CN110922176A - 一种石英陶瓷坩锅材料的生产工艺 - Google Patents

一种石英陶瓷坩锅材料的生产工艺 Download PDF

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CN110922176A
CN110922176A CN201911340089.5A CN201911340089A CN110922176A CN 110922176 A CN110922176 A CN 110922176A CN 201911340089 A CN201911340089 A CN 201911340089A CN 110922176 A CN110922176 A CN 110922176A
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ball milling
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ceramic crucible
bentonite
dispersion
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张黎明
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Jiangsu Comlola Special Ceramics Co Ltd
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Abstract

本发明公开了一种石英陶瓷坩锅材料的生产工艺，包括以下步骤：步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1000‑1500r/min。本发明石英陶瓷坩锅材料采用的基体为石英砂、陶瓷配制而成，采用的处理液处理后基体原料更易与耐腐助剂、辅料之间搭配，从而提高了原料之间的相容性，耐腐助剂中的钠沸石是沸石矿的主要矿物组分之一，通过在膨润土中分散更易与石英砂、陶瓷混合，辅料中的金刚石粉具有很强的耐腐性能，加入到材料中能够显著的提高材料的耐腐性能，原料之间相互搭配可提高材料的耐腐性能。

Description

一种石英陶瓷坩锅材料的生产工艺
技术领域
本发明涉及石英陶瓷坩锅技术领域，具体涉及一种石英陶瓷坩锅材料的生产工艺。
背景技术
石英陶瓷坩埚，全称为高纯熔融石英陶瓷坩埚(二氧化硅含量≥99.9％)。是以高纯熔融石英为原料做成的陶瓷质坩埚。一般情况下，其形状主要有方形和圆筒形。其中，方形的高纯石英坩埚用在多晶硅铸锭环节，充当多晶硅化料和长晶的容器；圆形的高纯石英坩埚则用在单晶硅中拉单晶的环节。高纯熔融石英由于具有结构精细、热导率低、热膨胀系数小、制成品尺寸精度高、高温不变形、热震稳定性好、电性能好、耐化学侵蚀性好等特点，因此在玻璃深加工行业、冶金工业、电子工业、化工工业、航空航天等领域得到广泛应用。
现有技术中的坩埚可具有耐高温性能，但是盐碱条件下，加上高温的煅烧，寿命会显著降低。
发明内容
发明目的：为了克服现有技术中存在的不足，本发明提供一种石英陶瓷坩锅材料的生产工艺。
技术方案：为实现上述目的，本发明提供如下技术方案：
一种石英陶瓷坩锅材料的生产工艺，包括以下步骤：
步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1000-1500r/min，球磨时间为30-40min，球磨结束，再送入到处理液中反应20-30min，反应温度为100-150℃，反应结束，离心、水洗，干燥，即可；
步骤二，耐腐助剂的制备：将沸石加入到球磨机中进行球磨，球磨过10-50目，随后送入到膨润土分散液中进行超分散，分散功率为300-1000W，分散时间为25-35min，然后过滤，干燥，得到耐腐助剂；
步骤三，辅料的称取：金刚石粉20-30份、硅酸铝5-10份、叶腊石4-8份、硅灰石4-8份；
步骤四，坩埚材料的制备：将步骤一制备的基体、步骤二制备的耐腐助剂、步骤三的辅料依次加入到共混机中进行共混，共混转速为100-500r/min，共混时间为 20-30min，随后再进行热压烧结，烧结结束，得到石英陶瓷坩锅。
优选地，所述处理液的制备方法为：将质量分数为20-30％的稀土氯化镧溶液送入到反应器中，然后再加入海藻酸钠溶液中，先以200-500r/min的转速搅拌20-30min，然后再加入20％的葡萄糖五丙酸酯，继续搅拌20-30min，搅拌结束，即可。
优选地，所述处理液中还添加水滑石粉。
优选地，所述步骤二中的沸石为钠沸石。
优选地，所述膨润土分散液的制备方法为：将膨润土先煅烧20-30min，煅烧温度为215-225℃，然后再置于硅烷偶联剂KH560中分散20-30min，分散结束，再向其中加入丙烯酸乳液，继续以20-100r/min的转速搅拌20-30min，搅拌结束，得到膨润土分散液。
优选地，所述热压烧结的烧结温度为1000-1500℃，热压时间为20-30min，热压压力为20-30MPa。
优选地，所述热压烧结的烧结温度为1250℃，热压时间为25min，热压压力为25MPa。
有益效果：本发明，有益效果如下：
1)本发明石英陶瓷坩锅材料采用的基体为石英砂、陶瓷配制而成，采用的处理液处理后基体原料更易与耐腐助剂、辅料之间搭配，从而提高了原料之间的相容性，耐腐助剂中的钠沸石是沸石矿的主要矿物组分之一，通过在膨润土中分散更易与石英砂、陶瓷混合，辅料中的金刚石粉具有很强的耐腐性能，加入到材料中能够显著的提高材料的耐腐性能，原料之间相互搭配可提高材料的耐腐性能。
