Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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nanomaterials Article Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy Bo-Chin Huang and Fei-Yi Hung * Department of Materials Science and Engineering, National Cheng Kung University, Tainan 701, Taiwan; frt4y6asd@gmail.com * Correspondence: fyhung@mail.ncku.edu.tw Abstract: This study investigated the microstructure, mechanical properties, impact toughness, and erosion characteristics of Al-10Si-Mg alloy specimens manufactured using the selective laser melting (SLM) method with or without subsequent T6 heat treatment. Furthermore, the erosion phase transformation behavior of the test specimens was analyzed, and the effect of the degradation mechanism on the tensile mechanical properties and impact toughness of the SLM Al-10Si-Mg alloy specimens before and after particle erosion was compared. The experimental results indicated that the Al-10Si-Mg alloy subjected to T6 heat treatment has better erosion resistance than the as-fabricated material. The tensile strength and fracture toughness of both specimen groups decreased due to the formation of microcracks on the surface caused by particle erosion. Nevertheless, the erosion-induced silicon nanoparticle solid solution softens the Al matrix and improves the elongation of the SLM Al-10Si-Mg alloy. Citation: Huang, B.-C.; Hung, F.-Y. Al2 O3 Particle Erosion Induced Phase Keywords: Al-Si-Mg alloy; selective laser melting (SLM); mechanical properties; impact toughness; Transformation: Structure, erosion wear Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy. Nanomaterials 2021, 11, 2131. https://doi.org/10.3390/ 1. Introduction nano11082131 Selective laser melting (SLM) is a type of powder bed fusion technology in which three-dimensional (3D) objects are gradually built layer by layer. This makes the technology Academic Editor: Jordi Sort suitable for manufacturing parts with complex geometric shapes. This emerging manufac- turing technology has been applied to different metallic materials such as cobalt-chromium Received: 2 July 2021 alloys [1], stainless steel [2,3], aluminum-based alloys [4,5], magnesium alloys [6,7], and Accepted: 19 August 2021 titanium alloys [8,9]. Published: 21 August 2021 Among Al alloys, Al-10Si-Mg alloy is one of the first to be subjected to SLM. The silicon content of Al-10Si-Mg alloy is close to the eutectic point of aluminum–silicon binary Publisher’s Note: MDPI stays neutral alloys, and the material has a small solidification range during melting, which makes it with regard to jurisdictional claims in suitable to be manufactured using SLM [10,11]. Moreover, Al-10Si-Mg alloy has good published maps and institutional affil- fluidity because its aluminum and silicon composition is close to the eutectic composition, iations. which makes it one of the most suitable candidates for the SLM process. Research on Al- 10Si-Mg alloy has focused on the specific microstructure and mechanical strength caused by the rapid cooling in the SLM process [10–15]. One study pointed out that specimens with different construction directions used in fatigue tests were fabricated using SLM [16] and Copyright: © 2021 by the authors. investigated the high cycle fatigue life of specimens with different construction directions Licensee MDPI, Basel, Switzerland. and subjected to different heat treatment conditions [14]. The results indicated that the This article is an open access article microstructure evolution characteristics and mechanical properties of SLM Al-10Si-Mg distributed under the terms and alloy were highly valuable. Notably, particle erosion is an important mechanism that causes conditions of the Creative Commons material damage in many engineering applications. However, few comprehensive reports Attribution (CC BY) license (https:// have discussed the wear resistance of Al-10Si-Mg alloy specimens [17–19]. Previously, we creativecommons.org/licenses/by/ 4.0/). used SiO2 particles to conduct erosion experiments for evaluating the wear resistance of Nanomaterials 2021, 11, 2131. https://doi.org/10.3390/nano11082131 https://www.mdpi.com/journal/nanomaterials
Nanomaterials 2021, 11, 2131 2 of 17 Al-10Si-Mg Nanomaterials 2021, alloy 11, x FOR PEER and commercial 4384 Al alloy and confirmed that Al-10Si-Mg alloy has 2 of 17 REVIEW excellent wear resistance [17]. In this study, Al2 O3 ceramic particles were used instead of SiO2 particles in erosion experiments to create reportsahave considerably discussed harsher the wearwear environment resistance for examining of Al-10Si-Mg the erosion- alloy specimens [17–19]. Previ- induced phase ously, we used SiO transformation 2 particles and to conduct material failure erosion experiments mechanism for evaluating of Al-10Si-Mg alloy.the Bywear re- sistance of using the SLM process Al-10Si-Mgfrom parameters alloy and [17],commercial 4384 Aland tensile, erosion, alloyimpact and confirmed that Al-10Si-Mg test specimens were fabricatedalloy fromhas excellent wear Al-10Si-Mg resistance alloy powder[17].by means of SLM to compare the effects In this study, Al 2O3 ceramic particles were used instead of SiO2 particles in erosion of heat treatment and erosion phase transformation behavior on the mechanical strength experiments to create a considerably harsher wear environment for examining the ero- and impact toughness of the material. The establishment of related wear degradation sion-induced phase transformation and material failure mechanism of Al-10Si-Mg alloy. mechanisms is important for academic research and to provide references for SLM Al-Si- By using the SLM process parameters from [17], tensile, erosion, and impact test speci- Mg alloy applications. mens were fabricated from Al-10Si-Mg alloy powder by means of SLM to compare the effects of heat treatment and erosion phase transformation behavior on the mechanical 2. Materials and Methods strength and impact toughness of the material. The establishment of related wear degra- In this study, wemechanisms