CN111018500A - 高纯氧化铝陶瓷的制备方法及陶瓷产品的制备方法 - Google Patents

高纯氧化铝陶瓷的制备方法及陶瓷产品的制备方法 Download PDF

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CN111018500A
CN111018500A CN201911350317.7A CN201911350317A CN111018500A CN 111018500 A CN111018500 A CN 111018500A CN 201911350317 A CN201911350317 A CN 201911350317A CN 111018500 A CN111018500 A CN 111018500A
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alumina ceramic
ceramic
alumina
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薛志岗
邱永斌
邱晨
朱军
郑兴益
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JIANGSU PROVINCE CERAMICS RESEARCH INSTITUTE CO LTD
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Abstract

本发明涉及一种氧化铝陶瓷的制备方法，尤其是高纯氧化铝陶瓷的制备方法，包括以下步骤：将多种直径的氧化铝陶瓷球混合；配置氧化铝粉，所述氧化铝粉与氧化铝陶瓷球的质量比为1:(1.5～3)；按照总重量的百分比加入以下辅料：0.5～2.5％拟薄水铝石、0.1～0.3％的硅溶胶、0.2～0.6％的氧化镁、0.1～0.6的氧化钇；将氧化铝陶瓷球、氧化铝粉、辅料均加入到球磨机中，同时加入0.1％～0.5％的分散剂，湿法球磨20～30h得到浆料；将球磨后的浆料酸化处理；将酸化处理后的浆料进行喷雾造粒，喷雾造粒得到高纯氧化铝陶瓷；将高纯氧化铝陶瓷在温度在20～45℃，湿度在40～65％的环境下均化处理24～48小时，得到高纯氧化铝陶瓷，所述高纯氧化铝陶瓷的氧化铝含量不低于99.5％。该高纯氧化铝陶瓷制备方便成本低、陶瓷性能好。

