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applied sciences Article Microstructure and Mechanical Properties of Magnesium Matrix Composites Interpenetrated by Different Reinforcement 1 1 , 1 1 2 Shuxu Wu , Shouren Wang *, Daosheng Wen , Gaoqi Wang and Yong Wang School of Mechanical Engineering, University of Jinan, Jinan 250022, China; Shuxu1994@gmail.com (S.W.); me_wends@ujn.edu.cn (D.W.); me_wanggq@ujn.edu.cn (G.W.) School of Physics and Technology, University of Jinan, Jinan 250022, China; ss_wangy@ujn.edu.cn * Correspondence: me_wangsr@ujn.edu.cn Received: 15 September 2018; Accepted: 19 October 2018; Published: 23 October 2018 Abstract: The present work discusses the microstructure and mechanical properties of the as-cast and as-extruded metal matrix composites interpenetrated by stainless steel (Fe–18Cr–9Ni), titanium alloy (Ti–6Al–4V), and aluminum alloy (Al–5Mg–3Zn) three-dimensional network reinforcement materials. The results show that the different reinforcement materials have different degrees of improvement on the microstructures and mechanical properties of the magnesium matrix composites. Among them, magnesium matrix composites interpenetrated by stainless steel reinforcement have maximum tensile strength, yield strength, and elongation, which are 355 MPa, 241 MPa, and 13%, respectively. Compared with the matrix, it increases by 47.9%, 60.7% and 85.7%, respectively. Moreover, compared with the as-cast state, the as-extruded sample has a relatively small grain size and a uniform size distribution. The grain size of the as-cast magnesium matrix composites is mainly concentrated at 200–300 m, whereas the extruded state is mainly concentrated at 10–30 m. The reason is that the coordination deformation of reinforcement and matrix, and the occurrence of dynamic recrystallization, cause grain refinement of magnesium matrix composite during the extrusion process, thereby improving its mechanical properties. Moreover, the improvement is attributed to the effect of the reinforcement itself, and the degree of grain refinement of the metal matrix composites. Keywords: microstructure; mechanical properties; interpenetrating composites; magnesium alloy; metal reinforcement; metal matrix composites 1. Introduction The metal matrix composites (MMCs) are a new type of structural material which is compounded by metal and alloy, as a matrix, through a certain process. The composite material has outstanding advantages, such as high specific modulus and specific strength, which is widely used in the fields of aviation, aerospace, and military protection [1,2]. In the area of the matrix, most metallic systems have been explored for use in metal matrix composites, including Al, Be, Ti, Mg, Fe, Ni, Co, and Ag, and, by far, the most mature technology is the preparation of aluminum matrix composites [3]. However, the traditional composite materials are usually reinforced by particles, fibers, and whiskers [4–6]. In recent years, with the requirement of the “structure–function” integration of composite materials and the development trend of increasing the volume fraction of the second phase particles, a new type of composite material has emerged, namely, the network interpenetrating structure of the reinforced the composite material. There is a new reinforcement method in which MMCs penetrate each other through three-dimensional network reinforcements, which have the mechanical characteristics of continuous enhancement, and the microstructure characteristics of intertwisting and interpenetrating with the Appl. Sci. 2018, 8, 2012; doi:10.3390/app8112012 www.mdpi.com/journal/applsci Appl. Sci. 2018, 8, 2012 2 of 14 matrix [7–9]. Since the matrix and reinforcement form a three-dimensional network structure in which the respective continuous and interpenetrating structures are formed in the space, the characteristics of each component constituting the network structure remain substantially unchanged, so its comprehensive reinforcement effect is generally better than the traditional reinforcement method, which makes it possible to obtain high-performance, multi-functional composite materials [10,11]. However, up to now, the metal matrix has been almost reinforced by ceramic, carbon nanotubes, or another brittle three-dimensional network reinforcement [12–14]. Due to the low toughness and shock resistance of brittle materials, these interpenetrating composites cannot undergo more machining deformation [15]. Particularly, in the case of fabricating structures having irregular cross-sectional shapes, their applications will be limited. In order to solve the above problems, the further development direction of the network interpenetrating metal matrix composites may be on the choice of the reinforcement materials, which can not only improve the strength of the composites, but also improve the plasticity [16]. Therefore, when metal is selected as a reinforcement for the composites, the metal matrix composites interpenetrated by metal reinforcement (MIMC) will have good forgeability and workability, which can be processed and deformed by multiple machining processes, such as torsion straining (TS), warm rolling (WR), twin-roll casting (TRC), and reciprocal extrusion (RE), etc. [17–19]. Among them, the extrusion process of the metal matrix composites can significantly improve the combined quality between matrix and reinforcement [20,21]. However, few researchers have studied the microstructure and mechanical properties of MIMC, especially magnesium matrix composites [22,23]. At the same time, magnesium and its alloy have the advantages of being lightweight, and having good casting performance, good damping, and shock absorbability, but their mechanical strength is poor [24,25]. Therefore, this article proposes a network interpenetrating bimetallic magnesium matrix composite using three metal-made network skeletons as reinforcements. This bimetallic magnesium matrix composite can not only make up for the deficiency of magnesium alloy in terms of strength and hardness, but also has a better toughness and absorbing properties as a metal material than ceramic materials. Therefore, the current work is mainly to manufacture the magnesium matrix composites interpenetrated by steel reinforcement, titanium reinforcement, and aluminum reinforcement and the subsequent extrusion process and, then, study the effects of different three-dimensional network reinforcement on the mechanical properties and microstructure of the magnesium matrix composites. 