dation used Al-10Si-Mg alloyfor is important specimens academic manufactured by the references research and to provide Industrialfor SLM Technology Research Al-Si-MgInstitute (ITRI; ITRI self-developed AM250, Hsinchu, Taiwan). More- alloy applications. over, the Al-10Si-Mg alloy powder (according to ASTM F3318, Taiwan Circle Metal Powder 2. Materials Co., Ltd., Tainan, Taiwan) and used Methods to fabricate these specimens was produced by ITRI. Its chemical composition In this study, we used is summarized Al-10Si-Mg in Table 1. Thealloy specimens powder has amanufactured by the Industrial spherical appearance and an average Technology particle sizeResearch of 35 µm.Institute (ITRI; ITRI self-developed A continuous-wave AM250, Hsinchu, laser with a wavelength of 1064 Taiwan). nm and a spot size of 100 µm was employed as the energy source. The laser power was Metal Moreover, the Al-10Si-Mg alloy powder (according to ASTM F3318, Taiwan Circle 300 W, scanningPowder speed 700Co., mm/s, Ltd., Tainan, hatchTaiwan) space 35used µm,toand fabricate powder these specimens layer was30produced thickness µm. by ITRI. Its chemical composition is summarized in Table 1. The powder has a spherical ap- The process parameters are summarized in Table 2. The relationship between the printed pearance and an average particle size of 35 μm. A continuous-wave laser with a wave- arrangement and construction direction of the SLM Al-10Si-Mg specimens on the substrate length of 1064 nm and a spot size of 100 μm was employed as the energy source. The laser and the specifications power wasof the300specimens W, scanning are illustrated speed in Figures 700 mm/s, 1 and hatch space 2, respectively, 35 μm, and powder and layer thick- the finished product is depicted in Figure 3. ness 30 μm. The process parameters are summarized in Table 2. The relationship between the printed arrangement and construction direction of the SLM Al-10Si-Mg specimens on Table 1. Chemicalthe composition of Al-10Si-Mg substrate and alloy. (wt.%). the specifications of the specimens are illustrated in Figures 1 and 2, respectively, and the finished product is depicted in Figure 3. Si Fe Cu Mn Mg Ni Zn Pb Sn Ti Al Composition 10.00 Table 0.551. Chemical 0.05 0.45 0.65of Al-10Si-Mg composition 0.05 0.10 0.05 alloy. (wt.%). 0.05 0.15 Bal. Si Fe Cu Mn Mg Ni Zn Pb Sn Ti Al Table 2. Composition Process 0.55 10.00 parameters employed 0.05 0.45 in this0.65 study. 0.05 0.10 0.05 0.05 0.15 Bal. Layer Laser Power Table 2. ProcessSpeed Scanning parameters employed in this study. Beam Size Hatch Space Thickness 300 W Laser700 Power mm/s Scanning Speed 35 µm Beam Size 100 µm Hatch Space30 µm Layer Thickness 300 W 700 mm/s 35 μm 100 μm 30 μm Figure 1. The relationship between the printed arrangement and construction direction of the Al-10Si-Mg specimens on the substrate.
Nanomaterials 2021, 11, x FOR PEER REVIEW 3 of 17 Nanomaterials 2021, 11, x FOR PEER REVIEW 3 of 17 Figure 1. The relationship between the printed arrangement and construction direction of the Al-10Si-Mg specimens on Nanomaterials 2021, 11, 2131 3 of 17 the substrate. Figure 1. The relationship between the printed arrangement and construction direction of the Al-10Si-Mg specimens on the substrate. Thedetailed Figure2.2.The Figure detailedspecifications specifications of of thethe specimens specimens used used in this in this study: study: (a)tensile (a) the the tensile test specimens; test speci- Figure 2. The detailed specifications of the specimens used in this study: (a) the tensile test speci- (b) the(b) mens; erosion test specimens; the erosion (c) (c) test specimens; thetheimpact toughness impact toughnessspecimens. specimens. mens; (b) the erosion test specimens; (c) the impact toughness specimens. Figure 3. The finished as-fabricated Al-10Si-Mg specimens. In this study, the specimens were subjected to T6 heat treatment, which involves two stages of solution Figure treatment 3. The finished at 510 °C forAl-10Si-Mg as-fabricated 2 h, followed by artificial aging treatment at 170 specimens. Figure 3. The finished as-fabricated Al-10Si-Mg specimens. °C for 6 h. The as-fabricated Al-10Si-Mg specimens were categorized as group F, and the specimens In In thissubjected this study, to T6 the study, the heat treatment specimens specimens werewere were categorized subjected subjected T6asheat to T6 to group heat FH. The naming treatment, treatment, whichprin- which involves two involves two ciples stages are summarized in Tableat3. 510 To examine the microstructure of the as-fabricated Al- stages of solution treatment at 510 C for 2 h, followed by artificial aging treatment170 of solution treatment °C◦ for 2 h, followed by artificial aging treatment at at 10Si-Mg specimens ◦ C 6for with different construction directions,were the plane perpendicular to the 170for °C h. 6The as-fabricated h. The Al-10Si-Mg as-fabricated Al-10Si-Mg specimens specimens were categorized categorizedas group F, and as group the F, and construction direction was defined as the z surface, and the planes parallel to the construc- specimens the specimens subjected to T6 heat subjected treatment werewere categorized as group FH. The naming prin- tion direction were defined to as T6 the heat treatment x surface and y surface, categorized as illustratedasingroup FigureFH. 4. The naming ciples are summarized principles are summarizedin Table 3. To3.examine in Table the the To examine microstructure microstructureof the as-fabricated of the Al- as-fabricated 10Si-Mg specimens Al-10Si-Mg specimenswith different with construction different directions, construction the the directions, plane perpendicular plane perpendicularto the to construction direction the construction was defined direction as the as was defined z surface, and theand the z surface, planestheparallel planes to the construc- parallel to the tion directiondirection construction were defined as the xas were defined surface and y surface, the x surface as illustrated and y surface, in Figure as illustrated 4. in Figure 4.
