CN110357622A - 一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法 - Google Patents

一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法 Download PDF

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CN110357622A
CN110357622A CN201910501666.8A CN201910501666A CN110357622A CN 110357622 A CN110357622 A CN 110357622A CN 201910501666 A CN201910501666 A CN 201910501666A CN 110357622 A CN110357622 A CN 110357622A
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crucible
artificial tooth
peeling
quartzy
coating layer
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游杰刚
司超伟
郎杰夫
张小芳
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University of Science and Technology Liaoning USTL
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Abstract

本发明涉及一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法，包括粉料和液态料，粉料占20％‑80％；粉料包括以下重量百分比的原料：ZrO2+HfO2≥90％；Y2O3 7％‑9％；SiO2 0‑5％，不包括0；其余为杂质；液态料包括去离子水和粘结剂。优点是：本发明的义齿坩埚涂层抗热震性能好，粘附良好。既可以起到缓解义齿坩埚在铸造过程中粘钢严重的问题，也可以有效抑制钢液对坩埚的侵蚀和剥落，同时使铸造合金不因石英义齿坩埚的溶蚀而遭到污染，且可以使得义齿坩埚的使用寿命得以延长。义齿坩埚涂层，在SEM观察下，涂层与坩埚内壁结合良好无裂纹；1100℃、抗水冷热震能力≥3次。

