WO2019119647A1 - 一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法 - Google Patents

一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法 Download PDF

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WO2019119647A1
WO2019119647A1 PCT/CN2018/077979 CN2018077979W WO2019119647A1 WO 2019119647 A1 WO2019119647 A1 WO 2019119647A1 CN 2018077979 W CN2018077979 W CN 2018077979W WO 2019119647 A1 WO2019119647 A1 WO 2019119647A1
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target
fullerene
graphene
layer
boron nitride
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PCT/CN2018/077979
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French (fr)
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张俊彦
张斌
王永富
强力
高凯雄
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中国科学院兰州化学物理研究所
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Publication of WO2019119647A1 publication Critical patent/WO2019119647A1/zh
Priority to US16/897,881 priority Critical patent/US11225710B2/en

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Definitions

  • the invention belongs to the field of lubrication and protection, and relates to a preparation method of a fullerene-like carbon layer/graphene-like boron nitride multi-layer composite super-lubricating film.
  • thin film materials have been widely used in various fields such as lubrication, computer field, cloud storage, sensors, precision sports machinery, microelectronics, aerospace and nuclear industry, and their application scope and functions are continuously expanding.
  • Thin film materials have been used in the field of lubrication for many years. Practice has shown that friction and wear mostly occur on the surface and subsurface of the material. Therefore, the key to improving the tribological properties of materials is how to improve the surface properties of the materials. By forming a film on the surface of the material, the tribological properties of the surface of the material can be effectively changed without changing the properties of the material itself, so that the material can meet different application requirements.
  • the fullerene-based carbon film has been favored by the scientific community and the industry as an advanced solid lubricating material because of its low friction coefficient, high hardness, good elastic recovery and excellent wear resistance.
  • Boron nitride has a layered structure similar to graphite. Each layer is composed of many flat hexagonal elements. The layers are combined by van der Waals force and the layers have very low shear force. The great potential of superlubricated materials. Very stable in the air, able to withstand 2270K high temperature, sublimation at 3270K. Therefore, hexagonal boron nitride can be attracting attention as a high-temperature solid lubricating material.
  • Multi-layer composite films will overcome the shortcomings of a single film, exert their respective advantages, and complement each other to obtain the high-quality film of the above requirements.
  • Multilayer composite films have attracted much attention due to their ease of achieving ultra-lubrication, low stress and wear resistance.
  • Ultra-lubrication refers to the phenomenon that the friction between two contact surfaces is almost zero or even disappears. It is generally considered that the friction coefficient must be less than 0.01. Therefore, it is a reality to combine the superior properties of two or more kinds of films to exert their respective advantages, so that the super-lubrication performance of the multilayer composite film is achieved.
  • the invention mainly combines the high load-bearing of a fullerene-like carbon film and the low shearing force of a graphene-like boron nitride film under high temperature conditions, thereby obtaining a high-temperature superlubricating composite film.
  • the invention obtains a multilayer structure of a fullerene-like film and a graphene-like boron nitride film, which effectively weakens the residual stress, significantly improves the bonding force between the film and the substrate, and solves the problem that the boron nitride film is high. Defects produced by density particle bombardment.
  • a preparation method of a fullerene-like carbon layer/graphene-like boron nitride multi-layer composite super-lubricating film characterized in that the specific steps are:
  • Step 3) and step 4) are repeated, and a multilayer composite film is obtained by superposition deposition in the order of ABAB ... ABA over 60-80 cycles.
  • the substrate is a metal or a ceramic.
  • the fullerene-like carbon layer has a thickness of 6 to 12 nm
  • the graphene-like boron nitride layer has a thickness of 2.1 to 3.5 nm
  • the multilayer composite film has a total thickness of 2 to 3.5 ⁇ m.
  • the fullerene-like carbon layer is prepared by high-vacuum medium-frequency magnetron sputtering of methane or acetylene.
  • the pressure in the chamber is controlled at 10-15 Pa
  • the pulse negative bias is controlled at 800-1000 V
  • the duty cycle is controlled at 60%-80. %
  • sputtering time is 10-50 min.
  • the graphene-like boron nitride layer is sputtered with an elemental boron target in a N 2 and Ar atmosphere by a high vacuum medium frequency magnetron sputtering coating device, the N 2 purity is greater than 99.99%, the flow rate is controlled at 55-95 sccm, and the Ar purity is greater than 99.99. %, flow control is 60-120sccm, cavity pressure is controlled at 0.4-0.5Pa, pulse negative bias is controlled at 400-1000V, duty cycle is controlled at 60%-80%, and sputtering time is 10-50min.
  • the target used for the magnetron sputtering is a rectangular target, a circular target, or a spin target.
  • the purity of the elemental boron target boron is greater than 99.9%, and is obtained by a hot press forming process, the target length is 60-90 cm, the target width is 10-20 cm, and the target height is 1-5 cm.
  • the multi-layer composite film of the invention can be applied to the wear resistance and the friction coefficient of the surface of metal and ceramic materials under high temperature conditions, and the friction coefficient is adjusted between 0.004 ⁇ 0.002 in the presence of high temperature aerobic conditions.
  • the fullerene-like carbon layer A and the graphene-like boron nitride layer B of the present invention are deposited layer by layer to obtain a multilayer composite film excellent in performance, and the hardness varies between 20 and 36 GPa.
  • the film prepared by the invention has high load-bearing, high-temperature resistance, oxidation resistance and super-lubricating property, the friction coefficient is as low as 0.004, and the wear rate is reduced by 70%.
  • the high temperature is increased to 600-2000 ° C, and the life is increased by 2-3 times.
  • Figure 1 is a schematic sectional view showing a multilayer film of the present invention.
  • Table 1 is a summary of the experimental conditions and results of friction and wear.
  • the film prepared above had a hardness of 25 GPa, a bonding force of 60 GPa, and a coefficient of friction of 0.004.
  • the performance of the fullerene-like carbon layer/graphene-nitride-boron multilayer super-lubricating film prepared by the invention was tested by BASALT-N2 friction and wear tester.
  • the test conditions were: ball-disk reciprocating friction mode, load 20N The frequency of 5 Hz, the stroke of 5 mm, the temperature of 27 ° C, the humidity of 38%, the film of the invention was prepared on a stainless steel sheet, and the dual ball was made of GCr15 bearing steel with a diameter of 6 mm.
  • the results showed that the coefficient of friction was stabilized at 0.006 and the wear rate was as low as 3.4 ⁇ 10 -9 m 3 /Nm, indicating that the film prepared by the present invention has ultra-lubrication and an extremely low wear rate.

