CN107459342B - 一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料 - Google Patents

一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料 Download PDF

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CN107459342B
CN107459342B CN201710737488.XA CN201710737488A CN107459342B CN 107459342 B CN107459342 B CN 107459342B CN 201710737488 A CN201710737488 A CN 201710737488A CN 107459342 B CN107459342 B CN 107459342B
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magnesite
silicon oxynitride
periclase
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CN107459342A (zh
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王玉霞
徐恩霞
董萌蕾
刘萍
李素萍
邓俊杰
李愿
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Sinosteel luonai Technology Co., Ltd
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Abstract

本发明公开了一种低电磁波吸收率，优异的透波性，高温体积稳定性好，抗热震性好，抗侵蚀优良的微波冶金窑车用方镁石‑氮氧化硅复合耐火材料及其制备方法。原始料的加入重量份数为：镁砂骨料65‑70份、镁砂细粉15‑23份、SiO2微粉2‑6份、Si粉10‑15份，结合剂加入量为原始料总重量的3‑6%。本发明性能如下：体积密度2.8‑2.95g/cm3，常温耐压强度：80‑120MPa，常温抗折强度：15‑25MPa，1400℃时热态抗折强度在5‑10MPa左右，按照YB/T376.1‑1995标准1100℃‑水冷次数为10‑20次，常温介电常数：8‑11，具有良好的抗侵蚀性。