Description

一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法
技术领域
本发明属于无机非金属材料领域，尤其涉及一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法，适用于离心铸造法生产合金义齿，同时也为钛合金义齿铸造用坩埚创造了可能。
背景技术
离心铸造法是合金义齿生产的一种重要方法，义齿铸造企业生产时，经常存在义齿铸造质量不过关，铸造义齿的坩埚容易粘钢，导致废弃，损耗资源，加大成本。在铸造过程中，义齿合金首先在义齿坩埚中加热快速熔化，然后在高速离心力的作用下将义齿坩埚中的熔融态合金高速注入到义齿型模中，冷却后经加工成为义齿。在此过程中，由于熔融石英质坩埚成本低，热震好而被广泛采用。然而熔融石英质坩埚在高温下非常不稳定，具有较高的氧势，容易造成合金氧化，形成氧化物夹杂，同时高温下二氧化硅也容易溶解在合金熔液中，从而影响义齿的铸造质量。特别是钛及钛合金在高温熔融状态下极易与氧反应，形成钛氧化物，从而影响钛及钛合金义齿的质量，同时铸造合金氧化所形成的合金氧化物极易与石英材质发生反应而粘附在坩埚涂层的内壁，使石英义齿坩埚的使用寿命大幅降低，因此在熔融石英坩埚内壁涂覆涂层成为了一种延长坩埚使用寿命和提高铸造义齿的重要方法。
发明内容
为克服现有技术的不足，本发明的目的是提供一种不粘钢、防剥落的石英义齿坩埚涂层及制备方法，抗热震性能高，粘附良好，抗剥落能力强，粘钢轻微。
为实现上述目的，本发明通过以下技术方案实现：
一种不粘钢、防剥落的石英义齿坩埚涂层，包括粉料和液态料，粉料占20％-80％；
粉料包括以下重量百分比的原料：ZrO2+HfO2≥90％；Y2O3 7％-9％；SiO2 0-5％，不包括0；其余为杂质；
液态料包括去离子水和粘结剂。
所述的粘结剂为有机硅烷、硅酸、多元醇、聚乙烯醇、丙烯酸酯中的一种。
一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，包括以下步骤：
1)以部分氧化钇稳定氧化锆为原料，加入去离子水，硅灰，粘结剂，混合均匀，形成混合料浆；
2)料浆涂覆义齿坩埚内壁，形成涂层；
3)对涂层坩埚进行干燥处理；
4)将干燥处理后的涂层义齿坩埚进行烧成处理。
步骤1)中所述的去离子水与粉料重量比为6：4；硅灰加入量为0-5wt.％，不包括0；粘结剂加入量为0-1wt.％，不包括0。
所述的部分氧化钇稳定氧化锆粒度为15-90μm，硅灰中SiO2含量≥92％，粒度为纳米级。
步骤1)中，利用行星球磨机进行部分氧化钇稳定氧化锆、去离子水、硅灰的混合，转数240-300r/min，时长6h以上；然后加入粘结剂混合，利用磁力搅拌器混合均匀。
步骤2)中，采用挂浆法将步骤1)所得混合浆料涂覆在义齿坩埚内壁，再置于通风干燥处24h以上，形成初次涂层。
步骤3)将步骤2)形成涂层的义齿坩埚置于恒温干燥箱中，干燥制度为温度80-110℃，时间12-24h。
步骤4)将干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，烧成制度为：3-5℃/min升温速率，温度为1200-1400℃，保温0.5h以上。
步骤4)烧成处理后的涂层在SEM观察下，涂层与坩埚内壁结合良好无裂纹；1100℃、抗水冷热震能力≥3次；铸造合金义齿20次不粘钢。
与现有技术相比，本发明的有益效果是：
本发明的义齿坩埚涂层抗热震性能好，粘附良好。既可以起到缓解义齿坩埚在铸造过程中粘钢严重的问题，也可以有效抑制钢液对坩埚的侵蚀和剥落，同时使铸造合金不因石英义齿坩埚的溶蚀而遭到污染，且可以使得义齿坩埚的使用寿命得以延长。本发明选取的部分氧化钇稳定氧化锆(PYD-AP)本身就具有较好的热震稳定性；选取的硅灰为烧结助剂，一方面可以降低氧化锆的烧结温度，使烧结涂层致密，可以减少和缓解熔融铸造合金的侵蚀和溶解；另一方面可以缓解氧化锆涂层和熔融石英之间的热膨胀差异，防止烧成和使用过程中涂层产生剥落。义齿坩埚涂层，在SEM观察下，涂层与坩埚内壁结合良好无裂纹；1100℃、抗水冷热震能力≥3次；铸造合金义齿20次不粘钢。
附图说明
图1是实施例一200倍SEM坩埚涂层图。
图2是实施例二200倍SEM坩埚涂层图。
具体实施方式
下面结合说明书附图对本发明进行详细地描述，但是应该指出本发明的实施不限于以下的实施方式。
一种不粘钢、防剥落的石英义齿坩埚涂层，其制备方法包括以下步骤：
(1)原料选择与配比：部分氧化钇稳定氧化锆(PYD-AP)为原料，硅灰为添加剂，加入去离子水，粘结剂为有机硅烷、硅酸、多元醇、聚乙烯醇和丙烯酸酯中的一种；优先地，去离子水与粉料比例为6：4，硅灰加入量为0-5wt.％，不包括0，粘结剂选择聚乙烯醇为0.5wt.％(粘结剂不局限于聚乙烯醇，还可从有机硅烷、硅酸、多元醇、丙烯酸酯选取)，且PYD-AP粒度为15-90μm，硅灰SiO2含量≥92％，粒度为纳米级；
(2)混料：对原料进行均匀混合，形成混合料浆；优先地，利用XQM-2行星球磨机进行原料和外加剂的混合，转数240-300r/min，时长6h；然后将料浆和粘结剂混合，利用磁力搅拌器混合均匀；粘结剂优选聚乙烯醇。
(3)成型：料浆涂覆义齿坩埚内壁，形成涂层；优先地，利用注浆法将步骤(2)所得的均匀浆料涂覆在义齿坩埚内壁，将其置于通风干燥处24h，形成一厚度约为0.3mm的涂层。
(4)干燥：对涂层的坩埚进行干燥处理；优先地，将形成涂层的义齿坩埚置于恒温干燥箱中，干燥制度为温度80-110℃，时间12-24h。
(5)烧成：将干燥处理后的义齿涂层坩埚进行烧成处理；优先地，干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，烧成制度为：3-5℃/min升温速率，温度为1200-1400℃，保温0.5h。
本发明的义齿坩埚涂层抗热震性能好，粘附良好。既可以起到缓解义齿坩埚在铸造过程中粘钢严重的问题，也可以有效抑制钢液对坩埚的侵蚀和剥落，同时使铸造合金不因石英义齿坩埚的溶蚀而遭到污染，且可以使得义齿坩埚的使用寿命得以延长。
实施例一
不粘钢、防剥落的石英义齿坩埚涂层的制备方法：
步骤一，以部分氧化钇稳定氧化锆(PYD-AP)为原料，加入去离子水与原料比例为6：4，1wt.％的硅灰，粘结剂选择聚乙烯醇加入量为0.5wt.％。
步骤二，粉料与去离子水置于球磨机内混合球磨6h，然后将料浆和粘结剂混合，利用磁力搅拌器混合均匀。
步骤三，利用挂浆法将上述所得均匀浆料涂覆在义齿坩埚内壁，将其置于通风干燥处24h，形成涂层。
步骤四，将形成涂层的义齿坩埚置于恒温干燥箱中，干燥温度为80℃，干燥时间12h。
步骤五，将干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，升温速度3℃/min，温度1300℃，保温0.5h。
本实例所得到义齿坩埚在扫描电子显微镜下的涂层SEM图片见图1，可见涂层厚度为0.1mm，涂层与坩埚粘附良好。涂层烧结良好，没有剥落，也几乎没有粘附铸造合金。
实施例二
不粘钢、防剥落的石英义齿坩埚涂层的制备方法：
步骤一，以PYD-AP为原料，加入去离子水与原料比例为6：4，1.5wt.％的硅灰，粘结剂选择聚乙烯醇加入量为0.5wt.％。
步骤二，原料与外加剂置于球磨机内混合球磨6h，然后将料浆和粘结剂混合，利用磁力搅拌器混合均匀。
步骤三，利用注浆法将上述所得均匀浆料涂覆在义齿坩埚内壁，将其置于通风干燥处24h，形成涂层。
步骤四，将形成涂层的义齿坩埚置于恒温干燥箱中，干燥温度为100℃，干燥时间18h。
步骤五，干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，4℃/min，温度1350℃，保温0.5h。
本实例所得到义齿坩埚在扫描电子显微镜下的涂层SEM图片见图2，可见涂层厚度约为0.1mm，涂层与坩埚粘附良好。涂层烧结良好，有少量的剥落，几乎没有粘附铸造合金。
实施例三
不粘钢、防剥落的石英义齿坩埚涂层的制备方法：
步骤一，以PYD-AP为原料，加入去离子水与原料比例为6：4，1wt.％的硅灰，粘结剂选择丙烯酸酯，加入量为0.3wt.％。
步骤二，原料与外加剂置于球磨机内混合球磨6h，然后将料浆和粘结剂混合，利用磁力搅拌器混合均匀。
步骤三，利用注浆法将上述所得均匀浆料涂覆在义齿坩埚内壁，将其置于通风干燥处24h，形成涂层。
步骤四，将形成涂层的义齿坩埚置于恒温干燥箱中，干燥温度为80℃，干燥时间16h。
步骤五，干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，5℃/min，温度1300℃，保温0.5h。

