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CN111570239B - 惰性环境中摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法 - Google Patents

惰性环境中摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法 Download PDF

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CN111570239B
CN111570239B CN202010406011.5A CN202010406011A CN111570239B CN 111570239 B CN111570239 B CN 111570239B CN 202010406011 A CN202010406011 A CN 202010406011A CN 111570239 B CN111570239 B CN 111570239B
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李红轩
吉利
高雪
刘晓红
周惠娣
陈建敏
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种惰性环境中利用摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法，是先将氧化石墨烯超声分散在挥发性溶剂中，并喷涂于基体表面形成氧化石墨烯涂层；然后在惰性环境中，采用具有化学活性键的摩擦配副，并施加正压力，在氧化石墨烯涂层表面进行干摩擦，在摩擦滑移轨道上原位形成完美结构的石墨烯涂层。在摩擦剪切力的作用下，氧化石墨烯的羟基官能团与摩擦配副上的活性键相互作用，氧化石墨烯上的C‑OH键发生断裂。断裂后碳原子由sp3态向能量更稳定的sp2态转化，实现六元环结构的修复，在摩擦滑移轨道上形成石墨烯结构。由于摩擦剪切力在摩擦滑移轨道上的氧化石墨烯涂层发生向完美石墨烯结构的原位大尺度转变，并且展现出优异的润滑性能。

