CN111004036A - 一种高致密度六方氮化硼基固体润滑复合材料及其制备方法 - Google Patents

一种高致密度六方氮化硼基固体润滑复合材料及其制备方法 Download PDF

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CN111004036A
CN111004036A CN201911352215.9A CN201911352215A CN111004036A CN 111004036 A CN111004036 A CN 111004036A CN 201911352215 A CN201911352215 A CN 201911352215A CN 111004036 A CN111004036 A CN 111004036A
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boron nitride
hexagonal boron
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sintering
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杨军
刘维民
陈娟娟
程军
朱圣宇
谈辉
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种高致密度六方氮化硼基固体润滑复合材料，是将h‑BN、SiC及复合烧结助剂于WC球磨罐中湿法球磨获得粉料，烘干，过筛后将粉料放入石墨模具中先预压，再将预压样与石墨模具一起装入放电等离子烧结炉中高温高压烧结，然后随炉冷却至室温，得到的毛坯样经打磨、抛光，即得六方氮化硼基复合材料。本发明采用放电等离子烧结技术，显著降低了六方氮化硼陶瓷的烧结温度，在较低温度、较短时间内可获得致密度达到95%以上的六方氮化硼基复合材料块体，节约制备成本，提高制备效率；引入碳化硅增强相，提高了复合材料的硬度；该复合材料在室温至900oC内具有良好的润滑性能，可用于高温环境中机械运动部件的润滑和密封件。

Description

一种高致密度六方氮化硼基固体润滑复合材料及其制备方法
技术领域
本发明涉及一种六方氮化硼基固体润滑复合材料，尤其涉及一种高致密度六方氮化硼基固体润滑复合材料的制备方法，属于陶瓷基固体润滑复合材料领域。
背景技术
六方氮化硼（h-BN）作为氮化硼诸多晶型中最为稳定的结构，具有类石墨的层状晶体结构特点，层内硼-氮原子间以强的共价键结合形成六角形网络，而相邻层之间以弱的范德华力结合，具有较低的剪切强度，容易发生层间滑移，赋予了h-BN良好的润滑性能。另外，h-BN具有较高的热导率，良好的热稳定性及化学稳定性，同时也是一种良好的高温固体润滑材料。目前，主要集中于将h-BN引入金属或其它陶瓷中作为固体润滑剂改善复合材料的摩擦学性能。文献1[Tribology International. 56 (2012) 58-65]中，在C/C复合材料表面制备了SiC/h-BN复合涂层，h-BN的加入不仅稳定了涂层室温下的摩擦系数，并且在高温下形成致密的层状结构的摩擦膜，使涂层的摩擦系数从室温时的0.60降低至800ºC时的0.28。而在镍基涂层中引入少量h-BN，可同时降低涂层的摩擦系数和磨损率[文献2：Surface & Coatings Technology 359 (2019) 485–494]。文献3[Applied Surface Science. 257 (2011) 10195-10200]中报道了h-BN热压烧结体室温至800ºC时的摩擦学行为，800ºC时，大气中的摩擦系数为0.38，水蒸汽环境中降低为0.22。文献4[RSC Advances. 5 (2015) 106239-106244]中利用第一性原理计算得到h-BN的摩擦系数为0.025~0.13。
虽然h-BN具有良好的润滑性能，但由于其本征强度低、硬度低、脆性大，且块体样品制备困难，限制了其广泛的应用。而制备复合材料是提高h-BN综合性能的一种有效途径，通过引入增强增韧相，制备h-BN基固体润滑复合材料，充分发挥h-BN结构陶瓷材料的固体润滑性能，可将其应用于高温环境中机械传动部件的润滑与密封件。
发明内容
本发明的目的在于提供一种低温、快速高效制备高致密度六方氮化硼基固体润滑复合材料的方法。
本发明制备六方氮化硼基固体润滑复合材料的方法，是将六方氮化硼（h-BN）、碳化硅（SiC）及复合烧结助剂于WC球磨罐中湿法球磨混合，获得混合均匀的粉料，烘干，过筛；所得粉料放入石墨模具中先进行预压，再将预压样与石墨模具一起装入放电等离子烧结炉中进行高温高压烧结，烧结结束后随炉冷却至室温，得到的毛坯样经打磨、抛光，即得块体六方氮化硼基复合材料。
原料六方氮化硼（h-BN）、碳化硅（SiC）及复合烧结助剂按以下质量百分数配比：六方氮化硼（h-BN）40~80%，碳化硅（SiC）10~50%，复合烧结助剂10%；其中复合烧结助剂由Al2O3和Y2O3以3:2的质量比复合。
所述湿法球磨混合在行星式球磨机上进行，球磨参数为：球磨介质为无水乙醇，球料比（3~5）:1；转速200~300r/min；球磨时间6~10 h。
所述粉料的烘干是在60~80oC的烘箱中干燥12~24 h。
所述粉料的预压是在10MPa的压力下预压1~10 min；
所述高温高压烧结，是在压力20~40 MPa，真空度10-2~10-1Pa下，以75~150oC/min的升温速率升温至1600~1800 oC，保温5~10 min。
图1为本发明制备的六方氮化硼基固体润滑复合材料的X射线衍射图谱。可见，复合材料的相组成主要为h-BN和SiC。
本发明制备的复合材料致密度达到95%以上，维氏硬度为1.5~3.8 GPa。复合材料在室温下的干摩擦系数为0.24~0.50，中高温（200~600oC）范围内摩擦系数为0.41~0.52；800oC时的摩擦系数为0.28~0.44，900oC时的摩擦系数为0.26~0.34。与文献3中h-BN热压烧结体800oC时在大气中的摩擦系数0.38相比，本发明制备的复合材料在更高的温度（900oC）下具有较低的摩擦系数，表现出良好的润滑性能。
综上所述，本发明相比现有技术具有以下优点：
1、采用放电等离子烧结技术，显著降低了h-BN陶瓷的烧结温度，在较低温度、较短时间内可获得致密度达到95%以上的六方氮化硼基复合材料块体，节约制备成本，提高制备效率；
2、通过引入碳化硅增强相，提高了复合材料的硬度和致密度，以此为基体的陶瓷基复合材料无需外加其它润滑相，在宽温域（室温~ 900oC）范围内具有良好的润滑性能，可将其应用于高温环境中机械传动部件的润滑与密封件。
附图说明
图1为六方氮化硼基固体润滑复合材料的X射线衍射图谱。
图2为实施例1制备的h-BN质量分数为65%的复合材料摩擦系数随温度的变化。
具体实施方式
下面通过实施例对本发明六方氮化硼基固体润滑复合材料的制备方法和摩擦系数作进一步说明。
实施例 1
按质量比65:25:6:4称取h-BN、SiC、Al2O3及Y2O3粉末，放入WC球磨罐中在行星式球磨机上湿法球磨：无水乙醇为介质，球料比5:1，转速200 r/min，球磨时间10 h。然后放入60oC的烘箱中干燥24 h，随后过120目筛，得到的粉料装入石墨模具中，10MPa预压成型，保压10min后移入放电等离子烧结炉中烧结：以100 oC/min的升温速率升温至1800oC保温5 min，升温过程中压力逐渐增加至20 MPa，整个烧结过程在真空中完成，真空度为10-2~10-1Pa。所得复合材料的致密度达到95%，维氏硬度为1.5GPa。该复合材料的室温干摩擦系数为0.25，中高温（200~600oC）范围内摩擦系数为0.43~0.52，800oC和900oC的摩擦系数分别为0.28和0.26。具体见图2。
实施例 2
按质量比60:30:6:4称取h-BN、SiC、Al2O3及Y2O3粉末，放入WC球磨罐中在行星式球磨机上湿法球磨：无水乙醇为介质，球料比4:1，转速250 r/min，球磨时间8 h。然后放入70oC的烘箱中干燥20 h，随后过100目筛，得到的粉料装入石墨模具中，10MPa预压成型，保压5 min后移入放电等离子烧结炉中烧结：以150 oC/min的升温速率升温至1700oC保温10 min，升温过程中压力逐渐增加至30 MPa，整个烧结过程在真空中完成，真空度为10-2~10-1Pa。所得复合材料的致密度达到97%，维氏硬度为1.6 GPa。该复合材料在室温及高温（800oC和900oC）时的摩擦系数为0.29~0.34，中高温（200~600oC）范围内摩擦系数稳定在0.43~0.45。
实施例 3
按质量比40:50:6:4称取h-BN、SiC、Al2O3及Y2O3粉末，放入WC球磨罐中在行星式球磨机上湿法球磨：无水乙醇为介质，球料比3:1，转速300 r/min，球磨时间6 h。然后放入80oC的烘箱中干燥12 h，随后过80目筛，得到的粉料装入石墨模具中，10MPa预压成型，保压1 min后移入放电等离子烧结炉中烧结：以75oC/min的升温速率升温至1600oC保温10 min，升温过程中压力逐渐增加至40 MPa，整个烧结过程在真空中完成，真空度为10-2~10-1Pa。所得复合材料的致密度达到99%，维氏硬度为3.8 GPa。该复合材料的室温干摩擦系数为0.50，中高温（200~600 oC）范围内摩擦系数为0.41~0.46，800oC和900oC时的摩擦系数分别为0.44和0.33。