2)由表1可知本发明实施例1-3、对比例1-2中本发明的材料耐20％盐酸为93％，而对比例2仅为80％，可知本发明的耐腐性能具有显著改善。
具体实施方式
实施例1：
本实施例的一种石英陶瓷坩锅材料的生产工艺，包括以下步骤：
步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1000r/min，球磨时间为30min，球磨结束，再送入到处理液中反应20min，反应温度为100℃，反应结束，离心、水洗，干燥，即可；
步骤二，耐腐助剂的制备：将沸石加入到球磨机中进行球磨，球磨过10目，随后送入到膨润土分散液中进行超分散，分散功率为300W，分散时间为25min，然后过滤，干燥，得到耐腐助剂；
步骤三，辅料的称取：金刚石粉20份、硅酸铝5份、叶腊石4份、硅灰石4份；
步骤四，坩埚材料的制备：将步骤一制备的基体、步骤二制备的耐腐助剂、步骤三的辅料依次加入到共混机中进行共混，共混转速为100r/min，共混时间为20min，随后再进行热压烧结，烧结结束，得到石英陶瓷坩锅。
本实施例的处理液的制备方法为：将质量分数为20％的稀土氯化镧溶液送入到反应器中，然后再加入海藻酸钠溶液中，先以200r/min的转速搅拌20min，然后再加入20％的葡萄糖五丙酸酯，继续搅拌20min，搅拌结束，即可。
本实施例的处理液中还添加水滑石粉。
本实施例的步骤二中的沸石为钠沸石。
本实施例的膨润土分散液的制备方法为：将膨润土先煅烧20min，煅烧温度为 215℃，然后再置于硅烷偶联剂KH560中分散20min，分散结束，再向其中加入丙烯酸乳液，继续以20r/min的转速搅拌20min，搅拌结束，得到膨润土分散液。
本实施例的热压烧结的烧结温度为1000℃，热压时间为20min，热压压力为20MPa。
实施例2：
本实施例的一种石英陶瓷坩锅材料的生产工艺，包括以下步骤：
步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1500r/min，球磨时间为40min，球磨结束，再送入到处理液中反应30min，反应温度为150℃，反应结束，离心、水洗，干燥，即可；
步骤二，耐腐助剂的制备：将沸石加入到球磨机中进行球磨，球磨过50目，随后送入到膨润土分散液中进行超分散，分散功率为1000W，分散时间为35min，然后过滤，干燥，得到耐腐助剂；
步骤三，辅料的称取：金刚石粉30份、硅酸铝10份、叶腊石8份、硅灰石8份；
步骤四，坩埚材料的制备：将步骤一制备的基体、步骤二制备的耐腐助剂、步骤三的辅料依次加入到共混机中进行共混，共混转速为500r/min，共混时间为30min，随后再进行热压烧结，烧结结束，得到石英陶瓷坩锅。
本实施例的处理液的制备方法为：将质量分数为30％的稀土氯化镧溶液送入到反应器中，然后再加入海藻酸钠溶液中，先以500r/min的转速搅拌30min，然后再加入20％的葡萄糖五丙酸酯，继续搅拌30min，搅拌结束，即可。
本实施例的处理液中还添加水滑石粉。
本实施例的步骤二中的沸石为钠沸石。
本实施例的膨润土分散液的制备方法为：将膨润土先煅烧30min，煅烧温度为 225℃，然后再置于硅烷偶联剂KH560中分散30min，分散结束，再向其中加入丙烯酸乳液，继续以100r/min的转速搅拌30min，搅拌结束，得到膨润土分散液。
本实施例的热压烧结的烧结温度为1500℃，热压时间为30min，热压压力为30MPa。
实施例3：
本实施例的一种石英陶瓷坩锅材料的生产工艺，包括以下步骤：
步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1250r/min，球磨时间为35min，球磨结束，再送入到处理液中反应25min，反应温度为125℃，反应结束，离心、水洗，干燥，即可；
步骤二，耐腐助剂的制备：将沸石加入到球磨机中进行球磨，球磨过30目，随后送入到膨润土分散液中进行超分散，分散功率为700W，分散时间为30min，然后过滤，干燥，得到耐腐助剂；
步骤三，辅料的称取：金刚石粉25份、硅酸铝7.5份、叶腊石6份、硅灰石6份；
步骤四，坩埚材料的制备：将步骤一制备的基体、步骤二制备的耐腐助剂、步骤三的辅料依次加入到共混机中进行共混，共混转速为300r/min，共混时间为25min，随后再进行热压烧结，烧结结束，得到石英陶瓷坩锅。
本实施例的处理液的制备方法为：将质量分数为25％的稀土氯化镧溶液送入到反应器中，然后再加入海藻酸钠溶液中，先以300r/min的转速搅拌25min，然后再加入20％的葡萄糖五丙酸酯，继续搅拌25min，搅拌结束，即可。
本实施例的处理液中还添加水滑石粉。
本实施例的步骤二中的沸石为钠沸石。
本实施例的膨润土分散液的制备方法为：将膨润土先煅烧25min，煅烧温度为 220℃，然后再置于硅烷偶联剂KH560中分散25min，分散结束，再向其中加入丙烯酸乳液，继续以60r/min的转速搅拌25min，搅拌结束，得到膨润土分散液。
本实施例的热压烧结的烧结温度为1250℃，热压时间为25min，热压压力为25MPa。
对比例1：
与实施例3的材料及制备工艺基本相同，唯有不同的是未添加耐腐助剂。
对比例2：
与实施例3的材料及制备工艺基本相同，唯有不同的是采用市场上常规的原料。
将实施例1-3及对比例1-2的材料进行性能测试，测试结果如表1所示
组别 耐20％盐酸程度(％)
实施例1 89
实施例2 91
实施例3 93
对比例1 86
对比例2 80
表1
由表1可知本发明实施例1-3、对比例1-2中本发明的材料耐20％盐酸为93％，而对比例2仅为80％。
以上所述仅是本发明的优选实施方式，应当指出：对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (7)

