CN111056833B - 一种氮化物结合的尖晶石滑板及其制备工艺 - Google Patents

一种氮化物结合的尖晶石滑板及其制备工艺 Download PDF

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CN111056833B
CN111056833B CN201911220941.5A CN201911220941A CN111056833B CN 111056833 B CN111056833 B CN 111056833B CN 201911220941 A CN201911220941 A CN 201911220941A CN 111056833 B CN111056833 B CN 111056833B
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spinel
powder
magnesium aluminate
nitride
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CN111056833A (zh
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陈松林
蒋正跃
刘士范
王俊涛
胡小成
闫昕
孙旭东
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Ruitai Technology Co ltd
YIXING REFRACTORY MATERIAL CO Ltd
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Abstract

本发明涉及一种氮化物结合尖晶石滑板及其制备工艺。以镁铝尖晶石为主要材料，加入金属硅粉或金属铝粉的一种或两种，在氮化气氛中高温烧成，金属硅粉和金属铝粉经氮化生成氮化硅和氮化铝，氮化硅和氮化铝和原料中的氧化铝、氧化镁或镁铝尖晶石反应原位反应，最后形成氮化硅、氮化铝、塞隆、阿隆、镁阿隆等氮化物中的一种或多种氮化物结合尖晶石质滑板。本发明突出优点是产品的力学强度高、高温抗折强度高、抗侵蚀性能好、抗热震性好，适用于各种钢种的冶炼和浇铸过程，且不对钢水有增碳污染。

