CN105967706B - 一种烧结锆刚玉耐火原料及其制备方法 - Google Patents
一种烧结锆刚玉耐火原料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种烧结锆刚玉耐火原料及其制备方法。其技术方案是:按氧化铝粉∶成球液体的质量比为1∶(0.16~0.22),将氧化铝粉置于成球机中,喷入成球液体,制得直径为18~28mm的坯球;将坯球送入高温竖窑的干燥室,在450~650℃条件下干燥70~100分钟,再送入高温竖窑的烧成室,在1850~1900℃条件下保温25~45分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。成球液体的制备方法是:以86~92wt%的氯氧化锆、4~9wt%的钙盐或镁盐、1~6.5wt%的氯化钇和0.5~3wt%的氯化铈为原料,按固液比为40~120g/L向原料中加入水,搅拌至澄清。本发明成本低廉和适于工业化生产,所制备的烧结锆刚玉耐火原料结构均匀和抗热震稳定性优良。
Description
技术领域
本发明属于刚玉耐火材料技术领域。具体涉及一种烧结锆刚玉耐火原料及其制备方法。
背景技术
刚玉质耐火材料由于具有一系列优异的高温性能,广泛应用于钢铁、铸造、陶瓷等行业,其中在钢铁行业的应用几乎涵盖了炼铁炼钢的全过程。但在某些工作环境苛刻部位,依然亟待进一步改善刚玉质耐火材料的抗热震稳定性。
近年来,各国学者提出了ZrO2不同的增韧机理,主要包括:1)相变增韧机理;2)微裂纹增韧机理;3)弥散增韧机理。依据上述ZrO2的增韧机理,在陶瓷领域,人们采用多相悬浮液混合法、溶胶-悬浮液混合法、溶胶-凝胶法、沉淀法、水热合成法等方法制备了氧化锆增韧氧化铝陶瓷,并在切削加工用刀具、耐磨部件、生物医用材料等领域获得广泛应用。但是上述方法制备的氧化锆增韧氧化铝陶瓷产量低、成本高,无法规模化制备耐火原料。在耐火材料领域,人们采用电熔的方法制备了电熔锆刚玉耐火原料,将电熔锆刚玉加入耐火材料中,提高了材料的断裂韧性及抗热震稳定性,使材料在滑板、水口、流道、玻璃炉窑等环境苛刻部位取得了较好的使用效果。但现行生产的电熔锆刚玉耐火原料存在以下主要问题:1)制备过程能耗大,加上ZrO2添加量较多,使得原料的制备成本较高;2)原料中ZrO2晶粒尺寸较大(一般在50μm以上),且分布不均匀,无法充分发挥ZrO2的增韧效果。
发明内容
本发明旨在克服现有技术缺陷,目的在于提供一种成本低廉和适于工业化生产的烧结锆刚玉耐火原料的制备方法,用该方法制备的烧结锆刚玉耐火原料结构均匀和抗热震稳定性优良。
为实现上述目的,本发明采用的技术方案是:按氧化铝粉∶成球液体的质量比为1∶(0.16~0.22),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为18~28mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在450~650℃条件下干燥70~100分钟,然后送入高温竖窑的烧成室中,在1850~1900℃条件下保温25~45分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以86~92wt%的氯氧化锆、4~9wt%的钙盐或镁盐、1~6.5wt%的氯化钇和0.5~3wt%的氯化铈为原料,按固液比为40~120g/L向原料中加入水,搅拌至澄清,即得成球液体。
所述氧化铝粉为工业氧化铝粉和α-氧化铝微粉中的一种,氧化铝粉的Al2O3含量>99.4 wt%。
所述钙盐为氯化钙和硝酸钙中的一种或两种。
所述镁盐为氯化镁和硝酸镁中的一种或两种。
所述氯化钇的YCl3含量>99.2 wt%,粒径<100μm。
所述氯化铈的CeCl3含量>99.5 wt%,粒径<100μm。
由于采用上述技术方案,本发明与现有技术相比具有如下积极效果:
本发明制备的烧结锆刚玉耐火原料是以溶液的形式引入氧化锆和复合稳定剂,引入量较少,工艺简单易操作,故生产成本低廉,适合规模化生产。以溶液的形式引入氧化锆,还能解决氧化锆在氧化铝基体中团聚的问题,使得氧化锆晶粒细小,在基体中均匀分布;引入的复合稳定剂对氧化锆具有很好的稳定效果,使绝大部分氧化锆以四方相形式存在,充分发挥了氧化锆的增韧效果。此外,烧结过程中部分固溶于ZrO2中的CaO或MgO会与Al2O3反应,在ZrO2晶粒表面分别生成六铝酸钙环或镁铝尖晶石环,同时基体中会形成微裂纹,进一步提高所制备的烧结锆刚玉耐火原料的抗热冲击能力,故具有优良的抗热震稳定性。
本发明所制得的烧结锆刚玉耐火原料经检测:体积密度为3.54~3.68g/cm3;显气孔率为2.2~4.8%;吸水率为0.6~1.2%;Al2O3晶粒尺寸为20~100μm;ZrO2晶粒尺寸为0.5~10μm;断裂韧性为9.5~14.5Mpa·m0.5。
因此,本发明所制备的烧结锆刚玉耐火原料具有成本低廉、结构均匀、抗热震稳定性优良和适于工业化生产的特点。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述,并非对其保护范围的限制:
为避免重复,先将本具体实施方式所涉及的原料技术参数统一描述如下,实施例中不再赘述:
