CN109516802A - 一种精密铸造用氧化锆坩埚及其热处理方法 - Google Patents

一种精密铸造用氧化锆坩埚及其热处理方法 Download PDF

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CN109516802A
CN109516802A CN201811504720.6A CN201811504720A CN109516802A CN 109516802 A CN109516802 A CN 109516802A CN 201811504720 A CN201811504720 A CN 201811504720A CN 109516802 A CN109516802 A CN 109516802A
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薛志岗
王帅
庞佳敏
董国强
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JIANGSU PROV CERAMIC RESEARCH INST Co Ltd
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Abstract

本发明公开了一种精密铸造用氧化锆坩埚，其特征在于，包括以下质量百分比的组分：10%～25%的150μm电熔单斜锆粉，10%～25%的150μm电熔稳定锆粉，5%～15%的75μm电熔单斜锆粉，5%～15%的3μm电熔单斜锆粉，5%～15%的0.8μm单斜锆粉，15%～25%的1.0μm化学镁稳定锆，3%～8%的0.8μm化学钇稳定锆和1%～4%的氧化镁。同时，本发明还公开了上述精密铸造用氧化锆坩埚的热处理方法。本发明对不同粒径氧化锆的稳定相和单斜相进行配比设计，对烧成后的坩埚采用特定工艺进行热处理，并对稳定剂采用复合设计，得到热膨胀系数较低、具有良好抗热震性能。

Description

一种精密铸造用氧化锆坩埚及其热处理方法
技术领域
本发明属于高温耐火材料领域，具体涉及一种精密铸造用氧化锆坩埚及其制备方法。
背景技术
氧化锆的熔点高达2700℃，即使加热到1900多摄氏度也不会与熔融的铝、铁、镍、铂等金属，硅酸盐和酸性炉渣等发生反应，所以用氧化锆材料制作的坩埚能成功地熔炼铂、钯、钌、铯等铂族贵金属及其合金，亦可用来熔炼钾、钠、石英玻璃以及氧化物和盐类等。但是，目前市场上提供的氧化锆坩埚产品往往抗热震性能较低，其主要原因如下：氧化锆具有单斜（Monoclinic）、四方（Tetragonal）、立方（Cubic）三种不同晶型，并且三种晶型随温度变化可以相互转变。在温度升到1170℃左右时，粒径在微米甚至更大尺寸的氧化锆晶体会发生从单斜相向四方相的转变（t-m相变），并伴有7%-9%的体积收缩，这种体积变化容易引起氧化锆材料的损伤，降低了氧化锆坩埚的抗热震性能，因此减轻t-m相变对材料的损伤是氧化锆坩埚制造的关键性技术。
目前采用的降低t-m相变对氧化锆材料损伤的方法是，在氧化锆中加入氧化镁、氧化钙、氧化钇等稳定剂，使氧化锆在高温下形成全稳定的立方氧化锆，这样就可以减少甚至消除在1170℃左右发生的t-m相变，减少因相变产生的体积变化而导致的损伤。
但是这个方法存在明显的不足：全稳定的立方相氧化锆具有较高的热膨胀系数（约11×10-6/K），而热膨胀系数越高则材料的抗热震性能越差，因此采用全稳定立方相的氧化锆坩埚，仍然不能够具备较好的抗热震性能。
发明内容
发明目的：本发明的目的在于针对现有技术的不足，提供一种精密铸造用氧化锆坩埚。
本发明的另一目的在于提供上述精密铸造用氧化锆坩埚的热处理方法。
技术方案：为了达到上述发明目的，本发明具体是这样来完成的：一种精密铸造用氧化锆坩埚，包括以下质量百分比的组分：10%～25%的150μm电熔单斜锆粉，10%～25%的150μm电熔稳定锆粉，5%～15%的75μm电熔单斜锆粉，5%～15%的3μm电熔单斜锆粉，5%～15%的0.8μm单斜锆粉，15%～25%的1.0μm化学镁稳定锆，3%～8%的0.8μm化学钇稳定锆和1%～4%的氧化镁。
其中，所述精密铸造用氧化锆坩埚的热处理方法，包括以下步骤：
（1）将制备好的坩埚置于加热炉中，开始加热升温；
（2）室温～1500℃：升温速度1℃/min ，升温至1500℃；
（3）1500℃：恒温保温3～6h；
（4）1500～1300℃：自然降温；
（5）1300℃：恒温保温3～6h；
（6）1300～1100℃：自然降温；
（7）1100℃：恒温保温3～6h；
（8）1100℃以下：自然降温至200℃或以下。
有益效果：本发明与传统技术相比，存在以下优点：
（1）本发明经热处理之后，两种颗粒的相转变温区产生差别：稳定相粗颗粒热处理产生的细晶单斜相在500℃～900℃发生相转变，降低了低温区膨胀率；单斜相粗颗粒由于晶粒尺寸较大，相转变滞后（1100℃～1400℃之间），降低了高温区膨胀率；通过此种设计，也使得集中在1100℃处进行相转变的单斜晶粒比例大大减少，从而避免了在此温区内，由于相转变的集中进行，而使得产品收缩开裂；
（2）本发明采用分步热处理的方法，相比于一般的热处理方法，分步热处理得到的氧化锆坩埚材料在常温下具有更多的单斜相含量，也具有更宽的相转变温度范围；
（3）本发明在1500℃、1300℃、1100℃分别进行保温处理，将稳定相的粗、细颗粒基本上转化为单斜相颗粒，从而降低了低温的膨胀率，并在升温的过程中单斜相颗粒逐步相转变，使整个升温过程中，产品的膨胀率波动达到设计要求；
（4）本发明中添加了3wt%～8wt%左右的氧化钇稳定氧化锆，为与其固溶的单斜晶粒相转变集中在1000℃～1100℃之间，从而缓解了1100℃～1200℃相转变时，膨胀率的突变。
具体实施方式
实施例1:
一种精密铸造用氧化锆坩埚，由以下质量百分比的组分组成：10%的150μm电熔单斜锆粉，25%的150μm电熔稳定锆粉，15%的75μm电熔单斜锆粉，15%的3μm电熔单斜锆粉，5%%的0.8μm单斜锆粉，25%的1.0μm化学镁稳定锆，4%的0.8μm化学钇稳定锆和1%的氧化镁。
实施例2:
一种精密铸造用氧化锆坩埚，由以下质量百分比的组分组成：15%的150μm电熔单斜锆粉，15%的150μm电熔稳定锆粉，12%的75μm电熔单斜锆粉，11%的3μm电熔单斜锆粉，15%的0.8μm单斜锆粉，20%的1.0μm化学镁稳定锆，8%的0.8μm化学钇稳定锆和4%的氧化镁。
实施例3:
一种精密铸造用氧化锆坩埚，由以下质量百分比的组分组成：20%的150μm电熔单斜锆粉，10%的150μm电熔稳定锆粉，10%的75μm电熔单斜锆粉，15%的3μm电熔单斜锆粉，15%的0.8μm单斜锆粉，25%的1.0μm化学镁稳定锆，3%的0.8μm化学钇稳定锆和2%的氧化镁。
实施例4:
一种精密铸造用氧化锆坩埚，由以下质量百分比的组分组成：25%的150μm电熔单斜锆粉，20%的150μm电熔稳定锆粉，15%的75μm电熔单斜锆粉，5%的3μm电熔单斜锆粉，12%的0.8μm单斜锆粉，15%的1.0μm化学镁稳定锆，5%的0.8μm化学钇稳定锆和3%的氧化镁。
实施例5:
一种精密铸造用氧化锆坩埚，由以下质量百分比的组分组成：25%的150μm电熔单斜锆粉，25%的150μm电熔稳定锆粉，5%的75μm电熔单斜锆粉，10%的3μm电熔单斜锆粉，10%的0.8μm单斜锆粉，15%的1.0μm化学镁稳定锆，7%的0.8μm化学钇稳定锆和3%的氧化镁。
实施例6:
一种精密铸造用氧化锆坩埚的热处理方法，包括将制备好的坩埚置于加热炉中，开始加热升温；在室温时进行速度1℃/min 的升温至1500℃；至1500℃后，恒温保温3～6h；随后进行1500～1300℃时的自然降温；至1300℃后恒温保温3～6h；再进行1300～1100℃时的自然降温；至1100℃后恒温保温3～6h；最后自然降温至200℃或以下。

