10C, (k) 20C and (l) 30C under tested load of 25 N and abrasive Al2 O3 particle size of 23 μm; (m) Al-Cu alloy, (n) 10C, (o) 20C and (p) 30C under tested load of 25 N and particle size of 23 µm; (m) Al-Cu alloy, (n) 10C, (o) 20C and (p) 30C under tested load of 25 N and abrasive Al2O3 particle size of 13 μm; (q) Al-Cu alloy, (r) 10C, (s) 20C and (t) 30C under tested load of abrasive Al2abrasive O3 particle size of 13 µm; (q) Al-Cu alloy, (r) 10C, (s) 20C and (t) 30C under tested load of 25 N and Al2O 3 particle size of 6.5 μm. 25 N and abrasive Al2 O3 particle size of 6.5 µm.
Figure 14 shows the comparisons in wear rate vs. applied load of the nanocomposites 30B, 30H, Figure 14 shows the comparisons in wear rate vs. applied load of the nanocomposites 30B, 30H, and 30C against the abrasive Al2O3 particle size of 23 μm, 13 μm, and 6.5 μm. It can be observed that and 30C against the abrasive Al2 O3 particle size of 23 µm, 13 µm, and 6.5 µm. It can be observed that the abrasive wear rates of the nanocomposite 30H were lower than those of the nanocomposites 30B theand abrasive wear rates of the nanocomposite 30H were lower than those of the nanocomposites 30B 30C at all the tested conditions. The nanocomposite 30H obtained higher abrasive wear resistance and 30C at all tested conditions. The nanocomposite obtained higher abrasive wear resistance than that of the the nanocomposites 30B and 30C. Figure 1530H shows the worn surfaces and corresponded than that of the nanocomposites 30B and 30C. Figure 15 shows the worn surfaces and corresponded EDS analysis results of the nanocomposites 30B, 30H, and 30C, which tested against the abrasive EDS results of the nanocomposites 30B, 30H, and 30C, which tested against the abrasive Al2 O3 Alanalysis 2O3 particle size of 23 μm and applied load of 5N. The distribution of Ti element in the EDS analysis particle of 23 µm appliedofload 5N. The particles distribution of Ti element in the As EDSobserved, analysis result resultsize indicated theand dispersion theof nano-TiC in the nanocomposites. the indicated the dispersion of the nano-TiC particles in the nanocomposites. As observed, the distribution distribution of Ti in nanocomposite 30H was much more homogenous than that in the of Ti in nanocomposite 30H was much more homogenous than that in the nanocomposites 30B and
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30C. The nanocomposite 30H30C. obtained much more homogenous distribution nano-TiC particles nanocomposites 30B and The nanocomposite 30H obtained much of more homogenous than that of the nanocomposites 30B and 30C, which was consistent with the results as shown distribution of nano-TiC particles than that of the nanocomposites 30B and 30C, which was consistentin Figure 3. results It can be the 3. better wear resistance ofabrasive the nanocomposites 30H with the as inferred shown inthat Figure It canabrasive be inferred that the better wear resistance of than the those of the nanocomposites 30B of and was attributed30B to the more homogenously-distributed nanocomposites 30H than those the30C nanocomposites andmuch 30C was attributed to the much more nano-TiC particles in the nanocomposite 30H. in the nanocomposite 30H. homogenously-distributed nano-TiC particles
Figure14. 14.The The comparisons comparisons in in wear wear rate rate vs. vs. applied applied load Figure load of of the the 30 30 vol.% vol.% TiC/Al-Cu TiC/Al-Cunanocomposites nanocomposites fabricated by different carbon sources tested under abrasive Al 2O3 particle size of (a) 23 μm, (b) 13 fabricated by different carbon sources tested under abrasive Al2 O3 particle size of (a) 23 µm, (b) 13 µm, μm,(c) and 6.5 μm. and 6.5(c) µm.
