CN108947493A - 一种高致密度纳米氧化镁基陶瓷的制备方法 - Google Patents

一种高致密度纳米氧化镁基陶瓷的制备方法 Download PDF

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CN108947493A
CN108947493A CN201810901429.6A CN201810901429A CN108947493A CN 108947493 A CN108947493 A CN 108947493A CN 201810901429 A CN201810901429 A CN 201810901429A CN 108947493 A CN108947493 A CN 108947493A
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莫云泽
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SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种高致密度纳米氧化镁基陶瓷的制备方法。该纳米氧化镁基陶瓷采用高纯度纳米氧化镁为原料，高纯度的氧化锆、氧化钇、氧化铝以及二氧化钛混合为添加剂制备而成，其中氧化镁含量≥85wt%、相对致密度≥95%，添加剂含量为15wt%。通过液相研磨混料、喷雾干燥造粒一体化、高压成型和高温烧结的工艺制备得到所述的纳米氧化镁基陶瓷。本发明的纳米氧化镁基陶瓷具有致密度高、纯度高、耐高温、耐腐蚀等特点，可长期应用于高温煅烧、金属冶炼等高温、高腐蚀性等环境，该制备工艺稳定、成品率高、适应范围广，适于批量化生产。

Description

一种高致密度纳米氧化镁基陶瓷的制备方法
技术领域
本发明属于功能材料的制备技术领域，具体地说是涉及一种高致密度纳米氧化镁基陶瓷的制备方法。
背景技术
氧化镁基陶瓷以氧化镁为主成分的陶瓷，属立方晶系，其抗拉强度、抗压强度及抗弯强度都比烧结氧化铝低得多，它的高温强度也较低。氧化镁是良好的绝缘体，室温下电阻率随温度升高，电阻率急剧降低。氧化镁陶瓷也是典型的碱性耐火材料，在氧化气氛或氮气保护下可稳定工作到2400℃。氧化镁陶瓷还可用作冶炼金属的坩埚，在原子能工业中也适于冶炼高纯度的铀和钍；还可用作热电偶保护套管。利用它能使电磁波通过的性质，作雷达罩及红外辐射的透射窗口材料等。
高纯度氧化镁陶瓷具有耐高温、耐腐蚀等优点，但高纯度氧化镁陶瓷较难致密烧结，使用高纯度纳米氧化镁为原料，由于其堆积密度低、反应活性强，使得制粉、成型有一定困难，特别是制备高致密度大尺寸氧化镁管、坩埚容易产生变形、开裂等现象。
本专利采用高纯度纳米氧化镁为原料，高纯度的氧化锆、氧化钇、氧化铝以及二氧化钛混合为添加剂制备而成。通过液相研磨混料、喷雾干燥造粒一体化、高压成型和高温烧结的工艺制备得到所述的纳米氧化镁基陶瓷。该方法大大提升了原料在混料过程中的均匀度，同时将干燥和造粒简化为一步，极大的提升了氧化镁基陶瓷的品质。
发明内容
本发明的目的在于克服现有技术制备氧化镁基陶瓷存在的品质低下、混料不均、成品率低的难题，提供了一种具有稳定的高致密度纳米氧化镁基陶瓷的制备方法。
为达到上述预期目的，本发明采用如下技术方案：
一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，采用高纯度纳米氧化镁为原料，高纯度的氧化锆、氧化钇、氧化铝以及二氧化钛混合为添加剂制备而成，其中氧化镁含量≥85wt%、相对致密度≥95%，添加剂含量为15wt%。该工艺包括如下步骤：
a．将纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体按照一定的比例组成称量，混合均匀；
b. 将步骤a混合均匀的粉体与水放入球磨罐或砂磨机中进行低温液相球磨，球磨介质为高纯度氧化钇稳定的氧化锆陶瓷球，湿磨混料2-40小时，得到均匀混合的陶瓷浆料；
c. 将步骤b制得的陶瓷浆料进行喷雾干燥，控制干燥后的粉体粒径，获得流动性好、颗粒尺寸为2-100 μm，堆积密度0.5-3.0g/cm3的陶瓷粉体，即完成造粒过程；
d. 将步骤c制得的造粒后的陶瓷粉体进行高压成型获得陶瓷坯体，通常采用的压力在10-300MPa 压力下保压2-30 分钟成型，即完成预加工处理；
e. 将步骤d制得的陶瓷坯体在高温烧结炉中按照预设烧结制度高温烧结获得基于纳米氧化镁基的氧化镁陶瓷。
所述的纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体的质量比为85：0~8：0~2：0~7：0~4。
