CN110950649A - 一种亚毫米级实心氧化铝陶瓷微珠的制备方法 - Google Patents

一种亚毫米级实心氧化铝陶瓷微珠的制备方法 Download PDF

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CN110950649A
CN110950649A CN201911290978.5A CN201911290978A CN110950649A CN 110950649 A CN110950649 A CN 110950649A CN 201911290978 A CN201911290978 A CN 201911290978A CN 110950649 A CN110950649 A CN 110950649A
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alumina
submillimeter
alumina ceramic
ceramic microspheres
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李蔚
孙小曼
宋雁翎
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East China University of Science and Technology
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Abstract

本发明涉及一种亚毫米级实心氧化铝陶瓷微珠制备方法。该氧化铝陶瓷微珠的制备方法如下：首先将喷雾造粒所得的氧化铝造粒粉利用筛分工艺进行筛分分级，获得不同粒径范围内的均匀的造粒粉。然后将一定粒径范围内的造粒粉与适量的石墨粉混合均匀。将混合后的粉料放在加盖的坩埚中在高温下煅烧，使氧化铝微珠完成致密化。然后将坩埚盖去掉，在低温下煅烧将多余的石墨粉除去。将煅烧后的产物过筛，即可获得所需要粒径范围的致密的、分散良好的氧化铝陶瓷微珠。

Description

一种亚毫米级实心氧化铝陶瓷微珠的制备方法
技术领域
本发明涉及陶瓷生产领域，特别涉及一种氧化铝陶瓷微珠制作方法。
背景技术
氧化铝陶瓷微珠，亦称氧化铝陶瓷微球，是指以氧化铝为主要原料，通过各种成型工艺制备而成的直径在微米级至毫米级的陶瓷球体或近似球体。氧化铝陶瓷微珠不仅有氧化铝陶瓷材料的优良性能，如具有强度高、热稳定性好、阻燃和绝缘性好、吸水率低、化学性能稳定等优点，同时还具有微珠颗粒的特点，如各向同性、点接触等。氧化铝陶瓷微珠因其独特的形状和优异的性能，被广泛应用于航空、航天、国防军工、医药、化工、建材、环保、核技术等行业。随着人们对氧化铝陶瓷微珠的研究越来越深入，其应用领域越来越广，制备方法也越来越丰富。但大多数方法如溶胶-凝胶法等成本很高，只能用于实验室研究，只有少数一些方法如火焰熔融法和喷雾造粒法等适合大规模生产。
火焰熔融法是将原料微粉输送至燃烧的火焰中，原料经火焰熔融后形成分散的小液滴，小液滴进入冷却区冷凝成球状的颗粒即制得球形颗粒。这种方法需要有很高的温度。如生产球形氧化铁所需的熔融温度达到2400℃以上，生产球形二氧化硅所需的熔融温度达到2000摄氏度左右。而制作球形氧化铝的熔融温度需控制大约在2050℃左右。因此存在设备要求高，生产成本高，能耗大等缺点。
喷雾造粒是将溶液或悬浮液等原料喷雾固化后制成一定形状和强度的细小颗粒，也可用于氧化铝陶瓷微珠的制备。但这种方法制备出来的氧化铝陶瓷微珠密度和强度都很低，很多场合不能直接使用（如作为研磨介质），必须通过进一步煅烧使其致密化，才能获得最后的产品。但是煅烧过程很容易让小颗粒之间因为烧结的作用而产生粘连，导致氧化铝陶瓷微珠的分散性和流动性大大降低。为了避免这种粘连，有人开发出梯度煅烧工艺，即将喷雾造粒所获得的陶瓷微珠以一定的温度间隔从低至高依次在不同温度下煅烧，每次煅烧后将粉体取出研磨以破坏有可能形成的粘连，直至最后获得致密的陶瓷微珠。但这种工艺过于繁琐，很难大规模应用。
发明内容
本发明的目的在于提供一种新的二步煅烧法制备氧化铝陶瓷实心微珠的方法。
为实现上述目的，本发明所采用的技术方案是：首先利用喷雾造粒设备制备出球形氧化铝粉，然后通过筛分工艺对所得造粒粉进行分级，将分级后的造粒粉与一定量的石墨粉混合，然后将混合好的粉体放在加盖的坩埚中以隔绝空气，在预定温度下煅烧，使球形氧化铝粉致密化。冷却后将坩埚盖除去，再在一定温度下将石墨粉烧掉，将粉体取出过筛，就获得制备出粒径均匀的亚毫米级氧化铝陶瓷微珠。
在上述技术方案中：石墨粉的添加量为5-50wt%，造粒粉与石墨粉混合时间为6-24h；去石墨粉的煅烧温度为900-1100℃，保温时间为2-10小时；
与现有技术相比，本发明最大的特点是：直接在高温下煅烧，获得致密的陶瓷微珠，同时通过混入的石墨粉阻止氧化铝颗粒间的粘连，之后再在低温下将石墨粉烧去。整个工艺简单可靠，适合规模化生产。
附图说明
图1是本发明所获得的致密的氧化铝陶瓷微珠。
图1用来提供对本发明的进一步理解，并且构成说明书的一部分，与本发明的实施例一起用于解释本发明，并不构成对本发明的限制。
具体实施方式
实施例一
取10kg喷雾造粒所得99氧化铝造粒粉，放在振动筛分机进行筛分，获得具有不同粒度尺寸范围的99氧化铝造粒原粉。取1kg筛分后的99氧化铝粉，添加200g石墨粉，装入球磨罐中，在普通球磨机上混合12小时。将混合好的粉置于刚玉坩埚中，加上盖，放入在马弗炉中，1650℃煅烧2h，使陶瓷微珠完成致密化。冷却后将刚玉坩埚的盖拿开，再升温到1000℃煅烧4h，将石墨粉烧去。冷却后，再将所得氧化铝陶瓷微珠过筛，获得所需要粒径范围的致密的、分散良好的氧化铝陶瓷微珠（如图1所示）。

