CN114318217B - 一种真空滑动电接触条件下具有超低摩擦低电噪音二硒化铌薄膜的制备方法 - Google Patents
一种真空滑动电接触条件下具有超低摩擦低电噪音二硒化铌薄膜的制备方法 Download PDFInfo
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Abstract
本发明涉及一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，是采用直流封闭场磁控溅射法制备，通过低沉积气压和低溅射能量的工艺设计，一方面保持了NbSe2溅射产物的纯度，避免了NbSe3等干扰相的产生，大幅改善了溅射NbSe2薄膜的导电性；另一方面形成了纳米晶/非晶超晶格复合结构，兼具了优异的力学和润滑性能，在真空滑动电接触条件下，与常见的电镀金涂层相比，摩擦系数由0.25降至0.02，磨损寿命提高7倍以上，达到100000次以上，电噪声降低50%左右。本发明技术可广泛适用于航天、航空领域导电滑环、滑桶、天线等滑动电接触运动部件的表面润滑处理。
Description
技术领域
本发明涉及一种二硒化铌润滑薄膜的制备方法，尤其涉及一种真空滑动电接触条件下具有超低摩擦和低电噪音二硒化铌（NbSe2）薄膜的制备方法，属于润滑材料技术领域。
背景技术
滑动电接触是一种特殊的机械设计，用于在滑动接触状态下传输电能和信号。在航空航天领域得到了广泛的应用，发挥着重要的作用。例如，导电滑环负责将太阳能电池板收集的能量传输到航天器系统。滑动电接触材料的润滑和耐磨性直接决定了整个系统的稳定性和可靠性。然而滑动电接触条件对润滑材料的损伤破坏极为严重，既受到机械因素的制约，又受到电流热效应的影响，同时还存在严重的电弧侵蚀损伤，极大地限制了润滑材料的选材与使用。特别是对于航空航天领域，还会涉及到真空环境下使用，目前主要采用了金、铂等贵金属。但贵金属摩擦副在载流时会表现出严重的粘着磨损，摩擦系数通常在0.3以上，严重影响其磨损寿命。
二硒化铌（NbSe2）材料具有类似于MoS2的层状易剪切结构，具有优异的润滑属性，同时由于其电子结构的特异性，表现出金属导电性，作为真空滑动电接触条件使用的新型润滑材料具有巨大的潜力。但是如何制备出能够耐受真空载流耦合苛刻条件的NbSe2表面处理技术是关键难点。CN202110844056.5公开一种NbSe2粘结固体涂层的方法，真空载流摩擦条件下摩擦系数可以稳定在0.05左右，相比于电镀金涂层已显现出明显的改善效果。但寿命改善效果还不明显，寿命约22000次循环，距离未来服役寿命要求还有差距。AppliedSurface Science 455, 2018, 1161和CN201810261644.4公开了射频磁控溅射法制备NbSe2薄膜，表现出大气非载流条件下的润滑和导电双重功能特性，但制备的薄膜中存在一些干扰物质，如NbSe3，这会对润滑和导电性能产生不利影响。如电阻率仅能达到1×10-3 Ω·cm量级，相对于现役的电镀金涂层（电阻率为2.4×10-6 Ω·cm）导电性仍相差三个数量级，尚不能耐受空间特殊的真空载流电接触苛刻工况，并且满足低摩擦、长寿命、高传输、低噪音等方面的高标准要求。
发明内容
本发明的目的在于提供一种真空滑动电接触条件下具有超低摩擦和低电噪音NbSe2润滑薄膜的制备方法。
一、NbSe2润滑薄膜的制备
本发明真空滑动电接触条件下具有超低摩擦和低电噪音NbSe2润滑薄膜的制备，采用直流封闭场磁控溅射法，通过低沉积气压和低溅射能量的工艺设计，保障了NbSe2溅射薄膜的纯度和晶体结构，赋予其优异的真空载流摩擦学性能。镀制过程在一个具有四个靶位的直流封闭场磁控溅射沉积系统上完成。其中两个靶装配钛靶材，连接有一台直流溅射电源进行激励；另两个靶装配NbSe2靶材，也连接有一台直流溅射电源进行激励；样品架连接有一台脉冲负偏压电源（20~60KHz）施加负电压。其结构示意图见图1。具体工艺如下：
（1）将表面清洁的待镀膜基底安置于镀膜腔体内样品台上，进行氩气等离子体清洗刻蚀，去除基底表面残留的杂质和污染物。待镀膜基底的材质为铜、铝、钛合金或钢。氩气等离子体清洗刻蚀工艺如下：镀膜腔体真空室本底真空气压低于3×10-3 Pa；清洗气压稳定在0.8~2.0 Pa，基体负偏压-400~-800V。
