CN112573910A - 一种耐磨石英陶瓷材料及其制备方法 - Google Patents

一种耐磨石英陶瓷材料及其制备方法 Download PDF

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CN112573910A
CN112573910A CN202011492719.3A CN202011492719A CN112573910A CN 112573910 A CN112573910 A CN 112573910A CN 202011492719 A CN202011492719 A CN 202011492719A CN 112573910 A CN112573910 A CN 112573910A
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parts
wear
powder
ceramic material
silicon
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杜孝硕
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Xuzhou Yasur High Tech Materials Co ltd
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Xuzhou Yasur High Tech Materials Co ltd
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    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

本发明涉及一种耐磨石英陶瓷材料，由以下原料制备而成：硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑、结合剂。本发明的耐磨石英陶瓷材料，具有良好的耐磨性能，在不同的温度下使用，仍然保持有良好的稳定性和耐候性，使用寿命长。本发明耐磨石英陶瓷材料的制备方法简单，可控性强、生产效率高、绿色环保。本发明的耐磨石英陶瓷材料，可以直接生产为高耐磨石英件，如耐磨石英管、石英陶瓷板，适应陶瓷坩埚，高精度的石英陶瓷件等。本发明的耐磨石英陶瓷材料产品，耐火温度为1800℃以上，莫氏硬度能达到8。