Abstract

本发明公开了一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法，具体步骤为：1)依次在无水乙醇和丙酮中超声清洗基底15min-30min；2)氩等离子体轰击清洗基底15min；3)利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；4)利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；5)重复步骤3)和步骤4)，经过60-80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。本发明制备的多层复合超润滑薄膜将克服单一薄膜的缺点，发挥各自的优点，取长补短，从而获得高承载、耐磨损、耐高温和超润滑的高性能薄膜。

Description

一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法 技术领域
本发明属于润滑与防护领域，涉及一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法。
背景技术
目前，薄膜材料已经广泛地应用于润滑领域、计算机领域、云储存、传感器、精密运动机械、微电子学、航空宇航和核工业等各个行业中，其应用范围和作用还在不断地扩大。
薄膜材料应用于润滑领域已有多年。实践表明，摩擦与磨损大多数发生在材料表面和亚表面。因此，提高材料摩擦学性能的关键是如何提高材料的表面性能。通过在材料的表面形成薄膜，可以在不改变材料本身性质的同时有效地改变材料表面的摩擦学性能，从而使材料满足不同的使用要求。
然而，随着航空宇航、云储存、大数据、柔性可穿戴等新技术产业的迅速发展，不仅对极端苛刻工况(真空、高低温交变、高速、高负载等)条件下服役的润滑薄膜材料提出了更加严格的要求，而且由于装备的高可靠、高精度和长寿命方面的要求，对具有超低摩擦和多环境适应性的新型润滑薄膜材料也提出了越来越迫切的需求。
类富勒烯结构碳膜，因其具有低的摩擦系数、高硬度、良好的弹性恢复以及优良的耐磨性能，已作为一种先进的固体润滑材料而受到科学界和工业界的青睐。
氮化硼(h-BN)，具有与石墨相似的层状结构，每一层由许多扁平的六角形单元构成，层间以范德华力相结合，层间具有极低的剪切力，具备成为超润滑材料的巨大潜质。在空气中非常稳定，能耐受2270K的高温，在3270K时升华。因此，六方氮化硼可以作为高温固体润滑材料而备受关注。
然而，薄膜材料的研制已经从单层、单一组分向复合化、梯度化和多层化发展。单一的薄膜已经无法满足苛刻的工况和众多设备对高可靠、高精度和长寿命方面的要求，迫切地需要我们制备出性能优异和多环境适应的可靠薄膜。多层复合薄膜将克服单一薄膜的缺点，发挥各自的优点，取长补短，而获得上述需求的 高质量薄膜。
多层复合薄膜因其易于实现超润滑、低应力和耐磨损而备受关注。超润滑是指两接触面间摩擦力几乎为零甚至消失的现象，通常认为摩擦系数须小于0.01。因此，综合两种或多种薄膜各自的优异性能，发挥各自优点，使得多层复合薄膜获得超润滑性能成为了现实。
发明内容
本发明的目的在于提供一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法。
本发明主要综合了类富勒烯碳膜的高承载和类石墨烯氮化硼薄膜在高温条件下的低剪切力特点，从而获得高温超润滑复合薄膜。本发明获得了类富勒烯薄膜和类石墨烯氮化硼薄膜的多层结构，该结构有效地削弱了残余应力，显著提高了薄膜与基底间的结合力，解决了氮化硼薄膜在高密度粒子轰击下产生的缺陷。
一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法，其特征在于具体步骤为：
1)依次在无水乙醇和丙酮中超声清洗基底15min-30min；
