CN108314450A - 通过球磨石墨球制备石墨/氧化锆自润滑复合陶瓷材料的方法 - Google Patents

通过球磨石墨球制备石墨/氧化锆自润滑复合陶瓷材料的方法 Download PDF

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CN108314450A
CN108314450A CN201810230873.XA CN201810230873A CN108314450A CN 108314450 A CN108314450 A CN 108314450A CN 201810230873 A CN201810230873 A CN 201810230873A CN 108314450 A CN108314450 A CN 108314450A
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zirconium oxide
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艾云龙
吕晨
陈卫华
何文
梁炳亮
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Nanchang Hangkong University
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Abstract

一种制备石墨/氧化锆自润滑复合陶瓷材料的方法。这种方法是通过称取适量的3mol%Y2O3稳定的亚微米级ZrO2粉体，加入尺寸合适的助磨ZrO2球和高纯石墨球，以无水乙醇为介质进行二次球磨，二次球磨后进行干燥，干燥后可获得石墨/氧化锆复合粉体。把获得的石墨/氧化锆复合粉体进行研磨造粒、过筛以及预压成型，再进行冷等静压，最后烧结成型。本发明石墨/氧化锆烧结体中的石墨分散均匀、细小，在此过程中未使用任何表面活性剂和粘结剂。

