CN113564525B - 一种石墨烯靶材的制备及其在磁控溅射沉积低摩擦碳薄膜中的应用 - Google Patents

一种石墨烯靶材的制备及其在磁控溅射沉积低摩擦碳薄膜中的应用 Download PDF

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CN113564525B
CN113564525B CN202110844040.4A CN202110844040A CN113564525B CN 113564525 B CN113564525 B CN 113564525B CN 202110844040 A CN202110844040 A CN 202110844040A CN 113564525 B CN113564525 B CN 113564525B
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张斌
贾倩
张俊彦
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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Abstract

本发明涉及一种石墨烯靶材的制备方法，是将石墨烯和乙二醇搅拌混合均匀，干燥至手捏可以成型的至半干状态，然后置于铣好的铜制靶座模具中，加载压力100~110 MPa，保压1~1.5小时，然后在真空中环境中干燥，即得石墨烯靶材。本发明以石墨烯靶材作为溅射碳靶，采用中频磁控溅射技术在基底上溅射沉积碳薄膜，碳薄膜具有良好的结合力，且在较宽的载荷范围内都具有稳定的摩擦学性能：在3‑11N的范围内摩擦系数稳定在0.068~0.072范围，远低于传统磁控溅射沉积的纯碳薄膜。本发明将石墨烯靶材用于溅射沉积碳薄膜，可以直接将石墨烯复合到不含氢碳薄膜中，获得优异摩擦学性能的纯碳薄膜。

Description

一种石墨烯靶材的制备及其在磁控溅射沉积低摩擦碳薄膜中 的应用
技术领域
本发明涉及一种石墨烯靶材的制备方法，同时还涉及石墨烯靶材在磁控溅射沉积低摩擦碳薄膜中的应用，属于磁控溅射技术领域和复合材料技术领域。
背景技术
碳基薄膜具有良好的机械、摩擦、生物等性能，在摩擦学领域得到了广泛的研究和应用。传统制备碳薄膜的方法主要有化学气相沉积法（CVD）、磁控溅射沉积法等。在磁控溅射沉积技术中，通常利用热解石墨等静压烧结成靶，制备的不含氢碳薄膜摩擦系数通常在0.2~0.7之间，磨损寿命短等问题，虽然可以通过等离子化学气相沉积获得含氢碳薄膜，摩擦系数可以低至0.06左右，但是因为含氢，在某些场合应用受到限制，在要求使用不含氢碳薄膜的场合，如何获得摩擦系数低至0.06，即和含氢碳薄膜摩擦系数相当的不含氢碳薄膜，一直是工程领域的挑战。
石墨烯是近代兴起的一种新材料，是目前发现的唯一存在的二维自由态原子晶体，是碳的二维材料。以sp²杂化连接的碳原子紧密堆积成单层二维蜂窝状晶格结构，是构筑零维富勒烯、一维碳纳米管、三维体相石墨等sp2杂化碳的基本结构单元。石墨烯因其特殊的六角型呈蜂巢晶格的平面结构而具有序多优异的电子及机械性能，如优异的光学、电学、力学特性，在材料学、微纳加工、能源、生物医学和药物传递等方面具有重要的应用前景，因此也被认为是一种未来革命性的材料。由于石墨烯的特殊性，由其制备的靶材应用于溅射沉积纯碳薄膜，可以直接将石墨烯复合到不含氢碳薄膜中，获得优异的摩擦学性能。
发明内容
针对上述目的，本发明提供一种了石墨烯靶材的制备方法，以用于采控溅射沉积碳薄膜的工艺中。
一、石墨烯靶的制备
本发明石墨烯靶材的制备方法，是将石墨烯和乙二醇搅拌混合均匀，干燥至手捏可以成型的至半干状态，然后置于铣好的铜制靶座模具中，加载压力100~110 MPa，保压1~1.5小时，然后在真空中环境中干燥，即得石墨烯靶材。石墨烯和乙二醇按4:1~6:1的质量比混合。其中，乙二醇仅作为分散液体起到融结作用；压靶后乙二醇挥发，对溅射形成的薄膜材料并不造成影响。
二、溅射沉积碳薄膜
采用磁控溅射技术，先在清洗后的基底表面溅射沉积Ti过渡层，然后溅射沉积碳薄膜；其具体沉积工艺：以Ti靶为靶材，使用氩气作为稀释气体，调节高功率脉冲溅射电压600~800 V，脉宽1500 ms，占空比45%，溅射沉积Ti过渡层，时间20 min；然后以石墨烯靶材为碳靶，调节气压为1.0~1.2 Pa，溅射电流为0.5~1.0 A，占空比为0.6，频率为50 kHz，偏压为-50 V，沉积不含氢碳薄膜，沉积时间为400 ~ 480 min。碳薄膜厚度为550 ~ 600nm。
使用摩擦实验机对获得碳薄膜进行测试，在较宽的载荷范围内（3~11N）都具有稳定的摩擦系数，摩擦系数在0.068~0.072范围。
本发明将石墨烯靶材用于溅射沉积碳薄膜，可以直接将石墨烯复合到不含氢碳薄膜中，获得优异摩擦学性能的纯碳薄膜。
具体实施方式
下面通过具体实施例对本发明石墨烯靶材的制备及应用作进一步说明。
实施例1
（1）石墨烯靶的制备：称量购置的石墨烯100g，乙二醇20g，于烧杯中混合均匀；将混合好的石墨烯置于干燥箱中至半干状态，手捏可以成型即可；将混合好石墨烯逐步倒入模具中，加载压力100 MPa，保压1.5小时，然后在真空中环境中保持24小时干燥，即得石墨烯靶材。
（2）碳薄膜的沉积制备及摩擦学性能
将硅片用丙酮清洗液、乙二醇清洗液对抛光后的不锈钢基底分别超声清洗20min，去除油污、锈点等表面杂质和有机污染物，然后用氮气吹干，置入镀膜真空室准备镀膜；
将真空系统抽至1.0×10-3 Pa及以下，通入氩气，调节气压为1.1 Pa，开启高偏压，偏压-800 V，对靶材表面和不锈钢样品表面进行刻蚀清洗；时间为10 min；
调节高功率脉冲溅射电压600 V，脉宽1500 ms，占空比45%，溅射沉积Ti过渡层，时间20 min；
调节溅射电流为0.5 A，占空比为0.6 ，频率为20 kHz，偏压为-50 V，溅射沉积不含氢碳薄膜，沉积时间为400 min，获得厚度约为550nm的碳薄膜；
使用摩擦实验机对获得碳薄膜进行测试，在较宽的载荷范围内（3-11N）都具有稳定的摩擦系数，摩擦系数为0.068。
实施例2
（1）石墨烯靶的制备：称量购置的石墨烯100g，乙二醇25g，于烧杯中混合均匀；将混合好的石墨烯置于干燥箱中至半干状态，手捏可以成型即可；将混合好石墨烯逐步倒入模具中，加载压力105 MPa，保压1小时，然后在真空中环境中保持24小时干燥，即得石墨烯靶材。
（2）碳薄膜的沉积制备及摩擦学性能
对抛光好的不锈钢基底进行清洗，分别用丙酮清洗液、乙二醇清洗液对硅基底超声清洗20 min，去除油污、锈点等表面杂质和有机污染物，然后用氮气吹干，置入镀膜真空室准备镀膜；
将真空系统抽至1.0×10-3 Pa及以下，通入氩气，调节气压为1.0 Pa，开启高偏压，偏压-800 V，对靶材表面和不锈钢样品表面进行刻蚀清洗；时间为10min；
调节高功率脉冲溅射电压800 V，脉宽1500 ms，占空比45%，溅射沉积Ti过渡层，时间20 min；
调节溅射电流为1.0 A，占空比为0.6 ，频率为20 kHz，偏压为-50 V，沉积不含氢碳薄膜，沉积时间为480 min，获得厚度约为600nm的碳薄膜；
使用摩擦实验机对获得碳薄膜进行测试，在较宽的载荷范围内（3~11N）都具有稳定的摩擦系数，摩擦系数为0.072。
实施例3
（1）石墨烯靶的制备
称量购置的石墨烯102g，乙二醇17g，于烧杯中混合均匀；将混合好的石墨烯置于干燥箱中至半干状态，手捏可以成型即可；将混合好石墨烯逐步倒入模具中，加载压力110MPa，保压1.5小时，然后在真空中环境中保持24小时干燥，即得石墨烯靶材。
（2）碳薄膜的沉积制备及摩擦学性能
对抛光好的轴承钢基底进行清洗，分别用丙酮清洗液、乙二醇清洗液对硅基底超声清洗20 min，去除油污、锈点等表面杂质和有机污染物，然后用氮气吹干，置入镀膜真空室准备镀膜；
将真空系统抽至1.0×10-3 Pa及以下，通入氩气，调节气压为1.2 Pa，开启高偏压，偏压-800 V，对靶材表面和不锈钢样品表面进行刻蚀清洗；时间为10min；
调节高功率脉冲溅射电压700 V，脉宽1500 ms，占空比45%，溅射沉积Ti过渡层，时间20 min；
调节溅射电流为0.8 A，占空比为0.6 ，频率为20 kHz，偏压为-50 V，沉积不含氢碳薄膜，沉积时间为480 min，获得厚度约为580nm的碳薄膜；
使用摩擦实验机对获得碳薄膜进行测试，在较宽的载荷范围内（3-11N）都具有稳定的摩擦系数，摩擦系数为 0.070。