所述的混合粉体与水的质量比为30-70：100，所述的低温液相球磨温度为0-10℃，所述的球磨介质大小为0.8mm或0.4mm。
所述的喷雾干燥的温度为180-300℃。
所述的预设烧结制度为以1℃/min-20℃/min 的升温速率从室温升温到300-400℃保温20-100 分钟，以1℃ /min-15℃ /min 的升温速率升温到 800℃-1000℃，保温20-100 分钟，以1℃ /min-10℃ /min 的升温速率升温到1400-1600℃保温1-10 小时，以1℃/min-5℃ /min 的升温速率升温到1700-1800℃保温1-10 小时，然后以1℃ /min-20℃ /min的降温速率冷却至室温。
本发明的有益效果：
本发明制得的纳米氧化镁基陶瓷具有致密度高、纯度高、耐高温、耐腐蚀等特点，可长期应用于高温煅烧、金属冶炼等高温、高腐蚀性等环境，本发明制备工艺稳定、成品率高、适应范围广，适于批量化生产，且不受具体陶瓷形状限制，适用于制备各种尺寸、形状的氧化镁陶瓷，成型后的陶瓷坯体烧结废品率几乎为零。
附图说明
图1 实施案例样品1的SEM图。
具体实施方式
本发明下面通过具体实例进行详细的描述，但是本发明的保护范围不受限于这些实施例子。
实施例1：将纳米氧化镁、氧化锆、氧化钇、氧化铝原料粉体按照85：8：2：5的比例组成称量，混合均匀；将混合均匀的粉体与水按30：100的质量比放入砂磨机中进行低温液相球磨，温度控制在0℃，球磨介质为0.8mm高纯度氧化钇稳定的氧化锆陶瓷球，湿磨混料2小时，得到均匀混合的陶瓷浆料；将陶瓷浆料进行喷雾干燥，温度为180℃，控制干燥后的粉体粒径，获得流动性好、颗粒尺寸为2-10 μm，堆积密度3.0g/cm3的陶瓷粉体，即完成造粒过程；将造粒后的陶瓷粉体进行高压成型获得陶瓷坯体，通常采用的压力在10MPa 压力下保压30 分钟成型，即完成预加工处理；将制得的陶瓷坯体在高温烧结炉中按照预设烧结制度高温烧结获得基于纳米氧化镁基的氧化镁陶瓷，预设烧结制度为以20℃/min 的升温速率从室温升温到300℃保温20分钟，以15℃ /min 的升温速率升温到 800℃，保温20分钟，以10℃ /min 的升温速率升温到1400℃保温1 小时，以5℃ /min 的升温速率升温到1700℃保温10 小时，然后以20℃ /min的降温速率冷却至室温。
实施例2：将纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体按照85：4：2：7：2的比例组成称量，混合均匀；将混合均匀的粉体与水按50：100的质量比放入球磨罐中进行低温液相球磨，温度控制在10℃，球磨介质为0.4mm高纯度氧化钇稳定的氧化锆陶瓷球，湿磨混料5小时，得到均匀混合的陶瓷浆料；将陶瓷浆料进行喷雾干燥，温度为300℃，控制干燥后的粉体粒径，获得流动性好、颗粒尺寸为50-100μm，堆积密度1.5g/cm3的陶瓷粉体，即完成造粒过程；将造粒后的陶瓷粉体进行高压成型获得陶瓷坯体，通常采用的压力在300MPa 压力下保压5分钟成型，即完成预加工处理；将制得的陶瓷坯体在高温烧结炉中按照预设烧结制度高温烧结获得基于纳米氧化镁基的氧化镁陶瓷，预设烧结制度为以20℃/min 的升温速率从室温升温到400℃保温50分钟，以15℃ /min 的升温速率升温到 900℃，保温50分钟，以10℃ /min 的升温速率升温到1500℃保温5 小时，以2℃ /min 的升温速率升温到1800℃保温4小时，然后以10℃ /min的降温速率冷却至室温。
实施例3：将纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体按照85：5：1：5：4的比例组成称量，混合均匀；将混合均匀的粉体与水按70：100的质量比放入球磨罐中进行低温液相球磨，温度控制在5℃，球磨介质为0.4mm高纯度氧化钇稳定的氧化锆陶瓷球，湿磨混料10小时，得到均匀混合的陶瓷浆料；将陶瓷浆料进行喷雾干燥，温度为230℃，控制干燥后的粉体粒径，获得流动性好、颗粒尺寸为20-50μm，堆积密度2.5g/cm3的陶瓷粉体，即完成造粒过程；将造粒后的陶瓷粉体进行高压成型获得陶瓷坯体，通常采用的压力在50MPa 压力下保压2 分钟成型，即完成预加工处理；将制得的陶瓷坯体在高温烧结炉中按照预设烧结制度高温烧结获得基于纳米氧化镁基的氧化镁陶瓷，预设烧结制度为以1℃/min 的升温速率从室温升温到400℃保温100分钟，以1℃ /min 的升温速率升温到 1000℃，保温100分钟，以1℃ /min 的升温速率升温到1600℃保温10 小时，以1℃ /min 的升温速率升温到1800℃保温1 小时，然后以1℃ /min的降温速率冷却至室温。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