Description

通过球磨石墨球制备石墨/氧化锆自润滑复合陶瓷材料的 方法
技术领域
本发明涉及陶瓷基自润滑复合材料领域，具体属于一种利用高纯石墨球磨珠制备石墨/氧化锆自润滑复合陶瓷材料的方法。
背景技术
氧化锆(TZP)具有高熔点、高硬度、耐高温、耐磨和良好的断裂韧性，一般应用在轴承、家用刀具、生物医用材料和密封件等领域。在不添加任何润滑剂的情况下，氧化锆陶瓷的摩擦性能并不理想，其摩擦系数和磨损率都相对较高，使其无法在轴承等领域上发挥出优异的性能。一般的润滑技术包括固体润滑、液体润滑和气体润滑等润滑技术，这些润滑技术都无法在同时满足苛刻条件下使用，比如：1、强腐蚀、高温、真空等环境下使用；2、无需补充或少补充；3、易于操作。
发明内容
本发明旨在提供利用石墨球磨珠制备石墨/氧化锆自润滑复合陶瓷材料的方法，目的是解决石墨在ZrO2陶瓷中分散不均匀、易团聚的问题。该过程所涉及的设备简单，操作简便，绿色环保，不添加任何表面活性剂和粘结剂。
本发明是解决石墨分散不均匀、易团聚所采用的技术方案，一种制备石墨/氧化锆自润滑复合陶瓷材料的方法，主要包括以下几个步骤：
步骤一：称取一定量的亚微米级ZrO2(3mol%Y2O3)粉体和试验所用的高纯石墨球放入球磨罐中，再加入尺寸、数量合适的助磨ZrO2球，以无水乙醇为介质，在行星球磨机中进行第一次球磨，第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉（使石墨达到预期的含量）进行第二次球磨；
步骤二：第二次球磨结束后，把浆料倒入烧杯中放进干燥箱中干燥；
步骤三：造粒，无需添加任何粘结剂，将复合粉体充分研磨，混合均匀，使用200目的标准分样筛过筛；
步骤四：将上述复合粉体进行预压成型、冷等静压，最后烧结成型。
亚微米级ZrO2粉体与高纯石墨球的重量比为1:1~1:15，高纯石墨球与助磨ZrO2球的数量比为1:1~1:20，高纯石墨球的直径为5~50mm，助磨ZrO2球的直径为1~30mm；球磨时间为2~96h，转速为100~1000rpm；预压成型压力为10~140Mpa，保压1~10min；冷等静压100~500Mpa，保压1~10min。
本发明的特点：使用高纯石墨球制备的石墨/氧化锆自润滑复合陶瓷材料，石墨能够均匀的分散在ZrO2基体上，该石墨片明显比直接加石墨粉球磨后所得到石墨/氧化锆复合粉体、烧结体中的石墨片薄、细很多。该方法无需使用任何表面活性剂，操作简单，价格适合，对环境也不会造成污染。
附图说明
图1、3、5分别是实例5得到的石墨/氧化锆复合粉体和石墨/氧化锆烧结体断口的SEM图，图2、4、6、7、8分别是实例2得到的石墨/氧化锆复合粉体、石墨/氧化锆烧结体断口的SEM图和石墨/氧化锆复合粉体XRD图以及石墨/氧化锆烧结体断口的XRD图，图9是实例5得到的石墨/氧化锆烧结体的摩擦系数，图10是实例2得到的石墨/氧化锆烧结体的摩擦系数。摩擦试验所用的对摩材料是Al2O3陶瓷球（浙江杰奈尔新材料有限公司），Al2O3陶瓷球硬度大于HRA90，表面粗糙度（Ra）为0.058µm，直径（Ф）为4mm。摩擦试验所用转速为0.2m/s，载荷为10N，测试时间为30min。
表1是实验使用仪器及设备，表2是两种不同方法（实例2和实例5）制备的石墨/氧化锆复合陶瓷材料的性能比较。
图1是本发明的10 vol.%石墨（石墨粉）/氧化锆复合粉体的SEM图。
图2是本发明的10 vol.%石墨（高纯石墨球）/氧化锆复合粉体的SEM图。
图3是本发明的10 vol.%石墨（石墨粉）/氧化锆烧结体断口的SEM图。
图4是本发明的10 vol.%石墨（高纯石墨球）/氧化锆烧结体断口的SEM图。
图5是本发明的10 vol.%石墨（石墨粉）/氧化锆烧结体断口的SEM图。
图6是本发明的10 vol.%石墨（高纯石墨球）/氧化锆烧结体断口的SEM图。
图7.10 vol.%石墨（高纯石墨球）/氧化锆复合粉体的XRD图。
图8.10 vol.%石墨（高纯石墨球）/氧化锆烧结体的XRD图。
图9是本发明的10 vol.%石墨（石墨粉）/氧化锆烧结体的摩擦系数示意图。
图10是本发明的10 vol.%石墨（高纯石墨球）/氧化锆烧结体的摩擦系数示意图。
具体实施方式
以下对本发明举例说明：
实例1：称取一定量亚微米级ZrO2(3mol%Y2O3)粉、尺寸合适的高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）混合放入球磨罐中，高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）数量比为1:5，球磨介质为无水乙醇，混料呈浆料状，使用行星球磨机进行第一次球磨，转速200rpm，球磨时间为12h。第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉（使石墨达到预期的含量）进行第二次球磨，第二次球磨罐中的ZrO2球和石墨/氧化锆复合粉体重量比为5:1，转速250rpm，球磨时间为24h。第二次球磨结束后，倒出浆料在干燥箱中90℃干燥。干燥后的复合粉体进行充分研磨和过筛，预压成型，在180Mpa下进行冷等静压，保压3-5min。通过微波烧结成型，烧结温度为1400℃，保温30min，升温速率为10℃/min，在1000℃时，保温10min。获得石墨/氧化锆烧结体。
实例2：称取一定量亚微米级ZrO2(3mol%Y2O3)粉、尺寸合适的高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）混合放入球磨罐中，高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）数量比为1:5，球磨介质为无水乙醇，混料呈浆料状，使用行星球磨机进行第一次球磨，转速200rpm，球磨时间为24h。第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉（使石墨达到预期的含量）进行第二次球磨，第二次球磨罐中的ZrO2球和石墨/氧化锆复合粉体重量比为5:1，转速250rpm，球磨时间为24h。第二次球磨结束后，倒出浆料在干燥箱中90℃干燥。干燥后的复合粉体进行充分研磨和过筛，预压成型，在180Mpa下进行冷等静压，保压3-5min。通过微波烧结成型，烧结温度为1400℃，保温30min，升温速率为10℃/min，在1000℃时，保温10min。获得石墨/氧化锆烧结体。
实例3：称取一定量亚微米级ZrO2(3mol%Y2O3)粉、尺寸合适的高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）混合放入球磨罐中，高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）数量比为1:5，球磨介质为无水乙醇，混料呈浆料状，使用行星球磨机进行第一次球磨，转速200rpm，球磨时间为24h。第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉（使石墨达到预期的含量）进行第二次球磨，第二次球磨罐中的ZrO2球和石墨/氧化锆复合粉体重量比为5:1，转速250rpm，球磨时间为48h。第二次球磨结束后，倒出浆料在干燥箱中90℃干燥。干燥后的复合粉体进行充分研磨和过筛，预压成型，在180Mpa下进行冷等静压，保压3-5min。通过微波烧结成型，烧结温度为1400℃，保温30min，升温速率为10℃/min，在1000℃时，保温10min。获得石墨/氧化锆烧结体。
实例4：称取一定量亚微米级ZrO2(3mol%Y2O3)粉、尺寸合适的高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）混合放入球磨罐中，高纯石墨球（Ф15mm）和助磨ZrO2球（Ф6mm）数量比为1:5，球磨介质为无水乙醇，混料呈浆料状，使用行星球磨机进行第一次球磨，转速200rpm，球磨时间为24h。第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉（使石墨达到预期的含量）进行第二次球磨，第二次球磨罐中的ZrO2球和石墨/氧化锆复合粉体重量比为5:1，转速300rpm，球磨时间为48h。第二次球磨结束后，倒出浆料在干燥箱中90℃干燥。干燥后的复合粉体进行充分研磨和过筛，预压成型，在180Mpa下进行冷等静压，保压3-5min。通过微波烧结成型，烧结温度为1400℃，保温30min，升温速率为10℃/min，在1000℃时，保温10min。获得石墨/氧化锆烧结体。
实例5：称取一定量亚微米级ZrO2(3mol%Y2O3)粉、石墨粉和尺寸、数量合适的ZrO2球混合放入球磨罐中，ZrO2球和石墨/氧化锆复合粉体重量比为5:1，球磨介质为无水乙醇，混料呈浆料状，使用行星球磨机进行球磨，转速250rpm，球磨时间为24h。球磨结束后，倒出浆料在干燥箱中90℃干燥。干燥后的复合粉体进行充分研磨和过筛，预压成型，在180Mpa下进行冷等静压，保压3-5min。通过微波烧结成型，烧结温度为1400℃，保温30min，升温速率为10℃/min，在1000℃时，保温10min。获得石墨/氧化锆烧结体。
表1. 实验使用仪器及设备
表2. 两种不同方法制备的石墨/ZrO2复合陶瓷材料的性能比较
。