2. Materials and Methods 2.1. MIMC Composites Fabrication Previously, our team used a three-dimensional network of Si N ceramic structure and 3 4 pressure-assisted and vacuum-driven permeation technique to reinforce magnesium matrix composites (Si N –Mg) [26]. The preparation process was as follows: a porous ceramic skeleton was prepared 3 4 from high-purity -Si N powder (97% of Si N and less than 100 m in diameter, Shanghai Silicon 3 4 3 4 Materials Plant, Shanghai, China). The porous reticulated polyurethane (PU) was selected as the original framework, and the porous prefabricated parts were prepared through the replication process. Figure 1a shows the porous network of Si N ceramic skeleton after impregnation and sintering. Then, 3 4 it was heated in a nitrogen-filled muffle furnace (SQFL-1700, Shanghai, China) until it reached the desired processing temperature of 750 C, at which time, the liquid magnesium alloy was infiltrated into the preform skeleton by means of pressure-assisted and vacuum-driven permeation techniques. Figure 1b shows a Si N –Mg metal matrix composite, in which zone “1” is the Si N three-dimensional 3 4 3 4 network skeleton, and zone “2” is the Mg matrix. Figure 1c shows the schematic diagram of the infiltration device, and the mechanical properties of Si N –Mg matrix composite are shown in Table 1, 3 4 which indicates that the ceramic network reinforcement significantly enhances the elastic modulus, rockwell hardness, and tensile strength of the matrix, while the elongation is decreased [27,28]. Appl. Sci. 2018, 8, 2012 3 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 3 of 14 Figure 1. SEM micrographs image and technical diagram: (a) Si3N4 reticulated ceramic skeleton; (b) Figure 1. SEM micrographs image and technical diagram: (a) Si N reticulated ceramic skeleton; 3 4 Si3N4–Mg composite; (c) the schematic diagram of infiltration equipment. (b) Si N –Mg composite; (c) the schematic diagram of infiltration equipment. 3 4 Table 1. The mechanical properties of Mg alloy and Si N –Mg composite. 3 4 Table 1. The mechanical properties of Mg alloy and Si3N4–Mg composite. Elastic Module Rockwell Hardness Elongation Tensile Strength Elastic Module Rockwell Hardness Elongation Tensile Strength Materials Materials (GPa) (HRB) (%) (MPa) (GPa) (HRB) (%) (MPa) Mg alloy 70 65 9.5 330 Mg alloy 70 65 9.5 330 12Si N –Mg 110 71 3.2 345 3 4 12Si3N4–Mg 110 71 3.2 345 25Si N –Mg 133 78 1.6 340 3 4 25Si3N4–Mg 133 78 1.6 340 Recently, however, our team tried a new and simple process to fabricate the magnesium matrix Recently, however, our team tried a new and simple process to fabricate the magnesium matrix composites. The network skeleton of the reinforcement designed by three-dimensional weaving composites. The network skeleton of the reinforcement designed by three-dimensional weaving technology was shown in Figure 2a, and the model of the metal matrix composite of the infiltrated technology was shown in Figure 2a, and the model of the metal matrix composite of the infiltrated reinforcement was shown in Figure 2b. The reinforcement skeleton materials were chosen as stainless reinforcement was shown in Figure 2b. The reinforcement skeleton materials were chosen as stainless steel (Fe–18Cr–9Ni), titanium alloy (Ti–6Al–4V), and aluminum alloy (Al–5Mg–3Zn), respectively, steel (Fe–18Cr–9Ni), titanium alloy (Ti–6Al–4V), and aluminum alloy (Al–5Mg–3Zn), respectively, while magnesium matrix was selected as AZ31(Mg–3.31Al–1.05Zn). The skeleton was fabricated using while magnesium matrix was selected as AZ31(Mg–3.31Al–1.05Zn). The skeleton was fabricated the three-dimensional weaving techniques, and measured by Archimedes measurements (ASTM C373), using the three-dimensional weaving techniques, and measured by Archimedes measurements with a reinforcement volume fraction of approximately 15%. Unlike the preparation of Si N –Mg 3 4 (ASTM C373), with a reinforcement volume fraction of approximately 15%. Unlike the preparation matrix composites, the MIMC composites’ fabrication processing was applied pressure infiltration of Si3N4–Mg matrix composites, the MIMC composites’ fabrication processing was applied pressure technology, which is shown in Figure 2c. The entire experiment was carried out under an inert gas infiltration technology, which is shown in Figure 2c. The entire experiment was carried out under an argon atmosphere. Firstly, in the inert atmosphere of a mixture of CO and SF , the furnace temperature 2 6 inert gas argon atmosphere. Firstly, in the inert atmosphere of a mixture of CO2 and SF6, the furnace was set to 720 C to melt the AZ31 alloy. Then, the molten magnesium alloy liquid was poured into temperature was set to 720 °C to melt the AZ31 alloy. Then, the molten magnesium alloy liquid was an infiltration mold having a temperature of 650 C and, finally, the pressure head started to be poured into an infiltration mold having a temperature of 650 °C and, finally, the pressure head started pressed. At last, the magnesium matrix composites interpenetrated by stainless steel reinforcement to be pressed. At last, the magnesium matrix composites interpenetrated by stainless steel (MISC), the magnesium matrix composites interpenetrated by titanium alloy reinforcement (MITC), reinforcement (MISC), the magnesium matrix composites interpenetrated by titanium alloy and the magnesium matrix composites interpenetrated by aluminum alloy reinforcement (MIAC), reinforcement (MITC), and the magnesium matrix composites interpenetrated by aluminum alloy were fabricated successfully. reinforcement (MIAC), were fabricated successfully. 