Claims (4)

1.一种用于磁控溅射沉积低摩擦碳薄膜石墨烯靶材的制备方法，是将石墨烯和乙二醇按4:1~6:1的质量比搅拌混合均匀，干燥至手捏可以成型的至半干状态，然后置于铣好的铜制靶座模具中，加载压力100~110 MPa，保压1~1.5小时，然后在真空中环境中干燥，即得石墨烯靶材。
2.如权利要求1所述方法制备的石墨烯靶材在溅射沉积碳薄膜中的应用，其特征在于：采用磁控溅射技术，先在清洗后的基底表面溅射沉积Ti过渡层，然后溅射沉积碳薄膜；其具体沉积工艺：以Ti靶为靶材，使用氩气作为稀释气体，调节高功率脉冲溅射电压600~800 V，脉宽1500 ms，占空比45%，溅射沉积Ti过渡层，时间20 min；然后以石墨烯靶材为碳靶，调节气压为1.0 ~ 1.2 Pa，溅射电流为0.5~1.0 A，占空比为0.6，频率为50 kHz，偏压为-50 V，沉积谈薄膜，沉积时间为400~480 min。
3.如权利要求2所述石墨烯靶材在溅射沉积碳薄膜中的应用，其特征在于：碳薄膜的沉积中，电流可以是中频电流或高功率脉冲电流。
4.如权利要求2所述石墨烯靶材在溅射沉积碳薄膜中的应用，其特征在于：所述基底为单晶硅、不锈钢、轴承钢中的一种。
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