Description

一种氮化物结合的尖晶石滑板及其制备工艺
技术领域
本发明属于无机非金属材料学科高温陶瓷和耐火材料领域，具体涉及一种氮化物结合尖晶石滑板及其制备工艺。
背景技术
在镁铝尖晶石构造中，Al-O、Mg-O之间都是较强的离子键，且静电键强度相等，结构牢固。因此，镁铝尖晶石晶体的饱和结构具有良好的耐化学侵蚀性和耐磨性，能够在氧化或还原气氛中保持较好的稳定性。镁铝尖晶石具有良好的耐高温、抗渣侵蚀、抗剥落性能，广泛用于耐火材料、钢铁冶炼，水泥回转窑及玻璃工业窑炉。碳结合的铝碳质及铝锆碳质滑板两种滑板抗Ca侵蚀能力差，难以适应特种钢连铸的要求，尖晶石质材料比氧化铝质适用性更广，碳结合的镁铝尖晶石滑板能适应钙处理钢、高氧钢、优质钢、沸腾钢、镇静钢、半镇静钢等特种钢连铸的要求。虽然能够满足生产的各项安全指标，但无法避免在连铸过程中对钢水增碳，影响洁净钢的质量。然而，碳结合材质无法避免在连铸过程中对钢水增碳，影响洁净钢的质量，本发明为了克服上述技术难题，开发出一种非碳结合的碱性滑板，以满足洁净钢的特种钢种需求。
发明内容
本发明涉及一种氮化物结合尖晶石滑板，原料配方以重量百分比计为：
（1）粒度4～2mm的镁铝尖晶石，25~33%；
（2）粒度2～1mm的镁铝尖晶石，20~30%；
（3）粒度1～0mm的镁铝尖晶石，22~33%；
（4）粒度≤0.088mm的镁铝尖晶石，13~18%；
（5）粒度0.002~0.005mm的富铝尖晶石A90，7~11%；
（6）粒度0.002~0.005mm的金属硅粉，7~15%；
（7）粒度0.002~0.005mm的金属铝粉，0~1%
（8）粒度0.002~0.005mm的α-Al2O3粉，2~3%
（9）粒度≤0.045mm碳化硼，0.5%；
（10）粒度≤0.045mm氮化硼，0.5%；
（11）糊精粉，2~3%；
（12）外加纸浆废液，+3~4%；
（13）氮气；
所述的原料（12）纸浆废液另外加入，不计入原料总质量百分比内；
原料（13）氮气气体用在烧成时的气氛炉内，不计入原料总重量百分比内，反应炉内保持0.2~0.4MPa的氮气气体压力。
上述氮化物结合尖晶石滑板的制备工艺，主要包括如下制备步骤：
（1）按比例称量粒度≤0.088mm的镁铝尖晶石、粒度0.002~0.005mm的富铝尖晶石A90、粒度0.002~0.005mm的金属硅粉、粒度0.002~0.005mm的金属铝粉、粒度0.002~0.005mm的α-Al2O3粉、粒度≤0.045mm碳化硼、粒度≤0.045mm氮化硼、糊精粉，进行强力预混，预混时间在15～20min，获得预混细粉料；
（2）按比例称量粒度4～2mm的镁铝尖晶石、粒度2～1mm的镁铝尖晶石，进行干混2~3min；然后加入纸浆废液，混合2~3min；再加入粒度1～0mm的镁铝尖晶石，混料2~3min，最后加入预混细粉料，强力混碾15～30min；
（3）密闭困料24～36h；
（4）压制成型；
（5）自然干燥24～48h后，再在120～140℃干燥24～48h；
（6）装入气氛炉内烧成，通0.2~0.4MPa压力的氮气气体，在1550～1650℃保温5~8h；
（7）烧成后自然冷却后磨削，打箍。
由于氮化硅、氮化铝、塞隆、阿隆、镁阿隆等氮化物具有很高的抗弯强度和断裂韧性，且对金属液体的润湿性差，在耐火材料中添加这些氮化物能大大增加材料的抗渣侵蚀性能。本发明就是在镁铝尖晶石为主要的原材料中，掺入金属硅粉或金属铝粉的一种或两种，在氮化气氛中高温烧成，金属硅粉和金属铝粉经氮化生成氮化硅和氮化铝，氮化硅和氮化铝和原料中的氧化铝、氧化镁或镁铝尖晶石反应原位反应，获得氮化硅、氮化铝、塞隆、阿隆、镁阿隆等氮化物中的一种或多种氮化物结合尖晶石滑板。该种产品性能突出优点是滑板砖的力学强度高、高温抗折强度高、抗侵蚀性能好、抗热震性好，适用于各种钢种的冶炼和浇铸过程，且不对钢水有增碳的污染。
实施例1
原料规格和配方（重量百分含量）如下：
（1）粒度4～2mm的镁铝尖晶石，25%；
（2）粒度2～1mm的镁铝尖晶石，27%；
（3）粒度1～0mm的镁铝尖晶石，22%；
（4）粒度≤0.088mm的镁铝尖晶石，2%；
（5）粒度0.002~0.005mm的富铝尖晶石（A90），9%；
（6）粒度0.002~0.005mm的α-Al2O3粉，3%
（7）粒度0.002~0.005mm的金属硅粉，7%；
（8）粒度0.002~0.005mm的金属铝粉，1%
（9）粒度≤0.045mm碳化硼，0.5%；
（10）粒度≤0.045mm氮化硼，0.5%；
（11）高岭土，3%；
（12）外加纸浆废液，+3%；
（13）氮气。
原料（12）纸浆废液另外加入，不计入原料总质量百分比内。原料（13）氮气气体用在烧成时的气氛炉内，不计入原料总重量百分比内，反应炉内保持0.2MPa的氮气气体压力。
本发明的具体工艺过程包括以下几部分：
（1）按比例称量粒度≤0.088mm的镁铝尖晶石、粒度0.002~0.005mm的富铝尖晶石（A90）、粒度0.002~0.005mm的金属硅粉、粒度0.002~0.005mm的金属铝粉、粒度0.002~0.005mm的α-Al2O3粉、粒度≤0.045mm碳化硼、粒度≤0.045mm氮化硼、高岭土，进行强力预混，预混时间在15min。获得预混细粉料。
（2）按比例称量粒度4～2mm的镁铝尖晶石、粒度2～1mm的镁铝尖晶石，进行干混2min。然后加入加入纸浆废液，混合2min。再加入粒度1～0mm的镁铝尖晶石，混料2min。最后加入预混细粉料，强力混碾15min。
（3）密闭困料24h。
（4）压制成型。