2.2. The Extrusion Process The diameter of the extruded blank was machined to 59 mm prior to extrusion of the metal matrix composite. Under the temperature of 300 C, the billet was extruded at a speed of 2 mm/s with an extrusion ratio of 30, and a half-angle of the extrusion die of 30 , as shown as in Figure 3a. The geometric model of extrusion die was shown in Figure 3b. The extruded material was immediately quenched to prevent the grain from growing. Appl. Sci. 2018, 8, x FOR PEER REVIEW 4 of 14 Appl. Sci. 2018, 8, 2012 4 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 4 of 14 Figure 2. Three-dimensional model image and technical diagram: (a) reinforcement; (b) MIMC composites; (c) the pressure infiltration technology. 2.2. The Extrusion Process The diameter of the extruded blank was machined to 59 mm prior to extrusion of the metal matrix composite. Under the temperature of 300 °C, the billet was extruded at a speed of 2 mm/s with an extrusion ratio of 30, and a half-angle of the extrusion die of 30°, as shown as in Figure 3a. The Figure Figure 2. 2. Thr Thr eee-dimensional e-dimensional m model odel imag image e and and tec technical hnical di diagram: agram: (( aa )) reinforcement; reinforcement; (( b b) ) M MIMC IMC geometric model of extrusion die was shown in Figure 3b. The extruded material was immediately co composites; mposites; ((c c)) the pres the pressur sure i e infiltration nfiltration ttechnology echnology.. quenched to prevent the grain from growing. 2.2. The Extrusion Process The diameter of the extruded blank was machined to 59 mm prior to extrusion of the metal matrix composite. Under the temperature of 300 °C, the billet was extruded at a speed of 2 mm/s with an extrusion ratio of 30, and a half-angle of the extrusion die of 30°, as shown as in Figure 3a. The geometric model of extrusion die was shown in Figure 3b. The extruded material was immediately quenched to prevent the grain from growing. Figure 3. The schematic diagram of extrusion process: (a) pressure infiltration processing of the Figure 3. The schematic diagram of extrusion process: (a) pressure infiltration processing of the extrusion process; (b) 1/4 extrusion die of matrix composites interpenetrated by metal reinforcement extrusion process; (b) 1/4 extrusion die of matrix composites interpenetrated by metal reinforcement (MIMC) composites. (MIMC) composites. 2.3. Microstructure Characterization 2.3. Microstructure Characterization The samples were mechanically polished using a polycrystalline diamond suspension ethylene The samples were mechanically polished using a polycrystalline diamond suspension glycol organic solution for observation of the optical microstructure (OM, Keyence VW-5000, Osaka, ethylene glycol organic solution for observation of the optical microstructure (OM, Keyence VW- Japan). Then, the samples were subjected to etching in a solution consisting of acetic acid (5 mL), Figure 3. The schematic diagram of extrusion process: (a) pressure infiltration processing of the 5000, Osaka, Japan). Then, the samples were subjected to etching in a solution consisting of acetic picric acid (5 g), ethanol (100 mL), and distilled water (10 mL), for 7 s, to reveal the crystal structure. extrusion process; (b) 1/4 extrusion die of matrix composites interpenetrated by metal reinforcement acid (5 mL), picric acid (5 g), ethanol (100 mL), and distilled water (10 mL), for 7 s, to reveal the The average grain size was analyzed by the Image Pro Plus (IPP, Media Cybernetics, Rockville, MD, (MIMC) composites. crystal structure. The average grain size was analyzed by the Image Pro Plus (IPP, Media USA). In addition, the EBSD samples were prepared by mechanical polishing using 2000# sandpaper Cybernetics, Rockville, MD, USA). In addition, the EBSD samples were prepared by mechanical and, then, by electric polishing in an electrolyte consisting of 400 mL butyl glycol (C H O , 99.5%), 2.3. Microstructure Characterization 4 10 2 polishing using 2000# sandpaper and, then, by electric polishing in an electrolyte consisting of 400 80 mL ethanol (C H O, 95%), and 40mL perchloric acid (HClO , 70%), at a voltage of 11 V for 2 6 4 mL butyl glycol (C4H10O2, 99.5%), 80 mL ethanol (C2H6O, 95%), and 40mL perchloric acid (HClO4, The samples were mechanically polished using a polycrystalline diamond suspension 120 s. Microstructure and morphology of MIMC composites were investigated by scanning electron 70%), at a voltage of 11 V for 120 s. Microstructure and morphology of MIMC composites were ethylene glycol organic solution for observation of the optical microstructure (OM, Keyence VW- microscopy (SEM, Hitachi S-4800, Tokyo, Japan), and the elemental composition of the samples was investigated by scanning electron microscopy (SEM, Hitachi S-4800, Tokyo, Japan), and the 5000, Osaka, Japan). Then, the samples were subjected to etching in a solution consisting of acetic determined by the energy dispersive spectroscopy (EDS, Oxford Instruments Inca Energy 350, Oxford, elemental composition of the samples was determined by the energy dispersive spectroscopy acid (5 mL), picric acid (5 g), ethanol (100 mL), and distilled water (10 mL), for 7 s, to reveal the UK), as well as grain distribution and diameter measurements, which were determined using electron (EDS, Oxford Instruments Inca Energy 350, Oxford, UK), as well as grain distribution and diameter crystal structure. The average grain size was analyzed by the Image Pro Plus (IPP, Media backscatter diffraction (EBSD, Oxford Instruments NordlysMax2, Oxford, UK). measurements, which were determined using electron backscatter diffraction (EBSD, Oxford Cybernetics, Rockville, MD, USA). In addition, the EBSD samples were prepared by mechanical Instruments NordlysMax2, Oxford, UK). polishing using 2000# sandpaper and, then, by electric polishing in an electrolyte consisting of 400 