1.一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，采用高纯度纳米氧化镁为原料，高纯度的氧化锆、氧化钇、氧化铝以及二氧化钛混合为添加剂制备而成，其中氧化镁含量≥85wt%、相对致密度≥95%，添加剂含量为15wt%。
2.该工艺包括如下步骤：
a．将纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体按照一定的比例组成称量，混合均匀；
b. 将步骤a混合均匀的粉体与水放入球磨罐或砂磨机中进行低温液相球磨，球磨介质为高纯度氧化钇稳定的氧化锆陶瓷球，湿磨混料2-40小时，得到均匀混合的陶瓷浆料；
c. 将步骤b制得的陶瓷浆料进行喷雾干燥，控制干燥后的粉体粒径，获得流动性好、颗粒尺寸为2-100 μm，堆积密度0.5-3.0g/cm3的陶瓷粉体，即完成造粒过程；
d. 将步骤c制得的造粒后的陶瓷粉体进行高压成型获得陶瓷坯体，通常采用的压力在10-300MPa 压力下保压2-30 分钟成型，即完成预加工处理；
e. 将步骤d制得的陶瓷坯体在高温烧结炉中按照预设烧结制度高温烧结获得基于纳米氧化镁基的氧化镁陶瓷。
3.根据权利要求1所述的一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，步骤a中所述的纳米氧化镁、氧化锆、氧化钇、氧化铝以及二氧化钛原料粉体的质量比为85：0~8：0~2：0~7：0~4。
4.根据权利要求1所述的一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，步骤b中所述的混合粉体与水的质量比为30-70：100，所述的低温液相球磨温度为0-10℃，所述的球磨介质大小为0.8mm或0.4mm。
5.根据权利要求1所述的一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，步骤c中所述的喷雾干燥的温度为180-300℃。
6.根据权利要求1所述的一种高致密度纳米氧化镁基陶瓷的制备方法，其特征在于，步骤e中，所述的预设烧结制度为以1℃/min-20℃/min 的升温速率从室温升温到300-400℃保温20-100 分钟，以1℃ /min-15℃ /min 的升温速率升温到 800℃-1000℃，保温20-100分钟，以1℃ /min-10℃ /min 的升温速率升温到1400-1600℃保温1-10 小时，以1℃ /min-5℃ /min 的升温速率升温到1700-1800℃保温1-10 小时，然后以1℃ /min-20℃ /min的降温速率冷却至室温。
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