CN110016378A - 一种新型离子液体润滑膜的制备方法 - Google Patents

一种新型离子液体润滑膜的制备方法 Download PDF

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CN110016378A
CN110016378A CN201910320087.3A CN201910320087A CN110016378A CN 110016378 A CN110016378 A CN 110016378A CN 201910320087 A CN201910320087 A CN 201910320087A CN 110016378 A CN110016378 A CN 110016378A
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methyl
film
lubricating film
ion liquid
villaumite
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CN110016378B (zh
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朱立业
刘汉臣
杨鑫
向硕
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Chengdu Quality Supervision Station Of Quartermaster Energy Quality Supervision Station Of Pla Joint Logistics Support Force
Army Service Academy of PLA
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Chinese People's Liberation Army Chengdu Military Command Oil Supervision Department
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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Abstract

本发明公开了一种新型离子液体润滑膜的制备方法，包含如下步骤：A.以单晶硅片抛光、清洗后作为基底材料；B.离子液体合成；C.滑膜成型处理。使用本方法合成的离子液体润滑膜，能够表现出较好的抗磨减摩性能和较长的耐磨寿命。

Description

一种新型离子液体润滑膜的制备方法
技术领域
本发明涉及一种新型离子液体润滑膜的制备方法。
背景技术
微机电系(Micro-electro-mechanical Systems，简称MEMS)是微/纳米技术研究的一个重要方向，在MEMS应用中存在严重的粘着、磨损和摩擦失效等摩擦学问题，因此最大限度地降低磨损减小摩擦，是保证微/纳米装置及MEMS功能和寿命的关键。
超薄膜润滑是指通过一定的实验技术，在MEMS材料表面制备出单或多分子层的超薄膜（厚度为纳米级），可以在不降低其承载能力的情况下，显著降低表面的摩擦系数，甚至出现超滑状态，被认为MEMS中最理想的润滑手段之一。根据成膜机理的不同，已研制出以下几种类型的分子膜：自组装膜（Self-assembled monolayer）、LB膜（Langmuir-Blodgett）、分子沉积膜（Molecular deposition film）等。由于离子液体具有非常优异的摩擦学性能、良好的导电性和分子中较强的静电力，使其在润滑薄膜方面显示出了潜在的应用价值，目前离子液体作为润滑材料在宏观摩擦学范畴已广泛应用，使利用离子液体超薄膜来改善微/纳米装置及MEMS中的摩擦和粘着问题成为可能。