Description

高纯氧化铝陶瓷的制备方法及陶瓷产品的制备方法
技术领域
本发明涉及一种氧化铝陶瓷的制备方法，尤其是高纯氧化铝陶瓷的制备方法及陶瓷产品的制备方法。
背景技术
氧化铝陶瓷作为基础陶瓷材料，以其良好的耐磨性、耐酸碱腐蚀性，较高的硬度、抗折强度等一系列性能广泛应用于各行各业。随着科学技术的发展，各行各业对于基础材料的性能要求也越来越高。氧化铝陶瓷制品的氧化铝含量从75％、85％、95％、99％逐渐提高到99.5％以上。
随着陶瓷材料中氧化铝含量的提高，氧化铝陶瓷制品的烧结也变得越来越困难，对于氧化铝粉体的烧结活性的要求也相应提高。然而传统的氧化铝粉体制备方法已经跟不上使用要求，传统方法制备的氧化铝粉体的粒径最小处于1～2微米之间，若要制备D50 0.5微米左右的粉体，则需要通过化学法或者采用砂磨机进行加工，粉体加工成本大幅度上升，导致D50 0.5微米及以下的粉体价格是传统氧化铝粉体的2～10倍，市场难以接受，暂时未能大范围使用。
常规的的99瓷材料密度3.85g/cm3左右，晶粒尺寸10～20μm、表面抛光光洁度Ra0.4～0.8、抗化学侵蚀性较差，达不到相关技术性能要求。而采用高纯超细粉体制备的陶瓷材料，由于原料价格昂贵，最终的制品价格昂贵，综合性价比较差。因此，采用新方法开发生产细晶、高致密99.5氧化铝陶瓷材料，不提高原料成本而提升材料的相关技术性能指标，具有重要意义。
发明内容
为解决上述问题，本发明提供一种氧化铝原料成本低、性能好的高纯氧化铝陶瓷的制备方法，具体技术方案为：
高纯氧化铝陶瓷的制备方法，包括以下步骤：
配置氧化铝陶瓷球，将多种直径的氧化铝陶瓷球混合；配置氧化铝粉，所述氧化铝粉与氧化铝陶瓷球的质量比为1:(1.5～3)；配置辅料，按照总重量的百分比加入以下辅料：0.5～2.5％拟薄水铝石、0.1～0.3％的硅溶胶、0.2～0.6％的氧化镁、0.1～0.6％的氧化钇；将氧化铝陶瓷球、氧化铝粉、辅料均加入到球磨机中，同时加入0.1％～0.5％的分散剂，然后进行湿法球磨，湿法球磨20～30h，球磨后形成浆料；酸化处理，将球磨后的浆料酸化处理；喷雾造粒，将酸化处理后的浆料进行喷雾造粒，喷雾造粒得到高纯氧化铝陶瓷；均化处理，将高纯氧化铝陶瓷在温度在20～45℃，湿度在40～65％的环境下均化处理24～48小时，得到高纯氧化铝陶瓷，所述高纯氧化铝陶瓷的氧化铝含量不低于99.5％。
进一步的，所述氧化铝陶瓷球按照以下的重量份数配置：8～10mm的氧化铝陶瓷球30～50份，4～6mm的氧化铝陶瓷球5～15份，1～3mm的氧化铝陶瓷球30～50份。
进一步的，所述氧化铝陶瓷球的氧化铝含量不低于99.5％。
进一步的，所述氧化铝粉的中位径在80μm、原晶中位径在1.7μm。
进一步的，所述氧化铝粉的氧化铝含量不低于99.85％。
进一步的，所述酸化处理时调整浆料的pH值为3～5，使拟薄水铝石胶溶包裹于氧化铝晶粒表面。
高纯氧化铝陶瓷产品的制备方法，包括以下步骤：将高纯氧化铝陶瓷用干压或等静压成型方法制备陶瓷坯体；将陶瓷坯体放入高温炉中，在1600～1650℃下保温3～5h烧结，按100～150℃/h进行快速降温，得到高纯氧化铝陶瓷产品。
高纯氧化铝陶瓷板的制备方法，包括以下步骤：将高纯氧化铝陶瓷装入定制形状的橡塑模具袋并密封，然后置入冷等静压机进行等静压成型，获得陶瓷板坯体，将压制的陶瓷板坯体放置在高温炉内，升温速率9℃/小时，最高温度不大于1620℃，保温5小时，按100～150℃/h快速降温，得到陶瓷板。
高纯氧化铝陶瓷轧辊的制备方法，包括以下步骤：将高纯氧化铝陶瓷装入高弹橡塑模具内，然后置入等静压机，在100MPa压力下成型得到陶瓷轧辊粗坯体，车加工得陶瓷轧辊坯体，将陶瓷轧辊坯体放置在高温炉内，升温速率21℃/小时，温度不大于1605℃，保温4小时，按100～150℃/h快速降温，得到陶瓷轧辊。
与现有技术相比本发明具有以下有益效果：
本发明提供的高纯氧化铝陶瓷的制备方法具有如下优点：
1)氧化铝陶瓷球为高纯氧化铝陶瓷微球，并按一定级配配比加入，提高了球磨机的研磨效率，减小粉体的晶粒尺寸，提高了粉体的烧成活性；
2)球磨过程中添加了拟薄水铝石，并对球磨后的浆料进行酸化处理，使拟薄水铝石胶溶覆盖于氧化铝晶粒表面，喷雾造粒后，在氧化铝晶粒表面形成高烧结活性的纳米氢氧化铝覆盖层，提高了陶瓷材料的烧成致密度和晶粒间的结合强度，提高了陶瓷材料的各项性能指标；
3)对造粒料环境温度、相对湿度进行控制，使造粒料的含水率和温度达到规定要求，提高了造粒料的成型性能；