2.4. Mechanical Properties Test mL butyl glycol (C4H10O2, 99.5% ), 80 mL ethanol (C2H6O, 95%), and 40mL perchloric acid (HClO4, The extruded samples used for tensile testing were processed on a CNC lathe (CJK6130L, Shanghai, 70%), at a voltage of 11 V for 120 s. Microstructure and morphology of MIMC composites were China), in accordance to the procedure outlined in American Society for Testing and Materials (ASTM investigated by scanning electron microscopy (SEM, Hitachi S-4800, Tokyo, Japan), and the E8M-96). There were no obvious processing marks on the surface of the test piece, nor were there any elemental composition of the samples was determined by the energy dispersive spectroscopy signs of breaking nucleation. The mechanical properties of the samples were tested using an Instron (EDS, Oxford Instruments Inca Energy 350, Oxford, UK), as well as grain distribution and diameter 5569 testing machine (Instron, Shanghai, China) with a crosshead moving speed of 0.1 mm/min, measurements, which were determined using electron backscatter diffraction (EBSD, Oxford and the strain was monitored by a strain gage of 20 mm in length. At the same time, the test Instruments NordlysMax2, Oxford, UK). Appl. Sci. 2018, 8, x FOR PEER REVIEW 5 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 5 of 14 2.4. Mechanical Properties Test 2.4. Mechanical Properties Test The extruded samples used for tensile testing were processed on a CNC lathe (CJK6130L, The extruded samples used for tensile testing were processed on a CNC lathe (CJK6130L, Shanghai, China), in accordance to the procedure outlined in American Society for Testing and Shanghai, China), in accordance to the procedure outlined in American Society for Testing and Materials (ASTM E8M-96). There were no obvious processing marks on the surface of the test piece, Materials (ASTM E8M-96). There were no obvious processing marks on the surface of the test piece, nor were there any signs of breaking nucleation. The mechanical properties of the samples were nor were there any signs of breaking nucleation. The mechanical properties of the samples were tested using an Instron 5569 testing machine (Instron, Shanghai, China) with a crosshead moving tested using an Instron 5569 testing machine (Instron, Shanghai, China) with a crosshead moving Appl. Sci. 2018, 8, 2012 5 of 14 speed of 0.1 mm/min, and the strain was monitored by a strain gage of 20 mm in length. At the same speed of 0.1 mm/min, and the strain was monitored by a strain gage of 20 mm in length. At the same time, the test comparisons of the AZ31 magnesium alloy were carried out, and each tensile value was time, the test comparisons of the AZ31 magnesium alloy were carried out, and each tensile value was the average of at least three measurements. the average of at least three measurements. comparisons of the AZ31 magnesium alloy were carried out, and each tensile value was the average of at least three measurements. 3. Results 3. Results 3. Results 3.1. Microstructure 3.1. Microstructure 3.1. Microstructure Figure 4 shows the surface microstructure and cross-section characteristics of MIMC composites. Figure 4 shows the surface microstructure and cross-section characteristics of MIMC composites. From Figur Figure e 4 4a, shows the the matr surface ix and micr reinostr forcuctur emene t and are interp cross-section enetrating characteristics , anisotropicof , and MIMC interwo composites. ven. In From Figure 4a, the matrix and reinforcement are interpenetrating, anisotropic, and interwoven. In add From ition, Figur in ethe 4a,long theitud matrix inal and direct reinfor ion, a cement portion ar of e th interpenetrating, e structure of the anisotr interpen opic, etrating and interwoven. network of addition, in the longitudinal direction, a portion of the structure of the interpenetrating network of reinf In addition, orcemen in tsthe is exp longitudinal osed from dir thection, e matrix a portion (white ci of rcles the )str , auctur nd ano e of ther thepo interpenetrating rtion of the reinf network orcemen of t reinforcements is exposed from the matrix (white circles), and another portion of the reinforcement is reinfor wrapped cements and is exposed buried by from magne the matrix sium matrix. (white cir Only cles), a and fewanother are exp por osed tion from of the thr e einfor matri cement x in this e is wrapped and buried by magnesium matrix. Only a few are exposed from the matrix in the wrapped transverse and direct buried ion (b by lamagnesium ck arrow). In matrix. addition, Only the a few matrix are exposed and reinffr orcem om the ent matrix form in a good the transverse interface transverse direction (black arrow). In addition, the matrix and reinforcement form a good interface com direction bination, (blac as k arr shown ow). as In iaddition, n Figure 4b. theF matrix urtherm and ore, reinfor the di cement stributio form n of ath good e chem interface ical element combination, s of the combination, as shown as in Figure 4b. Furthermore, the distribution of the chemical elements of the sa asmp shown les are as in examine Figured 4b. by Furthermor EDS, and e,subject the distribution ed to line of sc the anni chemical ng, as shown elements as of in the Fig samples ure 5. T ar he e samples are examined by EDS, and subjected to line scanning, as shown as in Figure 5. The reinf examined orcemby ents EDS, of thand e circular subjected area to are line staiscanning, nless steel as (cyan shown line as in in Figure Figur 5a e), 5.titan The iurm einfor alloy cements (blue line of reinforcements of the circular area are stainless steel (cyan line in Figure 5a), titanium alloy (blue line in theFcir igure cular 5b) ar , ea and ar alumin e stainless um alloy steel (cyan (cyan line line in in Figur Figure e 5c 5a), ), re titanium spectively. alloy Th (blue e magn line esium in Figur matrix e 5b), is in Figure 5b), and aluminum alloy (cyan line in Figure 5c), respectively. The magnesium matrix is represent and aluminum ed as a alloy red l(cyan ine inline the in MISC Figur an ed 5c), MIAC respectively composi . tes The , how magnesium ever, it ismatrix described is repr as esented a green as line a represented as a red line in the MISC and MIAC composites, however, it is described as a green line in MITC red line in com thepo MISC site. and MIAC composites, however, it is described as a green line in MITC composite. in MITC composite. Figure 4. SEM micrograph of MIMC composites: (a) the surface microstructure; (b) cross-section of Figure Figure 4. 