2021, 11, x FOR PEER REVIEW Nanomaterials 2021, 11, 2131 4 of 17 4 of 17 Table 3. The naming principles and post-processing conditions. Table 3. The naming principles and post-processing conditions. Group Post-Processing Conditions Group Post-Processing Conditions F Raw material FE F material after T6 heat treatment Raw Raw material FE Raw material after T6 heat treatment FH FH Raw material + Erosion wear Raw material + Erosion wear FHE Raw material FHE after T6 heat treatment + Erosion Raw material after wear T6 heat treatment + Erosion wear Figure 4. The naming principles of the relationship between different observation planes and the Figure 4. The naming principles of the relationship between different observation planes and the construction direction. construction direction. The F and FH specimens were cold embedded and ground in order using #80~#4000 The F and FH specimens were cold embedded and ground in order using #80~#4000 SiC sandpaper, followed by polishing using a 0.04 µm SiO2 polishing solution. The SiC sandpaper, followed specimens of each using by polishing groupawere0.04 immersed μm SiO2 polishing in Keller’s solution. etchingThe speci-(19 mL HNO + 9 mL solution 3 mens of each group were immersed in Keller’s etching solution (19 mL HNO 3 + 9 mL HCl HCl + 6 mL HF + 19 mL H2 O) for approximately 20 s, and the microstructures of the + 6 mL HF + 19 mL H O) for approximately z 2surface and x surface20 s, and were the microstructures observed using an optical of the z surface (OM; BX41M-LED, microscope and x surface were observed using an optical microscope (OM; BX41M-LED, Olympus, Olympus, Tokyo, Japan). Notably, only the z surface and x surface were analyzed herein. Tokyo, Japan). Notably, only the zthe Furthermore, surface and x were specimens surface were analyzed analyzed herein. Further- using a scanning electron microscope (SEM; more, the specimensSU-5000, were analyzed using a scanning electron microscope Hitachi, Japan) and an X-ray diffractometer (XRD; (SEM;D8 SU-5000, Discover, Bruker, Karlsruhe, Hitachi, Japan) and an X-ray diffractometer Germany) to observe the (XRD; D8 Discover, morphology Bruker,pool of the melting Karlsruhe, Ger- the phase structure, and examine many) to observe therespectively. morphology of the melting pool and examine the phase structure, respectively. A tensile test was performed in which the F and FH groups of specimens were A tensile test was performed stretched in which at a speed the F and and of 1 mm/min, FH the groups of specimens results of each group were were obtained as the stretched at a speedaverage of 1 mm/min, and theobtained of the values results ofineachfive group test runs.wereThe obtained hardness as theof the specimens was average of the valuesanalyzed obtainedininHRFfive test units runs. The hardness by using a Rockwell of the specimens hardness was(AR-10 tester ana- Hardness Testing lyzed in HRF units Machine, by using Mitutoyo, a Rockwell Taipei, Taiwan). An erosion test was conductedMa- hardness tester (AR-10 Hardness Testing in which the specimens chine, Mitutoyo, Taipei, wereTaiwan). placed on An theerosion carriertest waserosion of the conducted in which equipment the specimens (Figure 5). The erodent solid particles were placed on the carrier of theinerosion employed this testequipment were irregular(Figure Al25). O3 The erodent ceramic solid (hardness: particles particles 2000 HV, Rich Sou employed in this testTechnology were irregular Co.,Al 2O3 ceramic Ltd., Kaohsiung, particles Taiwan)(hardness: 2000ofHV, with sizes Rich Sou 125–150 µm. The erosion rate in Technology Co., Ltd., Kaohsiung, units of g/g was Taiwan) defined with as sizes of 125–150 the total mass ofμm. the The erosion removed rate individed by the total material mass as units of g/g was defined of the the total erodent mass particles hitting the of the removed specimen material surface. divided Following by the total the experimental mass of the erodentmethods particles used hittingin [20], the test was the specimen performed surface. Followingwith 200 g of Al2 O3 ceramic particles each the experimental time, 2 (the flying speed of Al O particle is methods used in [20], the and the inlet test was pressure performed was200 with fixed g ofatAl 3 2kg/cm O3 ceramic particles each 2 3 about 66was time, and the inlet pressure m/s).fixedTheatimpingement 3 kg/cm2 (theangle flying(the angle speed of between the erosion Al2O3 particle is direction of the erodent particles about 66 m/s). The impingement angle and theangle (the material surface) between the was gradually erosion direction of the from 15◦ to 90◦ in increased ◦ erodent particles andincrements the material of 15 . The was surface) maximum graduallyand increased minimumfrom erosion15°rates ofin to 90° thein-test pieces in both the F and the FH groups were 30 ◦ and 90◦ , respectively. The failure was dominated by the crements of 15°. The maximum and minimum erosion rates of the test pieces in both the F and the FH groupsductile cutting were 30° andmechanism. T6 heat 90°, respectively. Thetreatment failure wasimproved the ductility dominated by the of the material and
Nanomaterials 2021, 11, x FOR PEER REVIEW 5 of 17 Nanomaterials 2021, 11, 2131 5 of 17 ductile cutting mechanism. T6 heat treatment improved the ductility of the material and precipitatedthe precipitated thenano-strengthening nano-strengtheningMg Mg2Si Si phase, which can improve the wear resistance 2 phase, which can improve the wear resistance of the material. of the material. Figure5.5.(a) Figure (a)The Theerosion erosion test test equipment equipment developed developed by group; by our our group; (b)definition (b) the the definition of impingement of impingement angle. angle. To explore the differences in the wear mechanisms of the as-fabricated Al-10Si-Mg alloy To explore before specimens the differences and after inT6the heatwear mechanisms treatment, of themicroscope an electron as-fabricated andAl-10Si-Mg an optical alloy specimens before and after T6 heat treatment, an electron microscope microscope were used to observe the erosion surface morphology and erosion subsurface and an optical microscope were used to observe the erosion surface morphology and characteristics of the specimens, respectively. Moreover, in the erosion process, high- erosion subsurface characteristics speed impingementof the of specimens, the erodent Al respectively. Moreover, in the erosion process, high- 2 O3 particles on the specimen surface can generate a speed high impingement temperature of 400–500 ◦ of the erodent Al2O3 Under C [21–24]. particles theoninfluence the specimen surface of local can generate pressure and higha high temperature temperature, of 400–500 the matrix of the°CAl[21–24]. alloy isUnder the influence softened, of local are and microcracks pressure and high generated. In temperature, this the matrixthe light, to investigate of the Al alloyofiserosion influence softened, on and microcracksstrength the mechanical are generated. In this and fracture light, to investigate toughness of the SLMthe influencealloy, Al-10Si-Mg of erosion on FH the F and the groups mechanical strength after of specimens and erosion fracture toughness of the SLM Al-10Si-Mg alloy, the F and FH groups of specimens were denoted FE and FHE, respectively. The naming principles are summarized in Table after erosion 3. were In orderdenoted FE and to explore the FHE, phaserespectively. transformation Theand naming principles degradation are summarized behaviors caused byinsevere Table 3. In order particle to explore erosion the phase transformation [20], approximately 1000 g of Aland2 O3 degradation behaviors ceramic particles caused was used by se- to erode vere sides both particle erosion of the tensile[20], andapproximately 1000 g specimens, the impact toughness of Al2O3 ceramic and theparticles erosion was usedof direction to the erodent particles was parallel to the construction direction of the specimens (Figure 6).
