CN111056834A - 一种尖晶石-莫来石陶瓷匣钵的制备方法 - Google Patents

一种尖晶石-莫来石陶瓷匣钵的制备方法 Download PDF

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CN111056834A
CN111056834A CN201911298170.1A CN201911298170A CN111056834A CN 111056834 A CN111056834 A CN 111056834A CN 201911298170 A CN201911298170 A CN 201911298170A CN 111056834 A CN111056834 A CN 111056834A
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spinel
slurry
mullite
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张拯
雷复兴
魏少西
姜鹏
田守信
马文鹏
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Luoyang Ceramtech Material Co ltd
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Abstract

一种尖晶石‑莫来石陶瓷匣钵的制备方法，涉及一种尖晶石‑莫来石陶瓷匣钵，陶瓷匣钵基体由原料和胶体溶液制备而成，所述原料的组分按重量百分比计包括电熔镁铝尖晶石40~50%，电熔莫来石15~25%，氧化铝微粉15~20%，钛酸铝细粉4~8%，氧化锆5~10%，菱镁矿微粉3~5%，粘土细粉3~5%；胶体溶液为凝胶体，凝胶体的组分按重量百分比计包括丙烯酰胺10~14%，亚甲基双丙烯酰胺0.2~0.4%，过硫酸铵0.4~0.6%，四甲基乙二胺0.2~0.4%，其余为水；凝胶体的重量为原料总量的8%‑12%；通过浆料制备、注模成型、脱模、干燥和烧成步骤完成；本发明烧成后的制品体积密度高、强度高、热震稳定性高，使用性能优良。

