CN106083017B - 一种高性能低膨胀坩埚及其制备方法 - Google Patents

一种高性能低膨胀坩埚及其制备方法 Download PDF

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CN106083017B
CN106083017B CN201610452326.7A CN201610452326A CN106083017B CN 106083017 B CN106083017 B CN 106083017B CN 201610452326 A CN201610452326 A CN 201610452326A CN 106083017 B CN106083017 B CN 106083017B
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包启富
刘昆
董伟霞
周健儿
刘韩
杨瑞强
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Jingdezhen Ceramic Institute
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Abstract

本发明公开了一种高性能低膨胀坩埚及其制备方法，由坩埚基体材料和坩埚涂层材料构成，按质量百分比坩埚基体材料的组成为：叶长石40～60%、锂辉石5～15%、苏州土5～15%、子木节土1～3%、黑滑石1～5%、贵州土10～25%、白炭黑0～3%、氧化锆微粉5～10%，所述坩埚涂层材料的组成为：叶长石0～15%、功能材料微粉85～100%，外加分散剂0.1～0.5%和粘结剂0.1～0.5%。经配料混合、球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，将喷涂坩埚涂层材料到坩埚基体内表面，最后经烧成获得坩埚产品，本发明坩埚生产成本低、成型性能好，有效提高了产品的抗热震性能、机械强度和使用寿命，从而有利于促进坩埚产业的技术进步和应用发展。

Description

一种高性能低膨胀坩埚及其制备方法
技术领域
本发明涉及耐火材料技术领域，尤其涉及一种高性能低膨胀坩埚及其制备方法。
背景技术
陶瓷坩埚是耐火材料的重要组成部分，它是熔化和煅烧以及固液加热、反应的容器，是保证化学反应顺利进行的基础，也是制备高纯氧化物的必须用品。
坩埚的生产原料，可概括为三大类型。一是结晶质的天然石墨，二是氧化铝坩埚，三是石英坩埚。目前，用来煅烧氢氧化物获得高纯氧化物用坩埚一般都为石英坩埚，由于石英坩埚价格便宜，易获得，所以广泛使用。但是石英坩埚有致命的缺陷，使用寿命短，不稳定，石英在573℃的时候有晶型转变发生，伴随着体积膨胀，所以容易造成剥落和炸裂，使用次数低，甚至石英颗粒污染煅烧产品。另外生产特殊材料的产品使用的坩埚，如现在有生产铌钽的企业的坩埚采用铌和钽做坩埚，该坩埚很重，劳动强度大，再就是很贵，增加了企业负担。
发明内容
本发明的目的在于克服现有技术的不足，提供一种抗热震性能好、强度高、成本低、不易污染，并且使用寿命长的高性能低膨胀坩埚及其制备方法。
为解决以上技术问题，本发明的技术方案是：一种高性能低膨胀坩埚，其特征在于：由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石40～60%、锂辉石5～15%、苏州土5～15%、子木节土1～3%、黑滑石1～5%、贵州土10～25 %、白炭黑0～3%、氧化锆微粉5～10%，所述坩埚涂层材料的质量百分比组成为：叶长石0～15%、功能材料微粉85～100%，外加分散剂0.1～0.5%和粘结剂0.1～0.5%。
所述功能材料微粉为氧化锆微粉、稀土材料微粉、半导体材料中的一种，在800～1200℃煅烧获得的粉体材料。
所述稀土材料微粉为氧化镨微粉、氧化铈微粉、氧化镧微粉中的一种。
所述半导体材料为二氧化锡、氧化钛中的一种。
所述分散剂为聚丙烯酸胺、聚乙二醇、聚丙烯酸中的一种。
所述粘结剂为羟丙基甲基纤维素或聚乙烯醇。
所述氧化锆微粉、稀土材料微粉、半导体材料的细度为1～60µm。
所述氧化锆微粉、稀土材料微粉、半导体材料的细度为5～35µm。
上述的高性能低膨胀坩埚，其特征在于：所述高性能低膨胀坩埚其抗折强度为40～76MPa、膨胀系数为α（800～20℃）=1.1～1.6×10-6/℃。
所述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经10～12.5h慢烧至1310～1330℃。
本发明具有以下有益效果：
（1） 本发明高性能低膨胀坩埚具产品，生产成本低且成型性能好，通过在坯料中引入高性能低膨胀材料，能够有效提高产品的抗热震性能，并且提高了生产合格率；
（2）本发明坯料中引入了增强增韧材料进一步提高了产品的抗热震性能。配方体系通过氧化锆弥散、相变增韧原理，从而进一步大大提高了产品的强度；
（3）本发明所述高性能低膨胀坩埚其抗折强度为40～76MPa、膨胀系数为α（800～20℃）=1.1～1.6×10-6/℃。
具体实施方式
下面结合具体实施方式对本发明作进一步详细的说明。
实施例1
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石45%、锂辉石10%、苏州土10%、子木节土1%、黑滑石4%、贵州土20 %、白炭黑0%、氧化锆微粉10%；所述坩埚涂层材料的质量百分比组成为：叶长石15%、800℃煅烧后氧化锆微粉85%，外加聚丙烯酸胺0.1%和羟丙基甲基纤维素0.1%；所述氧化锆微粉的细度为10µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经10h慢烧至1310℃。
实施例2
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石58%、锂辉石5%、苏州土5%、子木节土2%、黑滑石1%、贵州土22%、白炭黑1%、氧化锆微粉6%，所述坩埚涂层材料的质量百分比组成为：叶长石12%、850℃煅烧后氧化镨微粉88%，外加聚乙二醇0.2%和聚乙烯醇0.2%；所述氧化锆微粉、氧化镨微粉的细度为15µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经10.5h慢烧至1320℃。
实施例3
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石50%、锂辉石15%、苏州土5%、子木节土1%、黑滑石1%、贵州土15 %、白炭黑3%、氧化锆微粉10%，所述坩埚涂层材料的质量百分比组成为：叶长石10%、1000℃煅烧后氧化镧微粉90%，外加聚丙烯酸0.3%和聚乙烯醇0.1%；所述氧化锆微粉、氧化镧微粉的细度为20µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经11h慢烧至1315℃。
实施例4
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石40%、锂辉石5%、苏州土15%、子木节土2%、黑滑石3%、贵州土25 %、白炭黑3%、氧化锆微粉7%，所述坩埚涂层材料的质量百分比组成为：叶长石8%、1000℃煅烧后二氧化锡92%，外加聚丙烯酸0.1%和聚乙烯醇0.4%；所述氧化锆微粉、二氧化锡微粉的细度为30µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经12h慢烧至1320℃。
实施例5
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石42%、锂辉石14%、苏州土6%、子木节土2%、黑滑石5%、贵州土20 %、白炭黑1%、氧化锆微粉10%，所述坩埚涂层材料的质量百分比组成为：叶长石2%、1100℃煅烧后氧化钛98%，外加聚丙烯酸0.4%和聚乙烯醇0.14%；所述氧化锆微粉、氧化钛的细度为40µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经12.5h慢烧至1330℃。
实施例6
一种高性能低膨胀坩埚，由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石50%、锂辉石10%、苏州土10%、子木节土3%、黑滑石1%、贵州土20 %、白炭黑1%、氧化锆微粉5%，所述坩埚涂层材料的质量百分比组成为：叶长石15%、1200℃煅烧后氧化铈微粉85%，外加聚丙烯酸0.2%和聚乙烯醇0.1%；所述氧化锆微粉、氧化铈微粉的细度为50µm。
上述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经12.5h慢烧至1320℃。
本发明实施例1-6高性能低膨胀坩埚的性能指标如下表所示：