1.一种石英陶瓷坩锅材料的生产工艺，其特征在于，包括以下步骤：
步骤一，基体的制备：将石英砂、陶瓷按照重量比2:1进行混合，然后送入到球磨机中进行球磨，球磨转速为1000-1500r/min，球磨时间为30-40min，球磨结束，再送入到处理液中反应20-30min，反应温度为100-150℃，反应结束，离心、水洗，干燥，即可；
步骤二，耐腐助剂的制备：将沸石加入到球磨机中进行球磨，球磨过10-50目，随后送入到膨润土分散液中进行超分散，分散功率为300-1000W，分散时间为25-35min，然后过滤，干燥，得到耐腐助剂；
步骤三，辅料的称取：金刚石粉20-30份、硅酸铝5-10份、叶腊石4-8份、硅灰石4-8份；
步骤四，坩埚材料的制备：将步骤一制备的基体、步骤二制备的耐腐助剂、步骤三的辅料依次加入到共混机中进行共混，共混转速为100-500r/min，共混时间为20-30min，随后再进行热压烧结，烧结结束，得到石英陶瓷坩锅。
2.根据权利要求1所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述处理液的制备方法为：将质量分数为20-30％的稀土氯化镧溶液送入到反应器中，然后再加入海藻酸钠溶液中，先以200-500r/min的转速搅拌20-30min，然后再加入20％的葡萄糖五丙酸酯，继续搅拌20-30min，搅拌结束，即可。
3.根据权利要求2所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述处理液中还添加水滑石粉。
4.根据权利要求1所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述步骤二中的沸石为钠沸石。
5.根据权利要求1所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述膨润土分散液的制备方法为：将膨润土先煅烧20-30min，煅烧温度为215-225℃，然后再置于硅烷偶联剂KH560中分散20-30min，分散结束，再向其中加入丙烯酸乳液，继续以20-100r/min的转速搅拌20-30min，搅拌结束，得到膨润土分散液。
6.根据权利要求1所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述热压烧结的烧结温度为1000-1500℃，热压时间为20-30min，热压压力为20-30MPa。
7.根据权利要求6所述的一种石英陶瓷坩锅材料的生产工艺，其特征在于，所述热压烧结的烧结温度为1250℃，热压时间为25min，热压压力为25MPa。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115636663A (zh) * 2022-10-20 2023-01-24 无锡市尚领石英科技有限公司 高强度高致密性石英坩埚的制备工艺
CN117447111A (zh) * 2023-10-26 2024-01-26 深圳市元子能科技有限公司 石英矿的处理方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115636663A (zh) * 2022-10-20 2023-01-24 无锡市尚领石英科技有限公司 高强度高致密性石英坩埚的制备工艺
CN115636663B (zh) * 2022-10-20 2023-05-16 无锡市尚领石英科技有限公司 高强度高致密性石英坩埚的制备工艺
CN117447111A (zh) * 2023-10-26 2024-01-26 深圳市元子能科技有限公司 石英矿的处理方法

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