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15. images SEM images worn surface and corresponded EDS analysis results of 30 vol.% TiC/Al-Cu Figure 15.Figure SEM of ofworn surface and corresponded EDS analysis results of 30 vol.% nanocomposites fabricated by carbon source of (a) C black, (b) hybrid C/CNTs, and (c) CNTs. TiC/Al‐Cu nanocomposites fabricated by carbon source of (a) C black, (b) hybrid C/CNTs, and (c) CNTs. Figure 16 shows the abrasive wear behavior diagrams of 30 vol.% TiC/Al-Cu nanocomposites
fabricated by different carbon sources. The nano-TiC particles played the role of load-supporting
Figure 16 shows the abrasive wear behavior diagrams of 30 vol.%The TiC/Al‐Cu elements and increased the hardness of the TiC/Al-Cu nanocomposites. penetrationnanocomposites depth as the carbon hardness sources. of the nanocomposites increased in the stages of a1, andof c1.load‐supporting As the fabricateddecreased by different The nano‐TiC particles played theb1,role abrasive wear proceeded, the abrasive Al2 O3 particles penetrated into the substrate and converted the elements and increased the hardness of the TiC/Al‐Cu nanocomposites. The penetration depth materials into the debris and chips (stages a2, b2, and c2). The abrasive wear loss of the nanocomposites decreasedoccurred as the hardness of the nanocomposites increased stages(stages of a1,a3, b1,b3,and during the reciprocating movements of the abrasive in Al2the O3 particle andc1. As the abrasive wear proceeded, Alformed 2O3 particles into inthe substrate and c3). The grooves andthe theabrasive wear debris on worn penetrated surface, as shown Figures 9, 11 and 13.converted As mentioned above, the nano-TiC particles obtained excellent interfacial bonding with the Al matrix, the materials into the debris and chips (stages a2, b2, and c2). The abrasive wear loss of the which obviously increased the strength and hardness of nanocomposites. It can be inferred that the nanocomposites occurred during the reciprocating movements of the abrasive Al2O3 particle (stages differences in the abrasive wear resistance of the nanocomposites 30B, 30H, and 30C were attributed a3, b3, andtoc3). The and grooves and the wear debrisparticles. formedThe on number worn surface, as shown 9, 11 the sizes distributions of the nano-TiC of nano-TiC particles in in Figures the and 13. Asnanocomposite mentioned above, nano‐TiC particles obtained excellent 30B was the smaller than that in the nanocomposite 30H due interfacial to the biggerbonding average with the size of nano-TiC particles in the nanocomposite 30B (239 nm) than that in the nanocomposite 30H It can be Al matrix, which obviously increased the strength and hardness of nanocomposites. (176 nm). As the number of nano-TiC particles increased, the direct contacting surface between the inferred that the differences in the abrasive wear resistance of the nanocomposites 30B, 30H, and 30C abrasive Al2 O3 particles and the Al substrate reduced which cause the decreased abrasive wear rates were attributed to the sizes The andnanocomposite distributions ofshowed the nano‐TiC particles. The number of the nanocomposites. 30H better abrasive wear resistance than thatof of nano‐TiC particles in the nanocomposite 30B was smaller than that in the nanocomposite 30H due to the bigger average size of nano‐TiC particles in the nanocomposite 30B (239 nm) than that in the nanocomposite 30H (176 nm). As the number of nano‐TiC particles increased, the direct contacting surface between the abrasive Al2O3 particles and the Al substrate reduced which cause the decreased abrasive wear rates of the nanocomposites. The nanocomposite 30H showed better abrasive wear
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the nanocomposite 30B. It is necessary to mention that the dispersions of nano-TiC particles in the nanocomposite 30C was not homogenous. The clusters of nano-TiC particles were to act as the preferential sites forideal crack nucleation, which inclined to form spalling pits andexpected increased act wear as therates preferential sites for crack nucleation, to in form spalling pits local and increased the of the nanocomposite at the stagewhich of c3, inclined as shown Figure 16c. The softened the Al wear rates of theenhancers nanocomposite at the stage of c3, as shown Figure 16c. softened Al matrix matrix without of nano-TiC particles was easilyinremoved byThe thelocal micro-ploughing and without enhancers of nano-TiC particles wasAl easily removed by the best micro-ploughing and resistance micro-cutting micro-cutting behaviors of the abrasive 2O3 particles. The abrasive wear of nanocomposite wasAlattributed to the amountwear of TiC particles and the homogenous behaviors of the 30H abrasive The high best abrasive resistance of nanocomposite 30H was 2 O3 particles. attributed toofthe high amount of TiC particles and the homogenous distribution of nano-TiC particles. distribution nano-TiC particles.
