CN110846644A - 镀镍黑磷纳米片润滑剂及其制备方法 - Google Patents
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
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- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/24—Compounds containing phosphorus, arsenic or antimony
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1882—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
Abstract
本发明涉及了一种镀镍黑磷纳米片润滑剂及其制备方法，具体是在黑磷纳米片表面镀上镍层，仍然保留其片层结构，黑磷与镍的摩尔比为：1:2.8‑4.6；和常规化学镀镍相比，镀镍层在黑磷纳米片表面覆盖均匀、可控，结合牢固，形成独特的纳米复合层状结构；该镀镍黑磷纳米片润滑剂同时显著提高了重载环境下摩擦副的减摩抗磨效果，在重载机械润滑领域具有重要应用价值。
Description
一、发明领域
本发明涉及一种纳米润滑剂及其制备方法，具体地说是一种镀镍黑磷纳米片润滑剂及其制备方法。
二、背景技术
润滑剂对于改善机械设备运动部件的润滑，降低摩擦部件磨损、提高设备效率具有非常重要的作用，开发新型润滑剂对于提高设备润滑效率、推动机械制造产业升级具有重要意义，特别是对于重型机械设备关键摩擦副的润滑显得尤为重要。
近年来，黑磷纳米片作为一种新兴二维材料受到了较多的关注，主要是由于特殊的褶皱层状结构赋予它具有许多优越的性能。Lv等[Tribology Letters,2018,66(2):61.]研究发现黑磷纳米片作为润滑添加剂能够明显改善复合材料的摩擦学性能，能起到较好的润滑作用，润滑机制是由于具有层状结构的材料在摩擦过程能起到层间滑移作用从而发挥润滑效果；然而，最近的摩擦学研究[ASME Journal of Tribology,2019,141(7):072101.]发现黑磷纳米片层状材料的承载能力欠佳，载荷较大时润滑效果就会降低，也即黑磷纳米片在重载条件下的润滑性能需要进一步提升。中国专利[公开号：CN110157516A]公开了一种将纳米二氧化钛与黑磷纳米片进行复合，形成一种新的复合润滑剂来改善黑磷纳米片在重载环境下的减摩润滑性能的方法，取得了一定的效果，但其抗磨性能仍需提升。因此，有必要同时改善黑磷纳米片在重载环境下摩擦副的减摩抗磨性能。
研究表明在材料表面镀镍可表现出较好的减摩和抗磨作用，因此，在黑磷纳米片表面镀镍，有望使其产生更加优异的减摩抗磨效果，然而，常规的化学镀镍方法在非金属表面镀镍效果差，镀层不均匀、成分难控制、结合松散等，因此，目前尚未见镀镍黑磷纳米片及其润滑性能的相关报道。
三、发明内容
本发明针对现有技术的不足，提供一种镀镍黑磷纳米片润滑剂及其制备方法，用以同时改善重载环境下摩擦副的减摩抗磨性能。
本发明通过以下技术方案来实现：
本发明一种镀镍黑磷纳米片，其特点在于：在黑磷纳米片表面镀上镍层，镀镍层在纳米片表面覆盖均匀、可控、结合牢固，形成独特的纳米复合层状结构；其中，黑磷纳米片厚度为2-10nm，黑磷与镍的摩尔比为：1:2.8-4.6。
如上所述的镀镍黑磷纳米片的制备方法，以质量份计，按以下方法进行制备，具体步骤为：
(1)预镀液配制：取200-500份NiSO4·6H2O搅拌溶解于10000份去离子水当中，接着依次加入900-1800份柠檬酸钠和700-1400份硫酸铵搅拌溶解，预镀液配制完成；
(2)表面修饰：取2-3份黑磷纳米片放入2000份质量浓度2％的银氨溶液中超声20-30min进行表面修饰，然后在12000-14000r/min转速下离心15-30min，取其沉淀，用无水乙醇清洗后，在真空环境40-60℃下干燥，得到表面修饰后的黑磷纳米片；
(3)镀镍处理：将黑磷纳米片放入步骤(1)制备的预镀液中超声20-30min，随后加入200-500份NaH2PO2·H2O，超声分散15-30min，调节溶液pH＝9-9.3，在80-85℃下加热搅拌反应，当不产生气泡时停止加热；溶液冷却后在3000-4000rpm转速下离心20-30min，取沉淀物，用去离子水冲洗，直到洗至中性，所得产物在真空环境60-80℃下干燥8-10h，得到镀镍黑磷纳米片。
与现有技术相比，本发明的优势在于：
1.本发明实现了在黑磷纳米片表面可控镀镍，成功制备出一种镀镍黑磷纳米片润滑剂，通过采用2-10nm黑磷纳米片原料及独特的制备工艺，镀镍后将黑磷与镍的摩尔比有效控制为：1:2.8-4.6，和常规化学镀镍相比，镀镍层在片层表面覆盖均匀、可控、结合牢固，形成独特的纳米复合层状结构。