（2）以氩气为溅射气体，钛靶为溅射靶材，在基底表面制备钛过渡层，以提高基底与NbSe2薄膜的膜基结合强度；Ti靶材纯度高于99.8%；溅射气压为0.1~0.5 Pa；靶溅射功率范围为0.5~10 W/cm2；基体负偏压为-50~-400 V；Ti层厚度为0.1~1 um。
（3）以氩气为溅射气体，NbSe2靶为溅射靶材，制备NbSe2润滑层。NbSe2靶材纯度高于99.9%；溅射气压为0.04~0.3 Pa；靶溅射功率范围为0.2~1 W/cm2；基体负偏压为-50~-400 V；NbSe2层厚度为1~5 um。
图2为本发明制备NbSe2润滑薄膜X射线衍射图谱。通过图2可以看出，仅显现出NbSe2晶相的衍射峰，并未有常见的NbSe3等不利于润滑和导电性质的干扰相产生。
图3为本发明制备NbSe2润滑薄膜高分辨透射电子显微镜照片。通过图3可以看出，NbSe2润滑薄膜具有纳米晶/非晶超晶格复合结构，可以有效阻止位错的迁移，而且还可以通过晶界滑移机制释放内应力，因而兼具优异的力学和润滑性能。
二、NbSe2润滑薄膜的性能
1、静态电阻率
测试方法：采用四探针法。
测试结果：本发明NbSe2润滑薄膜静态电阻率可达7.8×10-6 Ω·cm，与现役的电镀金涂层电阻率（2.4×10-6 Ω·cm）处于同一水平量级。
2、真空载流摩擦学性能
测试方法：真空载流摩擦磨损实验机，真空度1.0×10-5 mbar，球-盘接触线性往复运动模式，上试样为直径6mm的GCr15商品钢球，下试样为镀制有NbSe2润滑薄膜的平面铜试片，法向载荷为1 N，施加电流为1.0 A，往复滑动振幅为5mm，频率为5Hz。
测试结果：本发明NbSe2润滑薄膜与现役的电镀金涂层相比，在真空载流摩擦学性能方面有较大的改善。图4为本发明制备的NbSe2润滑薄膜与现役电镀金涂层的真空载流摩擦学性能对比：(a) 摩擦曲线；(b) 接触电噪音。可以看出，本发明NbSe2润滑薄膜的摩擦系数由0.25降至0.02，磨损寿命提高7倍以上，达到100000次仍未失效，接触电压和电镀金处于同一水平量级，电噪声降低50%左右。
综上所述，以真空等静压法压制的NbSe2块体为溅射靶材，以氩气为离化溅射气体，利用封闭场高离化率的优势，可以在低于常规溅射一个量级的沉积气压下溅射，并结合直流溅射低的溅射能量，极大地减少了溅射过程中对NbSe2溅射产物的破坏作用，避免了NbSe3等干扰相的产生，大幅改善了溅射NbSe2薄膜的导电性；同时形成了纳米晶/非晶超晶格复合结构，可以有效阻止位错的迁移，而且还可以通过晶界滑移机制释放内应力，兼具了优异的力学和润滑性能。最终使其能够耐受真空载流耦合苛刻条件，展现出超低的摩擦系数、长寿命和低电噪音综合性能优势，可广泛适用于航天、航空领域导电滑环、滑桶、天线等滑动电接触运动部件的表面润滑处理。
附图说明
图1为 NbSe2润滑薄膜直流封闭场磁控溅射沉积系统示意图；
图2为本发明制备NbSe2润滑薄膜X射线衍射图谱；
图3为本发明制备NbSe2润滑薄膜高分辨透射电子显微镜照片；
图4为本发明制备NbSe2润滑薄膜与现役电镀金涂层的真空载流摩擦学性能对比：（a）摩擦曲线；（b）接触电压；（c）接触电噪音。
具体实施方式
实施例1
1）氩气等离子体清洗待镀样品：将表面清洁的铜材质滑环及铜、铝、9Cr18、TC4试块安置于镀膜腔体内样品台上，真空腔内气压抽至3.0×10-3 Pa以下；通入高纯氩气至气压为1.8 Pa。打开负偏压电源，调节电压值为-600 V，进行氩气等离子体轰击清洗20 min，去除基底表面残留的杂质和污染物；
2）沉积钛过渡层：调节氩气流量，使腔体气压维持在0.1Pa，打开钛靶直流溅射电源和负偏压电源，调节钛靶溅射功率密度为0.3 W/cm2，负偏压为-50 V，沉积0.2 μm厚度；
3）沉积NbSe2导电润滑层：调节氩气流量，使腔体气压维持在0.05 Pa。关闭钛靶直流溅射电源，打开NbSe2靶直流溅射电源，调节NbSe2靶溅射功率为0.3 W/cm2，调节负偏压电源负偏压为-50 V，沉积2 μm厚度后原位充入Ar气自然冷却，当温度稳定至室温时，释放真空取出样品；
