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硅掺杂碳复合靶材的制备研究及溅射膜层生长形式分析
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有研资源环境技术研究院(北京)有限公司

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中图分类号:

TB321;TB44

基金项目:

有研科技集团有限公司青年基金资助(项目号13161)


Study on preparation of silicon doped carbon composite target and the growth form of sputtering film layer
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GRINM Resources and Environment Tech.Co.,Ltd,Beijing,10088

Fund Project:

Youth Fund projects of GRINM GROUP CORPRATION LIMITED

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    摘要:

    以石墨、碳化硅、硅粉体为原料,采用预处理工艺得到复合原料粉体,热压烧结制备C/Si 80/20 at%靶材。将制备的靶材在不同基片上溅射镀膜,分析薄膜的形貌及其生长模式。通过扫描电镜分析微观形貌、四探针测试电阻率、XRD结合拉曼光谱分析晶体结构,结果如下:(1)石墨和硅粉球磨混合48h可获得Si元素均匀分布的C/Si复合粉体;该粉体在1900 ℃下真空热处理时,C/Si通过互扩散生成等轴晶3C-SiC;(2)不同粒径的β-SiC粉体在1900 ℃真空热处理时,颈部生长速率和晶体结构转变存在显著差异。在高温下,纳米β-SiC粉体蒸汽压高,颈部增长速率快,通过蒸发-凝聚再结晶后可获得球形度良好的3C-SiC微米颗粒。(3)以C/Si/SiC 70/10/10 at%粉体为原料,采用球磨和高温真空热处理得到预处理粉体并热压制备C/Si 80/20 at%靶材,结果表明:与C/SiC 60/20 at%二元组分体系相比,三元组分预处理粉体制备靶材的均匀性好,平均电阻率3.9 mohm·cm,极差0.59,密度2.34 g/cm3,石墨化度0.17, 石墨晶体完整性好。(4)将制备的C/Si 80/20at%靶材分别在玻璃、硅片以及陶瓷基片上磁控溅射制备类金刚石薄膜,结果发现:在Si基体表面薄膜呈纵向生长模式,膜层微粒小于20 nm;在玻璃基体表面膜层呈层状生长模式且结合紧密;在陶瓷基体表面薄膜呈片状生长模式,膜层由微米级颗粒结合组成,与陶瓷基体的微观组织相似。

    Abstract:

    Using carbon, silicon carbide and silicon as raw material, the composite raw material powder was prepared by pretreatment process and C/Si 80/20at% target via hot pressing. The target material was then sputtered on different substrates. The micromorphology was analyzed by SEM; the resistivity was measured by four probes; the crystal structure was examined by XRD combined with Raman spectroscopy. The results yielded are: (1) Uniformly distributed C / Si powder of Si elements was obtained after consistent ball milling for 48 hours. While the powder is vacuum heat treated at 1900 ℃, liquid silicon and solid carbon generate equiaxed 3C-SiC through inter-diffusion. (2) Whenβ-SiC powders with different size were vacuum heat-treated at 1900 ℃, there was a significant disparity between neck growth rate and crystal structure transformation. Under high temperature, the nano-β-SiC powder had higher vapor pressure and its neck growth rate was relatively faster. Subsequently, pure 3C-SiC microparticles with higher sphericity were acquired after evaporation-coagulation and recrystallization. (3) Using C / Si / SiC 70/10/10 at% powder as raw materials and through ball milling /high-temperature vacuum heat treatment as pretreatment methods, C / Si 80/20 at% target was hot-pressed. The results show that: In comparison with the C / SiC 60/20 at% binary component system, the target prepared by the ternary component pretreatment powder has better uniformity, the average resistivity is 3.9×10-3 ohm · cm and the range is 0.59, the density is 2.34g / cm3, the degree of graphitization is 0.17, the graphite crystals have good integrity. (4) C / Si 80 / 20at% target was magnetron sputtered on glass, silicon wafer and ceramic substrate to deposit diamond-like thin films. The results exhibited that the film on the Si substrate had a longitudinal growth mode and the film particles were less than 20nm; The film layer on glass had a layered growth mode and were tightly bonded; The film on the ceramic substrate, composed of micron-sized particles that were similar to the microstructure of the ceramic matrix.

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白雪,刘宇阳,王星奇,桂涛,杨磊,王星明,储茂友.硅掺杂碳复合靶材的制备研究及溅射膜层生长形式分析[J].稀有金属材料与工程,2020,49(12):4207~4214.[Bai Xue, Liu Yuyang, Wang Xingqi, Gui Tao, Yang Lei, Wang Xingming, Chu Maoyou. Study on preparation of silicon doped carbon composite target and the growth form of sputtering film layer[J]. Rare Metal Materials and Engineering,2020,49(12):4207~4214.]
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  • 收稿日期:2020-05-03
  • 最后修改日期:2020-06-08
  • 录用日期:2020-06-09
  • 在线发布日期: 2021-01-13
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