4. SEM SEM micr microg ograph raph of of MIMC MIMC composites: composites: ( (a a) ) the the surface surface micr microstruc ostructur ture e; ; ( (b b) ) cr cross oss-section -section of of reinforcement with matrix. reinforcement wi reinforcement with th matrix matrix.. Figure 5. The energy dispersive spectroscopy (EDS) analysis of MIMC composites: (a) magnesium matrix composites interpenetrated by stainless steel reinforcement (MISC); (b) magnesium matrix composites interpenetrated by titanium alloy reinforcement (MITC); (c) magnesium matrix composites interpenetrated by aluminum alloy reinforcement (MIAC). Figure 6 shows the OM microstructure morphology and grain size distribution of magnesium matrix in three kinds of composite as-cast states. In MIMC composites, their grain distribution and grain size have the same characteristics, that is, the grain distribution does not obey a normal Appl. Sci. 2018, 8, 2012 6 of 14 distribution and is randomly distributed. In addition, the grain size is mainly concentrated in the range 200–300 m. Therefore, the results show that the grain and its area fraction are not affected by any of the reinforcement materials. However, compared with the as-cast state (Figure 6a,c,e), the micromorphology of the as-extruded samples has greater changes, which are shown in Figure 7a,c,e. The relatively small grain size of the as-extruded samples is owing to the accumulation of shear strain and dynamic recrystallization during extrusion. However, the grain refinement degree is different in three kinds of composites. In MISC composites, it can be seen, from Figure 7a, that the grain size follows a normal distribution. Moreover, most of the grain size is 10–20 m, so the average grain size is 14 m. In MITC composites, although the grain size does not conform to the normal distribution (Figure 7d), most of them are concentrated between 15–30 m. Therefore, the average grain size is 20 m. In MIAC composites, the grain size adheres to the Weibull distribution (Figure 7f), and most of them are concentrated between 20–30 m. The average grain size is 24 m. In short, the different reinforcement materials result in different microstructure characterization of magnesium matrix during deformation. The reason is that, due to the different strengths of reinforcement, the magnesium matrix bears a different stress from the reinforcement during extrusion. As we know, magnesium matrix alloys usually form a strong texture, resulting in the decreases of ductility at room temperature because of their intrinsic characterization of the hexagonal close-packed structure [29]. Since the room temperature-forming properties of the magnesium alloys are mainly affected by the initial crystal structure of the basal plane, the improvement of the crystal grains will significantly improve the formability of the MIMC composites [30]. In MISC composites, the three-dimensional network of stainless-steel has the highest strength, which leads to greater stress on magnesium grains, thus causing a till of the basal plane during coordinated deformation, and a minimum average grain size. Therefore, the dynamic recrystallization occurs in the vicinity of the reinforcement of magnesium matrix composite. Furthermore, the difference between size distribution and grain refinement can be explained by the changes in the grain orientation of magnesium matrix composite by EBSD test. Figure 8a shows that the grain orientation of the as-cast magnesium matrix composite (MIMC) is almost randomly distributed. Figure 8b–d reveal the grain orientation changes of the as-extruded magnesium matrix composite. From Figure 8b (MISC), the results show that during the extrusion, the grain orientation forms a strong peak at the center of the basal pole figure of {0001}. However, in the MIAC composites, {0001} basal pole figure exhibits a divergence state, due to a relatively small stress for the aluminum alloy imposed to magnesium matrix, as shown as in Figure 8d. From Figure 8c (MITC), it is shown that the grain orientation is between MISC and MIAC. 3.2. Mechanical Properties The MIMC composites exhibit different mechanical properties because of the difference of reinforcement materials. Figure 9 shows the mechanical properties change with different reinforcement materials. Compared with AZ31 magnesium alloy, the MIMC composites have a significant improvement in the yield strength (YS), ultimate tensile strength (UTS), and elongation (E). The improvement in mechanical performance is attributed to the following as (1) superior mechanical properties of the reinforcement itself; (2) the reinforcements have a good interface with the matrix; (3) effective load transfer can be carried out from matrix to reinforcement; and (4) fine and evenly distributed grain are produced during coordination deformation of the reinforcement and matrix. Appl. Sci. 2018, 8, 2012 7 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 7 of 14 Figure 6. The optical microstructure and the grain size distributions of magnesium matrix composite Figure 6. The optical microstructure and the grain size distributions of magnesium matrix composite in three kinds of reinforcement as-cast states: (a,b) MISC; (c,d) MITC; (e,f) MIAC. in three kinds of reinforcement as-cast states: (a,b) MISC; (c,d) MITC; (e,f) MIAC. Appl. Sci. 2018, 8, 2012 8 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 8 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 8 of 14 Figure 7. The SEM and the grain size