CN109354502B - 一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料 - Google Patents

一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料 Download PDF

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CN109354502B
CN109354502B CN201811017236.0A CN201811017236A CN109354502B CN 109354502 B CN109354502 B CN 109354502B CN 201811017236 A CN201811017236 A CN 201811017236A CN 109354502 B CN109354502 B CN 109354502B
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乔竹辉
刘炯杰
杨军
朱圣宇
程军
于源
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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温环境中具有高耐磨表面的自润滑氮化硅基复合材料，该复合材料通过以下方法制备得到：1）将α‑Si3N4和Ti2SnC放入球磨机进行球磨即得混合粉末；2）将混合粉末干燥过筛后装入石墨模具中进行预压；3）将步骤2）所得预压样进行高温高压烧结，随后随炉冷却，得到毛坯；4）将毛坯进行表面抛光、去毛刺处理即得自润滑氮化硅基复合材料。本发明所述自润滑复合材料利用金属锡的析出和氧化，可以实现高温环境中的自润滑与抗磨损，特别适合应用于高温条件下无润滑界面之间的器件材料。

Description

一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料
技术领域
本发明属于新材料技术领域，涉及一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料。
背景技术
普通的氮化硅材料本身具备有高强度、高硬度、抗热震性以及耐酸碱腐蚀等一系列优异性质，是工业应用中不可或缺的基础材料。但是，存在的主要问题是在干摩擦条件下氮化硅的自润滑能力和耐磨性能不佳，不能满足其作为一种结构陶瓷在工业中的应用；为了改善氮化硅在干摩条件下的摩擦学性能，在申请号为CN201710280311.1、CN201710119941.0、CN201711412039.4和CN201511027828.7的中国发明专利中，都是通过引入第二相 (增强相或润滑相)来改善复合材料的机械性能与摩擦学性能。然而，在这些说明书中，只是提供了复合材料在常温下的摩擦磨损情况，未找到任何有关氮化硅在高温环境中的性能参数。而在高温以及超高温条件下，热应力的作用会严重降低氮化硅的机械强度，使其易于发生磨损而不能长寿命使用。为了满足工业的需求，急需要开发出一种适用于高温环境中具有高耐磨表面的自润滑氮化硅基复合材料。
发明内容
本发明的目的在于提供一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料，该材料在高温环境中超耐磨且表面自润滑。
本发明主要是以Ti2SnC为前驱体，在烧结过程中利用原位生成的金属锡实现Si3N4基复合材料在高温下的自润滑，并且利用锡氧化形成的氧化膜实现超高的耐磨性。
一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料，其特征在于该复合材料通过以下方法制备得到：
1）将α-Si3N4和Ti2SnC放入球磨机进行球磨即得混合粉末；
2）将混合粉末干燥过筛后装入石墨模具中进行预压；
3）将步骤2）所得预压样进行高温高压烧结，随后随炉冷却，得到毛坯；
4）将毛坯进行表面抛光、去毛刺处理即得自润滑氮化硅基复合材料。
所述α-Si3N4和Ti2SnC在二者中的质量百分比依次为70～90 %、10～30 %。
所述α-Si3N4的粒度0.5～1.5 µm，纯度大于99%；Ti2SnC的粒度小于5 µm，纯度大于99%。
所述球磨的条件：每30 g混合粉末添加0.5 mL酒精作为分散剂，球料比5～8:1，球磨机转速为200～250 r/min，顺时针转30min，停歇5min，逆时针转30min，停歇5min，以此为一个周期，循环8～10个周期。
所述预压的条件：压力40MPa，保压时间20～30 s。
所述高温高压烧结的参数为：压力30～40 MPa，烧结温度1650～1700 ºC，升温速度100 ºC/min，保温时间10～15 min，真空度为10-2～10-1 Pa。
采用HT-1000高温摩擦磨损试验机进行摩擦磨损测试，对偶球为Si3N4陶瓷球，载荷为 10 N，滑动线速度为 0.13 m/s，摩擦半径为 3 mm，行程为 234 m，测试温度分别为 25ºC、200 ºC、400 ºC、600 ºC和800 ºC。摩擦系数和磨损率至少为3次实验平均值。
本发明所述自润滑氮化硅基复合材料具有以下优点：
1、本发明制备工艺简单可控，粉末无需特殊处理；成品自润滑效果优异，高温耐磨损性能极佳，大大延长了陶瓷在高温环境中的使用寿命，可以广泛应用于高温度条件下无润滑界面之间的器件材料。
2、改善纯Si3N4陶瓷在高温环境中高摩擦系数和磨损率的缺陷，基体中的锡在高温摩擦过程中会析出，降低摩擦系数；并且发生氧化而形成氧化锡，增强基体的耐磨损能力。
3、本发明所述复合材料在制备过程中首次将金属锡以润滑相的形式加入到陶瓷基体中，解决了低熔点金属在烧结过程中易于流出的难题，为金属-陶瓷复合材料的制备提供了一种新的思路。
附图说明
图1 为本发明实施例1所得复合材料在400 ºC的大气条件下热处理后表面的扫描电镜照片。
图2 为本发明实施例2所得复合材料在800 ºC的大气条件下热处理后表面的扫描电镜照片。
具体实施方式
实施例1
(1)混合粉末的制备：按照质量百分比，将10 % α-Si3N4和90 % Ti2SnC加入行星式球磨机进行均匀球混，每30 g混合粉料添加0.5 mL酒精作为分散剂，球料比5:1，球磨机转速为200r/min，顺时针转30min，停歇5min，逆时针转30min，停歇5min，以此为一个周期，循环8个周期。
(2)预压烘干：将步骤(1)的混合粉料干燥过筛后装入直径为25 mm圆柱形石墨模具中，压力40 MPa，保压时间30 s。
(3)高温高压烧结：对步骤(2)的预压样进行高温高压烧结，烧结参数为：压力为30MPa，烧结温度为1650 ºC，升温速度为100 ºC/min，保温时间10min，真空度为10-2Pa，随后随炉冷却，得到毛坯。
(4)将(3)所制备的毛坯进行表面磨削、去毛刺处理，得到所述的新型Si3N4基自润滑复合材料。随后将复合材料在400 ºC的大气条件下进行加热处理，图1显示了复合材料热处理后表面的扫描电镜照片。
实施例2
(1) 混合粉末的制备：按照质量百分比，将20 % α-Si3N4和80 % Ti2SnC加入行星式球磨机进行均匀球混，每30 g混合粉料添加0.5 mL酒精作为分散剂，球料比5:1，球磨机转速为200r/min，顺时针转30 min，停歇5 min，逆时针转30min，停歇5min，以此为一个周期，循环8个周期。
(2) 预压烘干：将步骤(1)的混合粉料干燥过筛后装入直径为25 mm圆柱形石墨模具中，压力40 MPa，保压时间30 s。
(3) 高温高压烧结：对步骤(2)的预压样进行高温高压烧结，烧结参数为：压力为30MPa，烧结温度为1650 ºC，升温速度为100 ºC/min，保温时间10min，真空度为10-2Pa，随后随炉冷却，得到毛坯。
(4) 将(3)所制备的毛坯进行表面磨削、去毛刺处理，得到所述的新型Si3N4基自润滑复合材料。随后将复合材料在800 ºC的大气条件下进行加热处理，图2显示了复合材料热处理后表面的扫描电镜照片。
实施例3
(1) 混合粉末的制备：按照质量百分比，将30 % α-Si3N4和70 % Ti2SnC加入行星式球磨机进行均匀球混，每30 g混合粉料添加0.5 mL酒精作为分散剂，球料比5:1，球磨机转速为200r/min，顺时针转30min，停歇5min，逆时针转30min，停歇5min，以此为一个周期，循环8个周期。
(2) 预压烘干：将步骤(1)的混合粉料干燥过筛后装入直径为25 mm圆柱形石墨模具中，压力40 MPa，保压时间30 s。
(3) 高温高压烧结：对步骤(2)的预压样进行高温高压烧结，烧结参数为：压力为30MPa，烧结温度为1650 ºC，升温速度为100 ºC/min，保温时间10min，真空度为10-2Pa，随后随炉冷却，得到毛坯。
(4) 将(3)所制备的毛坯进行表面磨削、去毛刺处理，得到所述的新型Si3N4基自润滑复合材料。纯Si3N4和新型Si3N4基复合材料在25 ºC、200 ºC、400 ºC、600ºC和800 ºC下的摩擦系数和磨损率如表1和表2所示。
表1：实施例3中纯Si3N4和新型Si3N4基复合材料在25 ºC、200 ºC、400 ºC、600 ºC和800 ºC下的摩擦系数。
Figure 684301DEST_PATH_IMAGE001
表2：实施例3中纯Si3N4和新型Si3N4基复合材料在25 ºC、200 ºC、400 ºC、600 ºC和800 ºC下的磨损率。
Figure 138897DEST_PATH_IMAGE002
。