发明内容
本发明的目的在于提供了一种新型离子液体润滑膜的制备方法。
本发明的目的主要通过以下技术方案实现：
提供一种新型离子液体润滑膜的制备方法，其特征在于，包含如下步骤：
A.基底材料的选择
单晶硅片抛光、清洗后作为基底材料；
B.离子液体合成
b1. 加入0.1mol N－甲基咪唑，在N2气保护加入0.1mol氯代正烷烃，得到中间体1－甲基－3－烷基咪唑氯盐；
b2. 将0.1mol1－甲基－3－烷基咪唑氯盐、0.12mol九氟丁磺酸钾和200ml去离子，在40°温度下水搅拌反应24h，静置冷却后加入200ml二氯甲烷；
b3. 抽滤步骤b2的反应溶液中，静置分层，取二氯甲烷层；
b4. 使用30ml去离子水多次洗涤b3的产物，旋蒸除去二氯甲烷，置于真空干燥箱中70温度真空干燥24h，得到1－甲基－3－烷基咪唑九氟丁磺酸盐；
C.滑膜成型处理
c1. 将离子液体溶于丙酮中，配制成质量百分浓度0.25wt%的溶液；
c2. 利用匀胶机在3000rpm的转速下旋涂于处理好的单晶硅片上；
c3. 在100℃下真空干燥箱中热处理2h。
进一步的，所述1－甲基－3－烷基咪唑九氟丁磺酸盐由通式I表示：
。
进一步的，所述通式I中R为C4H9、C6H3和C8H17中的一种。
进一步的，所述1－甲基－3－烷基咪唑氯盐为：1－甲基－3－丁基咪唑氯盐、1－甲基－3－已基咪唑氯盐和1－辛基－3－丁基咪唑氯盐中的一种。
综上所述，本发明具有以下有益效果：使用本方法合成的离子液体与硅基底表面的结合力较弱，因此具有合适的流动性，能够表现出最好的抗磨减摩性能和最长的耐磨寿命。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，下面结合实施例，对本发明作进一步的详细说明，本发明的示意性实施方式及其说明仅用于解释本发明，并不作为对本发明的限定。
实施例1：
A基底材料的处理：
对单晶硅片进行单面抛光，平整度TIR<0.5nm，厚度约为0.7mm。将单晶硅片切割成1cm×1cm的小片，分别在丙酮、无水乙醇中超声清洗10min，用二次蒸馏水将单晶硅片冼净后用氮气吹干。置入体积比为7:3的浓硫酸和30%过氧化氢的Piranha溶液中，90℃保温50min。用二次蒸馏水反复冲洗后用干燥氮气快速吹干，得到清洁的表面羟基化的单晶硅片待用。
B离子液体合成
试剂预处理：氯代烷烃，用前用浓硫酸洗涤，直至硫酸层无色，再用5% NaHCO3溶液洗三次，最后用蒸馏水洗至中性，用无水硫酸镁干燥过夜后，减压蒸馏备用；N－甲基咪唑，加入无水氯化钙干燥后减压蒸馏，密封保存备用；在避光的条件下，称量1.75g的AgNO3，用去离子水溶解，然后在容量瓶中稀释至100ml，得摩尔浓度为0.1mol/L的硝酸银溶液，于棕色瓶中保存备用。
b1. 加入0.1mol N－甲基咪唑，在N2气保护加入0.1mol氯代正烷烃，滴加完毕将烧瓶置于恒温水浴中升温至80℃，搅拌反应24h，室温静置冷却，将反应液倒入烧杯放入冰箱中冷冻2-3h，真空抽滤，将固体用乙酸乙酯清洗2-3次，置于真空干燥箱中，70℃真空干燥24h，得到中间体：1－甲基－3－丁基咪唑氯盐；
b2. 将0.1mol1－甲基－3－丁基咪唑氯盐、0.12mol九氟丁磺酸钾和200ml去离子，在40°温度下水搅拌反应24h，静置冷却后加入200ml二氯甲烷；
b3. 抽滤步骤b2的反应溶液中，静置分层，取二氯甲烷层；
b4. 使用30ml去离子水多次洗涤b3的产物，旋蒸除去二氯甲烷，置于真空干燥箱中70度真空干燥24h，得到1－甲基－3－丁基九氟丁磺酸盐。