Claims (7)

1.一种高性能低膨胀坩埚，其特征在于：由坩埚基体材料和坩埚涂层材料构成，所述坩埚基体材料的质量百分比组成为：叶长石40～60%、锂辉石5～15%、苏州土5～15%、子木节土1～3%、黑滑石1～5%、贵州土10～25 %、白炭黑0～3%、氧化锆微粉5～10%，所述坩埚涂层材料的质量百分比组成为：叶长石0～15%、功能材料微粉85～100%，外加分散剂0.1～0.5%和粘结剂0.1～0.5%；
所述功能材料微粉为氧化锆微粉、稀土材料微粉、半导体材料中的一种，在800～1200℃煅烧获得的粉体材料；
所述稀土材料微粉为氧化镨微粉、氧化铈微粉、氧化镧微粉中的一种；
所述半导体材料为二氧化锡、氧化钛中的一种。
2.根据权利要求1所述的高性能低膨胀坩埚，其特征在于：所述分散剂为聚丙烯酸胺、聚乙二醇、聚丙烯酸中的一种。
3.根据权利要求1所述的高性能低膨胀坩埚，其特征在于：所述粘结剂为羟丙基甲基纤维素或聚乙烯醇。
4.根据权利要求1所述的高性能低膨胀坩埚，其特征在于：所述氧化锆微粉、稀土材料微粉、半导体材料的细度为1～60µm。
5.根据权利要求1所述的高性能低膨胀坩埚，其特征在于：所述氧化锆微粉、稀土材料微粉、半导体材料的细度为5～35µm。
6.根据权利要求1-5任一所述的高性能低膨胀坩埚，其特征在于：所述高性能低膨胀坩埚其抗折强度为40～76MPa、膨胀系数为α（800～20℃）=1.1～1.6×10-6/℃。
7.根据权利要求1所述高性能低膨胀坩埚的制备方法，其特征在于：所述坩埚基体原料进行配料混合后，经球磨、过筛、压滤脱水、真空练泥、成型、干燥而得到坩埚坯体，然后将所述坩埚涂层材料配料后制备成流动性好的浆料，喷涂到坩埚基体内表面，最后经烧成获得高性能低膨胀坩埚产品，所述烧成工艺条件为在氧化气氛下从室温经10～12.5h慢烧至1310～1330℃。
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