4）薄膜性能：静态电阻率8.6×10-6Ω·cm，真空载流条件下摩擦系数0.025，磨损寿命100000次仍未失效。
实施例2
1）氩气等离子体清洗刻蚀待镀样品：将表面清洁的铜材质滑环及铜、铝、9Cr18、TC4试块安置于镀膜腔体内样品台上，真空腔内气压抽至3.0×10-3 Pa以下，通入高纯氩气至气压为0.8 Pa；打开负偏压电源，调节电压值为-800 V，进行氩气等离子体轰击清洗30min，去除基底表面残留的杂质和污染物；
2）沉积钛过渡层：调节氩气流量，使腔体气压维持在0.3 Pa；打开钛靶直流溅射电源和负偏压电源，调节钛靶溅射功率密度为1.5 W/cm2，负偏压为-200V，沉积0.4μm厚度；
3）沉积NbSe2导电润滑层：调节氩气流量，使腔体气压维持在0.15Pa。关闭钛靶直流溅射电源，打开NbSe2靶直流溅射电源，调节NbSe2靶溅射功率为0.5 W/cm2，调节负偏压电源负偏压为-150 V，沉积3.5μm厚度后原位充入Ar气自然冷却，当温度稳定至室温时，释放真空取出样品；
4）薄膜性能：静态电阻率7.8×10-6 Ω·cm，真空载流条件下摩擦系数0.022，磨损寿命100000次仍未失效。
实施例3
1）氩气等离子体清洗刻蚀待镀样品：将表面清洁的铜材质滑环及铜、铝、9Cr18、TC4试块安置于镀膜腔体内样品台上，真空腔内气压抽至3.0×10-3 Pa以下，通入高纯氩气至气压为1.2 Pa。打开负偏压电源，调节电压值为-400 V，进行氩气等离子体轰击清洗40min，去除基底表面残留的杂质和污染物；
2）沉积钛过渡层：调节氩气流量，使腔体气压维持在0.5 Pa，打开钛靶直流溅射电源和负偏压电源，调节钛靶溅射功率密度为8.5 W/cm2，负偏压为-350 V，沉积0.8 μm厚度；
3）沉积NbSe2导电润滑层：调节氩气流量，使腔体气压维持在0.3 Pa。关闭钛靶直流溅射电源，打开NbSe2靶直流溅射电源，调节NbSe2靶溅射功率为0.9 W/cm2，调节负偏压电源负偏压为-350 V，沉积4.5 μm厚度后原位充入Ar气自然冷却，当温度稳定至室温时，释放真空取出样品；
4）薄膜性能：静态电阻率9.2×10-6 Ω·cm，真空载流条件下摩擦系数0.029，磨损寿命100000次仍未失效。
Claims (5)
1.一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，其特征在于：采用直流封闭场磁控溅射法制备，采用低沉积气压和低溅射能量的工艺设计，包括以下步骤：
（1）将表面清洁的待镀膜基底安置于镀膜腔体内样品台上，进行氩气等离子体清洗刻蚀，去除基底表面残留的杂质和污染物；
（2）以氩气为溅射气体，钛靶为溅射靶材，在基底表面制备钛过渡层，以提高基底与NbSe2薄膜的膜基结合强度；
（3）以氩气为溅射气体，NbSe2靶为溅射靶材，制备NbSe2润滑层；溅射气压为0.04~0.3Pa；靶溅射功率范围为0.2~1 W/cm2；基体负偏压为-50~-400 V。
2.如权利要求书1所述一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，其特征在于：步骤（1）中，镀膜腔体真空室本底真空气压低于3×10-3 Pa；清洗气压稳定在0.8~2.0 Pa，基体负偏压-400~-800V。
3.如权利要求1所述一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，其特征在于：步骤（2）中，Ti靶材纯度高于99.8%；溅射气压为0.1~0.5 Pa；靶溅射功率范围为0.5~10 W/cm2；基体负偏压为-50~-400 V；Ti层厚度为0.1~1 um。
4.如权利要求1所述一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，其特征在于：NbSe2靶材纯度高于99.9%，NbSe2层厚度为1~5 um。
5.如权利要求1所述一种真空滑动电接触条件下具有超低摩擦低电噪音NbSe2薄膜的制备方法，其特征在于：待镀膜基底的材质为铜、铝、钛合金或钢。
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