Nanomaterials 2021, 11, x FOR PEER REVIEW 6 of 17 Nanomaterials 2021, 11, 2131 6 of 17 erode both sides of the tensile and the impact toughness specimens, and the erosion di- rection of the erodent particles was parallel to the construction direction of the specimens To our6). (Figure knowledge, no reports To our knowledge, noon the effect reports of effect on the particle erosion erosion of particle on the mechanical strength on the mechanical and impact strength and toughness of SLM Al-10Si-Mg impact toughness alloy arealloy of SLM Al-10Si-Mg available. In this study, are available. X-ray In this diffraction study, X-ray spectroscopy (Bruker AXS GmbH, Karlsruhe, Germany) was also used diffraction spectroscopy (Bruker AXS GmbH, Karlsruhe, Germany) was also used to ana-to analyze the phase structure of the erosion surfaces of the FE and FHE groups of specimens lyze the phase structure of the erosion surfaces of the FE and FHE groups of specimens toto demonstrate the generation demonstrate the mechanism of particle erosion generation mechanism induced of particle phase erosion transformation. induced XRD test uses phase transformation. copper XRD testas the copper uses target, Cu-Kα radiation as the target, with radiation Cu-Kα a wavelength withofa1.5418 Å, the scanning wavelength of 1.5418 range Å , theof 2θ is from 20 ◦ to 100◦ , and the scanning speed is 3◦ /min. scanning range of 2θ is from 20° to 100°, and the scanning speed is 3°/min. Figure 6.6. Figure Tensile Tensileand andimpact impacttoughness toughnesstest testspecimens specimensafter aftererosion. erosion. 3.3.Results Resultsand andDiscussion Discussion 3.1. 3.1.Microstructural MicrostructuralCharacteristics Characteristicsand andMaterial MaterialProperties Properties Figure Figure7 7presents presentsthe themicrostructures microstructures of the the as-fabricated as-fabricatedAl-10Si-Mg Al-10Si-Mgspecimens specimensbefore be- andand fore after T6T6 after heat heat treatment treatment(groups (groupsFFand andFH) FH) on on the surfaces surfaces parallel parallel(x (xsurface) surface)and and perpendicular (z surface) to the construction perpendicular (z surface) to the construction direction. direction. The microstructure microstructure of the F groupof of the F group ofspecimens specimenson onthethex xsurface surfacepresents presents melting meltingpools poolswith fish-scale-like with shapes, fish-scale-like shapes,as illustrated as illus- in Figure trated 7a, with in Figure a width 7a, with of approximately a width of approximately 100 µm,100 which μm, whichis close to thetospot is close size of the spot the size oflaser sourcesource the laser [25]. The[25].depth The of theseofmelting depth pools is approximately these melting 30 µm, and pools is approximately 30there μm, are andno microholes there between layers, are no microholes indicating between layers,that the SLMthat indicating process the SLMparameters process were appropriately parameters were controlled [26]. On the z surface, the laser source left a strip-shaped appropriately controlled [26]. On the z surface, the laser source left a strip-shaped laser laser scanning track, as illustrated in Figure 7b. The extremely fast cooling rate in the scanning track, as illustrated in Figure 7b. The extremely fast cooling rate in the SLM pro- SLM process caused segregation cess in the Al-10Si-Mg caused segregation alloy duringalloy in the Al-10Si-Mg solidification, leading to the during solidification, formation leading to theoffor- long dendritic crystals [27]. After T6 heat ◦ C, 2 h → (510 ◦ mation of long dendritic crystals [27].treatment (510 treatment After T6 heat 170 °C, C, 22h), h →the 170 outline °C, 2ofh), the melting the outlinepools of the and the scanning melting pools and trajectory disappeared, the scanning trajectory and coarse silicon disappeared, and particles were coarse sili- formed. con particlesThe supersaturated were formed. The silicon was redissolved supersaturated silicon was intoredissolved the aluminum into matrix, the aluminumand the resulting microstructure is depicted in Figure 7c,d. Notably, the fine matrix, and the resulting microstructure is depicted in Figure 7c,d. Notably, the fine grains grains distribute at the boundaries of melting pool, and on the above of fine grains present distribute at the boundaries of melting pool, and on the above of fine grains present radi- radiation-distributed columnar grains.columnar ation-distributed After T6 heat treatment, grains. After T6silicon heat precipitation treatment, silicontransformed into spherical precipitation trans- formed into spherical form, with grain distribution converted into equiaxed grains due and form, with grain distribution converted into equiaxed grains due to homogenization to recrystallization. homogenization and recrystallization. Considering that the silicon content in the aluminum matrix and the morphology of the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29], the detailed structure of the melting pools was observed using SEM, and the silicon content in different regions of the structure was analyzed using EDS. As illustrated in Figure 8, the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is close to the silicon content of the Al alloy powder used in this study. The silicon content at the boundary of the melting pools was approximately 18.40 wt.%. Therefore, the boundary zone was termed the Si-rich phase [10,13,17]. These organizational differences have an important effect on the subsequent erosion characteristics obtained in this study.
