CN105693259B - 一种刚玉质尖晶石固溶体耐火材料制备工艺 - Google Patents

一种刚玉质尖晶石固溶体耐火材料制备工艺 Download PDF

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CN105693259B
CN105693259B CN201610070854.6A CN201610070854A CN105693259B CN 105693259 B CN105693259 B CN 105693259B CN 201610070854 A CN201610070854 A CN 201610070854A CN 105693259 B CN105693259 B CN 105693259B
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李勇
马佳佳
薛文东
陈俊红
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Abstract

一种刚玉质尖晶石固溶体耐火材料制备工艺，属于无机非金属材料领域。本发明将以质量分数为60‑85％刚玉颗粒和细粉、10‑20％的镁砂细粉和5‑20％的金属铝粉为原料，并加入原料质量分数3‑5％的无机结合剂。在氮气气氛中烧结，基质中金属铝粉原位反应生成氮化铝，生成的氮化铝与氧化铝或新生成的尖晶石固溶形成阿隆或镁阿隆增强相。材料内部结构为富铝尖晶石固溶体和少量的阿隆或者镁阿隆增强相的结合结构，晶格常数较小，晶粒细小且致密，气孔较少，颗粒分布均匀。该耐火材料有较高的强度和熔点，优良的抗渣性能和抗热震稳定性，使用寿命长。该制备工艺操作简单，无需复杂的设备，且原料简单易得，生产和使用过程中对环境污染小，易于工业化推广。