4)坯体采用微电脑精密控温燃气窑高温烧成，高温烧成之后按100～150℃/h快速降温，使得陶瓷内部晶粒生长时间缩短，晶粒尺寸较小，小于8微米，提高了陶瓷材料的致密度、机械强度和后期抛光的表面光洁度。
与原有技术相比，本发明的提供的高纯氧化铝陶瓷可以按照预定的制造工艺进行控制，制成大规格精细高纯氧化铝陶瓷圆板、大尺寸陶瓷辊等一系列高纯氧化铝陶瓷制品，成本低。
附图说明
图1是采用本发明的高纯氧化铝陶瓷制成的产品的微观晶粒尺寸图。
具体实施方式
现结合附图对本发明作进一步说明。
实施例一
高纯氧化铝陶瓷的制备方法，包括以下步骤：
配置氧化铝陶瓷球，将多种直径的氧化铝陶瓷球混合；
配置氧化铝粉，所述氧化铝粉与氧化铝陶瓷球的质量比为1:(1.5～3)；
配置辅料，按照总重量的百分比加入以下辅料：
0.5～2.5％拟薄水铝石、0.1～0.3％的硅溶胶、0.2～0.6％的氧化镁、0.1～0.6％的氧化钇；
将氧化铝陶瓷球、氧化铝粉、辅料均加入到球磨机中，同时加入0.1％～0.5％分散剂，然后进行湿法球磨，湿法球磨20～30h，球磨后形成浆料；
酸化处理，将球磨后的浆料酸化处理；
喷雾造粒，将酸化处理后的浆料进行喷雾造粒，喷雾造粒得到高纯氧化铝陶瓷；
均化处理，将高纯氧化铝陶瓷在温度在20～45℃，湿度在40～65％的环境下均化处理24～48小时，得到高纯氧化铝陶瓷，所述高纯氧化铝陶瓷的氧化铝含量不低于99.5％。
氧化铝陶瓷球按照以下的重量份数配置：8～10mm的氧化铝陶瓷球30～50份，4～6mm的氧化铝陶瓷球5～15份，1～3mm的氧化铝陶瓷球30～50份。
氧化铝陶瓷球的氧化铝含量不低于99.5％。
氧化铝粉的中位径在80μm、原晶中位径在1.7μm。
氧化铝粉的氧化铝含量不低于99.85％。
酸化处理时调整浆料的pH值在3～5之间，使拟薄水铝石胶溶包裹于氧化铝晶粒表面。
喷雾造粒时加入PVA和润滑剂。
选用99.85％氧化铝原粉，加入0.5～2.5％拟薄水铝石、0.1～0.3％硅溶胶(固含量25％)、0.2～0.6％氧化镁、0.1～0.6％氧化钇，按比例加入氧化铝陶瓷球，球磨20～26hrs，喷雾干燥制备造粒料，经均化处理后，控制粉料温度在20～45℃，湿度在40～65％，采用干压或等静压成型，制得陶瓷坯体，将坯体放置在高温炉内，微电脑精密控温高温烧成，最高烧成温度1600～1650℃，保温3-5小时，烧成的陶瓷产品进行精密数控磨削加工，得到精细高纯氧化铝陶瓷制品。陶瓷制品有以下特征：产品尺寸100-2000mm，材料体积密度3.90-3.93g/cm3，硬度HRA≥90，抗弯强度>380Mpa，微观晶粒尺寸2-8μm左右。
实施例二
高纯氧化铝陶瓷产品的制备方法，包括以下步骤：
将高纯氧化铝陶瓷用等静压成型方法制备陶瓷坯体；将陶瓷坯体放入高温炉中，在1600～1650℃下保温3～5h烧结，得到高纯氧化铝陶瓷产品。
实施例三
选用99.85％氧化铝，加入2.5％拟薄水铝石、0.3％硅溶胶(固含量25％)、0.2％氧化镁、0.1％氧化钇，按比例加入氧化铝陶瓷球，湿法研磨22h，喷雾干燥制备造粒料，经均化处理后，控制粉料温度25℃，湿度45％，粉料装入定制形状的橡塑模具袋，密封，置入冷等静压机进行等静压成型，获得2400mm×300mm×50mm的陶瓷长板坯体，将压制的坯体放置在高温炉内，采用微电脑精密控温高温烧成，升温速率9℃/小时，最高温度1620℃，保温5小时，烧结后的陶瓷长板板通过磨削加工，得到一件精细99.5氧化铝陶瓷长板，其长度2000mm，宽度240mm,厚度35mm，无气孔，无细微裂纹，陶瓷材料的体积密度为3.91g/cm3，硬度HRA：91.7，加工后表面粗糙度0.2μm。
实施例四
选用99.9％氧化铝，加入1％拟薄水铝石、0.2％氧化镁、0.3％氧化钇，按比例加入氧化铝陶瓷球，湿法研磨26h，喷雾干燥制备造粒料，经均化处理后，控制粉料温度35℃，湿度55％，将粉料加入高弹橡塑模具内，置入等静压机内在100MPa压力下成型，获得φ450mm×500mm的陶瓷坯体，经车加工得到φ460mm×485mm坯体。放置高温炉内，微电脑精密控温烧成，升温速率21℃/小时，最高温度1605℃，保温4小时。烧结的陶瓷轧辊通过磨削加工、金属封装，得到φ350mm×400mm的结构件，表面光洁，无气孔，磨加工后表面光洁度Ra0.4；陶瓷材料的体积密度为3.90g/cm3，硬度HRA90.7。