C.滑膜成型处理
c1. 将离子液体溶于丙酮中，配制成质量百分浓度0.25wt%的溶液；
c2. 利用匀胶机在3000rpm的转速下旋涂于处理好的单晶硅片上；
c3. 在100℃下真空干燥箱中热处理2h。
1－甲基－3－丁基咪唑九氟丁磺酸盐，简写：PBS104，由下式表示：
。
实施例2：
A基底材料的处理：
对单晶硅片进行单面抛光，平整度TIR<0.5nm，厚度约为0.7mm。将单晶硅片切割成1cm×1cm的小片，分别在丙酮、无水乙醇中超声清洗10min，用二次蒸馏水将单晶硅片冼净后用氮气吹干。置入体积比为7:3的浓硫酸和30%过氧化氢的Piranha溶液中，90℃保温50min。用二次蒸馏水反复冲洗后用干燥氮气快速吹干，得到清洁的表面羟基化的单晶硅片待用。
B离子液体合成
试剂预处理：氯代烷烃，用前用浓硫酸洗涤，直至硫酸层无色，再用5% NaHCO3溶液洗三次，最后用蒸馏水洗至中性，用无水硫酸镁干燥过夜后，减压蒸馏备用；N－甲基咪唑，加入无水氯化钙干燥后减压蒸馏，密封保存备用；在避光的条件下，称量1.75g的AgNO3，用去离子水溶解，然后在容量瓶中稀释至100ml，得摩尔浓度为0.1mol/L的硝酸银溶液，于棕色瓶中保存备用。
b1. 加入0.1mol N－甲基咪唑，在N2气保护加入0.1mol氯代正烷烃，滴加完毕将烧瓶置于恒温水浴中升温至80℃，搅拌反应24h，室温静置冷却，将反应液倒入烧杯放入冰箱中冷冻2-3h，真空抽滤，将固体用乙酸乙酯清洗2-3次，置于真空干燥箱中，70℃真空干燥24h，得到中间体： 1－甲基－3－已基咪唑氯盐；
b2. 将0.1mol 1－甲基－3－已基咪唑氯盐、0.12mol九氟丁磺酸钾和200ml去离子，在40°温度下水搅拌反应24h，静置冷却后加入200ml二氯甲烷；
b3. 抽滤步骤b2的反应溶液中，静置分层，取二氯甲烷层；
b4. 使用30ml去离子水多次洗涤b3的产物，旋蒸除去二氯甲烷，置于真空干燥箱中70度真空干燥24h，得到1－甲基－3－已基咪唑九氟丁磺酸盐。
C.滑膜成型处理
c1. 将离子液体溶于丙酮中，配制成质量百分浓度0.25wt%的溶液；
c2. 利用匀胶机在3000rpm的转速下旋涂于处理好的单晶硅片上；
c3. 在100℃下真空干燥箱中热处理2h。
1－甲基－3－已基咪唑九氟丁磺酸盐，简写：PBS106，由下式表示：
。
实施例3：
A基底材料的处理：
对单晶硅片进行单面抛光，平整度TIR<0.5nm，厚度约为0.7mm。将单晶硅片切割成1cm×1cm的小片，分别在丙酮、无水乙醇中超声清洗10min，用二次蒸馏水将单晶硅片冼净后用氮气吹干。置入体积比为7:3的浓硫酸和30%过氧化氢的Piranha溶液中，90℃保温50min。用二次蒸馏水反复冲洗后用干燥氮气快速吹干，得到清洁的表面羟基化的单晶硅片待用。
B离子液体合成
b1. 加入0.1mol N－甲基咪唑，在N2气保护加入0.1mol氯代正烷烃，滴加完毕将烧瓶置于恒温水浴中升温至80℃，搅拌反应24h，室温静置冷却，将反应液倒入烧杯放入冰箱中冷冻2-3h，真空抽滤，将固体用乙酸乙酯清洗2-3次，置于真空干燥箱中，70℃真空干燥24h，得到中间体：1－辛基－3－丁基咪唑氯盐；
b2. 将0.1mol1－辛基－3－丁基咪唑氯盐、0.12mol九氟丁磺酸钾和200ml去离子，在40°温度下水搅拌反应24h，静置冷却后加入200ml二氯甲烷；
b3. 抽滤步骤b2的反应溶液中，静置分层，取二氯甲烷层；
b4. 使用30ml去离子水多次洗涤b3的产物，旋蒸除去二氯甲烷，置于真空干燥箱中70度真空干燥24h，得到1－甲基－3－辛基九氟丁磺酸盐。
C.滑膜成型处理
c1. 将离子液体溶于丙酮中，配制成质量百分浓度0.25wt%的溶液；