Nanomaterials 2021, 11, 2131 7 of 17 Nanomaterials 2021, 11, x FOR PEER REVIEW 7 of 17 Figure 7. Microstructure of the specimens in different observation planes: group F specimens on the planes (a) parallel and (b) perpendicular to the construction direction, and group FH specimens on the planes (c) parallel and (d) perpendicular to the construction direction. Considering that the silicon content in the aluminum matrix and the morphology of the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29], the detailed structure of the melting pools was observed using SEM, and the silicon con- tent in different regions of the structure was analyzed using EDS. As illustrated in Figure 8, the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is close to7.the Figure silicon content Microstructure of the Alinalloy of the specimens powder different usedplanes: observation in this study. group The silicon F specimens on thecontent Figure 7. Microstructure of the specimens in different observation planes: group F specimens on the at the boundary of the melting pools was approximately 18.40 wt.%. Therefore, the planes (a) parallel and (b) perpendicular to the construction direction, and group FH specimens on bound- planes (a) the zone parallel planeswas and (c) parallel (b) andtheperpendicular (d) perpendicularto the to the construction construction direction, direction. and group FH specimens on ary termed Si-rich phase [10,13,17]. These organizational differences have the planes (c) parallel and (d) perpendicular to the construction direction. an important effect on the subsequent erosion characteristics obtained in this study. Considering that the silicon content in the aluminum matrix and the morphology of the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29], the detailed structure of the melting pools was observed using SEM, and the silicon con- tent in different regions of the structure was analyzed using EDS. As illustrated in Figure 8, the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is close to the silicon content of the Al alloy powder used in this study. The silicon content at the boundary of the melting pools was approximately 18.40 wt.%. Therefore, the bound- ary zone was termed the Si-rich phase [10,13,17]. These organizational differences have an important effect on the subsequent erosion characteristics obtained in this study. Figure 8. (a) Detailed morphology of the melting pool and (b) silicon content in different regions of the melting pool. Figure 8. (a) Detailed morphology of the melting pool and (b) silicon content in different regions of the melting pool. The The SLM SLM process creates aa microstructure process creates microstructure with with aa nonuniform nonuniform distribution distribution of of silicon silicon particles particles inside insidethethematerial. material.The The evolution evolution of the phase of the structure phase structure afterafter heatheat treatment was treatment analyzed was analyzed usingusing XRD,XRD, and the andresults are presented the results are presented in Figure 9. The in Figure 9. diffraction The diffraction peaks cor- peaks responding to the α-Al phase clearly appeared in the XRD patterns corresponding to the α-Al phase clearly appeared in the XRD patterns of the F and FH of the F and FH groups of specimens. groups A comparison of specimens. betweenbetween A comparison FiguresFigures 8 and 98 revealed and 9 revealedthat the supersaturated that the supersat- Figure 8. (a) Detailed morphology silicon of thesolution solid melting pool and was (b) silicon content redissolved into inthe different regions of aluminum the melting matrix and pool. precipitated into urated silicon solid solution was redissolved into the aluminum matrix and precipitated coarse silicon into coarse particles, silicon thus causing particles, the diffraction peakpeak corresponding to silicon to rise. The SLM process creates thus causing a microstructure thewith diffraction a nonuniform corresponding distribution to silicon of silicon to In addition, rise. In the addition, magnesium the magnesium content in content theinAl-10Si-Mg the Al-10Si-Mgalloy was alloy 1 waswt.%, particles inside the material. The evolution of the phase structure after heat treatment was 1 and wt.%, because and becausethe the diffraction analyzed usingpeak XRD,corresponding and the results are to the Mg2 Si in presented nanoparticles Figure 9. The was close to diffraction the α-Al peaks cor- phase (Al (1 1 1)), the Mg responding to the α-Al Si phase diffraction peak was not clear in case of 2 phase clearly appeared in the XRD patterns of the F and FH groups the F and FH groups of specimens. A comparison between Figures 8 and 9 revealed that of specimens. Furthermore, the hardness data of the specimens are shown in Figure 10. the supersaturated silicon to Owing solid the solution extremelywasfine redissolved into the aluminum grains produced by the rapid matrix coolingand inprecipitated into the SLM process, the coarse silicon particles, thus causing the diffraction peak corresponding HRF hardness of the F group of specimens reached 98. The heat treatment process changed to silicon to rise. In addition, the the magnesium silicon structure content in and released the Al-10Si-Mg residual alloy was stress, which 1 wt.%,the reduced andhardness because the of the FH group of specimens to 75.
(1 1specimens. 1)), the MgFurthermore, 2Si phase diffraction peak data the hardness was not clear of the in case of specimens arethe F andinFH shown groups Figure 10. of Ow- specimens. ing to theFurthermore, extremely finethe grains hardness data of by produced the the specimens are shown rapid cooling in Figure in the 10. Ow-the SLM process, ingHRFto the extremely hardness of fine the Fgrains group produced by the reached of specimens rapid cooling 98. Thein the heatSLM process,process treatment the HRF hardness of the F group of specimens reached 98. The heat treatment changed the silicon structure and released residual stress, which reduced the hardness of process changed the FHthe silicon group structure and of specimens released residual stress, which reduced the hardness of to 75. Nanomaterials 2021, 11, 2131 8 of 17 the FH group of specimens to 75. Figure 9. XRD patterns of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment. FigureFigure 9. XRD9. patterns of the of XRD patterns as-fabricated Al-10Si-Mg the as-fabricated alloy before Al-10Si-Mg and after alloy before and T6 heat after T6treatment. heat treatment. Figure 10. HRF hardness of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment. Figure 10. HRF hardness of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment. 3.2. of Figure 10. HRF hardness Particle Erosion Wear the as-fabricated Mechanism Al-10Si-Mg alloy before and after T6 heat treatment. According 3.2. Particle Erosionto studies Wear in the literature [30–32], when a ductile metal material is hit Mechanism 3.2. Particle with Erosion erodent Wear Mechanism particles, the peak erosion rate appears at the ◦ –30◦ . According to studies in the literature [30–32], when a impingement ductile metal angles of 15 material is hit Theerodent with erosionto