Description

一种尖晶石-莫来石陶瓷匣钵的制备方法
技术领域
本发明涉及尖晶石-莫来石陶瓷领域，尤其是涉及一种尖晶石-莫来石陶瓷匣钵的制备方法。
背景技术
公知的，陶瓷匣钵被广泛地应用于锂电池行业正极材料的煅烧。锂电池正极材料主要含有大量的氢氧化锂或其他形式的锂盐化合物，由于锂离子的离子半径很小且具有很强的碱性，因此锂离子的渗透性和腐蚀性是非常强，这种非常苛刻的使用场合的使用要求也是非常苛刻的。
我国是全球最大的锂电池生产国，陶瓷匣钵的需求量非常大，但目前大都采用较为传统的机械压制的方法来成型。然而，由于匣钵属薄壁制品，采用机械压制成型方法无法保证匣钵四壁的密度和强度均匀性；因此，造成匣钵在使用过程中通常会出现密度低、强度低、耐腐蚀性差、表面剥落掉渣等现象，无法满足高品质锂电材料的使用要求。
发明内容
为了克服背景技术中的不足，本发明公开了一种尖晶石-莫来石陶瓷匣钵的制备方法。
为了实现所述发明目的，本发明采用如下技术方案：
一种尖晶石-莫来石陶瓷匣钵，陶瓷匣钵基体由原料和胶体溶液制备而成，所述原料的组分按重量百分比计包括电熔镁铝尖晶石40~50%，电熔莫来石15~25%，氧化铝微粉15~20%，钛酸铝细粉4~8%，氧化锆5~10%，菱镁矿微粉3~5%，粘土细粉3~5%；
胶体溶液为凝胶体，凝胶体的组分按重量百分比计包括丙烯酰胺10~14%，亚甲基双丙烯酰胺0.2~0.4%，过硫酸铵0.4~0.6%，四甲基乙二胺0.2~0.4%，其余为水；
凝胶体的重量为原料总量的8%-12%。
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：按所需重量份称取电熔镁铝尖晶石、电熔莫来石、氧化铝微粉、钛酸铝细粉、氧化锆、菱镁矿微粉、粘土细粉混合；按所需重量份称取丙烯酰胺、亚甲基双丙烯酰胺、过硫酸铵、四甲基乙二胺、水； 将上述原料和胶体溶液加入搅拌桶中搅拌，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到80-90℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在60~100℃温度下干燥，干燥时间为20~30小时；
（5）、烧成：干燥后的坯体经1300~1400℃烧成，保温时间为4~6小时；
所述的尖晶石-莫来石陶瓷匣钵的制备方法，步骤（1）中所述的搅拌速率为300转/分钟，搅拌时间为4-6小时。
由于采用了上述技术方案，本发明具有如下有益效果：
1、本发明所述的尖晶石-莫来石陶瓷匣钵的制备方法，电熔镁铝尖晶石、电熔莫来石作为骨料，电熔镁铝尖晶石为碱性材料，且结晶状态良好，具有很好的抗锂离子侵蚀性能；电熔莫来石属中性材料，但莫来石的热膨胀系数较低，对制品的耐急冷急热性有利；氧化铝微粉、钛酸铝细粉、氧化锆、菱镁矿微粉、粘土细粉为基质料，菱镁矿微粉经高温煅烧后形成碱性氧化镁，有利于抗锂离子侵蚀，钛酸铝细粉具有较低的热膨胀系数，有利于提高制品的耐急冷急热性，加入氧化锆也是为了提高耐侵蚀性，粘土粉为助烧剂；本发明的原料化学成分以碱性材料为主，能够有效地抵抗锂电材料的侵蚀。
2、本发明所述的凝胶体中，丙烯酰胺为有机单体，亚甲基双丙烯酰胺为交联剂，过硫酸胺为引发剂，四甲基乙二胺为催化剂，水为溶剂；其基本原理是有机单体与交联剂在引发剂和催化剂的作用下发生交联聚合反应形成具有较大分子链的稳定凝聚胶体；凝胶体为热凝型体系，即胶体溶液在常温下不会凝固，只有将胶体溶液加热到80~90℃才会发生聚合反应形成凝固体；本发明所述的含有凝胶体的浆料具有非常良好的性能，其具体表现为固体含量高、悬浮性好、不易沉淀、不易变质、流动性好；成型后的坯体的化学成分、微观结构及密度很均匀，因此烧成后的制品体积密度高、强度高、热震稳定性高，使用性能优良。
3、本发明所述的成型模具采用金属模具，可以成型任何复杂形状的及任意壁厚的陶瓷制品，尤其对于成型薄壁陶瓷匣钵、薄壁陶瓷坩埚及薄壁陶瓷管件具有很大的优势。
具体实施方式
通过下面的实施例可以详细的解释本发明，公开本发明的目的旨在保护本发明范围内的一切技术改进。
本发明所述的尖晶石-莫来石陶瓷匣钵，陶瓷匣钵基体由原料和胶体溶液制备而成，所述原料的组分按重量百分比计包括电熔镁铝尖晶石40~50%，电熔莫来石15~25%，氧化铝微粉15~20%，钛酸铝细粉4~8%，氧化锆5~10%，菱镁矿微粉3~5%，粘土细粉3~5%；
胶体溶液为凝胶体，凝胶体的组分按重量百分比计包括丙烯酰胺10~14%，亚甲基双丙烯酰胺0.2~0.4%，过硫酸铵0.4~0.6%，四甲基乙二胺0.2~0.4%，其余为水；
凝胶体的重量为原料总量的8%-12%。
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：按所需重量份称取电熔镁铝尖晶石、电熔莫来石、氧化铝微粉、钛酸铝细粉、氧化锆、菱镁矿微粉、粘土细粉混合；按所需重量份称取丙烯酰胺、亚甲基双丙烯酰胺、过硫酸铵、四甲基乙二胺、水； 将上述原料和胶体溶液加入搅拌桶中搅拌，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到80-90℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在60~100℃温度下干燥，干燥时间为20~30小时；
（5）、烧成：干燥后的坯体经1300~1400℃烧成，保温时间为4~6小时；
所述的尖晶石-莫来石陶瓷匣钵的制备方法，步骤（1）中所述的搅拌速率为300转/分钟，搅拌时间为4-6小时。
实施例1
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：称取重量份电熔镁铝尖晶石40%、电熔莫来石25%、氧化铝微粉15%、钛酸铝细粉5%、氧化锆5%、菱镁矿微粉5%、粘土细粉5%；称取重量份丙烯酰胺10%、亚甲基双丙烯酰胺0.4%、过硫酸铵0.6%、四甲基乙二胺0.4%、水88.6%； 将100Kg原料和8Kg胶体溶液加入搅拌桶中搅拌4小时，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到80℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在60℃温度下干燥，干燥时间为30小时；
（5）、烧成：干燥后的坯体经1300℃烧成，保温时间为6小时。
实施例2
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：称取重量份的电熔镁铝尖晶石50%、电熔莫来石15%、氧化铝微粉20%、钛酸铝细粉4%、氧化锆5%、菱镁矿微粉3%、粘土细粉3%；称取重量份的丙烯酰胺14%、亚甲基双丙烯酰胺0.3%、过硫酸铵0.5%、四甲基乙二胺0.3%、水84.9%； 将100Kg原料和12Kg胶体溶液加入搅拌桶中搅拌6小时，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到90℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在100℃温度下干燥，干燥时间为20小时；
（5）、烧成：干燥后的坯体经1400℃烧成，保温时间为4小时。
实施例3
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：称取重量份的电熔镁铝尖晶石45%、电熔莫来石20%、氧化铝微粉16%、钛酸铝细粉6%、氧化锆6%、菱镁矿微粉4%、粘土细粉3%；称取重量份的丙烯酰胺12%、亚甲基双丙烯酰胺0.2%、过硫酸铵0.4%、四甲基乙二胺0.2%、水87.2%； 将100Kg原料和10Kg胶体溶液加入搅拌桶中搅拌5小时，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到85℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在80℃温度下干燥，干燥时间为25小时；
（5）、烧成：干燥后的坯体经1350℃烧成，保温时间为4小时。
实施例4
一种尖晶石-莫来石陶瓷匣钵的制备方法，其具体操作步骤如下：
（1）、浆料制备：称取重量份的电熔镁铝尖晶石41%、电熔莫来石16%、氧化铝微粉18%、钛酸铝细粉8%、氧化锆10%、菱镁矿微粉3%、粘土细粉4%；称取重量份的丙烯酰胺13%、亚甲基双丙烯酰胺0.3%、过硫酸铵0.5%、四甲基乙二胺0.3%、水85.9%； 将100Kg原料和11Kg胶体溶液加入搅拌桶中搅拌5小时，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到88℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在70℃温度下干燥，干燥时间为28小时；
（5）、烧成：干燥后的坯体经1380℃烧成，保温时间为5小时。
本发明未详述部分为现有技术。
为了公开本发明的发明目的而在本文中选用的实施例，当前认为是适宜的，但是，应了解的是，本发明旨在包括一切属于本构思和发明范围内的实施例的所有变化和改进。

