CN109336618A - 一种高效制备高分散氧化锆陶瓷粉的方法 - Google Patents

一种高效制备高分散氧化锆陶瓷粉的方法 Download PDF

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CN109336618A
CN109336618A CN201811307812.5A CN201811307812A CN109336618A CN 109336618 A CN109336618 A CN 109336618A CN 201811307812 A CN201811307812 A CN 201811307812A CN 109336618 A CN109336618 A CN 109336618A
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江婷婷
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ZHEJIANG JINKUN ZIRCONIUM INDUSTRY Co Ltd
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Abstract

本发明公开一种高效制备高分散氧化锆陶瓷粉的方法，包括如下步骤：步骤一、将化学共沉淀得到的氢氧化锆洗涤并压制成固态滤饼；步骤二、将滤饼与去离子水混合，进行球磨；步骤三、将球磨后浆料滤出，并烘干；步骤四、将烘干后物料进窑炉煅烧，得到氧化锆粉体。本发明方法可提高球磨效率，大大减少磨损引入的杂质，煅烧所需温度可降低至700～900℃，节省能源并利于提高生产效率；有效去除团聚，避免了对氧化锆球磨，减少其因外力作用造成的t→m相变；适用范围广。

Description

一种高效制备高分散氧化锆陶瓷粉的方法
技术领域
本发明涉及材料技术领域，具体涉及一种高效制备高分散氧化锆陶瓷粉的方法。
背景技术
制造高性能陶瓷材料对所用的粉料有很高的要求，除对粉料的化学组成和相组成要求准确、均匀、杂质含量低之外，对粉料中的颗粒形状和尺寸有严格要求。大致可归纳如下：
1)颗粒尺寸小；
2)颗粒尺寸分布范围窄；
3)颗粒形状最好为球形或等轴粒状；
4)颗粒之间无团聚或团聚程度小。
目前氧化锆陶瓷的粉体大多使用化学共沉淀法生产，但其易产生团聚，造成粒度分布宽等问题。
发明内容
本发明的目的是提供一种高效制备高分散氧化锆陶瓷粉的方法，以解决现有技术的不足。
本发明采用以下技术方案：
一种高效制备高分散氧化锆陶瓷粉的方法，包括如下步骤：
步骤一、将化学共沉淀得到的氢氧化锆洗涤并压制成固态滤饼；
步骤二、将滤饼与去离子水混合，进行球磨；
步骤三、将球磨后浆料滤出，并烘干；
步骤四、将烘干后物料进窑炉煅烧，得到氧化锆粉体。
进一步地，步骤二滤饼与去离子水按质量比1:1～2:1混合。
进一步地，步骤二以280～350r/min球磨时间1～2h。
进一步地，步骤四700～900℃煅烧3～5h。
本发明的有益效果：
1、本发明通过对上游段氢氧化锆直接进行球磨细化，由于氢氧化锆硬度远小于氧化锆，故可提高球磨效率，且球磨时间的减少对于磨损引入的杂质大大减少；由于在煅烧前就对其进行了细化、表面改性，其煅烧所需温度可降低至700～900℃，节省能源并利于提高生产效率。
2、化学共沉淀法制备氧化锆粉体，沉淀生成及洗涤段最易发生团聚，而本发明直接作用在洗涤之后，可有效地去除团聚；避免了直接对氧化锆球磨，减少其因外力作用造成的t→m相变。
3、本发明方法适用于大多稳定剂稳定的氧化锆粉，如氧化钇、氧化镁、氧化铈、氧化钙等，适用范围广。
附图说明
图1为本发明方法与现有方法对比。
图2为实施例1中粉料在球磨前、球磨后、煅烧后的粒度分布。
图3为实施例2中粉料在球磨前、球磨后、煅烧后的粒度分布。
图4为按图1中现有方法制得的3Y氧化锆粉煅烧后、球磨后的粒度分布。
具体实施方式
下面结合实施例和附图对本发明做更进一步地解释。下列实施例仅用于说明本发明，但并不用来限定本发明的实施范围。
一种高效制备高分散氧化锆陶瓷粉的方法，包括如下步骤：
步骤一、将化学共沉淀得到的氢氧化锆洗涤并压制成固态滤饼；
步骤二、将滤饼与去离子水按质量比1:1～2:1混合，以280～350r/min球磨1～2h；
步骤三、将球磨后浆料滤出，并烘干；
步骤四、将烘干后物料进窑炉700～900℃煅烧3～5h，得到氧化锆粉体。
实施例1：
按3Y的比例称取171.2g氧氯化锆(含有结晶水)、六水合硝酸钇11.85g，溶于250ml去离子水中，取过量的氨水(25％浓度、600ml)，将两溶液按一定流速滴定共沉淀反应，保持反应过程pH在8～10之间，反应过程中要一直搅拌；滴定结束后持续搅拌1h，后洗涤沉淀物至氯离子含量小于10mg/L，此沉淀前驱体主要为氢氧化锆，测此时的沉淀物粒度(本文粒度测量均使用OMEC ls-pop6型号激光粒度仪)，结果如图2a所示。
将沉淀物用滤纸析出取120g，与去离子水按质量比2:1加入到球磨罐中，然后以300r/min球磨1h，取样测此时前驱体粒度，结果如图2b所示。
用滤纸析出浆料，烘干，并置于窑炉中煅烧(最高温度800℃、保温3h)；煅烧后粉体为氧化锆，取样测粒度结果如图2c所示；比表面积为15.463m2/g。
实施例2：
称取171.2g氧氯化锆(含有结晶水)、氧化镁2.23g，溶于250ml去离子水中，取过量的氨水(25％浓度、600ml)，将两溶液按一定流速滴定共沉淀反应，保持反应过程pH在8～10之间，反应过程中要一直搅拌；滴定结束后持续搅拌1h，后洗涤沉淀物至氯离子含量小于10mg/L，此沉淀前驱体主要为氢氧化锆，测此时的沉淀物粒度，结果如图3a所示。
将沉淀物用滤纸析出取120g，与去离子水按质量比2:1加入到球磨罐中，然后以300r/min球磨1h，取样测此时前驱体粒度，结果如图3b所示。
用滤纸析出浆料，烘干，并置于窑炉中煅烧(最高温度800℃、保温3h)；煅烧后粉体为氧化锆，取样测粒度结果如图3c所示；比表面积为16.356m2/g。
对比例1
按3Y的比例称取171.2g氧氯化锆(含有结晶水)、六水合硝酸钇11.85g，溶于250ml去离子水中，取过量的氨水(25％浓度、600ml)，将两溶液按一定流速滴定共沉淀反应，保持反应过程pH在8～10之间，反应过程中要一直搅拌；滴定结束后持续搅拌1h，后洗涤沉淀物至氯离子含量小于10mg/L，此沉淀前驱体主要为氢氧化锆，测此时的沉淀物粒度，结果如图2a所示。
将沉淀物用滤纸析出取120g，1000℃下煅烧4h，得到氧化锆粉体，取样测此时氧化锆粉体粒度，结果如图4a所示，将煅烧后得到的氧化锆粉体加入到球磨罐中，以300r/min球磨10h，取样测此时球磨后氧化锆粉体粒度，结果如图4b所示。