Description

一种耐磨石英陶瓷材料及其制备方法
技术领域
本发明属于石英陶瓷材料领域，具体地，涉及一种耐磨石英陶瓷材料及其制备方法。
背景技术
常见的陶瓷材料有粘土、氧化铝、高岭土等，陶瓷材料一般硬度较高，但可塑性较差，除了使用于食器、装饰上外，陶瓷在科学、技术的发展中亦扮演着重要角色，陶瓷原料是地球原有的大量资源黏土经过淬取而成，而粘土的性质具韧性，常温遇水可塑，微干可雕，全干可磨；烧至700度可成陶器能装水；烧至1230度则瓷化，可几乎完全不吸水且耐高温耐腐蚀。
陶瓷材料越硬，其耐磨性越好，硬度越高，冲击韧性越低，材料越脆。硬质合金材料对其中不少新材料的加工难以胜任。另一方面，现在国际上硬质合金产量己达20000-25000t，每年消耗大量的金属，如W、Co、Ta和Nb等。这些金属的矿产资源正日益减少，价格上涨，按日前消耗速度，用不了几十年有些资源将耗尽。而陶瓷材料在此背景下发展起来，现有的陶瓷材料相对于硬质合金耐磨性有了提高，但在加工高精度复杂件时其耐磨性还有待提高，因此急需一种高耐磨性的陶瓷刀具是当前所要解决的问题。
现有技术中，石英陶瓷又称熔融石英陶瓷、石英玻璃陶瓷、石英玻璃烧结制品、熔融石英烧结制品，他是采用熔融石英为原料，经过粉碎、成形、烧成等一系列陶瓷工艺制备的制品。
石英陶瓷具有成本低、高温荷重软化温度高、热膨胀系数小、热稳定系好、耐化学腐蚀性能好、介电性高等优良特性，可以应用于多个领域。现有的石英陶瓷隔热性一般，耐磨性较差，同时易炸裂，导致使用成本升高。
发明内容
发明目的：本发明的目的在于提供一种耐磨石英陶瓷材料的制备方法，工艺过程简单、可控性强、成本低，生产效率高、绿色环保，能生产出耐磨损、高强度、高韧性、质量轻的铝硅合金板材料。
本发明所采用的技术方案：本发明提供了一种耐磨石英陶瓷材料，由以下重量份的组分制备而成：
硅微粉 90-120份
碳酸钡 15-20份
二硼化钛 7-12份
氮化铝 10-15份
氮化硼 10-15份
氧化锆 3-8份
氮化硅 9-13份
滑石粉 8-12份
陶瓷粉 3-8份
碳化硅 5-8份
碳酸氢钠 3-5份
三氧化二锑 2-5份
结合剂 5-10份。
进一步的，所述硅微粉为亚纳米的球形硅微粉。
进一步的，所述结合剂由以下重量份的组分组成：乙酸乙酯6-10份、水性树脂聚丙烯酰胺3-5份、聚乙二醇5-8份。
进一步的，所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
进一步的，所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
进一步的，所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨4h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到450~500℃，保持12~16min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1450-1500℃，待细硅粉熔融，保持8~12min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用旋风集尘，得到硅微粉。
进一步的，所述步骤（d）的惰性保护气为氩气。
进一步的，所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
进一步的，所述的一种耐磨石英陶瓷材料的制备方法，包括如下步骤：（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨，得到混合料；（2）在惰性气氛下，向步骤（1）的混合料中加入结合剂，搅拌15-20min后，升温至140-150℃，保温反应30-40min；（3）将步骤（2）的混合料放入石墨模具内干压成型，并进行冷等静压处理，压力为100MPa，保压时间30min，得到生坯；（4）将步骤（3）得到的生坯转移至高温氮气炉内于流动氮气保护下先于1000-1200℃保温25-35min，随后升温至1700-1800℃保温2-2.5h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
进一步的，所述耐磨石英陶瓷材料产品的耐火温度为1800℃以上，莫氏硬度能达到8。
本发明的有益效果是：
（1）本发明的耐磨石英陶瓷材料，具有良好的耐磨性能，在不同的温度下使用，仍然保持有良好的稳定性和耐候性，使用寿命长，具有耐磨、硬度高、热膨胀系数小、热稳定性好、耐化学腐蚀性能好、介电性高等优点。本发明耐磨石英陶瓷材料的制备方法简单，可控性强、生产效率高、绿色环保。本发明的耐磨石英陶瓷材料，可以直接生产为高耐磨石英件，如耐磨石英管、石英陶瓷板，适应陶瓷坩埚，高精度的石英陶瓷件等。本发明的耐磨石英陶瓷材料产品，耐火温度为1800℃以上，莫氏硬度能达到8。
具体实施方式
下面将通过几个具体实施例，进一步阐明本发明，这些实施例只是为了说明问题，并不是一种限制。
实施例1：
一种耐磨石英陶瓷材料，由以下重量份的组分制备而成：
硅微粉 100份
碳酸钡 15份
二硼化钛 10份
氮化铝 12份
氮化硼 10份
氧化锆 6份
氮化硅 12份
滑石粉 8份
陶瓷粉 6份
碳化硅 7份
碳酸氢钠 5份
三氧化二锑 3份
结合剂 8份。
进一步的，所述硅微粉为亚纳米的球形硅微粉。
进一步的，所述结合剂由以下重量份的组分组成：乙酸乙酯8份、水性树脂聚丙烯酰胺4份、聚乙二醇5份。
进一步的，所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
进一步的，所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
进一步的，所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨4h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到480℃，保持15min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1500℃，待细硅粉熔融，保持10min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用布袋、旋风或者静电集尘，得到硅微粉。
进一步的，所述惰性保护气为氩气。
进一步的，所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
进一步的，（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨；（2）在惰性气氛下，向步骤（1）的产物中加入结合剂，搅拌18min后，升温至145℃，保温反应35min；（3）经过滤后放入高温氮气炉内于流动氮气保护下先于1100℃保温30min，随后升温至1800℃保温2h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
进一步的，所述耐磨石英陶瓷材料产品的耐火温度为1800℃以上，莫氏硬度能达到8.2。将所得到的耐磨石英陶瓷材料产品放在冰水混合液中，10分钟后拿出来，放于80-100℃的热水中，耐磨石英陶瓷材料产品完好无损，没有破裂的情况。