所述氧化铝粉为工业氧化铝粉和α-氧化铝微粉中的一种,氧化铝粉的Al2O3含量>99.4 wt%。
所述钙盐为氯化钙和硝酸钙中的一种或两种。
所述镁盐为氯化镁和硝酸镁中的一种或两种。
所述氯化钇的YCl3含量>99.2 wt%,粒径<100μm。
所述氯化铈的CeCl3含量>99.5 wt%,粒径<100μm。
实施例1
一种烧结锆刚玉耐火原料及其制备方法。按工业氧化铝粉∶成球液体的质量比为1∶(0.16~0.18),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为18~25mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在450~500℃条件下干燥70~80分钟,然后送入高温竖窑的烧成室中,在1850~1870℃条件下保温25~30分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以86~88wt%的氯氧化锆、7~9wt%的氯化钙、1~3wt%的氯化钇和2~3wt%的氯化铈为原料,按固液比为40~60g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例1所制得的烧结锆刚玉耐火原料经检测:体积密度为3.54~3.58g/cm3,显气孔率为4.2~4.8%,吸水率为1.0~1.2%,Al2O3晶粒尺寸为20~70μm,ZrO2晶粒尺寸为0.5~7μm,断裂韧性为9.5~11.5Mpa·m0.5。
实施例2
一种烧结锆刚玉耐火原料及其制备方法。按α-氧化铝粉∶成球液体的质量比为1∶(0.17~0.19),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为19~26mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在500~550℃条件下干燥80~90分钟,然后送入高温竖窑的烧成室中,在1870~1890℃条件下保温30~35分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以88~90wt%的氯氧化锆、5~7wt%的硝酸钙、3~5wt%的氯化钇和1~2wt%的氯化铈为原料,按固液比为60~80g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例2所制得的烧结锆刚玉耐火原料经检测:体积密度为3.58~3.62g/cm3;显气孔率为3.6~4.2%;吸水率为0.9~1.1%;Al2O3晶粒尺寸为20~90μm;ZrO2晶粒尺寸为2~8μm;断裂韧性为10.5~12.5Mpa·m0.5。
实施例3
一种烧结锆刚玉耐火原料及其制备方法。按α-氧化铝粉∶成球液体的质量比为1∶(0.18~0.20),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为20~27mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在550~600℃条件下干燥90~100分钟,然后送入高温竖窑的烧成室中,在1880~1900℃条件下保温35~40分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以90~92wt%的氯氧化锆、4~6wt%的氯化镁、4.5~6.5wt%的氯化钇和0.5~1.5wt%的氯化铈为原料,按固液比为80~100g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例3所制得的烧结锆刚玉耐火原料经检测:体积密度为3.64~3.68g/cm3;显气孔率为2.2~2.8%;吸水率为0.6~0.8%;Al2O3晶粒尺寸为30~100μm;ZrO2晶粒尺寸为3~10μm;断裂韧性为11.5~13.5Mpa·m0.5。
实施例4
一种烧结锆刚玉耐火原料及其制备方法。按工业氧化铝粉∶成球液体的质量比为1∶(0.19~0.21),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为21~28mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在600~650℃条件下干燥75~85分钟,然后送入高温竖窑的烧成室中,在1860~1880℃条件下保温40~45分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以87~89wt%的氯氧化锆、6~8wt%的硝酸镁、2~4wt%的氯化钇和1~2wt%的氯化铈为原料,按固液比为100~120g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例4所制得的烧结锆刚玉耐火原料经检测:体积密度为3.60~3.64g/cm3;显气孔率为3.2~3.8%;吸水率为0.8~1.0%;Al2O3晶粒尺寸为20~80μm;ZrO2晶粒尺寸为2~9μm;断裂韧性为12.5~14.5Mpa·m0.5。
实施例5