Claims (4)

1.一种亚毫米级实心氧化铝陶瓷微珠的制备方法，其基本工艺是：利用筛分工艺将喷雾造粒所得的氧化铝造粒粉进行筛分分级，将分级后的造粒粉与一定量的石墨粉混合，将混合好的粉体放在加盖的坩埚中，在预定温度下煅烧，使球形氧化铝粉致密化；冷却后将坩埚盖除去，在一定温度下将石墨粉烧掉；将所得的氧化铝微珠取出过筛，就获得制备出粒径均匀的亚毫米级陶瓷微珠。
2.根据权利要求1所述一种亚毫米级实心氧化铝陶瓷微珠的制备方法，其特征在于：制备氧化铝微珠的原料为喷雾造粒氧化铝粉。
3.根据权利要求1所述一种亚毫米级实心氧化铝陶瓷微珠的制备方法，其特征在于：先将喷雾造粒氧化铝粉进行预先筛分成不同粒径范围的粒径均匀的球形粉；筛分后的氧化铝微球与一定量的石墨分散剂混合，石墨粉的添加量为5-50wt%，造粒粉与石墨粉混合时间为6-24h。
4.根据权利要求1所述一种亚毫米级实心氧化铝陶瓷微珠的制备方法，其特征在于：造粒粉首先在隔绝空气的条件下高温煅烧完成致密化，之后在空气中低温下煅烧除去石墨粉。
CN201911290978.5A 2019-12-16 2019-12-16 一种亚毫米级实心氧化铝陶瓷微珠的制备方法 Pending CN110950649A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113060746A (zh) * 2021-04-14 2021-07-02 雅安百图高新材料股份有限公司 一种大粒径氧化铝原料制备方法及其球形氧化铝产品

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113060746A (zh) * 2021-04-14 2021-07-02 雅安百图高新材料股份有限公司 一种大粒径氧化铝原料制备方法及其球形氧化铝产品

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