（5）自然干燥24h后，再在120℃干燥24h。
（6）装入气氛炉内烧成，通0.2MPa压力的氮气气体，在1650℃保温3h。
（7）烧成后自然冷却后磨削，打箍。
表1列出了本实施例的原料规格和配方及其性能。性能测试结果表明氮化物结合尖晶石滑板在低温时耐压强度较高，达196MPa；在1400℃高温耐压强度较高变化很小，仍然163MPa。其抗折强度在常温时38MPa，在1100℃高温抗折强度35 MPa，说明发明的氮化物结合尖晶石滑板的强度对温度的敏感性很低。其抗热震性能也较好，1100℃×0.5h时抗热震次数达8次。应用于某山钢厂浇铸温度1620～1650℃，钙处理钢水，连滑5次。
实施例2
原料规格和配方（重量百分含量）如下：
（1）粒度4～2mm的镁铝尖晶石，28%；
（2）粒度2～1mm的镁铝尖晶石，18%；
（3）粒度1～0mm的镁铝尖晶石，19%；
（4）粒度≤0.088mm的镁铝尖晶石，5%；
（5）粒度0.002~0.005mm的富铝尖晶石（A90），13%；
（6）粒度0.002~0.005mm的α-Al2O3粉，3%
（7）粒度0.002~0.005mm的金属硅粉，9%；
（8）粒度0.002~0.005mm的金属铝粉，1%
（9）粒度≤0.045mm碳化硼，0.5%；
（10）粒度≤0.045mm氮化硼，0.5%；
（11）高岭土，3%；
（12）外加纸浆废液，+3%；
（13）氮气。
原料（12）纸浆废液另外加入，不计入原料总质量百分比内。原料（13）氮气气体用在烧成时的气氛炉内，不计入原料总重量百分比内，反应炉内保持0.3MPa的氮气气体压力。
本发明的具体工艺过程包括以下几部分：
（1）按比例称量粒度≤0.088mm的镁铝尖晶石、粒度0.002~0.005mm的富铝尖晶石（A90）、粒度0.002~0.005mm的金属硅粉、粒度0.002~0.005mm的金属铝粉、粒度0.002~0.005mm的α-Al2O3粉、粒度≤0.045mm碳化硼、粒度≤0.045mm氮化硼、高岭土，进行强力预混，预混时间在15min。获得预混细粉料。
（2）按比例称量粒度4～2mm的镁铝尖晶石、粒度2～1mm的镁铝尖晶石，进行干混2min。然后加入加入纸浆废液，混合3min。再加入粒度1～0mm的镁铝尖晶石，混料3min。最后加入预混细粉料，强力混碾20min。
（3）密闭困料24h。
（4）压制成型。
（5）自然干燥24h后，再在120℃干燥24h。
（6）装入气氛炉内烧成，通0.3MPa压力的氮气气体，在1600℃保温6h。
（7）烧成后自然冷却后磨削，打箍。
表1列出了本实施例的原料规格和配方及其性能。性能测试结果表明氮化物结合尖晶石滑板在低温时耐压强度较高，达198MPa；在1400℃高温耐压强度较高变化很小，仍然166MPa。其抗折强度在常温时39MPa，在1100℃高温抗折强度35 MPa，说明发明的氮化物结合尖晶石滑板的强度对温度的敏感性很低。其抗热震性能也较好，1100℃×0.5h时抗热震次数达8次。应用于某武钢厂300吨氧气顶吹钢包，浇铸硅钢品种钢，连滑5次。
实施例3
原料规格和配方（重量百分含量）如下：
（1）粒度4～2mm的镁铝尖晶石，33%；
（2）粒度2～1mm的镁铝尖晶石，9%；
（3）粒度1～0mm的镁铝尖晶石，15%；
（4）粒度≤0.088mm的镁铝尖晶石，8%；
（5）粒度0.002~0.005mm的富铝尖晶石（A90），18%；
（6）粒度0.002~0.005mm的α-Al2O3粉，2%
（7）粒度0.002~0.005mm的金属硅粉，11%；
（8）粒度0.002~0.005mm的金属铝粉，0%
（9）粒度≤0.045mm碳化硼，0.5%；
（10）粒度≤0.045mm氮化硼，0.5%；
（11）高岭土，3%；
（12）外加纸浆废液，+4%；
（13）氮气。
原料（12）纸浆废液另外加入，不计入原料总质量百分比内。原料（13）氮气气体用在烧成时的气氛炉内，不计入原料总重量百分比内，反应炉内保持0.4MPa的氮气气体压力。
本发明的具体工艺过程包括以下几部分：
（1）按比例称量粒度≤0.088mm的镁铝尖晶石、粒度0.002~0.005mm的富铝尖晶石（A90）、粒度0.002~0.005mm的金属硅粉、粒度0.002~0.005mm的金属铝粉、粒度0.002~0.005mm的α-Al2O3粉、粒度≤0.045mm碳化硼、粒度≤0.045mm氮化硼、高岭土，进行强力预混，预混时间在20min。获得预混细粉料。
（2）按比例称量粒度4～2mm的镁铝尖晶石、粒度2～1mm的镁铝尖晶石，进行干混3min。然后加入加入纸浆废液，混合3min。再加入粒度1～0mm的镁铝尖晶石，混料3min。最后加入预混细粉料，强力混碾20min。
（3）密闭困料36h。
（4）压制成型。
（5）自然干燥48h后，再在140℃干燥24h。
（6）装入气氛炉内烧成，通0.4MPa压力的氮气气体，在1550℃保温10h。
（7）烧成后自然冷却后磨削，打箍。
表1列出了本实施例的原料规格和配方及其性能。性能测试结果表明氮化物结合尖晶石滑板在低温时耐压强度较高，达218MPa；在1400℃高温耐压强度较高变化很小，仍然179MPa。其抗折强度在常温时49MPa，在1100℃高温抗折强度43MPa，说明发明的氮化物结合尖晶石滑板的强度对温度的敏感性很低。其抗热震性能也较好，1100℃×0.5h时抗热震次数达10次。应用于某港钢厂浇铸温度1550～1650℃，经钙处理钢水，连滑6次。
表1氮化物结合尖晶石滑板的实施实例的原料规格、配方及其性能对照表
Figure 272137DEST_PATH_IMAGE002