一种烧结锆刚玉耐火原料及其制备方法。按α-氧化铝粉∶成球液体的质量比为1∶(0.20~0.22),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为19~26mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在550~600℃条件下干燥85~95分钟,然后送入高温竖窑的烧成室中,在1880~1900℃条件下保温37~42分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以89~91wt%的氯氧化锆、4~6wt%的氯化钙和硝酸钙、1~3wt%的氯化钇和2~3wt%的氯化铈为原料,按固液比为90~110g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例5所制得的烧结锆刚玉耐火原料经检测:体积密度为3.62~3.66g/cm3;显气孔率为2.8~3.4%;吸水率为0.7~0.9%;Al2O3晶粒尺寸为20~90μm;ZrO2晶粒尺寸为2~8μm;断裂韧性为10.2~12.2Mpa·m0.5。
实施例6
一种烧结锆刚玉耐火原料及其制备方法。按α-氧化铝粉∶成球液体的质量比为1∶(0.18~0.20),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为19~26mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在500~550℃条件下干燥80~90分钟,然后送入高温竖窑的烧成室中,在1860~1880℃条件下保温35~40分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料。
所述成球液体的制备方法是:以87~89wt%的氯氧化锆、6~8wt%的钙氯化镁和硝酸镁、2~4wt%的氯化钇和1~2wt%的氯化铈为原料,按固液比为80~100g/L向原料中加入水,搅拌至澄清,即得成球液体。
本实施例6所制得的烧结锆刚玉耐火原料经检测:体积密度为3.61~3.65g/cm3;显气孔率为3.1~3.7%;吸水率为0.6~0.8%;Al2O3晶粒尺寸为20~90μm;ZrO2晶粒尺寸为2~9μm;断裂韧性为11.4~13.4Mpa·m0.5。
本具体实施方式与现有技术相比具有如下积极效果:
本具体实施方式制备的烧结锆刚玉耐火原料是以溶液的形式引入氧化锆和复合稳定剂,引入量较少,工艺简单易操作,故生产成本低廉,适合规模化生产。以溶液的形式引入氧化锆,还能解决氧化锆在氧化铝基体中团聚的问题,使得氧化锆晶粒细小,在基体中均匀分布;引入的复合稳定剂对氧化锆具有很好的稳定效果,使绝大部分氧化锆以四方相形式存在,充分发挥了氧化锆的增韧效果。此外,烧结过程中部分固溶于ZrO2中的CaO或MgO会与Al2O3反应,在ZrO2晶粒表面分别生成六铝酸钙环或镁铝尖晶石环,同时基体中会形成微裂纹,进一步提高所制备的烧结锆刚玉耐火原料的抗热冲击能力,故具有优良的抗热震稳定性。
本具体实施方式所制得的烧结锆刚玉耐火原料经检测:体积密度为3.54~3.68g/cm3;显气孔率为2.2~4.8%;吸水率为0.6~1.2%;Al2O3晶粒尺寸为20~100μm;ZrO2晶粒尺寸为0.5~10μm;断裂韧性为9.5~14.5Mpa·m0.5。
因此,本具体实施方式所制备的烧结锆刚玉耐火原料具有成本低廉、结构均匀、抗热震稳定性优良和适于工业化生产的特点。
Claims (7)
1.一种烧结锆刚玉耐火原料的制备方法,其特征在于:按氧化铝粉∶成球液体的质量比为1∶(0.16~0.22),先将所述氧化铝粉置于成球机中,喷入所述成球液体,制得直径为18~28mm的坯球;再将所述坯球送入高温竖窑的干燥室中,在450~650℃条件下干燥70~100分钟,然后送入高温竖窑的烧成室中,在1850~1900℃条件下保温25~45分钟,随炉冷却,破碎,筛分,包装,即得烧结锆刚玉耐火原料;
所述成球液体的制备方法是:以86~92wt%的氯氧化锆、4~9wt%的钙盐或镁盐、1~6.5wt%的氯化钇和0.5~3wt%的氯化铈为原料,按固液比为40~120g/L向原料中加入水,搅拌至澄清,即得成球液体。
2.根据权利要求1所述的烧结锆刚玉耐火原料的制备方法,其特征在于所述氧化铝粉为工业氧化铝粉和α-氧化铝微粉中的一种,氧化铝粉的Al2O3含量>99.4wt%。
3.根据权利要求1所述的烧结锆刚玉耐火原料的制备方法,其特征在于所述钙盐为氯化钙和硝酸钙中的一种或两种。
4.根据权利要求1所述的烧结锆刚玉耐火原料的制备方法,其特征在于所述镁盐为氯化镁和硝酸镁中的一种或两种。
5.根据权利要求1所述的烧结锆刚玉耐火原料的制备方法,其特征在于所述氯化钇的YCl3含量>99.2wt%,粒径<100μm。
6.根据权利要求1所述的烧结锆刚玉耐火原料的制备方法,其特征在于所述氯化铈的CeCl3含量>99.5wt%,粒径<100μm。
7.一种烧结锆刚玉耐火原料,其特征在于所述烧结锆刚玉耐火原料是根据权利要求1~6项中任一项所述的烧结锆刚玉耐火原料的制备方法所制备的烧结锆刚玉耐火原料。
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