Claims (6)

1.一种高致密度六方氮化硼基固体润滑复合材料的制备方法，是将六方氮化硼、碳化硅及复合烧结助剂于WC球磨罐中湿法球磨混合，获得混合均匀的粉料，烘干，过筛；所得粉料放入石墨模具中先进行预压，再将预压样与石墨模具一起装入放电等离子烧结炉中进行高温高压烧结，烧结结束后随炉冷却至室温，得到的毛坯样经打磨、抛光，即得块体六方氮化硼基复合材料；所述复合烧结助剂是由Al2O3和Y2O3以3:2的质量比复合。
2.如权利要求1所述一种高致密度六方氮化硼基固体润滑复合材料的制备方法，其特征在于：六方氮化硼、碳化硅及复合烧结助剂按以下质量百分数配比：六方氮化硼40~80%，碳化硅10~50%，复合烧结助剂10%。
3.如权利要求1所述一种高致密度六方氮化硼基固体润滑复合材料的制备方法，其特征在于：所述湿法球磨混合在行星式球磨机上进行，球磨参数为：球磨介质为无水乙醇，球料比（3~5）:1；转速200~300r/min；球磨时间6~10 h。
4.如权利要求1所述一种高致密度六方氮化硼基固体润滑复合材料的制备方法，其特征在于：所述粉料的烘干是在60~80oC的烘箱中干燥12~24 h。
5.如权利要求1所述一种高致密度六方氮化硼基固体润滑复合材料的制备方法，其特征在于：所述粉料的预压是在10MPa的压力下预压1~10 min。
6.如权利要求1所述一种高致密度六方氮化硼基固体润滑复合材料的制备方法，其特征在于：所述高温高压烧结，是在压力20~40 MPa，真空度10-2~10-1Pa下，以75~150oC/min的升温速率升温至1600~1800 oC，保温5~10 min。
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