distributions of magnesium matrix composite in three kinds of Figure 7. The SEM and the grain size distributions of magnesium matrix composite in three kinds of Figure 7. The SEM and the grain size distributions of magnesium matrix composite in three kinds of reinforcement as-extruded states: (a,b) MISC; (c,d) MITC; (e,f) MIAC. reinforcement as-extruded states: (a,b) MISC; (c,d) MITC; (e,f) MIAC. reinforcement as-extruded states: (a,b) MISC; (c,d) MITC; (e,f) MIAC. Figure 8. The {0001} basal pole figures: (a) cast states of MIMC; (b) extruded state of MISC; (c) Figure 8. The {0001} basal pole figures: (a) cast states of MIMC; (b) extruded state of MISC; (c) Figure 8. The {0001} basal pole figures: (a) cast states of MIMC; (b) extruded state of MISC; (c) extruded extruded state of MITC; (d) extruded state of MIAC. extruded state of MITC; (d) extruded state of MIAC. state of MITC; (d) extruded state of MIAC. 3.2. Mechanical Properties 3.2. Mechanical Properties The MIMC composites exhibit different mechanical properties because of the difference of The MIMC composites exhibit different mechanical properties because of the difference of reinforcement materials. Figure 9 shows the mechanical properties change with different reinforcement materials. Figure 9 shows the mechanical properties change with different reinforcement materials. Compared with AZ31 magnesium alloy, the MIMC composites have a reinforcement materials. Compared with AZ31 magnesium alloy, the MIMC composites have a significant improvement in the yield strength (YS), ultimate tensile strength (UTS), and elongation significant improvement in the yield strength (YS), ultimate tensile strength (UTS), and elongation Appl. Sci. 2018, 8, x FOR PEER REVIEW 9 of 14 (E). The improvement in mechanical performance is attributed to the following as (1) superior mechanical properties of the reinforcement itself; (2) the reinforcements have a good interface with the matrix; (3) effective load transfer can be carried out from matrix to reinforcement; and (4) fine and evenly distributed grain are produced during coordination deformation of the reinforcement and matrix. Among the three kinds of composites, the MISC composites have the maximum values of UTS (Figure 9a), YS (Figure 9b), and E (Figure 9c), which are 355 MPa, 241 MPa, and 13%. For each parameter, comparing with the AZ31, the increase is 47.9%, 60.7%, and 85.7%, respectively, while the MITC composites followed, the mechanical properties are 340 MPa, 220 MPa, and 12%, increasing by 41.7%, 46.7%, and 71.4%, respectively. The MIAC composites are the minimum, the mechanical properties of which are 280 MPa, 175 MPa, and 8%, increasing by 16.7%, 16.7%, and 14.3%, respectively. These changes are ascribed to two factors. One is the influence of reinforcement itself, and the mechanical properties of the three network reinforcements are shown in Table 2. Another is Appl. Sci. 2018, 8, 2012 9 of 14 the influence of the grain refinement degree of matrix alloy. Figure 9. The mechanical properties of AZ31, MISC, MITC, and MIAC: (a) UTS; (b) YS; (c) E. Figure 9. The mechanical properties of AZ31, MISC, MITC, and MIAC: (a) UTS; (b) YS; (c) E. Among the thr Table ee kinds 2. The m of composites, echanical prop the ertie MISC s of the composites three network have reinforcemen the maximum ts. values of UTS (Figure 9a), YS (Figure 9b), and E (Figure 9c), which are 355 MPa, 241 MPa, and 13%. For each Tensile Strength Yield Strength Elongation Materials parameter, comparing with the AZ31, the increase is 47.9%, 60.7%, and 85.7%, respectively, while the (MPa) (MPa) (%) MITC composites followed, the mechanical properties are 340 MPa, 220 MPa, and 12%, increasing Fe–18Cr–9Ni 893 824 36 by 41.7%, 46.7%, and 71.4%, respectively. The MIAC composites are the minimum, the mechanical Ti–6Al–4V 790 710 21 properties of which are 280 MPa, 175 MPa, and 8%, increasing by 16.7%, 16.7%, and 14.3%, respectively. Al–5Mg–3Zn 542 520 11 These changes are ascribed to two factors. One is the influence of reinforcement itself, and the mechanical properties of the three network reinforcements are shown in Table 2. Another is the 4. Discussions influence of the grain refinement degree of matrix alloy. The reinforcement and matrix of MIMC composites are regarded as two interpenetrating pore structures or network structures, which are shown in Figure 10a. Owing to that one kind of metal Table 2. The mechanical properties of the three network reinforcements. phase is interpenetrated by another metal phase, the mechanical models of the network structure of Tensile Strength Yield Strength Elongation MIMC composites does not follow the brittle fracture mode which is shown in Figure 10b, it follows Materials (MPa) (MPa) (%) the elastic plastic mode which is shown in Figure 10c, and this deformation mode is the main failure Fe–18Cr–9Ni 893 824 36 mode of MIMC composites [31,32]. Considering the linear elastic elements, the elastic modulus of Ti–6Al–4V 790 710 21 interpenetrating composites is estimated as Equation (1), according to the mixing rule Al–5Mg–3Zn 542 520 11 E =E V +E V , (1) C M M R R 4. Discussions where EC, EM, and ER are, respectively, the elastic modulus of composites (C), matrix (M), and reinforcement (R), and VM and VR are, respectively, the volume fraction of matrix and reinforcement. The reinforcement and matrix of MIMC composites are regarded as two interpenetrating pore structures or network structures, which are shown in Figure 10a. Owing to that one kind of metal phase is interpenetrated by another metal phase, the mechanical models of the network structure of MIMC composites does not follow the brittle fracture mode which is shown in Figure 10b, it follows the elastic plastic mode which is shown in Figure 10c, and this deformation mode is the main failure mode of MIMC composites [31,32]. Considering the linear elastic elements, the elastic modulus of interpenetrating composites is estimated as Equation (1), according to the mixing rule