c2. 利用匀胶机在3000rpm的转速下旋涂于处理好的单晶硅片上；
c3. 在100℃下真空干燥箱中热处理2h。
1－甲基－3－辛基咪唑九氟丁磺酸盐，简写：PBS108，由下式表示：
。
对照例1：
再本对照例中离子液体采用：四氟硼酸盐，简写：LB104。
对照例2：
再本对照例中离子液体采用：双三氟甲磺酰亚胺盐离子液体，简写： LF104。
实验例1：
离子液体薄膜摩擦学性能测定在UMT-2MT摩擦试验机（CETR公司，USA）上进行。采用往复运动模式，接触形式为球－盘接触，往复行程为5mm，法向负荷80~1000mN，频率为1~3Hz。当摩擦系数升至0.50（基底的摩擦系数）时认为薄膜已被磨穿，以薄膜所经历的时间表示薄膜的耐磨寿命。上试球选用直径为3mm的GCr15（SAE 52100）钢球，试验前在丙酮中超声清洗10min。所有的测试均在室温20~25℃，相对湿度30~40%中进行。
由表可见，在200mN载荷下，各薄膜的耐磨寿命都达到3600s以上，说明经过1小时的摩擦后薄膜仍没有被磨破，但随着载荷的增加，各薄膜的耐磨寿命出现不同的变化：对于含有不同阴离子的离子液体薄膜，LB104的耐磨寿命迅速缩短，在300mN载荷下就只持续了228s，再增大载荷寿命都低于20s；LF104的耐磨寿命也明显缩短，在400mN载荷下持续了338s，再增大载荷薄膜迅速失效；PBS类离子液体薄膜表现出最长的耐磨寿命，特别是PBS104，在600mN载荷下耐磨寿命仍能达到3600s以上。对于含有不同链长的PBS类离子液体薄膜，随着链长的增加，离子液体薄膜的耐磨寿命呈现明显的降低，如在600mN下的耐磨寿命，PBS104为大于3600s，而PBS108只有806s。
实验例2：
本实验例中滑动频率为4Hz。
由表可见，随着载荷的增加，各薄膜的耐磨寿命出现不同的变化：对于含有不同阴离子的离子液体薄膜，当滑动速度增大后，LB104薄膜变得非常脆弱，耐磨寿命急剧减小，LB104薄膜在200mN载荷下只持续了470s，再增大载荷薄膜几乎在摩擦的初始阶段就被破坏；LF104薄膜的耐磨寿命也明显缩短，在300mN载荷下只能持续343s，再增大载荷薄膜迅速失效；PBS104和PBS106薄膜的耐磨寿命受滑动速度的影响相对较小，仍能表现出较长的耐磨寿命，特别是PBS104薄膜在400mN载荷下耐磨寿命仍能达到3600s以上；而PBS108薄膜的耐磨寿命受滑动速度的影响较大，其在高频高载荷下的耐磨寿命降低明显，如在载荷为600mN时，薄膜只持续了277s就被磨破，其耐磨寿命仅为低频时的1/3。
从实验例1和2的试验结果可见，PBS类离子液体与硅基底表面的结合，表现出最好的抗磨减摩性能和最长的耐磨寿命。
同时，也发现随着链长的增加PBS类离子液体薄膜的润滑效果和耐磨寿命都呈现降低的趋势，这主要是因为链长的增加，一方面使离子液体与表面的结合力进一步减弱，从而导致其很容易被完全挤出，另一方面使离子液体的粘度增大，从而导致其流动性变差，特别是当滑动速度加大时，所以PBS108薄膜的减摩抗磨效果较PBS104薄膜明显降低。
实验例3
本实验例中滑动频率为1Hz。
由表可见，LB104薄膜在80mN和100mN下的平均摩擦系数相近约为0.15，当载荷增加到200mN时，平均摩擦系数降低到0.12，并在测试时间内保持稳定。载荷继续增加到300mN时，在经历了228s后薄膜的摩擦系数突增到0.5以上，表明薄膜已经失效，再增加载荷到400mN时，薄膜在20s内迅速失效。
LF104薄膜在80mN下的平均摩擦系数为0.072，并在测定时间内保持稳定，当载荷增加到100mN和200mN时，平均摩擦系数减小到约0.051，并在测定时间内保持稳定，当载荷增加到300mN时，摩擦系数稳定保持1130s后突增到0.5以上，表明薄膜已经磨破，当载荷增加到400mN时，薄膜的耐磨寿命进一步降低到338s，再增加载荷到500mN时，薄膜在10s内立即失效。