Claims (3)

1.一种尖晶石-莫来石陶瓷匣钵，陶瓷匣钵基体由原料和胶体溶液制备而成，其特征是：所述原料的组分按重量百分比计包括电熔镁铝尖晶石40~50%，电熔莫来石15~25%，氧化铝微粉15~20%，钛酸铝细粉4~8%，氧化锆5~10%，菱镁矿微粉3~5%，粘土细粉3~5%；
胶体溶液为凝胶体，凝胶体的组分按重量百分比计包括丙烯酰胺10~14%，亚甲基双丙烯酰胺0.2~0.4%，过硫酸铵0.4~0.6%，四甲基乙二胺0.2~0.4%，其余为水；
凝胶体的重量为原料总量的8%-12%。
2.一种尖晶石-莫来石陶瓷匣钵的制备方法，其特征是：其具体操作步骤如下：
（1）、浆料制备：按所需重量份称取电熔镁铝尖晶石、电熔莫来石、氧化铝微粉、钛酸铝细粉、氧化锆、菱镁矿微粉、粘土细粉混合；按所需重量份称取丙烯酰胺、亚甲基双丙烯酰胺、过硫酸铵、四甲基乙二胺、水； 将上述原料和胶体溶液加入搅拌桶中搅拌，制成浆料；
（2）、注模成型：将上一步骤中所述的浆料经过真空处理除去浆料中的气泡，再用压力泵注入金属模具中，并将模具加热到80-90℃，浆料形成凝固体；
（3）、脱模：上一步骤所述的金属模具打开，取出坯体；
（4）、干燥：将坯体在60~100℃温度下干燥，干燥时间为20~30小时；
（5）、烧成：干燥后的坯体经1300~1400℃烧成，保温时间为4~6小时。
3.根据权利要求2所述的尖晶石-莫来石陶瓷匣钵的制备方法，其特征是：步骤（1）中所述的搅拌速率为300转/分钟，搅拌时间为4-6小时。
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