CN114032129B - 一种过渡金属硫化物表面修饰方法及其应用 - Google Patents

一种过渡金属硫化物表面修饰方法及其应用 Download PDF

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CN114032129B
CN114032129B CN202111291598.0A CN202111291598A CN114032129B CN 114032129 B CN114032129 B CN 114032129B CN 202111291598 A CN202111291598 A CN 202111291598A CN 114032129 B CN114032129 B CN 114032129B
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张春风
孙丁伟
张晓军
张伟
路捷
常晓峰
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Shanxi Lu'an Taihang Lubrication Technology Co ltd
Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种过渡金属硫化物表面修饰有机联硼化合物的方法及其作为润滑油添加剂的应用。有机联硼化合物包括双（频那醇合）二硼，双（邻苯二酚）二硼酸酯，四（二甲氨基）二硼和四羟基二硼。过渡金属硫化物主要包括二硫化钼（MoS2），二硫化钨（WS2），二硒化钼（MoSe2）和二硒化钨（WSe2）。有机联硼修饰的过渡金属硫化物在润滑油中可形成非常稳定的分散体系，并且在升高温度（150 oC）、变化载荷（50～200 N）条件下表现出优异的减摩抗磨性能。

Description

一种过渡金属硫化物表面修饰方法及其应用
技术领域
本发明涉及一种过渡金属硫化物的表面修饰方法及其作为润滑油添加剂的应用。
背景技术
过渡金属二硫化物(TMDCs，例如MoS2和WS2)是一类性能非常优异的固体润滑剂，其沉积膜被广泛应用于卫星、人造飞船、空间实验室、空间站等各种航天器的润滑。另外，作为润滑添加剂，MoS2和WS2粉体可稳定分散于工业润滑脂和工程塑料中，用于增加其润滑性、极压性和抗磨损性能。
近些年来，大量研究表明MoS2和WS2纳米颗粒作为润滑油添加剂具有非常显著的减摩和抗磨性能。但是固体纳米颗粒在润滑油中不能稳定存在是制约其应用的最大障碍。为了增强MoS2和WS2纳米颗粒在润滑油中的分散稳定性，将油溶性良好的有机官能团结合到MoS2和WS2表面是一种非常有效的途径。例如，Chen Shahar等在类富勒烯WS2(IF-WS2)表面修饰不同碳链的烷基硅涂层(Langmuir,2010,26,4409-4414)，Chen Zhe等制备了表面修饰油酸胺的超薄MoS2纳米片(Sci.Rep.,2015,5,12869)。上述通过化学方法将有机官能团结合到MoS2和WS2表面均可大幅度增强固体纳米颗粒在润滑油中的分散稳定性，但是这些方法的制备过程复杂、所产生的废气废液会对环境造成危害。探索绿色无污染的高效的MoS2和WS2表面修饰方法是拓宽其应用的一种重要途径。
发明内容
本发明的目的在于提供一种表面功能化过渡金属硫化物，以及一种过渡金属硫化物表面功能化方法，并开拓其作为润滑油添加剂的应用。
本发明的一种表面功能化过渡金属硫化物，其特征在于，该表面功能化过渡金属硫化物为有机联硼修饰的过渡金属硫化物。
本发明所述的过渡金属硫化物表面功能化方法是：将有机联硼与过渡金属硫化物在惰性气体保护下(手套箱)按照一定质量比混合，置于研钵中研磨一定时间，所得产物即为有机联硼修饰的过渡金属硫化物(B-MS2)。
进一步的，所述的有机联硼为双(频那醇合)二硼，双(邻苯二酚)二硼酸酯，四(二甲氨基)二硼和四羟基二硼(分别简称为B1，B2，B3和B4，其结构式如图1所示)。
进一步的，所述的过渡金属硫化物为二硫化钼(MoS2)，二硫化钨(WS2)，二硒化钼(MoSe2)和二硒化钨(WSe2)。
进一步的，所述的有机联硼与过渡金属硫化物质量比为0.5:1～10:1。
进一步的，所述的研磨时间为10min～60min。
本发明所述的B-MS2作为润滑油添加剂的在润滑油中的应用。
本发明的B-MS2在润滑油中形成稳定的分散体系，在升高温度(150℃)、变化载荷(50～200N)条件下表现出优异的减摩抗磨性能。
本发明所述B-MS2在润滑油中的添加量为0.5wt％～1.5wt％。
本发明所述润滑油为合成油、矿物油中的任意一种或其混合物及成品油。
所述合成油为CTL10(煤制基础油)及5W-30SP汽油机油等。