Description

惰性环境中摩擦力还原氧化石墨烯原位制备石墨烯涂层的 方法
技术领域
本发明涉及了一种石墨烯涂层的制备方法，尤其涉及一种在惰性环境中利用摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法，属于纳米材料和固体润滑领域。
背景技术
得益于石墨烯独特的六角型呈蜂巢晶格的二维碳纳米结构，研究者们发现了石墨烯具有许多优异的特性，包括电学、光学、力学以及摩擦学等。但是这些特性强烈依赖于石墨烯的完美二维结构，一旦理想二维结构破坏，许多特性就会丧失。以摩擦学性能为例，研究发现当微观的纳米针尖在理想的石墨烯片上层发生相对运动时，会出现摩擦系数接近为零的超润滑状态，但当有缺陷存在或者官能团（如氧化石墨烯、氟化石墨烯等）存在时，摩擦系数就会显著变大。因此如何实现宏观大尺寸理想石墨烯结构的可控制备是非常重要的，对于实现石墨烯众多优异特性的工程实用化具有极大的价值。
研究者们致力于在不同领域尝试不同方法以求制备高质量、大面积石墨烯材料。CVD法制备的石墨烯薄膜结构较为完美，尺寸较大，但由于较小的产量以及较薄的厚度，在工程应用中受到限制。氧化石墨烯作为石墨烯的衍生物，较石墨烯具有分散性好、机械强度高、易批量制备等优势，具有更大的工程应用价值。目前规模化产量的石墨烯主要来源于还原氧化石墨烯粉末材料，但在还原过程中需要高温、强还原剂等苛刻反应条件，并且还存在着大量的缺陷和其他官能团，通常需要进一步结构缺陷以获得高质量的石墨烯。文献1（Wei, Z. et al. Nanoscale tunable reduction of graphene oxide for grapheneelectronics. Science 328, 1373-1376（2010）.）和文献2（Raghuraman, S., Elinski,M.B., Batteas, J.D. & Felts, J.R. Driving surface chemistry at the nanometerscale using localized heat and stress. Nano letters 17, 2111-2117（2017）.）报道了以氧化石墨烯为前驱物，通过纳米针尖局部加热或者加压实现氧化石墨烯向石墨烯原位转化的方法，这有助于阐明氧化石墨烯结构原位调控和转化。但这一方法是在纳米尺度上实现的，离工程化大尺度应用尚存在很大差距。
发明内容
本发明的目的在于提供一种利用摩擦力还原氧化石墨烯原位大尺度，简单易行制备石墨烯涂层的方法。
一、石墨烯涂层的原位制备
本发明制备石墨烯涂层的方法，是以氧化石墨烯涂层为原材料，在惰性环境中利用摩擦剪切力原位形成石墨烯涂层。具体制备方法包括以下步骤：
（1）将氧化石墨烯超声分散在挥发性溶剂中，并喷涂于基体表面形成氧化石墨烯涂层。
挥发性溶剂采用丙酮、丁酮、无水乙醇、甲苯等。氧化石墨烯在挥发性溶剂中的质量比百分数为0.2-1.0%。超声分散时间为2-6小时。
基体可以为钢、钛、铝等金属，也可以为硅、玻璃等非金属。
氧化石墨烯涂层厚度为2~6μm。
（2）在惰性环境中，采用具有化学活性键的摩擦配副，并施加0.2-1N的正压力，在氧化石墨烯涂层表面进行干摩擦，在摩擦滑移轨道上原位形成完美结构的石墨烯涂层。
惰性环境为氩气、氮气、氦气和真空（<10-2Pa）。
具有化学活性键的摩擦配副为钢、钛、铝等金属，也可以为硅、玻璃、diamond-likecarbon等非金属。
摩擦配副干摩擦的滑动速度2~5 cm/s。
石墨烯原位形成：在摩擦剪切力的作用下，氧化石墨烯的羟基官能团与摩擦配副上的活性键相互作用，氧化石墨烯上的C-OH键发生断裂。断裂后碳原子由sp3态向能量更稳定的sp2态转化，实现六元环结构的修复，在摩擦滑移轨道上形成石墨烯结构。由于摩擦剪切力在摩擦滑移轨道上的氧化石墨烯涂层发生向完美石墨烯结构的原位大尺度转变，并且展现出优异的润滑性能。
二、石墨烯涂层的结构和性能
对本发明制备的石墨烯涂层进行Raman光谱表征。作为对比，对原始的氧化石墨烯也进行了Raman光谱表征。
图1是采用的原始氧化石墨烯涂层Raman光谱，可以看出，原始氧化石墨烯涂层以浅绿色为主，Raman光谱中D峰显著，2D峰宽且强度低，这是氧化石墨烯典型特征。
图2是本发明方法制备的石墨烯涂层Raman光谱。在摩擦滑移轨道上，石墨烯涂层呈现黑色、紫色和蓝色，D峰强度很弱，2D峰增强并且尖锐，这是石墨烯典型特征。
对本发明制备的石墨烯涂层进行摩擦学性能测试。采用球盘摩擦试验机测试涂层的摩擦学性能，摩擦环境为惰性氩气，摩擦配副为Φ 6 mm的GCr15钢球，接触压力为0.5N，滑动速度5 cm/s，测试结果如图3所示。可以看出，石墨烯涂层稳定阶段平均摩擦系数在0.05，展现出优异的润滑性能。
附图说明
图1 为原始氧化石墨烯涂层的Raman光谱。
图2 为本发明制备的石墨烯涂层Raman 光谱。
图3为本发明制备的石墨烯涂层摩擦系数随时间的变化曲线。
具体实施方式
为了更好的理解本发明，下面通过具体实施例对本发明石墨烯涂层的制备方法和摩擦性能做进一步说明。
实施例1
（1）称取1g氧化石墨烯粉末，分散在200g无水乙醇中，超声分散3小时，喷涂于GCr15钢表面形成氧化石墨烯涂层，涂层厚度为4μm；
（2）在惰性氩气环境中，采用GCR15钢球作为摩擦配副，与氧化石墨烯涂层干摩擦，施加0.5N的正压力，滑动速度5 cm/s，在摩擦滑移轨道上原位形成石墨烯涂层；
（3）石墨烯涂层的摩擦性能：石墨烯涂层稳定阶段平均摩擦系数为0.05，展现出优异的润滑性能。
实施例2
（1）称取1g氧化石墨烯粉末，分散在100g丙酮中，超声分散6小时，喷涂于硅片表面形成氧化石墨烯涂层；涂层厚度为6μm；
（2）在真空（<10-2Pa）环境中，采用镀有diamond-like carbon薄膜的钢片作为摩擦配副，使diamond-like carbon薄膜与氧化石墨烯涂层干摩擦，施加1N的正压力，滑动速度3cm/s，在摩擦滑移轨道上原位形成石墨烯涂层；
（3）石墨烯涂层的摩擦性能：石墨烯涂层稳定阶段平均摩擦系数为0.03，展现出优异的润滑性能。
实施例3
（1）称取1g氧化石墨烯粉末，分散在500g甲苯中，超声分散2小时，喷涂于玻璃表面形成氧化石墨烯涂层；涂层厚度为2μm；
（2）在惰性氮气环境中，采用TC4钛片作为摩擦配副，与氧化石墨烯涂层干摩擦，施加0.2N的正压力，滑动速度5 cm/s，在摩擦滑移轨道上原位形成石墨烯涂层；
（3）石墨烯涂层的摩擦性能：石墨烯涂层稳定阶段平均摩擦系数为0.06，展现出优异的润滑性能。
实施例4
（1）称取1g氧化石墨烯粉末，分散在200g丁酮中，超声分散4小时，喷涂于钛表面形成氧化石墨烯涂层；涂层厚度为4μm；
（2）在惰性氦气环境中，采用硅片作为摩擦配副，与氧化石墨烯涂层干摩擦，施加0.5N的正压力，滑动速度5 cm/s，在摩擦滑移轨道上原位形成石墨烯涂层；
（3）石墨烯涂层的摩擦性能：石墨烯涂层稳定阶段平均摩擦系数为0.06，展现出优异的润滑性能。

Claims (3)

1.惰性环境中利用摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法，包括以下步骤：
（1）将氧化石墨烯超声分散在挥发性溶剂中，并喷涂于基体表面形成氧化石墨烯涂层；氧化石墨烯在挥发性溶剂中的质量比百分数为0.2-1.0%；基体为钢、钛、铝、硅、玻璃；
（2）在惰性环境中，采用具有化学活性键的摩擦配副，并施加正压力，在氧化石墨烯涂层表面进行干摩擦，在摩擦滑移轨道上原位形成完美结构的石墨烯涂层；惰性环境为氩气、氮气、氦气、真空<10-2Pa；具有化学活性键的摩擦配副为钢、钛、铝、硅、玻璃；施加的正压力在0.2-1N。
2.如权利要求1所述惰性环境中利用摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法，其特征在于：挥发性溶剂为丙酮、丁酮、无水乙醇、甲苯。
3.如权利要求1所述惰性环境中利用摩擦力还原氧化石墨烯原位制备石墨烯涂层的方法，其特征在于：超声分散时间为2-6小时。
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