Claims (2)

1.一种精密铸造用氧化锆坩埚，其特征在于，包括以下质量百分比的组分：10%～25%的150μm电熔单斜锆粉，10%～25%的150μm电熔稳定锆粉，5%～15%的75μm电熔单斜锆粉，5%～15%的3μm电熔单斜锆粉，5%～15%的0.8μm单斜锆粉，15%～25%的1.0μm化学镁稳定锆，3%～8%的0.8μm化学钇稳定锆和1%～4%的氧化镁。
2.制备权利要求1所述精密铸造用氧化锆坩埚的热处理方法，其特征在于，包括以下步骤：
（1）将制备好的坩埚置于加热炉中，开始加热升温；
（2）室温～1500℃：升温速度1℃/min ，升温至1500℃；
（3）1500℃：恒温保温3～6h；
（4）1500～1300℃：自然降温；
（5）1300℃：恒温保温3～6h；
（6）1300～1100℃：自然降温；
（7）1100℃：恒温保温3～6h；
（8）1100℃以下：自然降温至200℃或以下。
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CN112408979A (zh) * 2020-11-13 2021-02-26 浙江自立控股有限公司 转炉挡渣滑板用氧化锆陶瓷及其制备方法
CN116082035A (zh) * 2023-02-01 2023-05-09 中钢集团洛阳耐火材料研究院有限公司 一种高光洁度、高抗热震性薄壁氧化锆坩埚的制备方法

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