E = E V +E V , (1) C M M R R where E , E , and E are, respectively, the elastic modulus of composites (C), matrix (M), C M R and reinforcement (R), and V and V are, respectively, the volume fraction of matrix M R and reinforcement. Appl. Sci. 2018, 8, 2012 10 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 10 of 14 Figure 10. The mechanical model of network structure: (a) the unit model; (b) the brittle model; (c) Figure 10. The mechanical model of network structure: (a) the unit model; (b) the brittle model; (c) the the elastic plastic model. elastic plastic model. Considering the elastic modulus influence, the constitutive mechanical mode of MIMC is proposed Considering the elastic modulus influence, the constitutive mechanical mode of MIMC is according to mixture law of composites, as shown in Equations (2) and (3). proposed according to mixture law of composites, as shown in Equations (2) and (3). Upper limit model: E X =∑ E X V , (2) C C i=1 i i i Upper limit model : E X = E X V , (2) C C å i i i i=1 E E V C i i Lower limit model: = , (3) i=1 X X C i E E V C i i Lower limit model : = , (3) where XC represents the mechanical properties of composite materials, and Xi and Vi represent the X X i=1 mechanical properties and volume fractions of different composite phase, respectively. For two where X represents the mechanical properties of composite materials, and X and V represent the phases C interpenetrating composites, the mechanical properties, such as tensile strength, yield i i mechanical properties and volume fractions of different composite phase, respectively. For two strength, and elongation, are rewritten as Equations (4)–(7), according to the above equations, phases interpenetrating composites, the mechanical properties, such as tensile strength, yield strength, E σ =E V σ +E V σ , (4) C C M M M R R R and elongation, are rewritten as Equations (4)–(7), according to the above equations, E V V C M R E s = E =EV s ++ E E V, s , (5) (4) C C M MM M R R R R σ σ σ C M R E V V C M R = E + E , (5) M R (6) E δ =E V δ +E V δ , C C M M M R R R s s s M R E d = E V d + E V d , (6) C C E M MVM V R R R C M R =E +E , (7) M R E V V δ δ δ C M R C M R = E + E , (7) M R d d d C M R where σ and V represent, respectively, the tensile strength or yield strength and volume fractions of where s and V represent, respectively, the tensile strength or yield strength and volume fractions the matrix (M) and reinforcement (R), and δ represents the elongation of the matrix (M) and of the matrix (M) and reinforcement (R), and d represents the elongation of the matrix (M) and reinforcement (R). reinforcement (R). Combining Equation (1) to Equations (4)–(7), the following Equations (8)–(11) are obtained: Combining Equation (1) to Equations (4)–(7), the following Equations (8)–(11) are obtained: E E M R Upper limit model: σ = V σ + V σ , (8) C M M R R E V +E V E V +E V M M R R M M R R E E M R Upper limit model : s = V s + V s , (8) C M M R R 1 E V E V E V + E VM M E V R + E R V M M R R M M R R Lower limit model: = + , (9) σ E V +E V σ E V +E V σ C M M R R M M M R R R 1 E V E V M M R R Lower limit model : = + , (9) E E M R s E V + E V s E V + E V s Upper limit model: δ = V δ + V δ , C M M R R M M M R R R (10) C M M R R E V +E V E V +E V M M R R M M R R E E M R Upper limit model : d = V d + V d , (10) C M M R R 1 E V E V M M R R E V + E V E V + E V Lower limit model: M M = R R + M M .R R (11) δ E V +E V δ E V +E V δ C M M R R M M M R R R 1 E V E V M M R R Lower limit model : = + . (11) According to the above mathematics model, the relationship between volume fraction and d E V + E V d E V + E V d C M M R R M M M R R R tensile strength of magnesium matrix composites interpenetrated by different reinforcement is According to the above mathematics model, the relationship between volume fraction and tensile shown in Figure 11. The results show that as the volume fraction of reinforcement increases, the strength of magnesium matrix composites interpenetrated by different reinforcement is shown in continuous improving trend of tensile strength is more obvious. Similarly, the yield strength and Figure 11. The results show that as the volume fraction of reinforcement increases, the continuous elongation also have the same regularity. Compared with the tested results in Figure 9, the results of improving trend of tensile strength is more obvious. Similarly, the yield strength and elongation also the mathematics model are the same. Therefore, it can be considered that the mathematics model of Appl. Sci. 2018, 8, 2012 11 of 14 Appl. Sci. 2018, 8, x FOR PEER REVIEW 11 of 14 have the same regularity. Compared with the tested results in Figure 9, the results of the mathematics model are the same. Therefore, it can be considered that the mathematics model of the composite the composite material, derived from this paper, is correct and provides a good theoretical guidance material, derived from this paper, is correct and provides a good theoretical guidance for the test. for the test. Figure 11. The relationship between tensile strength and volume fraction of magnesium matrix Figure 11. The relationship between tensile strength and volume fraction of magnesium matrix composites interpenetrated by different reinforcement. composites interpenetrated by different reinforcement. 