实施例2：
一种耐磨石英陶瓷材料，由以下重量份的组分制备而成：
硅微粉 90份
碳酸钡 17份
二硼化钛 12份
氮化铝 10份
氮化硼 12份
氧化锆 3份
氮化硅 9份
滑石粉 10份
陶瓷粉 3份
碳化硅 6份
碳酸氢钠 4份
三氧化二锑 2份
结合剂 5份。
进一步的，所述硅微粉为亚纳米的球形硅微粉。
进一步的，所述结合剂由以下重量份的组分组成：乙酸乙酯10份、水性树脂聚丙烯酰胺4份、聚乙二醇6份。
进一步的，所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
进一步的，所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
进一步的，所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨3h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到450℃，保持16min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1450℃，待细硅粉熔融，保持12min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用布袋、旋风或者静电集尘，得到硅微粉。
进一步的，所述惰性保护气为氩气。
进一步的，所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
进一步的，（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨；（2）在惰性气氛下，向步骤（1）的产物中加入结合剂，搅拌15min后，升温至150℃，保温反应30min；（3）经过滤后放入高温氮气炉内于流动氮气保护下先于1000℃保温35min，随后升温至1750℃保温2h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
进一步的，所述耐磨石英陶瓷材料产品的耐火温度为1750℃以上，莫氏硬度能达到8.0。将所得到的耐磨石英陶瓷材料产品放在冰水混合液中，10分钟后拿出来，放于80-100℃的热水中，耐磨石英陶瓷材料产品完好无损，没有破裂的情况。
实施例3：
一种耐磨石英陶瓷材料，由以下重量份的组分制备而成：
硅微粉 110份
碳酸钡 19份
二硼化钛 8份
氮化铝 13份
氮化硼 15份
氧化锆 8份
氮化硅 11份
滑石粉 12份
陶瓷粉 8份
碳化硅 5份
碳酸氢钠 5份
三氧化二锑 5份
结合剂 10份。
进一步的，所述硅微粉为亚纳米的球形硅微粉。
进一步的，所述结合剂由以下重量份的组分组成：乙酸乙酯6份、水性树脂聚丙烯酰胺4份、聚乙二醇7份。
进一步的，所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
进一步的，所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
进一步的，所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨3h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到500℃，保持12min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1480℃，待细硅粉熔融，保持10min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用布袋、旋风或者静电集尘，得到硅微粉。
进一步的，所述惰性保护气为氩气。
进一步的，所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
进一步的，（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨；（2）在惰性气氛下，向步骤（1）的产物中加入结合剂，搅拌20min后，升温至150℃，保温反应30min；（3）经过滤后放入高温氮气炉内于流动氮气保护下先于1200℃保温25min，随后升温至1700℃保温2.5h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
进一步的，所述耐磨石英陶瓷材料产品的耐火温度为1700℃以上，莫氏硬度能达到8.1。将所得到的耐磨石英陶瓷材料产品放在冰水混合液中，10分钟后拿出来，放于80-100℃的热水中，耐磨石英陶瓷材料产品完好无损，没有破裂的情况。
实施例4
一种耐磨石英陶瓷材料，由以下重量份的组分制备而成：
硅微粉 120份
碳酸钡 20份
二硼化钛 11份
氮化铝 15份
氮化硼 13份
氧化锆 5份
氮化硅 13份
滑石粉 9份
陶瓷粉 5份
碳化硅 8份
碳酸氢钠 3份
三氧化二锑 4份
结合剂 7份。
进一步的，所述硅微粉为亚纳米的球形硅微粉。
进一步的，所述结合剂由以下重量份的组分组成：乙酸乙酯9份、水性树脂聚丙烯酰胺3份、聚乙二醇8份。
进一步的，所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
进一步的，所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
进一步的，所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨3~4h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到480℃，保持14min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1500℃，待细硅粉熔融，保持8min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用布袋、旋风或者静电集尘，得到硅微粉。
进一步的，所述惰性保护气为氩气。
进一步的，所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
进一步的，（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨；（2）在惰性气氛下，向步骤（1）的产物中加入结合剂，搅拌18min后，升温至145℃，保温反应40min；（3）经过滤后放入高温氮气炉内于流动氮气保护下先于1100℃保温30min，随后升温至1750℃保温2.5h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
进一步的，所述耐磨石英陶瓷材料产品的耐火温度为1750℃以上，莫氏硬度能达到8.0。将所得到的耐磨石英陶瓷材料产品放在冰水混合液中，10分钟后拿出来，放于80-100℃的热水中，耐磨石英陶瓷材料产品完好无损，没有破裂的情况。
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，这些改进也应视为本发明的保护范围。