2)氩(Ar)等离子体轰击清洗基底15min；
3)利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；
4)利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；
5)重复步骤3)和步骤4)，经过60-80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。
所述基底为金属或陶瓷。
所述类富勒烯碳层的厚度为6-12nm，类石墨烯氮化硼层的厚度为2.1-3.5nm，多层复合薄膜的总厚度为2-3.5μm。
所述类富勒烯碳层由甲烷或乙炔经高真空中频磁控溅射制备，腔体内压力控制在10-15Pa，脉冲负偏压控制在800-1000V，占空比控制在60％-80％，溅射时间为10-50min。
所述类石墨烯氮化硼层利用高真空中频磁控溅射镀膜设备在N 2和Ar氛围中溅射单质硼靶，N 2纯度大于99.99％，流量控制在55-95sccm，Ar纯度大于99.99％， 流量控制在60-120sccm，腔体内压力控制在0.4-0.5Pa，脉冲负偏压控制在400-1000V，占空比控制在60％-80％，溅射时间为10-50min。
所述磁控溅射所用靶为矩形靶、圆靶或旋转柱靶。
所述单质硼靶硼的纯净度大于99.9％，采用热压成型工艺获得，靶长60-90cm，靶宽10-20cm，靶高1-5cm。
本发明所述多层复合薄膜可以应用于高温条件下金属和陶瓷材质表面的耐磨损和降低摩擦系数，在高温有氧存在的条件下摩擦系数在0.004±0.002之间调整。
本发明所述类富勒烯碳层A和类石墨烯氮化硼层B逐层叠加沉积，获得性能优异的多层复合薄膜，硬度在20-36GPa之间变化。
和单层类富勒烯薄膜以及单层氮化硼薄膜相比较，本发明制备的薄膜具有高承载、耐高温、抗氧化和超润滑性能，摩擦系数低至0.004，磨损率降低70％，承受的高温提升至600-2000℃，寿命提高2-3倍。
附图说明
图1是本发明多层薄膜的断面示意图。
表1是摩擦磨损实验条件及结果汇总表。
具体实施方式
实施例1
1.类富勒烯碳层/类石墨烯氮化硼多层复合薄膜的制备步骤如下所述：
(1)超声清洗基片：首先用无水乙醇和丙酮超声清洗304不锈钢片15min，用氮气吹干，将基片置于腔体中与靶相距80mm，开始抽真空；
(2)溅射清洗基片：当腔体中压力低于5×10 -5Pa，通入氩气，氩气流量为120sccm，脉冲偏压-1000V，占空比70％，氩(Ar)等离子体轰击清洗基片15min，已去除基片表面的氧化物和其他杂质；
(3)类富勒烯碳膜的沉积：打开CH 4气体，调节CH 4流量为80sccm，调节Ar流量120sccm,保持腔体内压强为15Pa，偏压调节至-800V，溅射时间30min；
(4)类石墨烯氮化硼的沉积：关闭CH 4气体，打开N 2，调节N 2流量为80sccm，Ar流量为90sccm，保持腔体内压强为0.45Pa，打开单质硼靶挡板，硼靶通电，调节溅射靶电流为1A，脉冲偏压从-400V开始，每5min偏压升高-100V，偏压 升至-600V后保持10min，溅射时间总共20min；
(5)重复步骤(3)和(4)，连续镀膜80个周期，总厚度1.04μm；
(6)上述所制备薄膜硬度25GPa，结合力60GPa,摩擦系数0.004。
2.采用BASALT-N2摩擦磨损试验机对本发明制备的类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜进行性能测试，测试条件为：球-盘往复摩擦模式，载荷20N，频率5Hz，行程5㎜，温度27℃，湿度38％，在不锈钢片上制备有本发明的薄膜，对偶球采用GCr15轴承钢，直径6mm。结果显示，摩擦系数稳定在0.006，磨损率低至3.4×10 -9m 3/Nm，表明本发明制备的薄膜具有超润滑和极低的磨损率。