5. Conclusions 5. Conclusions 1. The magnesium matrix composites reinforced by stainless steel (Fe–18Cr–9Ni), titanium alloy 1. The magnesium matrix composites reinforced by stainless steel (Fe–18Cr–9Ni), titanium alloy (Ti–6Al–4V), and aluminum alloy (Al–5Mg–3Zn), were prepared by the pressure infiltration technology. (Ti–6Al–4V), and aluminum alloy (Al–5Mg–3Zn), were prepared by the pressure infiltration The reinforcements of the composites are interwoven with the matrix and have an integrated interface. technology. The reinforcements of the composites are interwoven with the matrix and have an 2. The grain size and distribution in the as-cast magnesium matrix composites have the same integrated interface. characteristics, and their sizes are mainly concentrated at 200–300 m, and the size distribution is 2. The grain size and distribution in the as-cast magnesium matrix composites have the same random and does not obey normal distribution. However, during the extrusion process, the grain size characteristics, and their sizes are mainly concentrated at 200–300 μm, and the size distribution is of magnesium matrix composite is more refined than that of the as-cast state, because of the dynamic random and does not obey normal distribution. However, during the extrusion process, the grain recrystallization and the superposition of shear strain, and its size is mostly concentrated at 10–30 m. size of magnesium matrix composite is more refined than that of the as-cast state, because of the In addition, the grain size distributions of MISC and MIAC follow the normal distribution and the dynamic recrystallization and the superposition of shear strain, and its size is mostly concentrated at Wien distribution, respectively. 10–30 μm. In addition, the grain size distributions of MISC and MIAC follow the normal distribution 3. Different reinforcement materials result in different microstructure characterization of and the Wien distribution, respectively. magnesium matrix during extrusion. The average grain sizes of magnesium matrix composites 3. Different reinforcement materials result in different microstructure characterization of with the reinforcements of MISC, MITC, and MIAC are 14, 20, and 24 m, respectively. magnesium matrix during extrusion. The average grain sizes of magnesium matrix composites with 4. Compared with AZ31, the mechanical properties of metal composites interpenetrated by the reinforcements of MISC, MITC, and MIAC are 14, 20, and 24 μm, respectively. metal reinforcement have a significant improvement. Different MIMCs with different reinforcements 4. Compared with AZ31, the mechanical properties of metal composites interpenetrated by exhibit different mechanical properties. Among the three composite materials, the tensile strength, metal reinforcement have a significant improvement. Different MIMCs with different reinforcements yield strength, and elongation of MISC are 355 MPa, 241 MPa, and 13%, with an increase of 47.9%, exhibit different mechanical properties. Among the three composite materials, the tensile strength, 60.7%, and 85.7%, respectively; while for MITC, they are 340 MPa, 220 MPa, and 12%, with an increase yield strength, and elongation of MISC are 355 MPa, 241 MPa, and 13%, with an increase of 47.9%, of 41.7%, 46.7%, and 71.4%, respectively; and for MIAC, are 280 MPa, 175 MPa, and 8%, an increase of 60.7%, and 85.7%, respectively; while for MITC, they are 340 MPa, 220 MPa, and 12%, with an increase 16.7%, 16.7%, and 14.3%, respectively. of 41.7%, 46.7%, and 71.4%, respectively; and for MIAC, are 280 MPa, 175 MPa, and 8%, an increase of 16.7%, 16.7%, and 14.3%, respectively. Author Contributions: S.W. (Shouren Wang) wrote the main part of the manuscript and developed the planning of the experiment. S.W. (Shuxu Wu) and Y.W. carried out the preparation of different composite materials and Author Contributions: S.W. (Shouren Wang) wrote the main part of the manuscript and developed the planning tested the mechanical properties. D.W. and G.W. performed characterization of the microstructure of the samples. of the experiment. S.W. (Shuxu Wu) and Y.W. carried out the preparation of different composite materials and S.W. (Shouren Wang) summed up the article and conducted a final review. S.W. (Shuxu Wu) made the final typesetting of the article. tested the mechanical properties. D.W. and G.W. performed characterization of the microstructure of the samples. S.W. (Shouren Wang) summed up the article and conducted a final review. S.W. (Shuxu Wu) made the final typesetting of the article. Funding: This research was funded by the National Natural Science Foundation of China (No. 51872122), Shandong Key Research and Development Plan, China (No.: 2017GGX30140, 2016JMRH0218) Shandong Provincial Natural Science Foundation, China (No.: ZR2017BEE055), Distinguished Middle-Aged and Young Appl. Sci. 2018, 8, 2012 12 of 14 Funding: This research was funded by the National Natural Science Foundation of China (No. 51872122), Shandong Key Research and Development Plan, China (No.: 2017GGX30140, 2016JMRH0218) Shandong Provincial Natural Science Foundation, China (No.: ZR2017BEE055), Distinguished Middle-Aged and Young Scientist Encourage and Reward Foundation of Shandong Province (No.: ZR2016EMB01) and Taishan Scholar Engineering Special Funding (2016–2020). Conflicts of Interest: The authors declare no conflict of interest. Nomenclature MMCs metal matrix composites MIMC metal matrix composites interpenetrated by metal reinforcement MISC magnesium matrix composites interpenetrated by stainless steel reinforcement MITC magnesium matrix composites interpenetrated by titanium alloy reinforcement MIAC magnesium matrix composites interpenetrated by aluminum alloy reinforcement WR warm rolling TS torsion straining TRC twin-roll casting RE reciprocal extrusion OM optical microstructure SEM scanning electron microscopy EDS energy dispersive spectroscopy EBSD electron backscatter diffraction CNC computer numerical control YS yield strength UTS ultimate tensile strength E elongation E , E and E the elastic modulus of composites, matrix, and reinforcement C M R V and V the volume fraction of matrix and reinforcement M R X the mechanical properties of composite materials X and V the mechanical properties and volume fractions of different composite phase i i s and V the tensile strength or yield strength and volume fractions of the matrix and reinforcement d the elongation of the matrix and reinforcement References 1. 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Applied Sciences – Multidisciplinary Digital Publishing Institute
Published: Oct 23, 2018
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