CN106588024A - 一种Al7O3N5结合刚玉质复合耐火材料的制备方法 - Google Patents

一种Al7O3N5结合刚玉质复合耐火材料的制备方法 Download PDF

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CN106588024A
CN106588024A CN201710007248.4A CN201710007248A CN106588024A CN 106588024 A CN106588024 A CN 106588024A CN 201710007248 A CN201710007248 A CN 201710007248A CN 106588024 A CN106588024 A CN 106588024A
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李勇
秦海霞
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Abstract

本发明属于无机非金属材料领域，涉及Al7O3N5结合刚玉质耐火材料的制备方法，用于炼铁高炉、炼钢钢包、炉外精炼炉和水泥窑用耐火材料的领域。本发明采用烧结刚玉、电熔刚玉、活性氧化铝微粉作为原料，添加沥青作为结合剂，经压制成型后氮化烧结而成。原料简单易得，无需添加稀有金属氧化物、金属Al等添加剂；合成时无需添加Al7O3N5作为晶核；伴随着Al7O3N5的形成将，碳以CO气相移除，可制备出低碳的材料；所制备的Al7O3N5呈相互交错的片状，可大大提高耐火材料的强度、抗侵蚀性、抗氧化性等性能。该方法原料来源广泛、价格较低、工艺简单，可实现大规模工业化推广。

Description

一种Al7O3N5结合刚玉质复合耐火材料的制备方法
技术领域
本发明属于无机非金属材料领域，涉及Al7O3N5结合刚玉质耐火材料的制备方法，用于炼铁高炉、炼钢钢包、炉外精炼炉和水泥窑用耐火材料的领域。
根据晶体结构，人们将Al2O3-AlN二元系的AlON固溶体分为纤维锌矿和尖晶石两大类。目前对于AlON的研究主要集中在尖晶石型领域，对于纤维锌矿型的AlON，人们将其称为多型体。Al7O3N5即为一种纤维锌矿结构的AlON多型体。AlON具有高硬度、高熔点、高热传导率和优异的抗化学侵蚀性以及抗氧化性能，其应用范围很广，尤其是高温材料领域和透明材料领域。AlON陶瓷材料的制备方法主要是以Al2O3和AlN为原料，在高温热压的条件下或者通过添加稀有金属添加剂；或者金属Al、Al2O3为原料，进行氮化烧成制备AlON陶瓷。这两种方法的成本都较高，前者由于高温热压条件难以在工业上实现，稀有金属较为昂贵；后者由于金属铝成本较高、且保存时有爆炸的危险，因此这两种方法都难以实现大规模工业化推广。此外还有一种应用较广的制备方法为碳热还原氮化Al2O3制备AlON陶瓷，该方法采用Al2O3粉和石墨或者碳粉作为原料，无需加入添加剂，通过无压烧结即可制备AlON陶瓷。然而该方法的难点在于Al2O3/C的比例难以控制，C含量太少Al2O3不能完全转化为AlON；C含量太多会将Al2O3还原为AlN。因此，为控制反应，人们往往通过多步合成法，先在较低温度合成AlN，再添加Al2O3合成AlON；而且为降低材料中最终的C含量，需要最终采用除碳工艺移除多余的C。
通常为合成AlON增强的耐火材料，人们通常先合成AlON粉或者添加商业AlON粉；或者添加稀有金属添加剂，可制备出抗铁水侵蚀、抗碱侵蚀性能优越的高强度耐火材料。由于热力学数据缺失、相图尚有争议，关于Al7O3N5研究较少，Al7O3N5结合刚玉耐火材料的制备也鲜有报道。
发明内容
针对现有技术中Al7O3N5结合刚玉耐火材料制备方法有限，成本较高的缺陷不足，本发明提供了一种可用于炼铁高炉、炼钢钢包、炉外精炼炉和水泥窑耐火材料的制备方法。
一种Al7O3N5结合刚玉质复合耐火材料的制备方法，本发明以烧结刚玉颗粒、电熔刚玉粉、活性氧化铝微粉作为原料，另外添加沥青作为结合剂，将原料混合后进行混炼，经压制成型，在流动氮气中烧结，氮化烧结后自然冷却。烧成过程中，沥青高温烧结后的残炭对活性Al2O3微粉碳热还原氮化，在烧结过程中，原位合成基质中的活性氧化铝微粉经反应形成片状的Al7O3N5，其微观结构呈互相交织的层片状，作为结合相增强刚玉质材料。
沥青高温烧结后的残炭对活性Al2O3微粉碳热还原氮化，在烧结过程中原位合成，其微观结构呈互相交织的层片状，可增强耐火材料基质。
进一步的所述烧结刚玉颗粒粒径为3-1mm，1-0mm，质量百分数分别为40-50％，10-20％，电熔刚玉粉粒径小于88μm，质量百分数为15-25％，活性氧化铝微粉粒径为5-20μm，质量百分数为5-25％，结合剂沥青质量百分数为3-5％。
进一步的压制成型压力为15-40MPa，氮气纯度为不小于99.99％，氮化烧结温度1350-1550℃，氮化时间8-24h。
本发明所制备的Al7O3N5结合刚玉质复合耐火材料的性能气孔率12-20％，体积密度3.00-3.30g/cm3，常温耐压强度120-300MPa。
本发明的基本构思是以沥青作为结合剂，在烧结过程中沥青分解的残碳，作用与氧化铝，形成Al7O3N5增强相，得到一种低碳的高性能的耐火材料。突破了传统碳热还原法使用石墨、炭黑的局限。与其他制备方法相比，原料简单易得，无需添加稀有金属氧化物、金属Al等添加剂；合成时无需添加Al7O3N5作为晶核；随着Al7O3N5的形成，碳将以CO气相移除，得到低碳的材料；所制备的Al7O3N5呈相互交错的片状，可大大提高耐火材料的强度、抗侵蚀性、抗氧化性等性能。该方法原料来源广泛、价格较低、工艺简单，可实现大规模工业化推广。
具体实施方式
取粒径为3-1mm，1-0mm的烧结刚玉颗粒，以及粒径小于88μm的电熔刚玉粉，粒径为5-20μm的活性氧化铝微粉，其质量百分数分别为40-50％，10-20％，15-25％，5-25％为原料，另外添加3-5％的沥青作为结合剂。将原料混合后进行混炼，在15-40MPa下压制成型。将压制成型后的试样放入烧结炉中，通纯度为不小于99.99％氮气，在1350-1550℃进行氮化8-24h后自然冷却。
实例1
取粒径为3-1mm，1-0mm的烧结刚玉颗粒，以及粒径小于88μm的电熔刚玉粉，粒径为5-20μm的活性氧化铝微粉，其质量百分数分别为40％，20％，15％，25％为原料，另外添加3％的沥青作为结合剂。将原料混合后进行混炼，在15MPa下压制成型。将压制成型后的试样放入烧结炉中，通纯度为不小于99.99％氮气，在1500℃进行氮化24h后自然冷却。
实例2
取粒径为3-1mm，1-0mm的烧结刚玉颗粒，以及粒径小于88μm的电熔刚玉粉，粒径为5-20μm的活性氧化铝微粉，其质量百分数分别为50％，10％，25％，15％为原料，另外添加5％的沥青作为结合剂。将原料混合后进行混炼，在40MPa下压制成型。将压制成型后的试样放入烧结炉中，通纯度为不小于99.99％氮气，在1450℃进行氮化24h后自然冷却。
实例3：
取粒径为3-1mm，1-0mm的烧结刚玉颗粒，以及粒径小于88μm的电熔刚玉粉，粒径为5-20μm的活性氧化铝微粉，其质量百分数分别为40％，20％，15％，25％为原料，另外添加5％的沥青作为结合剂。将原料混合后进行混炼，在30MPa下压制成型。将压制成型后的试样放入烧结炉中，通纯度为不小于99.99％氮气，在1550℃进行氮化12h后自然冷却。

