CN111848137A - 一种高抗热震氧化铝陶瓷及其制备方法 - Google Patents

一种高抗热震氧化铝陶瓷及其制备方法 Download PDF

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CN111848137A
CN111848137A CN202010532530.6A CN202010532530A CN111848137A CN 111848137 A CN111848137 A CN 111848137A CN 202010532530 A CN202010532530 A CN 202010532530A CN 111848137 A CN111848137 A CN 111848137A
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rare earth
alumina ceramic
thermal shock
high thermal
alumina
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狄玉丽
罗茜
黄海燕
焦钰
靳必强
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Xichang College
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Abstract

本发明公开了一种高抗热震氧化铝陶瓷及其制备方法；所述高抗热震氧化铝陶瓷，按质量百分比计算，包括95～98%微米级α‑Al2O3粉、0.5～1%SiO2、0.5～1%CaCO3、0.5～1%滑石粉、0.5～1%粘结剂、0～0.5%稀土氧化物或稀土氟化物。本发明选择微米级的氧化铝粉，添加稀土氧化物或氟化物，选择滑石粉、二氧化硅、碳酸钙为助烧剂，聚乙烯醇为粘结剂，经过混合－压制－烧结三大步骤即可制得氧化铝陶瓷制品，工艺简单，易操作，且能在较低烧结温度（1580‑1600℃）下烧结成型，且制备所得的氧化铝具有高抗热震性能。本发明可节约制备氧化铝成本且使其在高温环境（≥800℃）下的使用寿命增加。

Description

一种高抗热震氧化铝陶瓷及其制备方法
技术领域
本发明涉及材料制备技术领域，特别涉及一种高抗热震氧化铝陶瓷及其制备方法。
背景技术
氧化铝具有高强度、高硬度、耐腐蚀、耐磨损等优异性能，且其价格相对较低，在陶瓷、化工、建材、机械、冶金等领域得到了广泛的应用。现有技术的原料使用纳米级氧化铝以降低氧化铝的烧结温度，成本较高，且烧结温度较高1700℃（烧结48小时），或使用热等静压法制备氧化铝，其操作过程繁杂，步骤较多，难以实现工业化。
现有氧化铝陶瓷为了降低烧结温度提高性能，一般原料选择纳米氧化铝粉，然后与助烧剂、添加剂（稀土氧化物、其他陶瓷粉末等）球磨混合后，在液压机在压制成型（形状以模具而定，可为圆柱形，可为长方形、正方形或其他形状，有热压、冷等静压等方法）后，选择真空烧结、微波烧结、放电等离子烧结、热压烧结等方法烧结成型，烧结温度较高1600-1700℃，保温时间2-48小时，且制备所得的氧化铝的高温抗热震性能较差，从而限制其更广泛的应用。
发明内容
本发明的目的在于提供一种高抗热震氧化铝陶瓷及其制备方法，解决以下现有氧化铝陶瓷材料塑性及韧性差，脆性大，高温（≥800℃）抗热震性能差，且其烧结温度较高的问题。
本发明的技术方案为：
一种高抗热震氧化铝陶瓷，按质量百分比计算，包括95～98%微米级α-Al2O3粉、0.5～1%SiO2、0.5～1%CaCO3、0.5～1%滑石粉、0.5～1%粘结剂、0～0.5%稀土氧化物或稀土氟化物。
优选地，所述微米级α-Al2O3粉的纯度≥99.9%。
优选地，所述粘结剂为聚乙烯醇，其纯度≥98%。
优选地，稀土氧化物或稀土氟化物的纯度≥99.9%；所述稀土氧化物为Nd2O3或Pr6O11，所述稀土氟化物为LaF3。
一种高抗热震氧化铝陶瓷的制备方法，包括以下步骤：
（1）按比例称取上述微米级α-Al2O3粉、SiO2、CaCO3、滑石粉、粘结剂、稀土氧化物或稀土氟化物；放入变频行星式球磨机中干法研磨混合，转速为250～300r/min，混合1～2h后取出干燥；
（2）采用液压机进行干压成型，压制压强为100～200MPa保压1～5min后成型，生坯形状根据模具形状而定；
（3）压制后试样放置于箱式电阻炉中进行烧结，设置烧结温度为1580～1600℃，保温时间2～3h；保温冷却后取出，制得高抗热震氧化铝陶瓷。
优选地，所述步骤（3）中箱式电阻炉先升温至100℃保温30min后再升温到1000℃保温60min以去除粘结剂，于升温至1580～1600℃，保温2-3h后降温至400℃后随炉冷却后取出成品；整个烧结的升温速率≤10℃/min。
本发明的有益效果是：
本发明选择微米级的α-氧化铝粉末，添加稀土氧化物或氟化物，选择滑石粉、二氧化硅、碳酸钙为助烧剂，聚乙烯醇为粘结剂，使用工艺简单且易操作；通过干压法制备氧化铝生坯后在较低烧结温度（1580～1600℃）烧结制备获得高抗热震性能的氧化铝陶瓷；可节约制备氧化铝成本且使其在高温环境（≥800℃）下的使用寿命增加。
具体实施方式
下面结合实施例对本发明作进一步描述，但不限制本发明的保护范围和应用范围。
一种高抗热震氧化铝陶瓷的制备方法，包括以下步骤：
（1）按比例称取微米级α-Al2O3粉（70%颗粒尺寸分布在10～200μm之间，其平均粒径为163μm，纯度≥99.9％）、SiO2、CaCO3、滑石粉、粘结剂聚乙烯醇（PVC，纯度≥98％）、稀土氧化物或稀土氟化物（近90%的颗粒粒径在1～8μm之间，且平均粒径为3.85μm，纯度≥99.9%）；放入变频行星式球磨机中干法研磨混合，转速为250～300r/min，混合1～2h后取出干燥；
（2）采用液压机进行干压成型，压制压强为100～200MPa保压1～5min后成型，生坯形状根据模具形状而定；
（3）压制后试样放置于箱式电阻炉中进行烧结，设置烧结温度为1580～1600℃，保温时间2～3h；具体地，箱式电阻炉先升温至100℃保温30min后再升温到1000℃保温60min以去除粘结剂，于升温至1580～1600℃，保温2-3h后降温至400℃后随炉冷却后取出成品；整个烧结的升温速率≤10℃/min。
采用上述制备方法，所述步骤（1）中原料配比按表1所示进行称取，制得实施例1至实施例7样品。
表1 原料配比表（质量百分比，%）
实施例 α－Al<sub>2</sub>O<sub>3</sub> SiO<sub>2</sub> CaCO<sub>3</sub> 滑石粉 PVC LaF<sub>3</sub> Nd<sub>2</sub>O<sub>3</sub> Pr<sub>6</sub>O<sub>11</sub>
1 96 1 1 1 1 0 0 0
2 95.9 1 1 1 1 0.1 0 0
3 95.8 1 1 1 1 0.2 0 0
4 95.9 1 1 1 1 0 0.1 0
5 95.8 1 1 1 1 0 0.2 0
6 95,5 1 1 1 1 0 0 0.5
7 95 1 1 1 1 0 0 1
实施例1为对比例即不加入任何稀土情况下时制备所得的氧化铝陶瓷，而实施例2-7分别为加入不同稀土添加量的氟化镧（LaF3）、氧化钕（Nd2O3）、氧化镨（Pr6O11）的氧化铝陶瓷。
采用如下抗热震检测方法：将成品在25℃常温下放入1100℃的箱式电阻炉内保温30min，然后取出放入流动水槽中10min，然后静置5min后观察是否出现裂纹，重复实验直至出现裂纹、破损从而停止实验，从而记录抗热震次数，抗热震次数至少使用3个样品进行检测，并且求平均值后四舍五入后使用，检测其抗热震次数如表２所示，说明添加稀土元素进去可以有效提高氧化铝陶瓷的抗热震性能。
表2 氧化铝陶瓷的抗热震性能
Figure 396939DEST_PATH_IMAGE002
本发明选择微米级的氧化铝粉，添加稀土氧化物或氟化物，选择滑石粉、二氧化硅、碳酸钙为助烧剂，聚乙烯醇为粘结剂，经过混合－压制－烧结三大步骤即可制得氧化铝陶瓷制品，工艺简单，易操作，且能在较低烧结温度（1580-1600℃）下烧结成型，且制备所得的氧化铝具有高抗热震性能。本发明可节约制备氧化铝成本且使其在高温环境（≥800℃）下的使用寿命增加。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何不经过创造性劳动想到的变化或简单替换，都应该涵盖在本发明的保护范围之内。