本发明的有益效果：本发明提供了一种新颖、简单、环境友好的过渡金属硫化物表面修饰方法。这种方法所制备的表面功能化过渡金属硫化物不仅在溶剂和润滑基础油中表现出良好的分散稳定性，并且在升高温度的条件下表现出更好的减摩抗磨效果。
附图说明
图1为联硼有机化合物的结构示意图。
图2为表面修饰双(频那醇合)二硼(B1)的WS2(B1-WS2，实施例1中所制备)的透射电子显微镜(TEM)形貌图。
图3为未修饰WS2(I)和B1-WS2(II)(实施例1中所制备)在二氯甲烷中分散1小时和24小时后的图像。
图4为未修饰WS2和B1-WS2(实施例1中所制备)分散在CTL10(煤制基础油)基础油中，在100℃，25Hz，载荷分别为50N(a)，100N(b)，150N(c)和200N(c)条件下的摩擦曲线图。
图5为CTL10(煤制基础油)和CTL10(煤制基础油)中分别添加未修饰WS2和B1-WS2(实施例1中所制备)在100℃，频率25Hz，载荷分别为50N(a)，100N(b)，150N(c)和200N(c)条件下对应磨斑的磨损量。
具体实施方式
实施例1
将2.0g双(频那醇合)二硼(B1)和1.0g商品纳米WS2在氮气保护下加入玛瑙研钵中(手套箱中操作)，并在手套箱中研磨30min，所得产物即为B1修饰的WS2纳米颗粒(B1-WS2)。
在CTL10(煤制基础油)基础油中添加1％WS2和1wt％B1-WS2，超声分散均匀后测试其摩擦学性能。
实施例2
将2.0g双(频那醇合)二硼(B1)和1.0g商品纳米MoS2在氮气保护下加入玛瑙研钵中(手套箱中操作)，并在手套箱中研磨30min，所得产物即为B1修饰的MoS2纳米颗粒(B1-MoS2)。
在CTL10(煤制基础油)基础油中添加1％MoS2和1wt％B1-MoS2，超声分散均匀后测试其摩擦学性能。
实施例3
将2.0g双(邻苯二酚)二硼酸酯(B2)和1.0g商品纳米WS2在氮气保护下加入玛瑙研钵中(手套箱中操作)，并在手套箱中研磨30min，所得产物即为B2修饰的WS2纳米颗粒(B2-WS2)。
在5W-30SP汽油机油中添加1％WS2和1wt％B2-WS2，超声分散均匀后测试其摩擦学性能。
实施例4
将2.0g四(二甲氨基)二硼(B3)和1.0g商品纳米WS2在氮气保护下加入玛瑙研钵中(手套箱中操作)，并在手套箱中研磨30min，所得产物即为B3修饰的WS2纳米颗粒(B3-WS2)。
在5W-30SP汽油机油中添加1％WS2和1wt％B3-WS2，超声分散均匀后测试其摩擦学性能。
实施例5
将2.0g四羟基二硼(B4)和1.0g商品纳米WS2在氮气保护下加入玛瑙研钵中(手套箱中操作)，并在手套箱中研磨30min，所得产物即为B4修饰的WS2纳米颗粒(B4-WS2)。
在5W-30SP汽油机油中添加1％WS2和1wt％B4-WS2，超声分散均匀后测试其摩擦学性能。
产物的结构表征
采用日本电子株式会社(JEOL)公司生产的型号为JEM-1200EX透射电镜(TEM)对实施例1中所制备的B1-WS2纳米颗粒的形貌和结构进行表征，过程中所使用的加速电压为100KV，形貌图见附图2。从图中可以清楚的看出，WS2表面具大量的有机层，并且大部分有机相的厚度大于10nm，表明联硼有机化合物被成功修饰到WS2表面。
产物在润滑油中的稳定性表征
图3中Ⅰ号样品为在CTL10(煤制基础油)基础油中添加1％WS2，Ⅱ号样品为在CTL10(煤制基础油)基础油中添加1wt％本发明实施例1制备的B1-WS2，Ⅰ号样品和Ⅱ号样品超声分散均匀后静置，静置1h和24h后样品稳定性照片见图3。从图3可以看出，本发明制备的B1-WS2在CTL10(煤制基础油)基础油中能够稳定存在。
产物的摩擦学性能评价
1.采用德国Optimol油脂公司生产的SRV-IV微振动摩擦磨损试验机测试实施例1中制备的CTL10(煤制基础油)添加1％WS2和1wt％B1-WS2在温度100℃、频率25Hz、振幅1mm、变化载荷50～200N、长磨30min时的摩擦系数f。试验所用钢球为Φ＝10mm的GCr15轴承钢，下试样为Φ24×7.9mm的GCr15钢块。结果见附图4。测量结果表明在100℃不同载荷条件下，1％B1-WS2能够显著降低CTL10(煤制基础油)的摩擦系数，并且在CTL10(煤制基础油)中添加B1-WS2的减摩性能显著优于CTL10(煤制基础油)中添加未修饰的WS2。
2.采用MicroXAM 3D非接触的表面测试仪测试实施例1中制备的CTL10(煤制基础油)添加1％WS2和1wt％B1-WS2在温度100℃、频率25Hz、振幅1mm、变化载荷50～200N、长磨30min时对应磨斑的磨损量，如附图5所示。结果表明在100℃不同载荷条件下，1％B1-WS2能够大幅度增强CTL10(煤制基础油)的抗磨损性能,并且B1-WS2的抗磨损性能明显优于未修饰的WS2。