Claims (10)

1. 一种耐磨石英陶瓷材料，其特征在于：由以下重量份的组分制备而成：
硅微粉 90-120份
碳酸钡 15-20份
二硼化钛 7-12份
氮化铝 10-15份
氮化硼 10-15份
氧化锆 3-8份
氮化硅 9-13份
滑石粉 8-12份
陶瓷粉 3-8份
碳化硅 5-8份
碳酸氢钠 3-5份
三氧化二锑 2-5份
结合剂 5-10份。
2.根据权利要求1所述的一种耐磨石英陶瓷材料，其特征在于：所述硅微粉为亚纳米的球形硅微粉。
3.根据权利权利要求1所述的一种耐磨石英陶瓷材料，其特征在于：所述结合剂由以下重量份的组分组成：乙酸乙酯6-10份、水性树脂聚丙烯酰胺3-5份、聚乙二醇5-8份。
4.根据权利权利要求1所述的一种耐磨石英陶瓷材料，其特征在于：所述陶瓷粉为白云母、镁铝尖晶石和方解石的粉末。
5.根据权利权利要求4所述的一种耐磨石英陶瓷材料的制备方法，其特征在于：所述陶瓷粉中白云母、镁铝尖晶石、方解石粉末的质量比为6:3:2。
6.根据权利权利要求1所述的一种耐磨石英陶瓷材料，其特征在于：所述硅微粉的制备方法包括如下步骤：（a）硅粉研磨：选取高纯度硅粉浸入研磨液，在研磨盘上研磨3~4h得到细硅粉，彻底清洗除去研磨液；（b）筛分：采用多级筛盘筛分细硅粉，然后选取200-300目的细硅粉置入等离子反应炉中；（c）预反应：将等离子反应炉抽真空至1~3Pa，然后通电加热到450~500℃，保持12~16min；（d）反应：向等离子反应炉中通入惰性保护气，然后升温至1450-1500℃，待细硅粉熔融，保持8~12min后迅速充入氧气；（e）冷却：充入氧气后的熔融细硅粉迅速成为二氧化硅微尘，用引风装置被带入骤冷器进行冷却，形成球形微粒，用旋风集尘，得到硅微粉。
7.根据权利权利要求6所述的一种耐磨石英陶瓷材料，其特征在于：所述步骤（d）的惰性保护气为氩气。
8.根据权利权利要求6所述的一种耐磨石英陶瓷材料，其特征在于：所述步骤（d）的等离子反应炉的升温过程为：先以15~20℃/min、再以7.5~12℃/min、最后以3~5℃/min的速率升温。
9.根据权利要求1-8任意一项所述的一种耐磨石英陶瓷材料的制备方法，其特征在于：包括如下步骤：（1）按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、、氮化硼、氧化锆、氮化硅、滑石粉、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑，加入高压均质机中混合均匀，充分球磨，得到混合料；（2）在惰性气氛下，向步骤（1）的混合料中加入结合剂，搅拌15-20min后，升温至140-150℃，保温反应30-40min；（3）将步骤（2）的混合料放入石墨模具内干压成型，并进行冷等静压处理，压力为100MPa，保压时间30min，得到生坯；（4）将步骤（3）得到的生坯转移至高温氮气炉内于流动氮气保护下先于1000-1200℃保温25-35min，随后升温至1700-1800℃保温2-2.5h进行烧结，待反应冷却后即可得到所述耐磨石英陶瓷材料产品。
10.根据权利要求9所述的一种耐磨石英陶瓷材料，其特征在于：所述耐磨石英陶瓷材料产品的耐火温度为1800℃以上，莫氏硬度能达到8。
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