Claims (10)

1.一种不粘钢、防剥落的石英义齿坩埚涂层，其特征在于，包括粉料和液态料，粉料占20％-80％；
粉料包括以下重量百分比的原料：ZrO2+HfO2≥90％；Y2O3 7％-9％；SiO2 0-5％，不包括0；其余为杂质；
液态料包括去离子水和粘结剂。
2.根据权利要求1所述的一种不粘钢、防剥落的石英义齿坩埚涂层，其特征在于，所述的粘结剂为有机硅烷、硅酸、多元醇、聚乙烯醇、丙烯酸酯中的一种。
3.一种根据权利要求1所述的不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，包括以下步骤：
1)以部分氧化钇稳定氧化锆为原料，加入去离子水，硅灰，粘结剂，混合均匀，形成混合料浆；
2)料浆涂覆义齿坩埚内壁，形成涂层；
3)对涂层坩埚进行干燥处理；
4)将干燥处理后的涂层义齿坩埚进行烧成处理。
4.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤1)中所述的去离子水与粉料重量比为6：4；硅灰加入量为0-5wt.％，不包括0；粘结剂添加量为0-1wt.％，不包括0。
5.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，所述的部分氧化钇稳定氧化锆粒度为15-90μm，硅灰中SiO2含量≥92％，粒度为纳米级。
6.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤1)中，利用行星球磨机进行部分氧化钇稳定氧化锆、去离子水、硅灰的混合，转数240-300r/min，时长6h以上；然后加入粘结剂混合，利用磁力搅拌器混合均匀。
7.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤2)中，采用挂浆法将步骤1)所得混合浆料涂覆在义齿坩埚内壁，再置于通风干燥处24h以上，形成初次涂层。
8.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤3)将步骤2)形成涂层的义齿坩埚置于恒温干燥箱中，干燥制度为温度80-110℃，时间12-24h。
9.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤4)将干燥后的形成涂层的义齿坩埚置于箱式电阻炉中烧结，烧成制度为：3-5℃/min升温速率，温度为1200-1400℃，保温0.5h以上。
10.根据权利要求3所述的一种不粘钢、防剥落的石英义齿坩埚涂层的制备方法，其特征在于，步骤4)烧成处理后的涂层在SEM观察下，涂层与坩埚内壁结合良好无裂纹；1100℃、抗水冷热震能力≥3次；铸造合金义齿20次不粘钢。
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