Claims (10)

1.一种表面功能化过渡金属硫化物，其特征在于，该表面功能化过渡金属硫化物为有机联硼修饰的过渡金属硫化物（B-MS2）。
2.如权利要求1表面功能化过渡金属硫化物，其特征在于，所述的有机联硼选自双（频那醇合）二硼，双（邻苯二酚）二硼酸酯，四（二甲氨基）二硼和四羟基二硼。
3.如权利要求1表面功能化过渡金属硫化物，其特征在于，所述的过渡金属硫化物为二硫化钼（MoS2）或二硫化钨（WS2）。
4.如权利要求1表面功能化过渡金属硫化物，其特征在于，所述的有机联硼与过渡金属硫化物质量比为0 .5:1～10:1。
5.如权利要求1所述表面功能化过渡金属硫化物的制备方法，其特征在于，制备方法具体为：将有机联硼与过渡金属硫化物在惰性气体保护下按照一定质量比混合，置于研钵中研磨一定时间，所得产物即为有机联硼修饰的过渡金属硫化物（B-MS2）。
6.如权利要求5表面功能化过渡金属硫化物的制备方法，其特征在于，所述的研磨时间为10 min～60 min。
7.如权利要求1所述表面功能化过渡金属硫化物的应用，其特征在于，所述的B-MS2作为润滑油添加剂的在润滑油中的应用。
8.如权利要求1所述表面功能化过渡金属硫化物的应用，其特征在于，B-MS2在润滑油中形成稳定的分散体系，在升高温度、变化载荷条件下表现出优异的减摩抗磨性能。
9.如权利要求7所述表面功能化过渡金属硫化物的应用，其特征在于，所述B-MS2在润滑油中的添加量为0 .5wt%～1 .5 wt %。
10.如权利要求7所述表面功能化过渡金属硫化物的应用，其特征在于，所述润滑油为合成油、矿物油中的任意一种或其混合物。
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