Claims (4)

1.一种Al7O3N5结合刚玉质复合耐火材料的制备方法，其特征在于以烧结刚玉颗粒、电熔刚玉粉、活性氧化铝微粉作为原料，另外添加沥青作为结合剂，将原料混合后进行混炼，经压制成型，在流动氮气中烧结，氮化烧结后自然冷却。烧成过程中，沥青高温烧结后的残炭对活性Al2O3微粉碳热还原氮化，在烧结过程中，原位合成基质中的活性氧化铝微粉经反应形成片状的Al7O3N5，其微观结构呈互相交织的层片状，作为结合相增强刚玉质材料。
2.根据权利要求1所述的Al7O3N5结合刚玉质复合耐火材料，其特征在于所述烧结刚玉颗粒粒径为3-1mm，1-0mm，质量百分数分别为40-50％，10-20％，电熔刚玉粉粒径小于88μm，质量百分数为15-25％，活性氧化铝微粉粒径为5-20μm，质量百分数为5-25％，结合剂沥青质量百分数为3-5％。
3.根据权利要求1所述的Al7O3N5结合刚玉质复合耐火材料，其特征在于所述压制成型压力为15-40MPa，氮气纯度为不小于99.99％，氮化烧结温度1350-1550℃，氮化时间8-24h。
4.根据权利要求1所述的Al7O3N5结合刚玉质复合耐火材料，其特征在于所制备Al7O3N5结合刚玉质复合耐火材料的性能气孔率12-20％，体积密度3.00-3.30g/cm3，常温耐压强度120-300MPa。
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Cited By (2)

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CN110997596A (zh) * 2017-10-04 2020-04-10 里弗雷克特里知识产权两合公司 用于制造耐火产品的批料、制造耐火产品的方法、耐火产品以及合成原材料的用途
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EP3564201A4 (en) * 2016-12-28 2020-08-19 Krosakiharima Corporation BRICK FOR FURNACES AND FURNACES AS WELL AS A PROCESS FOR MANUFACTURING BRICK FOR FURNACES
CN110997596A (zh) * 2017-10-04 2020-04-10 里弗雷克特里知识产权两合公司 用于制造耐火产品的批料、制造耐火产品的方法、耐火产品以及合成原材料的用途
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