Claims (4)

1.一种高效制备高分散氧化锆陶瓷粉的方法，其特征在于，包括如下步骤：
步骤一、将化学共沉淀得到的氢氧化锆洗涤并压制成固态滤饼；
步骤二、将滤饼与去离子水混合，进行球磨；
步骤三、将球磨后浆料滤出，并烘干；
步骤四、将烘干后物料进窑炉煅烧，得到氧化锆粉体。
2.根据权利要求1所述的高效制备高分散氧化锆陶瓷粉的方法，其特征在于，步骤二滤饼与去离子水按质量比1:1～2:1混合。
3.根据权利要求1所述的高效制备高分散氧化锆陶瓷粉的方法，其特征在于，步骤二以280～350r/min球磨时间1～2h。
4.根据权利要求1所述的高效制备高分散氧化锆陶瓷粉的方法，其特征在于，步骤四700～900℃煅烧3～5h。
CN201811307812.5A 2018-11-05 2018-11-05 一种高效制备高分散氧化锆陶瓷粉的方法 Pending CN109336618A (zh)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1033750A (zh) * 1987-12-26 1989-07-12 冶金部洛阳耐火材料研究所 高温陶瓷氧化物微粉生产方法
JPH02129032A (ja) * 1988-11-09 1990-05-17 Sumitomo Seika Chem Co Ltd Ｐｌｚｔ粉末の製造法
CN101098828A (zh) * 2004-12-13 2008-01-02 多诺克斯颜料股份有限公司 微粒锆钛酸铅、锆钛水合物和钛酸锆及其制备方法
CN101698509A (zh) * 2009-09-11 2010-04-28 淄博广通化工有限责任公司 纳米氧化锆的生产方法
CN101993248A (zh) * 2009-08-10 2011-03-30 上海锦奕新材料科技有限公司 一种低温烧成钇稳定氧化锆的添加剂

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1033750A (zh) * 1987-12-26 1989-07-12 冶金部洛阳耐火材料研究所 高温陶瓷氧化物微粉生产方法
JPH02129032A (ja) * 1988-11-09 1990-05-17 Sumitomo Seika Chem Co Ltd Ｐｌｚｔ粉末の製造法
CN101098828A (zh) * 2004-12-13 2008-01-02 多诺克斯颜料股份有限公司 微粒锆钛酸铅、锆钛水合物和钛酸锆及其制备方法
CN101993248A (zh) * 2009-08-10 2011-03-30 上海锦奕新材料科技有限公司 一种低温烧成钇稳定氧化锆的添加剂
CN101698509A (zh) * 2009-09-11 2010-04-28 淄博广通化工有限责任公司 纳米氧化锆的生产方法

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