Preparation and properties of tungsten micro-deposited on diamond (100)-(111) facets/Cu composites
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摘要: 金刚石/铜复合材料具有密度低、热导率高及热膨胀系数(CTE)可调等优点，与核心芯片具有良好的热匹配性能，在高热流密度电子封装领域具有广泛的应用前景。然而，金刚石与铜界面润湿性差，限制了其应用。为了改善金刚石与铜之间的润湿性，采用真空微沉积技术在金刚石表面沉积钨膜，并结合放电等离子烧结(SPS)技术制备了金刚石/铜复合材料。研究了金刚石(100)和(111)面钨镀层的形成、结构、复合材料断口形貌、致密性(RD)及导热性能(TC)。结果表明：在1050℃高温下，当沉积时间为60 min时，镀层表面较均匀、光滑、致密性高，且金刚石(100)面镀层的形成优先于(111)面。镀层外延生长在金刚石表面，生成了WC-W2C-W的梯度结构。复合材料的断裂由金刚石颗粒与铜基体的脱黏及铜基体的韧性断裂组成，界面结合紧密。在沉积工艺为1050℃且50 min时，镀钨金刚石颗粒镀层厚度为331.46 nm，制备的金刚石/铜复合材料致密度与导热率最高，分别为99.71%和459 W/(m·K)。Abstract: Diamond/Cu composites have the advantage of low density, high thermal conductivity and tailorable coefficient of thermal expansion (CTE), then possess a good thermal matching performance with core chips. Therefore, it has a widespread application prospect in electronic packaging with high heat flux density and other fields. However, due to the poor wettability between diamond and Cu, which restricts its application. To improve the wettability between diamond and copper, tungsten-coated diamond particles as the reinforcement particles, which were coated on diamond particles by vacuum micro-evaporation method, and diamond/copper composites were prepared by Spark plasma sintering (SPS) technique. The formation and structure of tungsten coating on diamond (100) and (111) facets, fracture morphology, relative density (RD) and thermal conductivity (TC) of the compo-sites were studied. The results show that the coating surface is uniform, smooth and compact at the high tempera-ture of 1050oC for 60 min, and the formation of diamond coating on (100) surface is preferentially compared with that on (111) surface, the gradient structure of WC-W2C-W grows epitaxial on the diamond surface. The fracture mode of the composites is composed of debonding diamond particles from copper matrix and the ductile fracture of copper, and tight interface bonding between diamond and copper are formed. The coat thickness of tungsten-coated diamond particles is 331.46 nm at 1050℃ for 50 min, and the maximum RD and TC of diamond/copper composites are 99.71% and 459 W/(m·K), respectively.
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图 2 沉积法制备镀钨金刚石/铜复合材料的流程示意图
Figure 2. Schematic of W coated diamond particles/copper composites deposited by micro-deposition method
TC—Thermal conductivity; SPS—Spark plasma sintering
图 3 放电等离子烧结技术(SPS)制备金刚石微沉积钨/铜复合材料工艺曲线
Figure 3. Process of diamond/copper composite by spark plasma sintering (SPS)
图 4 在1050℃下不同沉积时间镀钨金刚石(100)面微观组织
Figure 4. Microstructures of W-coated diamond (100) facet at 1050℃ for different holding time
图 5 在1050℃下不同沉积时间镀钨金刚石(111)面微观组织
Figure 5. Microstructure of W-coated diamond (111) facet at 1050℃ for different holding time
图 6 在1050℃下不同沉积时间镀钨金刚石XRD图谱
Figure 6. XRD patterns of W-coated diamond at 1050℃ for different holding time
图 7 金刚石镀层厚度理论与实验值对比分析
Figure 7. Theoretical and experimental thickness analysis of diamond coating
图 8 在1050oC下不同沉积时间镀钨金刚石镀层厚度
Figure 8. Thickness of W-coated diamond at 1050℃ for different holding time
D—Plating thickness
图 9 在1050℃下不同沉积时间镀钨金刚石/铜复合材料断口形貌
Figure 9. Fracture morphologies of W-coated diamond/copper composites surface at 1050℃ for different plating time
图 10 在1050℃下沉积50 min时镀钨金刚石/铜复合材料断口形貌
Figure 10. Fracture morphologies of W-coated diamond/copper composites surface at 1050℃ for 50 min
图 11 在1050℃下沉积不同时间镀钨金刚石/铜复合材料XRD图谱
Figure 11. XRD patterns of W coated diamond particles/copper composites deposited at 1050℃ for different plating time
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