PBS104薄膜在200mN下的平均摩擦系数为0.071，并在测定时间内保持稳定，当载荷增加到400mN和600mN时，平均摩擦系数降低到0.064和0.047，并在测定时间内保持稳定，当载荷继续增加到800mN时，平均摩擦系数增加到0.055，仍在测定时间内保持稳定，直到载荷增大到900mN时，摩擦系数稳定保持1154s后发生突变，再增加载荷到9001N时，薄膜对硅片的润滑防护作用仍然持续了854s才失效。
PBS106薄膜在200mN下的平均摩擦系数为0.084，并在测定时间内保持稳定，当载荷增加到400mN和600mN时，平均摩擦系数降低到约0.077，并在测定时间内保持稳定，当载荷继续增加到800mN时，摩擦系数稍有增加且持续1705s后发生突增，表明薄膜未能坚持到测定时间完就已经磨破了，再增加载荷到800mN时，薄膜的减摩抗磨作用仅仅持续了351s就失效。
PBS108薄膜在100mN下的平均摩擦系数为0.089，并在测定时间内保持稳定，当载荷增加到200mN和400mN时，平均摩擦系数降低到0.086和0.078，并在测定时间内保持稳定，当载荷继续增加到600mN时，摩擦系数变化不大但在经历了806秒后突增到0.5以上，表明薄膜已经磨破，再增加载荷到700mN时，薄膜在130s后迅速失效。
LB104薄膜在300mN以下具有一定的减摩作用，但摩擦系数较高，同时薄膜的承载能力较差，与LB104薄膜相比，LF104薄膜的减摩效果较好，摩擦系数较低，但承载能力依然较差。PBS104薄膜的减摩效果与LF104薄膜相当，摩擦系数稍低，但承载能力较LF104薄膜有了大幅提高，与PBS104薄膜相比，PBS106薄膜的减摩效果和承载能力都有所下降，与PBS104薄膜相比，PBS108薄膜的减摩效果和承载能力都明显下降。所以，PBS类离子液体薄膜有较好的承载能力和抗磨效果。

Claims (4)

1.一种新型离子液体润滑膜的制备方法，其特征在于，包含如下步骤：
A.基底材料的选择
单晶硅片抛光、清洗后作为基底材料；
B.离子液体合成
b1. 加入0.1mol N－甲基咪唑，在N2气保护加入0.1mol氯代正烷烃，得到中间体1－甲基－3－烷基咪唑氯盐；
b2. 将0.1mol1－甲基－3－烷基咪唑氯盐、0.12mol九氟丁磺酸钾和200ml去离子，在40度温度下水搅拌反应24h，静置冷却后加入200ml二氯甲烷；
b3. 抽滤步骤b2的反应溶液中，静置分层，取二氯甲烷层；
b4. 使用30ml去离子水多次洗涤b3的产物，旋蒸除去二氯甲烷，置于真空干燥箱中70度温度真空干燥24h，得到1－甲基－3－烷基咪唑九氟丁磺酸盐；
C.滑膜成型处理
c1. 将离子液体溶于丙酮中，配制成质量百分浓度0.25wt%的溶液；
c2. 利用匀胶机在3000rpm的转速下旋涂于处理好的单晶硅片上；
c3. 在100℃下真空干燥箱中热处理2h。
2.根据权利要求1所述的一种新型离子液体润滑膜的制备方法，其特征在于，所述1－甲基－3－烷基咪唑九氟丁磺酸盐由通式（I）表示：
。
3.根据权利要求2所述的一种新型离子液体润滑膜的制备方法，其特征在于，所述通式（I）中R为C4H9、C6H3和C8H17中的一种。
4.根据权利要求1所述的一种新型离子液体润滑膜的制备方法，其特征在于，所述1－甲基－3－烷基咪唑氯盐为：1－甲基－3－丁基咪唑氯盐、1－甲基－3－已基咪唑氯盐和1－辛基－3－丁基咪唑氯盐中的一种。
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