According rates of the studies particles, in Fthe the and peak FH groups literature erosion ofappears [30–32], rate specimens whenatathe as impingement functions ductile metalof the impingement material angles isofhit 15°– with angle erodentare illustrated particles, in the Figure peak 11. erosionThe erosion rate rates appears of at the the specimens impingement in 30°. The erosion rates of the F and◦ FH groups of specimens as functions of the impinge- both anglesgroups of peaked 15°– at an 30°.ment The impingement erosion angle arerates angle of the illustrated F of 30 inand FH, 11. Figure while Thethe groups of minimum specimens erosion erosion rates ofasthe rate occurred functions specimens of the 90◦ . The at groups impinge- in both erosion rate decreasedinasFigure the impingement angle increased ◦ after 30 rate , which ment angleatare peaked anillustrated impingement angle 11. Thewhile of 30°, erosiontherates of the specimens minimum erosion bothindicated inoccurred groups that at 90°. the ductile cutting mechanism dominated the wear fracture of peaked at an impingement angle of 30°, while the minimum erosion rate occurred at 90°. both groups. In general, the metallic materials with higher hardness have better wear resistance, but the results presented in Figure 11 indicated that the wear resistance of the FH group of specimens was superior to that of the group F specimens under all impingement angles. To clarify the wear mechanism, we inspected the morphology of the erosion surface by using SEM (Figure 12), and the results indicated that under impingement by irregularly shaped erodent particles, many sharp grooves were formed in the F group of specimens because the Al2 O3 particles cut through the material surface. By contrast, the FH group of specimens had a softer matrix due to the heat treatment; the scratches on the erosion surface were gentler, and many lip structures were formed adjacent to the erosion grooves. The main reason is
sults presented in Figure 11 indicated that the wear resistance of the FH group of speci- mens was superior to that of the group F specimens under all impingement angles. To clarify the wear mechanism, we inspected the morphology of the erosion surface by using SEM (Figure 12), and the results indicated that under impingement by irregularly shaped Nanomaterials 2021, 11, 2131 erodent particles, many sharp grooves were formed in the F group of specimens because 9 of 17 the Al2O3 particles cut through the material surface. By contrast, the FH group of speci- mens had a softer matrix due to the heat treatment; the scratches on the erosion surface were gentler, and many lip structures were formed adjacent to the erosion grooves. The main reason is that that heat heat treatment treatment can generate can generate strengthening strengthening MgMg 2Si nanoprecipitates in 2 Si nanoprecipitates in the aluminum the aluminum matrix [33,34], which increases the resistance of the material matrix [33,34], which increases the resistance of the materialtoto wear wearandand microcrack microcrack formation. Therefore, the lip structures were not completely separated from formation. Therefore, the lip structures were not completely separated from the surface, the surface, which led to the superior wear resistance of the Al-10Si-Mg alloy [21,24]. which led to the superior wear resistance of the Al-10Si-Mg alloy [21,24]. Moreover, based Moreover, based on the erosion subsurface morphologies corresponding to different im- pingementon the erosion angles, subsurface as depicted morphologies in Figure corresponding 13, the FH group of specimens tohad different a higherimpingement sur- angles, as depicted face roughness in Figure than the F group13, of the FH group specimens of specimens because had a of the softer matrix higher surface the former led roughness than the F group to the formation of lipofstructures. specimens because However, the softer because matrix changes in the ofmomentum the formercompo- led to the formation of liptostructures. nent normal However, the erosion surface of the because changes Al2O3 particles in theincrease gradually momentum component normal to as the impinge- the erosion ment angle increases,surface of the many pits Al2 O3inparticles appeared gradually both groups at highincrease impingementas the impingement angle angles. Therefore, in the follow-up increases, many pits experiments, appeared1000 g of Al in both 2O3 particles groups at high wasimpingement used to study angles. the Therefore, erosion-induced phase transformation in the follow-up experiments, of 1000 both groups g of Alof O 2 3specimens particles at an was impingement used to study the erosion- angle ofinduced 90°. Furthermore, the effects ofof phase transformation the phase both transformation groups of specimens induced at anby the heat impingement angle of 90◦ . generated due to particle Furthermore, theimpingement effects of theand erosion-induced phase transformation microcracks inducedonbythe mechan- the heat generated due to ical properties and impact toughness of the SLM Al-10Si-Mg alloy were evaluated. particle impingement and erosion-induced microcracks on the mechanical properties and impact toughness of the SLM Al-10Si-Mg alloy were evaluated. Figure 11. Erosion rate of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment as a Nanomaterials 2021, 11, x FOR PEER Figure 11.REVIEW Erosion rate of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment as a 10 of 17 functionfunction of the impingement of the impingement angle. angle. Figure Figure 12.12. Erosion Erosion surface surface morphology morphology of as-fabricated of the the as-fabricated Al-10Si-Mg Al-10Si-Mg alloy alloy beforebefore andT6 and after after heatT6 heat treatment. treatment.
Nanomaterials 2021, 11, 2131 10 of 17 Figure 12. Erosion surface morphology of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment. Figure Figure 13. 13. Erosion Erosion subsurface subsurface morphology morphology of of the the as-fabricated as-fabricated Al-10Si-Mg alloy before Al-10Si-Mg alloy before and and after after T6 T6 heat heat treatment. treatment. 3.3. 