Claims (9)

1.高纯氧化铝陶瓷的制备方法，其特征在于，包括以下步骤：
配置氧化铝陶瓷球，将多种直径的氧化铝陶瓷球混合；
配置氧化铝粉，所述氧化铝粉与氧化铝陶瓷球的质量比为1:(1.5～3)；
配置辅料，按照总重量的百分比加入以下辅料：
0.5～2.5％拟薄水铝石、0.1～0.3％的硅溶胶、0.2～0.6％的氧化镁、0.1～0.6％的氧化钇；
将氧化铝陶瓷球、氧化铝粉、辅料均加入到球磨机中，同时加入0.1％～0.5％的分散剂，然后进行湿法球磨，湿法球磨20～30h，球磨后形成浆料；
酸化处理，将球磨后的浆料酸化处理；
喷雾造粒，将酸化处理后的浆料进行喷雾造粒，喷雾造粒得到高纯氧化铝陶瓷；
均化处理，将高纯氧化铝陶瓷在温度在20～45℃，湿度在40～65％的环境下均化处理24～48小时，得到高纯氧化铝陶瓷，所述高纯氧化铝陶瓷的氧化铝含量不低于99.5％。
2.根据权利要求1所述的高纯氧化铝陶瓷的制备方法，其特征在于，所述氧化铝陶瓷球按照以下的重量份数配置：
8～10mm的氧化铝陶瓷球30～50份，4～6mm的氧化铝陶瓷球5～15份，1～3mm的氧化铝陶瓷球30～50份。
3.根据权利要求2所述的高纯氧化铝陶瓷的制备方法，其特征在于，所述氧化铝陶瓷球的氧化铝含量不低于99.5％。
4.根据权利要求1所述的高纯氧化铝陶瓷的制备方法，其特征在于，所述氧化铝粉的中位径在80μm、原晶中位径在1.7μm。
5.根据权利要求4所述的高纯氧化铝陶瓷的制备方法，其特征在于，所述氧化铝粉的氧化铝含量不低于99.85％。
6.根据权利要求1所述的高纯氧化铝陶瓷的制备方法，其特征在于，所述酸化处理时调整浆料的pH值为3～5，使拟薄水铝石胶溶包裹于氧化铝晶粒表面。
7.高纯氧化铝陶瓷产品的制备方法，其特征在于，包括以下步骤：
将高纯氧化铝陶瓷用干压或等静压成型方法制备陶瓷坯体；
将陶瓷坯体放入高温炉中，在1600～1650℃下保温3～5h烧结，按100～150℃/h进行快速降温，得到高纯氧化铝陶瓷产品。
8.高纯氧化铝陶瓷板的制备方法，其特征在于，包括以下步骤：
将高纯氧化铝陶瓷装入定制形状的橡塑模具袋并密封，然后置入冷等静压机进行等静压成型，获得陶瓷板坯体，将压制的陶瓷板坯体放置在高温炉内，升温速率9℃/小时，最高温度不大于1620℃，保温5小时，按100～150℃/h快速降温，得到陶瓷板。
9.高纯氧化铝陶瓷轧辊的制备方法，其特征在于，包括以下步骤：
将高纯氧化铝陶瓷装入高弹橡塑模具内，然后置入等静压机，在100MPa压力下成型得到陶瓷轧辊粗坯体，车加工得陶瓷轧辊坯体，将陶瓷轧辊坯体放置在高温炉内，升温速率21℃/小时，温度不大于1605℃，保温4小时，按100～150℃/h快速降温，得到陶瓷轧辊。
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Application publication date: 20200417