Description

一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料
技术领域
本发明涉及一种微波冶金窑车用耐火材料，尤其涉及一种通过添加Si粉和Si02粉原位反应制备方镁石-氧氮化硅复合耐火材料及其制备方法。
背景技术
随着科技的不断发展，环境保护在生活、生产中得到越来越高的重视。传统重工业特别是金属冶炼等高温工业，迫切需要改变生产方式以适应国家发展要求。微波加热技术的出现使得高温加热有了更节能环保的加热方式，其中用微波加热的方式来冶炼金属被称为绿色冶金，是近年来兴起的新技术。
由于微波冶金技术的出现，微波冶金窑车用耐火材料主要作为承载物料的窑车载体使用，物料在窑车上从窑炉进入，经过微波冶炼后从窑尾出料，由于微波加热的快速升温和出料时窑车直接在室温下卸料，所以对窑车用耐火材料有较高的性能要求：（1）低电磁波吸收率和优异的透波性：一是防止在电磁波作用下耐火材料自身吸收较多的电磁能造成温度过高而对材料造成破坏，二是可以节约能源，使有限的电磁能被冶金物料所吸收，缩短冶炼时间；（2）优良的抗热震性：在微波加热快速升温过程中能抵抗较大的热应力对材料的冲击；（3）良好的高温力学性能：在微波冶金反应过程中炉衬材料要承受各种结构应力机械作用；（4）抗侵蚀性优良：耐火材料在高温下长时间与冶金物料接触，容易与冶金物料发生化学反应导致耐火材料结构被破坏。
目前还没有针对微波冶金用耐火材料系统的研究，如果能够研发制备出符合微波冶金使用的耐火材料，对冶金新技术的进步将起到促进作用。
发明内容
为解决目前耐火材料不能满足微波冶金窑车对其性能的要求，本发明提供一种低电磁波吸收率，优异的透波性，高温体积稳定性好，抗热震性好，抗侵蚀优良的微波冶金窑车用方镁石-氮氧化硅复合耐火材料及其制备方法。
为了实现上述目的，本发明采用的技术方案为：
一种方镁石-氧氮化硅复合耐火材料，原始料为：镁砂骨料和细粉、SiO2微粉、Si粉，采用压制成形方法成形，在N2气氛下通过原位氮化反应烧结制备得到。
本发明原始料的加入重量份数为：镁砂骨料65-70份、镁砂细粉15-23份、SiO2微粉2-6份、Si粉10-15份，结合剂加入量为原始料总重量的3-6%。
所述镁砂骨料为电熔镁砂或烧结镁砂中的一种或两种，粒度≤3mm；
所述镁砂细粉为电熔镁砂或烧结镁砂中的一种或两种，粒度≤0.075mm；
所述SiO2粉为超细天然石英砂粉、硅微粉和气相氧化硅微粉中的一种或两种以上；纯度≥98%，粒径小于10μm；
其中SiO2粉的粒度要求是为了：SiO2粒度达到了微粉级，SiO2粉可充分渗入原料的缝隙中，可以使最终产品的晶相为原位生成的氮氧化硅晶相，因为生成的氮氧化硅晶相具有低电磁波吸收率和优异的透波性。
所述Si粉纯度≥99%，粒度≤0.045mm；
其中Si粉在烧成过程中与氮气反应原位生成氮化硅、氧氮化硅等物相，促进了材料的烧结，提高了复合材料热态强度和透波性的同时，增加了材料的致密度提高抗侵蚀性。Si粉粒度≤0.045mm；目的是为了让硅粉更容易在制备温度下完全氮化形成氮氧化硅。
其中加入的镁砂骨料和细粉是材料的主晶相起骨架作用，基质中的SiO2微粉和Si粉在高温流动氮气中原位生成Si2N2O并与镁砂骨料结合在一起，由于Si粉的过剩及部分超微粉镁砂的存在，基质中除了Si2N2O外还有部分Si3N4和Sialon相生成。Si2N2O等非氧化物晶相呈柱状生长在镁砂骨料表面，不仅提高了最终产品的材料强度及透波性，而且缓冲了材料内部热应力，提高了复合材料的韧性，有利于热震稳定性提高和膨胀系数的降低。
所述结合剂为糊精、聚乙烯醇、羧甲基纤维素、树脂、纸浆废液中的一种或几种复合。
本发明的这种方镁石-氧氮化硅复合耐火材料的制备方法为：
步骤一、先将镁砂细粉15-23份、SiO2微粉2-6份、Si粉10-15份，放入球磨机中按照刚玉球和物料比1:1，在转速为1000~1200rpm下，研磨120-180分钟，得到预混合细粉；
步骤二、将镁砂骨料65-70份倒入混碾机中，然后加入3-6wt%结合剂，打开混碾机搅拌5-10min，使结合剂均匀粘附在镁砂颗粒表面与其润湿，再加入步骤一得到的预混合细粉，搅拌10-20min，使物料充分混合均匀；
步骤三、将混合后的物料装入密封袋中在室温下空气湿度为50-60%的空气气氛中置放12-24h困料；
步骤四、困料后，将混合均匀的物料用液压机在120MPa压力下制成砖坯，将成型后的砖坯在120℃干燥箱中干燥48小时；
步骤五、将干燥后的试样称重后运入氮化炉中，密封炉门通入氮气，在微正压流动氮气气氛下以5-8℃/min的升温速率升温至1100℃，保温2小时后再以1-5℃/min速率升温至1450℃并保温24小时，然后随炉冷却至室温，即可得到方镁石-氧氮化硅复合耐火材料。
其中步骤一先把镁砂细粉、SiO2粉和Si粉进行预混合，目的是为了SiO2粉，Si粉和镁砂细粉能均匀混合，使氮化后形成的短柱状晶体氧氮化硅均匀分布，增强材料的强度和透波性。
其中步骤三目的是为了使其结合剂中的水分均匀分布，改善坯料的成型性能，使砖坯骨料和细粉均匀分布，不产生偏析，从而使最终产品具有低电磁波吸收率和优异的透波性。
其中步骤五中1100℃下保温因为在此温度下氮化反应开始，1450℃长时间保温有利于更多的氮氧化硅生成和材料的进一步烧结。
本发明通过镁砂为基料，引入一定量的氧化硅微粉和硅粉、原料的优化组合、合理的粒度配比、采用高温氮气气氛下原位氮化反应一步烧成制备出方镁石-氮氧化硅复合耐火材料，该材料的主晶相为方镁石和氮氧化硅，有少量β-Si3N4相生成。因此具有优异的透波性，良好的高温体积稳定性、抗热震性和抗侵蚀性能。
本发明采用了原位反应烧成制备方镁石-氮氧化硅复合材料，而不采用直接在原料加入氮氧化硅，这是因为氮氧化硅与方镁石都属于高熔点物相，需要较高的烧成温度或加助烧剂，本发明采用了原位反应烧成制备方镁石-氮氧化硅复合材料，不仅可以降低烧结温度，原位生成的氮氧化硅可以更好与镁砂结合，同时制备过程中生成的少量的β-Si3N4相生成，这些生成物都对材料的透波性，热膨胀及强度有较大的提高。