Claims (7)

  1. 一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法，其特征在于具体步骤为：
    1)依次在无水乙醇和丙酮中超声清洗基底15min-30min；
    2)氩等离子体轰击清洗基底15min；
    3)利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；
    4)利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；
    5)重复步骤3)和步骤4)，经过60-80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。
  2. 如权利要求1所述的制备方法，其特征在于所述基底为金属或陶瓷。
  3. 如权利要求1所述的制备方法，其特征在于所述类富勒烯碳层的厚度为6-12nm，类石墨烯氮化硼层的厚度为2.1-3.5nm，多层复合薄膜的总厚度为2-3.5μm。
  4. 如权利要求1所述的制备方法，其特征在于所述类富勒烯碳层由甲烷或乙炔经高真空中频磁控溅射制备，腔体内压力控制在10-15Pa，脉冲负偏压控制在800-1000V，占空比控制在60％-80％，溅射时间为10-50min。
  5. 如权利要求1所述的制备方法，其特征在于所述类石墨烯氮化硼层利用高真空中频磁控溅射镀膜设备在N 2和Ar氛围中溅射单质硼靶，N 2纯度大于99.99％，流量控制在55-95sccm，Ar纯度大于99.99％，流量控制在60-120sccm，腔体内压力控制在0.4-0.5Pa，脉冲负偏压控制在400-1000V，占空比控制在60％-80％，溅射时间为10-50min。
  6. 如权利要求1所述的制备方法，其特征在于所述磁控溅射所用靶为矩形靶、圆靶或旋转柱靶。
  7. 如权利要求1所述的制备方法，其特征在于所述单质硼靶硼的纯净度大于99.9％，采用热压成型工艺获得，靶长60-90cm，靶宽10-20cm，靶高1-5cm。
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