Preparation and high temperature tribological properties of core-shell MoS2@SiO2 nanocomposites
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摘要: 二硫化钼(MoS2)在高温条件使用易发生氧化导致其摩擦学性能大幅劣化，表现出较高的摩擦系数。为了改善MoS2润滑剂在高温环境下的摩擦学性能，本文通过水热法和改良Stöber法生成核-壳MoS2@SiO2纳米复合材料。通过透射电子显微镜(TEM)、扫描电子显微镜(SEM)及X射线衍射仪(XRD)等对制备的纳米材料的形态、尺寸和组成进行表征。微观结果显示了核-壳结构复合材料的成功制备，平均粒径250 nm。对制备的MoS2@SiO2固体润滑涂层进行高温摩擦实验，并以MoS2涂层作为对比。采用SEM、XRD等对涂层的形貌、结构进行了表征，采用三维轮廓仪对涂层磨损率进行表征。结果表明：MoS2@SiO2涂层在680℃下的摩擦系数为0.2且较平稳，MoS2涂层则迅速失效。MoS2@SiO2涂层耐磨性更好，磨损率比MoS2涂层低25.86%。摩擦实验后MoS2@SiO2涂层磨痕区域仍存在MoS2，有润滑膜覆盖；而MoS2涂层磨痕区的基体完全暴露。由此表明，SiO2外壳的包覆延缓了MoS2在高温下的迅速氧化，且两者协同润滑，延长了涂层的使用寿命。Abstract: Molybdenum disulfide (MoS2) is easy to be oxidized when used at high temperature, which leads to significant deterioration of its tribological properties, showing a high friction coefficient. In order to improve the tribological properties of MoS2 lubricant under high temperature environment, core-shell MoS2@SiO2 nanocomposites was formed by hydrothermal method and improved Stöber method. The morphology, size and composition of the nano materials were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The micro results show that the core-shell structure composite is successfully prepared, with an average particle size of 250 nm. The high temperature friction test of prepared MoS2@SiO2 solid lubrication coating was carried out, and the MoS2 coating was used as a comparison. The morphology and structure of the coating were characterized by SEM and XRD, and the wear rate of the coating was characterized by a 3D profiler. The results show that the friction coefficient of the MoS2@SiO2 coating at 680℃ is 0.2 and relatively stable, while MoS2 coating rapidly fail. The MoS2@SiO2 coating had better wear resistance, with a wear rate at 25.86%, lower than that of MoS2 coating. After the friction tests, MoS2 still existed in the wear scar area of the MoS2@SiO2 coating, which was covered by the lubricating film. However, the substrate in the wear zone of MoS2 coating was completely exposed. It is thus shown that the encapsulation of the SiO2 shell retards the rapid oxidation of MoS2 at high temperatures and the two synergistically lubricate to prolong the service life of the coating.
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Key words:
- core-shell structure /
- molybdenum disulfide /
- solid lubricating /
- high temperature /
- composites
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图 1 (a) MoS2@SiO2的合成示意图；(b) 摩擦磨损试验示意图
TAA—Thioacetamide; PVP—Polyvinylpyrrolidone; TEOS—Tetraethyl orthosilicate
Figure 1. (a) Schematic of the preparation of MoS2@SiO2; (b) Schematic of friction and wear tests
图 2 MoS2 (a)和MoS2@SiO2 (b)的SEM图像；MoS2 (c)和MoS2@SiO2 (d)的TEM图像
Figure 2. SEM images of MoS2 (a) and MoS2@SiO2 (b); TEM images of MoS2 (c) and MoS2@SiO2 (d)
图 3 (a) MoS2@SiO2的EDS面扫描图像；相应的EDS元素分布图：(b) Si；(c) O；(d) Mo；(e) S；(f) MoS2@SiO2的EDS光谱数据
Figure 3. (a) EDS map scanning profile across the MoS2@SiO2; Corresponding EDS elemental mapping: (b) Si; (c) O; (d) Mo; (e) S; (f) EDS spectrum data of MoS2@SiO2
图 4 (a) MoS2和MoS2@SiO2的XRD衍射图谱；(b) MoS2和MoS2@SiO2的拉曼图谱
E12g—In-plane vibration mode of MoS2; A1g—Interlayer vibration mode of MoS2
Figure 4. (a) XRD patterns of MoS2 and MoS2@SiO2; (b) Raman spectra of MoS2 and MoS2@SiO2
图 6 MoS2和MoS2@SiO2在纯水中的粒径分布曲线
D10, D50, D90—Particle size with a cumulative distribution of 10%, 50%, 90%
Figure 6. Particle size distribution curves of MoS2 and MoS2@SiO2 in water
图 7 MoS2涂层 (a) 和MoS2@SiO2涂层(b)的SEM图像和元素分布
Figure 7. SEM images and elemental distributions of MoS2 coating (a) and MoS2@SiO2 coating (b)
图 8 (a) MoS2涂层和MoS2@SiO2涂层的XRD图谱；(b) MoS2涂层和MoS2@SiO2涂层在680℃高温摩擦实验之后的XRD图谱
Figure 8. (a) XRD patterns of MoS2 coating and MoS2@SiO2 coating; (b) XRD patterns of MoS2 coating and MoS2@SiO2 coating after high temperature friction test at 680℃
图 9 MoS2涂层和MoS2@SiO2涂层在680℃和室温(RT)下的摩擦系数曲线
Figure 9. Friction coefficient curves of MoS2 coating and MoS2@SiO2 coating at 680℃ and room temperature (RT)
图 10 ((a), (b)) MoS2涂层和MoS2@SiO2涂层高温摩擦实验后的对偶球形貌；((c), (d)) MoS2涂层和MoS2@SiO2涂层高温摩擦实验后的磨痕
Figure 10. ((a), (b)) Friction pairs of MoS2 coating and MoS2@SiO2 coating after friction test; ((c), (d)) Wear scar of MoS2 coating and MoS2@SiO2 coating after friction test
图 11 MoS2涂层(a)和MoS2@SiO2涂层(b) 磨损表面的三维形貌和磨痕深度曲线
Figure 11. 3D morphology and wear scar depth curve of MoS2 coating (a) and MoS2@SiO2 coating (b)
图 12 MoS2涂层(a)和MoS2@SiO2涂层(b)的磨损表面形貌和元素分布
Figure 12. Surface morphology and element distribution at wear scar of MoS2 coating (a) and MoS2@SiO2 coating (b)
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