Figure Figure 16. 16. The The abrasive abrasive wear wear behavior behavior diagrams diagrams of of TiC/Al-Cu TiC/Al-Cunanocomposites nanocompositesfabricated fabricatedby bycarbon carbon sourceof of (a) (a) C C black black (nanocomposite (nanocomposite 30B), 30B), (b) (b) hybrid hybrid C/CNTs C/CNTs(nanocomposite (nanocomposite30H), 30H),and and(c) (c)CNTs CNTs source (nanocomposite 30C). 30C). (nanocomposite
4. 4. Conclusions Conclusions The The in in situ situ TiC/Al-Cu TiC/Al-Cunanocomposites nanocompositeswere weresynthesized synthesizedininthe theAl-Ti-C Al-Ti-C systems systems with with various various carbon sources(pure (pureC black, C black, hybrid C/CNTs, and CNTs) pure by CNTs) by the combined method of carbon sources hybrid C/CNTs, and pure the combined method of combustion combustion synthesis, and hotThe extrusion. average sizes ofparticles nano-TiC particles synthesis, hot pressinghot andpressing hot extrusion. averageThe sizes of nano-TiC ranged fromranged 67 nm from nmintothe 239fabricated nm in the nanocomposites. fabricated nanocomposites. The sizes of synthesized particles to 23967nm The sizes of synthesized nano-TiC nano-TiC particles increased increased with the TiCcontent particles content increasing, while with decreased with the transfersource of carbon with the TiC particles increasing, while decreased the transfer of carbon from source C black, hybrid C/CNTs toThe pureTiC/Al-Cu CNTs. Thenanocomposites TiC/Al-Cu nanocomposites pure Cfrom black,pure hybrid C/CNTs to pure CNTs. fabricated by fabricated the hybrid by the hybrid C/CNTs more homogenously distributed nano-TiC particles that in the C/CNTs obtained moreobtained homogenously distributed nano-TiC particles than that in the than nanocomposites nanocomposites synthesized by pure C black and pure CNTs. The 30 vol.% TiC/Al-Cu synthesized by pure C black and pure CNTs. The 30 vol.% TiC/Al-Cu nanocomposite (nanocomposite nanocomposite 30H) fabricated bybest thecomprehensive hybrid C/CNTs exhibited the (yield best 30H) fabricated (nanocomposite by the hybrid C/CNTs exhibited the tensile properties comprehensive tensiletensile properties (yield(656 strength (531 MPa), tensile (656the MPa), fracture strain strength (531 MPa), strength MPa), fracture strain strength (3.0%), and highest hardness (3.0%), and The the highest (331.2 HV). superior properties and abrasive wear (331.2 HV). superiorhardness tensile properties andThe abrasive weartensile resistance of the nanocomposite 30H resistance of the to nanocomposite 30H were attributed to the higher nano-TiC particles content, were attributed the higher nano-TiC particles content, better Orowan strengthening effects,better much Orowan strengthening effects,nano-TiC much more homogenously-dispersed nano-TiC particles, and more homogenously-dispersed particles, and excellent Al-TiC interface bonding. excellent Al-TiC interface bonding. Author Contributions: Y.-Y.G., F.Q. and Q.-C.J. conceived and designed the initial idea; Y.-Y.G., T.-S.L. and J.-G.C. Author Contributions: Y.-Y.G., F.Q. and Q.-C.J. conceived and designed theand initial Y.-Y.G., T.-S.L. and J.performed the experiments; Y.-Y.G. wrote the article manuscript; Y.-Y.G. F.Q.idea; analyzed and interpreted G.C. performed thedata; experiments; Y.-Y.G. wrote the article andQ.-C.J. F.Q. analyzed the experimental Y.-Y.G. and Q.-L.Z. collected andmanuscript; assembledY.-Y.G. data; and revised and the interpreted manuscript for experimental publication. data; Y.-Y.G. and Q.-L.Z. collected and assembled data; and Q.-C.J. revised the manuscript for the publication. Funding: This research is supported by the National Natural Science Foundation of China (NNSFC, No. 51571101 and No. 51771081), the Source Innovation Plan of Qingdao City, China (No. 18-2-2-1-jch), the Science and Funding: This research isProgram supported by Province, the National Natural Science Foundation of China (NNSFC, No. Technology Development of Jilin China (20170101178JC), and the Project 985-High Properties 51571101 No.University. 51771081), the Source Innovation Plan of Qingdao City, China (No. 18-2-2-1-jch), the Science Materialsand of Jilin and Technology Development Program of Jilin Province, China (20170101178JC), and the Project 985-High Conflicts of Interest: The authors declare that there is no conflict of interest regarding the publication of this paper. Properties Materials of Jilin University.
Conflicts of Interest: The authors declare that there is no conflict of interest regarding the publication of this paper. References 1.
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