Claims (4)

1.一种制备石墨/氧化锆自润滑复合陶瓷材料的方法，步骤如下：
步骤一：称取一定量的亚微米级ZrO2(3mol%Y2O3)粉体和试验所用的高纯石墨球放入球磨罐中，再加入尺寸、数量合适的助磨ZrO2球，以无水乙醇为介质，在行星球磨机中进行第一次球磨，第一次球磨结束后将高纯石墨球取出，冲净后将其干燥，称取其重量，计算石墨的磨量，再加入尺寸、数量合适的ZrO2球和所需量的ZrO2(3Y)粉,使石墨达到预期的含量，进行第二次球磨；
步骤二：第二次球磨结束后，把浆料倒入烧杯中放进干燥箱中干燥；
步骤三：造粒，无需添加任何粘结剂，将复合粉体充分研磨，混合均匀，使用200目的标准分样筛过筛；
步骤四：将上述复合粉体进行预压成型、冷等静压，最后烧结成型。
2.根据权利要求1所述的一种制备石墨/氧化锆自润滑复合陶瓷材料的方法，它包括：亚微米级ZrO2粉体与高纯石墨球的重量比为1:1~1:15，高纯石墨球与助磨ZrO2球的数量比为1:1~1:20，高纯石墨球的直径为5~50mm，助磨ZrO2球的直径为1~30mm。
3.根据权利要求1所述的一种制备石墨/氧化锆自润滑复合陶瓷材料的方法，其特征在于：所述球磨时间为2~96h，转速为100~1000rpm。
4.根据权利要求1所述的一种制备石墨/氧化锆自润滑复合陶瓷材料的方法，其特征在于：所述预压成型压力为10~140Mpa，保压1~10min；冷等静压100~500Mpa，保压1~10min。
CN201810230873.XA 2018-03-20 2018-03-20 通过球磨石墨球制备石墨/氧化锆自润滑复合陶瓷材料的方法 Pending CN108314450A (zh)

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