3.3. Erosion Erosion Induced Induced Phase Phase Transformation Transformation In In particle erosion, theceramic particle erosion, the ceramic particles particleshithit thethesurface surfaceof the of metal specimens the metal at high specimens at speed, and their kinetic energy is converted into heat energy, which high speed, and their kinetic energy is converted into heat energy, which can generate can generate temper- atures of 400–500 temperatures °C instantaneously of 400–500 [22,23,31] ◦ C instantaneously and cause [22,23,31] andsurface oxidation cause surface to formtoAlform oxidation 2O3. As depicted in Figure 14a,b, the F group of specimens transformed Al2 O3 . As depicted in Figure 14a,b, the F group of specimens transformed into the FE into the FE group of specimens after erosion. The diffraction peaks corresponding group of specimens after erosion. The diffraction peaks corresponding to Al2 O3 were to Al 2O3 were generated at six specificatdiffraction generated six specificangles 2θ, and diffraction the 2θ, angles same andresults the samewere obtained results werefor the F group obtained for theofF specimens transformed group of specimens into the FE transformed intogroup the FEof group specimens. A comparison of specimens. of the XRD A comparison patterns of the XRD of the F, of patterns FE,the FH, F, and FE, FH,FHEand groups FHEof specimens groups with thatwith of specimens of the thatAlof 2Othe 3 ceramic Al2 O3 particles ceramic used in the particles used erosion in the experiment revealedrevealed erosion experiment that only sixonly that specific diffraction six specific peaks peaks diffraction corre- sponding to the Al O phase of the erodent particles appeared in corresponding to the Al2 O3 phase of the erodent particles appeared in the patterns of the 2 3 the patterns of the FE and FHE groups of specimens. Notably, no ceramic particles remained FE and FHE groups of specimens. Notably, no ceramic particles remained on the erosion on the erosion sur- face of the surface specimens of the specimens observed observed using usingSEM SEM (Figure (Figure12). 12).ItItcan canbebeinferred inferredthat that the the particle erosion caused (1) the formation formation of of a surface surface Al Al22O33 film; film; (2) (2) high high temperature temperature of the surface to lead to redissolution of the supersaturated silicon into the α-Al matrix, resulting in a slight dip in the silicon phase diffraction peak of the specimens specimens after after the the particle particle erosion; erosion; (3) deformation of the grains after erosion and microcrack formation [34]. In this light, it is interesting to investigate the effect of particle erosion on the mechanical strength and fracture toughness of the SLM Al-10Si-Mg alloy. alloy. 3.4. Changes in Tensile Mechanical Properties Caused by Erosion The F and FH groups of specimens were compared, as illustrated in Figure 15a,b. The yield strength (YS) and ultimate tensile strength (UTS) of the F group of specimens reached 181.63 and 297.75 MPa, respectively, but their uniform elongation (UE) and total elongation (TE) were both 1.87% (low ductility). After T6 heat treatment, the UTS decreased from 297.75 to 286.02 MPa; YS increased from 181.63 to 221.09 MPa; UE and TE increased to 2.33% and 2.70% (ductility improvement), respectively. The morphologies of the tensile fracture surface and the tensile fracture subsurface of the F and FH groups of specimens are depicted in Figure 16a,b. The F group of specimens had insufficient ductility and broke before necking. By contrast, the FH group of specimens, on which small dimples were observed upon tensile fracture, had higher ductility. Based on a comparison of the tensile fracture subsurface presented in Figure 16c,d, the F group of specimens fractured within an extremely short time, resulting in a sharper fracture subsurface profile than that of the FH group of specimens. The difference between the two groups can be compared more clearly by using the enlarged views presented in Figure 16e,f. The failure of the FH group
Nanomaterials 2021, 11, 2131 11 of 17 of specimens was attributed to the maximum shear stress induced by the tensile force, and Nanomaterials 2021, 11, x FOR PEER REVIEW 11 of 1 the fracture subsurface profile was undulating and oriented at approximately 45◦ with respect to the tensile direction. Figure 14. XRD pattern: (a) XRD Figure 14. the F pattern: group of(a)specimens converted the F group to FEconverted of specimens after erosion; to FE(b) theerosion; after FH group of specimens (b) the FH group con- verted to FHE after of erosion. specimens converted to FHE after erosion. According to thein 3.4. Changes literature [23], the local Tensile Mechanical high temperature Properties and high pressure gener- Caused by Erosion ated by the impact of high-speed particles during erosion softened The F and FH groups of specimens were compared, as theillustrated matrix in in theFigure region15a,b. Th close to 200 yield strength (YS) and ultimate tensile strength (UTS) of the F group ofthespecimen µm below the Al-alloy surface. In addition, ceramic particles accompanying fluid hit the surface reached of the 181.63 metal and specimen 297.75 at high speeds, MPa, respectively, but which distorted their uniform and deformed elongation (UE) and tota the crystal grains near the surface and generated microcracks [35]. Thus, elongation (TE) were both 1.87% (low ductility). After T6 heat treatment, in this study, the the UTS de F and FHcreased groupsfrom of specimens were subjected to particle erosion with an impingement 297.75 to 286.02 MPa; YS increased from 181.63 to 221.09 MPa; UE and TE angle of 90 ◦ on both sides to analyze the changes in their mechanical properties and impact increased to 2.33% and 2.70% (ductility improvement), respectively. The morphologies o toughness (Figure 6). the tensile fracture surface and the tensile fracture subsurface of the F and FH groups o specimens are depicted in Figure 16a,b. The F group of specimens had insufficient ductil ity and broke before necking. By contrast, the FH group of specimens, on which smal dimples were observed upon tensile fracture, had higher ductility. Based on a comparison of the tensile fracture subsurface presented in Figure 16c,d, the F group of specimens frac tured within an extremely short time, resulting in a sharper fracture subsurface profil
Nanomaterials 2021, 11, 2131 12 of 17 After erosion, the YS and UTS of the FE group of specimens decreased from 182.63 and 297.75 MPa to 145.77 and 261.86 MPa, respectively, compared with the F group of specimens. The YS and UTS of the FHE group of specimens decreased from 221.09 and 286.02 MPa to 147.74 and 197.03 MPa, respectively, compared with the FH group of specimens. By contrast, the UE and TE of the FE group of specimens increased from 1.87% to 4.93%, compared with the F group of specimens. The UE and TE of the FE group Nanomaterials 2021, 11, x FOR PEER REVIEW 12 of of 17 specimens increased from 2.33%. The experimental results indicate that under severe erosion conditions, the tensile strength of the as-fabricated Al-10Si-Mg alloy decreases, but the softening of the Al matrix due to the high surface temperature increases the elongation than that of the significantly. FH group ofafter Furthermore, specimens. erosion,The difference Young’s between moduli of the the two groups specimens can of the twobe compared more clearly by using the enlarged views presented in Figure 16e,f. The groups tend to decrease (Figure 16), indicating that erosion not only affects the changes in failure of the FH tensile groupand strength of specimens elongation was attributed but also directlytodegrades the maximum shear material stress induced elasticity. by the The coefficient tensile force, and the fracture subsurface profile was undulating and oriented at approxi- of elasticity (Figure 17). These results directly affect the impact toughness of SLM Al-10Si- mately Mg 45° with respect to the tensile direction. alloy. Figure 15. (a) Mechanical strength and (b) elongation of the F, FH, FE, and FHE groups of specimens. Figure 15. (a) Mechanical strength and (b) elongation of the F, FH, FE, and FHE groups of speci- mens.