由于本发明所用的材质主要为镁砂，本发明作为窑车的耐火材料，具有抗碱性渣的侵蚀性好，适用于冶金物料碱性较强的窑炉中使用。
镁质材料是普通冶金过程中常有的耐火材料，对碱性熔渣具有优良的抗侵蚀性，但不足之处是热膨胀系数大, 抗热震性差，因此在快速生降温的微波冶金条件下该材料容易开裂而无法正常使用。氧氮化硅和氮化硅等非氧化物材料热膨胀系数小抗热震性优良，且具有优良的透波性，因此可以通过氮氧化硅与镁质材料的复合，使其优势互补，制备满足微波冶金用的耐火材料。
本发明为了实现氧氮化硅与耐火材料的复合，克服现有方镁石耐火材料性能的不足，开拓氧化物-非氧化物复合材料在微波冶金新领域的应用。
本发明通过引入一定量的氧化硅微粉和硅粉、原料的优化组合、合理的粒度配比、采用原位氮化反应一步烧成制备出了热震稳定性好、透波性好、抗侵蚀优良、生产成本低的方镁石-氧氮化硅复合耐火材料。
本发明所得产品为非氧化物与氧化物的复合材料，通过方镁石-氧氮化硅复合耐火材料中断口形貌图，可以看到短柱状的氧氮化硅与粒状的方镁石结合良好，在材料内部起到缓冲应力的作用，提高了复合材料的韧性，有利于材料热震稳定性提升和膨胀系数的降低。
本发明所述的方镁石-氧氮化硅复合耐火材料的性能如下：体积密度2.8-2.95g/cm3，常温耐压强度：80-120MPa，常温抗折强度：15-25MPa，1400℃时热态抗折强度在5-10MPa左右，按照YB/T376.1-1995标准1100℃-水冷次数为10-20次，常温介电常数：8-11，具有良好的抗侵蚀性。
具体实施方式
下面举例说明本发明的实施及特点，但本发明不局限于下述实施例。
实施例1：
步骤一、先将镁砂细粉15份、SiO2微粉6份、SiO2粉粒径1-5μm ，Si粉10份，放入球磨机中按照刚玉球和物料比1:1，在转速为1000~1200rpm下，研磨120-180分钟，得到预混合细粉；
步骤二、将镁砂骨料69份倒入混碾机中，然后加入6wt%结合剂，打开混碾机搅拌5-10min，使结合剂均匀粘附在镁砂颗粒表面与其润湿，再加入步骤一得到的预混合细粉，搅拌10-20min，使物料充分混合均匀；
步骤三、将混合后的物料装入密封袋中在室温下空气湿度为50-60%的空气气氛中置放12-24h困料；
步骤四、困料后，将混合均匀的物料用液压机在120MPa压力下制成砖坯，将成型后的砖坯在120℃干燥箱中干燥48小时；
步骤五、将干燥后的试样称重后运入氮化炉中，密封炉门通入氮气，在微正压流动氮气气氛下以5-8℃/min的升温速率升温至1100℃，保温2小时后再以1-5℃/min速率升温至1450℃并保温24小时，然后随炉冷却至室温，即可得到方镁石-氧氮化硅复合耐火材料。
所得产品的性能指标为：显气孔率：15.80%，体积密度：2.90g/cm3，常温耐压强度：84.00MPa，常温抗折强度：15.84MPa，1400℃时热态抗折强度：5.67MPa左右，按照YB/T376.1-1995标准1100℃-水冷次数:10次，常温介电常数：8.47，抵抗微波冶炼镍铁矿物料的侵蚀效果最好。
实施例2：
步骤一、先将镁砂细粉20份、SiO2微粉4份、SiO2粉粒径5-8μm， Si粉11份，放入球磨机中按照刚玉球和物料比1:1，在转速为1000~1200rpm下，研磨120-180分钟，得到预混合细粉；
步骤二、将镁砂骨料65份倒入混碾机中，然后加入3wt%结合剂，打开混碾机搅拌5-10min，使结合剂均匀粘附在镁砂颗粒表面与其润湿，再加入步骤一得到的预混合细粉，搅拌10-20min，使物料充分混合均匀；
步骤三、将混合后的物料装入密封袋中在室温下空气湿度为50-60%的空气气氛中置放12-24h困料；
步骤四、困料后，将混合均匀的物料用液压机在120MPa压力下制成砖坯，将成型后的砖坯在120℃干燥箱中干燥48小时；
步骤五、将干燥后的试样称重后运入氮化炉中，密封炉门通入氮气，在微正压流动氮气气氛下以5-8℃/min的升温速率升温至1100℃，保温2小时后再以1-5℃/min速率升温至1450℃并保温24小时，然后随炉冷却至室温，即可得到方镁石-氧氮化硅复合耐火材料。
所得产品的性能指标为：显气孔率：16.2%，体积密度：2.87g/cm3，常温耐压强度：94.32MPa，常温抗折强度：19.53MPa，1400℃时热态抗折强度：8.45MPa，按照YB/T376.1-1995标准1100℃-水冷次数:16次，常温介电常数：10.13，抵抗微波冶炼镍铁矿物料的侵蚀效果最好。
实施例3：
步骤一、先将镁砂细粉15份、SiO2微粉3份、SiO2粉粒径1-10μm， Si粉12份，放入球磨机中按照刚玉球和物料比1:1，在转速为1000~1200rpm下，研磨120-180分钟，得到预混合细粉；
步骤二、将镁砂骨料70份倒入混碾机中，然后加入3-6wt%结合剂，打开混碾机搅拌5-10min，使结合剂均匀粘附在镁砂颗粒表面与其润湿，再加入步骤一得到的预混合细粉，搅拌10-20min，使物料充分混合均匀；
步骤三、将混合后的物料装入密封袋中在室温下空气湿度为50-60%的空气气氛中置放12-24h困料；
步骤四、困料后，将混合均匀的物料用液压机在120MPa压力下制成砖坯，将成型后的砖坯在120℃干燥箱中干燥48小时；
步骤五、将干燥后的试样称重后运入氮化炉中，密封炉门通入氮气，在微正压流动氮气气氛下以5-8℃/min的升温速率升温至1100℃，保温2小时后再以1-5℃/min速率升温至1450℃并保温24小时，然后随炉冷却至室温，即可得到方镁石-氧氮化硅复合耐火材料。
所得产品的性能指标为：显气孔率：17.3%，体积密度：2.81g/cm3，常温耐压强度：118.71MPa，常温抗折强度：24.50MPa，1400℃时热态抗折强度：9.23MPa左右，按照YB/T376.1-1995标准1100℃-水冷次数:27次，常温介电常数：9.07，抵抗微波冶炼镍铁矿物料的侵蚀渗透效果较好。