Claims (2)

1.一种氮化物结合尖晶石滑板，原料配方以重量百分比计为：
（1）粒度4～2mm的镁铝尖晶石，25~33%；
（2）粒度2～1mm的镁铝尖晶石，20~30%；
（3）粒度1～0mm的镁铝尖晶石，22~33%；
（4）粒度≤0.088mm的镁铝尖晶石，13~18%；
（5）粒度0.002~0.005mm的富铝尖晶石A90，7~11%；
（6）粒度0.002~0.005mm的金属硅粉，7~15%；
（7）粒度0.002~0.005mm的金属铝粉，0~1%
（8）粒度0.002~0.005mm的α-Al2O3粉，2~3%
（9）粒度≤0.045mm碳化硼，0.5%；
（10）粒度≤0.045mm氮化硼，0.5%；
（11）糊精粉，2~3%；
（12）外加纸浆废液，3~4%；
（13）氮气；
所述的原料（12）纸浆废液另外加入，不计入原料总质量百分比内；
原料（13）氮气气体用在烧成时的气氛炉内，不计入原料总重量百分比内，反应炉内保持0.2~0.4MPa的氮气气体压力。
2.一种权利要求1所述的氮化物结合尖晶石滑板的制备工艺，主要包括如下制备步骤：
（1）按比例称量粒度≤0.088mm的镁铝尖晶石、粒度0.002~0.005mm的富铝尖晶石A90、粒度0.002~0.005mm的金属硅粉、粒度0.002~0.005mm的金属铝粉、粒度0.002~0.005mm的α-Al2O3粉、粒度≤0.045mm碳化硼、粒度≤0.045mm氮化硼、糊精粉，进行强力预混，预混时间在15～20min，获得预混细粉料；
（2）按比例称量粒度4～2mm的镁铝尖晶石、粒度2～1mm的镁铝尖晶石，进行干混2~3min；然后加入纸浆废液，混合2~3min；再加入粒度1～0mm的镁铝尖晶石，混料2~3min，最后加入预混细粉料，强力混碾15～30min；
（3）密闭困料24～36h；
（4）压制成型；
（5）自然干燥24～48h后，再在120～140℃干燥24～48h；
（6）装入气氛炉内烧成，通0.2~0.4MPa压力的氮气气体，在1550～1650℃保温5~8h；
（7）烧成后自然冷却后磨削，打箍。
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