Nanomaterials 2021, 11, 2131 13 of 17 Nanomaterials 2021, 11, x FOR PEER REVIEW 13 of Nanomaterials 2021, 11, x FOR PEER REVIEW 14 of 17 tensile Figure 16. (a,b) Tensile strength fracture andmorphology; surface elongation (c,d) but also directly fracture degrades subsurface; materialviews (e,f) enlarged elasticity. of the The coeffi- fracture subsur- Figure 16. cient of (a,b) Tensile fracture surface morphology; (c,d) fracture subsurface; (e,f) enlarged views face of F and FH groups of elasticity specimens.(Figure 17). These results directly affect the impact toughness of SLM ofAl-10Si-Mg the fracture subsurface alloy. of F and FH groups of specimens. According to the literature [23], the local high temperature and high pressure gene ated by the impact of high-speed particles during erosion softened the matrix in the regi close to 200 μm below the Al-alloy surface. In addition, ceramic particles accompanyi the fluid hit the surface of the metal specimen at high speeds, which distorted and d formed the crystal grains near the surface and generated microcracks [35]. Thus, in th study, the F and FH groups of specimens were subjected to particle erosion with an im pingement angle of 90° on both sides to analyze the changes in their mechanical propert and impact toughness (Figure 6). After erosion, the YS and UTS of the FE group of specimens decreased from 182. and 297.75 MPa to 145.77 and 261.86 MPa, respectively, compared with the F group specimens. The YS and UTS of the FHE group of specimens decreased from 221.09 a 286.02 MPa to 147.74 and 197.03 MPa, respectively, compared with the FH group of spe imens. By contrast, the UE and TE of the FE group of specimens increased from 1.87% 4.93%, compared with the F group of specimens. The UE and TE of the FE group of spe Changes in the stress–strain imens curve of increased SLM from alloy Al-10Si-Mg 2.33%. Theand before experimental afterafter results erosion: indicate (a) groups that F andFFE under and severe erosi Figure 17.17. Figure Changes in the stress–strain curve of SLM Al-10Si-Mg alloy before and erosion: (a) groups and FE(b) and groups FH and (b) groups FHFHE. and FHE. conditions, the tensile strength of the as-fabricated Al-10Si-Mg alloy decreases, but t softening of the Al matrix due to the high surface temperature increases the elongati significantly. 3.5. Changes Furthermore, in Impact Toughness Causedafter erosion, Young’s moduli of the specimens of the tw by Erosion groups tend to decrease (Figure 16), indicating that erosion not only affects the changes In this study, an impact fracture test was performed to evaluate the impact toughness of the specimens from the four groups. The energy absorbed per unit area was calculated at the point of specimen fracture. The morphology of the impact fracture surface was ob- served with SEM to clarify the fracture mechanism. Figure 18 shows that the impact frac- ture toughness of the specimens increased by approximately 20% after the T6 heat treat- ment. However, due to the composite effect of microcracks and the matrix softening
Nanomaterials 2021, 11, 2131 14 of 17 3.5. Changes in Impact Toughness Caused by Erosion In this study, an impact fracture test was performed to evaluate the impact toughness of the specimens from the four groups. The energy absorbed per unit area was calculated at the point of specimen fracture. The morphology of the impact fracture surface was observed with SEM to clarify the fracture mechanism. Figure 18 shows that the impact fracture toughness of the specimens increased by approximately 20% after the T6 heat treatment. However, due to the composite effect of microcracks and the matrix softening caused by the erosion, the impact toughness of the specimens decreased. Comparing group F and FE, as well as group FH and FHE, respectively, the impact toughness decreased by about 11%. The surface morphology of the region near the starting point of the fracture was inspected using SEM (Figure 19). The F group of specimens exhibited superior ductility, and their fracture-induced dimples were smaller and denser than those of the FH group of specimens. Compared with the characteristics of tensile failure, the specimens are subjected to the shear force, which is rapid and parallel to the fracture surface during the impact, so that the specimens of groups FE and FHE have the same cracking wave pattern as the impact direction. After erosion, the surface layer of the SLM Al-10Si-Mg alloy was softened at high temperatures, and the microcracks induced by erosion directly decreased Young’s Nanomaterials 2021, 11, x FOR PEER REVIEW modulus of the material, thus leading to a decrease in the impact toughness of the15SLM of 17 Al-10Si-Mg alloy. Figure 18.Impact Figure18. Impacttoughness toughnessofofspecimens specimensfrom fromeach group each before group (F, (F, before FH)FH) andand afterafter (FE,(FE, FHE) erosion FHE) ero- in terms sion of theofenergy in terms absorbed the energy per unit absorbed perarea. unit area.
Nanomaterials 2021, 11, 2131 15 of 17 Figure 18. Impact toughness of specimens from each group before (F, FH) and after (FE, FHE) ero- sion in terms of the energy absorbed per unit area. Figure 19. Impact fracture surfaces of the (a) F, (b) FE, (c) FH, and (d) FHE groups of specimens. Figure 19. Impact fracture surfaces of the (a) F, (b) FE, (c) FH, and (d) FHE groups of specimens. 4. Conclusions (1) After the T6 heat treatment of SLM Al-10Si-Mg alloy, the supersaturated silicon solid redissolved into the aluminum matrix and formed strengthening Mg2 Si nanopre- cipitates in the aluminum matrix. The SLM process produced extremely fine grains with high hardness. After the T6 heat treatment, the microstructure of the material changed, and stress was released, which reduced the hardness of the material. (2) The maximum and minimum erosion rates of the F and FH groups of specimens occurred at 30◦ and 90◦ , respectively. The erosion fracture was dominated by the ductile cutting mechanism. The T6 heat treatment improved the ductility of the material and generated strengthening Mg2 Si nanoprecipitates, which can improve the wear resistance of the material. (3) The tensile strength of the SLM Al-10Si-Mg alloy decreased after erosion. The high surface temperature induced by particle impingement softened the aluminum matrix and increased the elongation significantly. Moreover, erosion of the die reduced Young’s modulus and impact toughness of the SLM Al-10Si-Mg alloy. Author Contributions: Methodology, B.-C.H.; investigation, B.-C.H.; data curation, B.-C.H.; writing— original draft preparation, B.-C.H.; writing—review and editing, F.-Y.H.; supervision, F.-Y.H. All authors have read and agreed to the published version of the manuscript. Funding: This research received no external funding. Institutional Review Board Statement: Not applicable. Informed Consent Statement: Not applicable. Data Availability Statement: The data presented in this study are available on request from the corresponding author. Acknowledgments: The authors are grateful to the Instrument Center of National Cheng Kung University and the Ministry of Science and Technology of Taiwan (Grant No. MOST 108-2221-E-006- 140-MY3) for their financial support. Conflicts of Interest: The authors declare no conflict of interest.
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