Claims (4)

1.一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料，其特征在于: 原始料的加入重量份数为：镁砂骨料65-70份、镁砂细粉15-23份、SiO2微粉2-6份、Si粉10-15份，结合剂加入量为原始料总重量的3-6%；SiO2粉为超细天然石英砂粉、硅微粉和气相氧化硅微粉中的一种或两种以上；纯度≥98%，粒径小于10μm； Si粉纯度≥99%，粒度≤0.045mm；制备方法，其特征在于：步骤一、先将镁砂细粉15-23份、SiO2微粉2-6份、Si粉10-15份，放入球磨机中按照刚玉球和物料比1:1，在转速为1000~1200rpm下，研磨120-180分钟，得到预混合细粉；步骤二、将镁砂骨料65-70份倒入混碾机中，然后加入3-6wt%结合剂，打开混碾机搅拌5-10min，使结合剂均匀粘附在镁砂颗粒表面与其润湿，再加入步骤一得到的预混合细粉，搅拌10-20min，使物料充分混合均匀；步骤三、将混合后的物料装入密封袋中在室温下空气湿度为50-60%的空气气氛中置放12-24h困料；步骤四、困料后，将混合均匀的物料用液压机在120MPa压力下制成砖坯，将成型后的砖坯在120℃干燥箱中干燥48小时；步骤五、将干燥后的试样称重后运入氮化炉中，密封炉门通入氮气，在微正压流动氮气气氛下以5-8℃/min的升温速率升温至1100℃，保温2小时后再以1-5℃/min速率升温至1450℃并保温24小时，然后随炉冷却至室温，即可得到方镁石-氧氮化硅复合耐火材料；其主晶相为方镁石和氮氧化硅，有β-Si3N4相生成；适用于冶金物料碱性较强的微波冶金窑车使用。
2.根据权利要求1所述的一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料，其特征在于：镁砂骨料为电熔镁砂或烧结镁砂中的一种或两种，粒度≤3mm。
3.根据权利要求1所述的一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料，其特征在于：镁砂细粉为电熔镁砂或烧结镁砂中的一种或两种，粒度≤0.075mm。
4.根据权利要求1所述的一种微波冶金窑车用方镁石-氧氮化硅复合耐火材料，其特征在于：结合剂为糊精、聚乙烯醇、羧甲基纤维素、树脂、纸浆废液中的一种或几种复合。
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