Claims (6)

1.一种高抗热震氧化铝陶瓷，其特征在于：按质量百分比计算，包括95～98%微米级α-Al2O3粉、0.5～1%SiO2、0.5～1%CaCO3、0.5～1%滑石粉、0.5～1%粘结剂、0～0.5%稀土氧化物或稀土氟化物。
2.根据权利要求1所述的高抗热震氧化铝陶瓷，其特征在于：所述微米级α-Al2O3粉的纯度≥99.9%。
3.根据权利要求1所述的高抗热震氧化铝陶瓷，其特征在于：所述粘结剂为聚乙烯醇，其纯度≥98%。
4.根据权利要求1所述的高抗热震氧化铝陶瓷，其特征在于：稀土氧化物或稀土氟化物的纯度≥99.9%；所述稀土氧化物为Nd2O3或Pr6O11，所述稀土氟化物为LaF3。
5.根据权利要求1-4任一所述的高抗热震氧化铝陶瓷的制备方法，其特征在于，包括以下步骤：
（1）按比例称取上述微米级α-Al2O3粉、SiO2、CaCO3、滑石粉、粘结剂、稀土氧化物或稀土氟化物；放入变频行星式球磨机中干法研磨混合，转速为250～300r/min，混合1～2h后取出干燥；
（2）采用液压机进行干压成型，压制压强为100～200M Pa保压1～5min后成型，生坯形状根据模具形状而定；
（3）压制后试样放置于箱式电阻炉中进行烧结，设置烧结温度为1580～1600℃，保温时间2～3h；保温冷却后取出，制得高抗热震氧化铝陶瓷。
6.根据权利要求5所述的高抗热震氧化铝陶瓷的其制备方法，其特征在于：所述步骤（3）中箱式电阻炉先升温至100℃保温30min后再升温到1000℃保温60min以去除粘结剂，于升温至1580～1600℃，保温2-3h后降温至400℃后随炉冷却后取出成品；整个烧结的升温速率≤10℃/min。
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