Claims (2)

1.一种高温环境中具有高耐磨表面的自润滑氮化硅基复合材料，其特征在于该复合材料通过以下方法制备得到：
1）将α-Si3N4和Ti2SnC放入球磨机进行球磨即得混合粉末；所述α-Si3N4和Ti2SnC在二者中的质量百分比依次为70～90 %、10～30 %；所述α-Si3N4的粒度0.5～1.5 µm，纯度大于99%；Ti2SnC的粒度小于5 µm，纯度大于99%；
2）将混合粉末干燥过筛后装入石墨模具中进行预压；所述预压的条件：压力40 MPa，保压时间20～30 s；
3）将步骤2）所得预压样进行高温高压烧结，随后随炉冷却，得到毛坯；所述高温高压烧结的参数为：压力30～40MPa，烧结温度1650～1700 ºC，升温速度100 ºC/min，保温时间10～15 min，真空度为10 -2 ～10 -1 Pa；
4）将毛坯进行表面抛光、去毛刺处理即得自润滑氮化硅基复合材料。
2.如权利要求1所述的复合材料，其特征在于所述球磨的条件：每30 g混合粉末添加0.5 mL酒精作为分散剂，球料比5～8:1，球磨机转速为200～250 r/min，顺时针转30min，停歇5min，逆时针转30min，停歇5min，以此为一个周期，循环8～10个周期。
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