2.本发明的镀镍黑磷纳米片润滑剂显著提高了黑磷纳米片在接触应力4GPa以上重载环境下摩擦副的减摩抗磨作用，摩擦副的摩擦系数和磨损量同时显著降低。
3.本发明的镀镍黑磷纳米片的制备工艺简便，成本较低，容易实现。
四、附图说明
图1(a)为镀镍前黑磷纳米片的拉曼光谱图；
图1(b)为本发明方法制备的镀镍黑磷纳米片的拉曼光谱图。
图2为本发明方法制备的镀镍黑磷纳米片的扫描电镜照片。
五、具体实施例
为了更好的理解本发明，通过以下具体实施例说明本发明镀镍黑磷纳米片润滑剂的制备方法及其润滑性能。需要指出的是，这些实施例并不限制本发明所要保护的内容。以下实施例中采用的黑磷纳米片原料厚度为2-10nm。
实施例1
首先取2g NiSO4·6H2O搅拌溶解于50mL去离子水当中，接着依次加入8g柠檬酸钠和6.5g硫酸铵，搅拌溶解，预镀液配制完成。将11.4mg黑磷纳米片放入10.15g质量浓度2％银氨溶液中超声20min进行表面修饰，然后在14000rpm转速下离心15min取其沉淀，用无水乙醇清洗后，在真空环境60℃下干燥，得到修饰后的黑磷纳米片。将修饰后的黑磷纳米片放入之前配制的预镀液中超声30min，往其中加入2.2g NaH2PO2·H2O超声分散15min，调节溶液pH＝9，在80℃加热搅拌反应，当不产生气泡时结束加热。待溶液冷却后，在4000rpm转速下离心30min，取其沉淀用去离子水冲洗，洗涤至中性，所得产物在真空环境80℃下干燥8-10h，即得镀镍黑磷纳米片。
由图1(a)和图1(b)镀镍前后黑磷纳米片的拉曼光谱图可知，镀镍前黑磷纳米片存在3个典型特征峰A1g，B2g和A2g(分别位于～358cm-1，～435cm-1和～462cm-1)；镀镍后，黑磷纳米片的拉曼特征峰消失，表明镍相已均匀覆盖在黑磷纳米片表面。
从图2镀镍黑磷纳米片的扫描电镜照片中也可以直观地看到镀镍层在黑磷纳米片表面覆盖均匀、结合牢固，形成独特的纳米复合层状结构。
实施例2
取1.2g NiSO4·6H2O搅拌溶解于50mL去离子水当中，接着依次加入4.8g柠檬酸钠和3.9g硫酸铵，搅拌溶解，镀液便配制完成。将11mg黑磷纳米片放入10.15g质量浓度2％银氨溶液中超声30min进行表面修饰，然后在12000rpm转速下离心20min取其沉淀，用无水乙醇清洗后，在真空环境60℃下干燥，得到修饰后的黑磷纳米片。将修饰后的黑磷纳米片放入之前调配的镀液中超声30min，往其中加入1.32g NaH2PO2·H2O超声分散15min，调节溶液pH＝9，在80℃加热搅拌反应，当不产生气泡时结束加热。待溶液冷却后，在3000rpm转速下离心20min，取其沉淀用去离子水冲洗，洗涤至中性，所得产物在真空环境80℃下干燥8-10h，即得镀镍黑磷纳米片。
为了检测本发明润滑剂的润滑效果，将黑磷纳米片、实施例1和实施例2制备的镀镍黑磷纳米片分别以0.01wt％的浓度分散在PAO6基础油中，采用往复摩擦试验进行考察其润滑性能。试验机的接触形式为球盘接触，运动方式为直线往复式，摩擦副材料均为GCr15，参数设置为载荷100N(接触应力为4.6GPa)，转速500r/min，行程5mm。三种润滑剂的润滑性能数据如表1所示，从表中数据可以看出，相对于黑磷纳米片，本发明的镀镍黑磷纳米片在重载环境下润滑，系统摩擦系数和磨斑直径显著降低，也即同时实现了摩擦副减摩抗磨性能的显著提升。
表1三种润滑剂的润滑性能比较
Claims (2)
1.一种镀镍黑磷纳米片润滑剂，其特征在于：在黑磷纳米片表面镀上镍层，镀镍层在纳米片表面覆盖均匀、可控、结合牢固，形成独特的纳米复合层状结构；其中，黑磷纳米片厚度为2-10nm，黑磷与镍的摩尔比为：1:2.8-4.6。
2.一种权利要求1所述的镀镍黑磷纳米片的制备方法，其特征在于：以质量份计，具体步骤为：
(1)预镀液配制：取200-500份NiSO4·6H2O搅拌溶解于10000份去离子水当中，接着依次加入900-1800份柠檬酸钠和700-1400份硫酸铵搅拌溶解，预镀液配制完成；
(2)表面修饰：取2-3份黑磷纳米片放入2000份质量浓度2％的银氨溶液中超声20-30min进行表面修饰，然后在12000-14000r/min转速下离心15-30min，取其沉淀，用无水乙醇清洗后，在真空环境40-60℃下干燥，得到表面修饰后的黑磷纳米片；
(3)镀镍处理：将表面修饰后的黑磷纳米片放入步骤(1)制备的预镀液中超声20-30min，随后加入200-500份NaH2PO2·H2O，超声分散15-30min，调节溶液pH＝9-9.3，在80-85℃下加热搅拌反应，当不产生气泡时停止加热；溶液冷却后在3000-4000rpm转速下离心20-30min，取沉淀物，用去离子水冲洗，直到洗至中性，所得产物在真空环境60-80℃下干燥8-10h，得到镀镍黑磷纳米片。
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