Description

一种刚玉质尖晶石固溶体耐火材料制备工艺
技术领域
本发明属于无机非金属材料领域，涉及炼钢钢包、炉外精炼和连铸功能材料用耐火材料的制备方法，具体一种刚玉质尖晶石固溶体耐火材料制备工艺。
镁铝尖晶石的化学式为MgAl2O4熔点为2135℃，只是MgO-Al2O3二元体系其中一个化合物，MgO-Al2O3二元体系所形成的有限固溶体都称之为尖晶石固溶体，可知其化学组成在一个较大范围的固溶体区域内，在高温下方镁石在尖晶石中的溶解度可达10wt％，刚玉在尖晶石中的溶解度更高。
尖晶石质耐火材料耐高温，抗高温蠕变，抗炉渣侵蚀性好，热震稳定性好，耐磨损，抗腐蚀性气体及气氛波动，具有一系列优良的综合性能。作为一种高级耐火材料，方镁石-尖晶石砖广泛应用于炼钢钢包、炉外精炼、连铸用功能耐火材料和水泥回转窑的过渡带或烧成带和玻璃窑蓄热室等。理论组成附近的镁铝尖晶石质耐火材料的耐侵蚀性更好，并且尖晶石固溶体中氧化铝含量的增加使得尖晶石的晶粒发育缓慢，颗粒分布均匀，气孔率更低。氧化铝和尖晶石的线膨胀系数相差不大，抗剥落性能好。因此，刚玉质尖晶石固溶体耐火材料比方镁石-尖晶石复合耐火材料更加适用于炼钢钢包和炉外精炼。
耐火材料正在由氧化物复合材料向着氧化物-非氧化物复合和氧化物-非氧化物-金属复合的方向发展，先后出现了一系列综合性能较好的新型耐火材料，其中阿隆和镁阿隆就在其中，镁阿隆是针对阿隆材料在1640℃下不稳定的特性，加入氧化镁或者尖晶石热力学稳定剂后形成的新相。它们都具有更好的机械性能、抗高温性能、热震稳定性、抗侵蚀性能和抗剥落性。结合上述阿隆和镁阿隆的优良性能，我们想到如果将它们用于镁铝尖晶石中作为增强相应该会给镁铝尖晶石带来更加优良的性能。
随着金属塑性相工艺的提出和发展，硅粉和铝粉是目前使用最广泛的金属塑性添加剂。在本工艺中，铝作为过渡塑性相引入，在烧结过程中，基质中铝粉在660℃时变成液态铝先与氮气反应生成氮化铝，新生成的氮化铝和氧化铝、氧化镁或者氧化铝氧化镁新生成的尖晶石反应，生成了阿隆和镁阿隆增强相，它们的生成填充了铝液化和气化留下的气孔，增加了基质与基质，基质与大颗粒之间的联系并且起到弥散增韧的效果。并且铝粉的液化使得铝粉作为一种助烧剂，使得液相烧结在低温下可以实现，加速了反应进程。如果生产直接结合尖晶石质砖，需要使用纯度较高的原料，高压成型，高温烧成(1900-1800℃)，最好1800℃以上。而本工艺1700℃时已经能完全形成刚玉质尖晶石固溶体了。最后未反应的铝粉在高温的使用过程中以液相的形式存在于材料中吸收温度变化及钢水冲刷产生的应力，进一步提高了材料的抗热震性。
发明内容：针对现有技术不足，本发明提供了炼钢钢包、炉外精炼和连铸功能材料用耐火材料的制备方法，具体一种刚玉质尖晶石固溶体耐火材料制备工艺。
与纯镁铝尖晶石耐火材料相比，刚玉质尖晶石固溶体耐火材料内部是富铝的尖晶石固溶体基体与阿隆、镁阿隆增强相的结合，内部结构更加致密，常温耐压强度有较大提高，高温性能更好，应用范围更广泛，并且反应温度更低，反应更容易进行。
一种刚玉质尖晶石固溶体耐火材料制备工艺，其特征在于：所述的材料采用刚玉颗粒、镁砂细粉和金属铝粉作为原料氮化而成；具体制备工艺是取质量分数为60-85％刚玉颗粒和细粉、10-20％的镁砂细粉和5-20％的金属铝粉为原料，另外加入原料质量3-5％的结合剂。将原料混合后进行混炼，并在100-160MPa下压制成型。将压制成型后的试样放入烧结炉中，在1600-1900℃进行氮化8-24h后自然冷却；
在烧结过程中金属铝粉氮化，在基质中原位生成氮化铝，生成的氮化铝与氧化铝或新生成的尖晶石固溶形成阿隆或者镁阿隆增强相。所制备的材料内部结构为富铝尖晶石固溶体和少量的阿隆、镁阿隆增强相的结合结构。
其中刚玉为电熔刚玉或烧结刚玉中的至少一种，所含Al2O3纯度≥99.4％，颗粒级配分别有5-≥3mm，3-≥1mm、1-＞0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％。
镁砂为烧结镁砂或电熔镁砂中的至少一种，所含MgO纯度≥97.3％，以≤0.088mm的细粉存在于基质中(基质即富铝尖晶石固溶体和少量的阿隆、镁阿隆增强相的结合体)。
铝粉纯度≥99.3％，以≤0.088mm的细粉存在于基质中。
结合剂是三聚磷酸钠和六偏磷酸钠中的一种或两种。
本发明的基本构思是以刚玉为颗粒，氧化镁为细粉，添加金属铝粉为原料，在氮气气氛中烧结氮化，原位反应生成氮化铝，从而制备出以富铝的尖晶石固溶体为基体结合阿隆、镁阿隆增强相的材料。本发明创新之处在于设计原料使生成刚玉质镁铝尖晶石固溶体而非刚玉尖晶石复合耐火材料，晶粒更加细小均匀而致密，使物理性能和高温性能更加优良；并且在耐火材料中使用金属塑性相工艺，通过添加金属铝粉，在基质中原位生成增强相，使烧成之后的耐火材料具有更高的强度，更好抗渣性能，抗热震稳定性和抗剥落性，使用寿命更长，质量更好。
本发明以刚玉、镁砂和铝粉为原料，压制成砖坯，在氮气气氛中氮化，原位生成阿隆和镁阿隆结合相，制备出刚玉质尖晶石固溶体和阿隆、镁阿隆相的复合材料。本发明以刚玉、镁砂和铝粉为原料，压制成砖坯，在氮气气氛中氮化，原位生成阿隆和镁阿隆结合相，制备出刚玉质尖晶石固溶体和阿隆、镁阿隆的复合材料。该方法操作工艺简单，无需复杂的设备，且原料简单易得，生产过程对环境污染小，易于工业化推广。
本发明所制备的刚玉质尖晶石固溶体耐火材料，其性能为：所制备的材料气孔率10-18％，体积密度2.55-3.18g/cm3，常温耐压强度100-240MPa,是一种强度较大的砖，其高温性能也较好，适宜作为高炉钢包和炉外精炼用耐火材料。
具体实施工艺：
1选取纯度为99.4％以上电熔或者烧结刚玉。分别选取颗粒级配为：5-3mm、3-1mm、1-0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％。
2按质量分数取60-85％刚玉颗粒和细粉、10-20％的镁砂细粉和5-20％的金属铝粉为原料，加入3-5％三聚磷酸钠或者六偏磷酸钠作为结合剂。将原料混合后进行混炼，并在100-160MPa下压制成型。将压制成型后的试样放入烧结炉中，在1600-1900℃进行氮化8-24h后自然冷却即可获得一种刚玉质尖晶石固溶体耐火材料。
实例1
1选取纯度为99.4％以上电熔或者烧结刚玉。分别选取颗粒级配为：5-3mm、3-1mm、1-0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％。
2按质量分数取80％刚玉颗粒和细粉、13％的镁砂细粉和7％的金属铝粉为原料，加入3-5％三聚磷酸钠或者六偏磷酸钠作为结合剂。将原料混合后进行混炼，并在150MPa下压制成型。将压制成型后的试样放入烧结炉中，在1700℃进行氮化10h后自然冷却即可获得一种刚玉质尖晶石固溶体耐火材料。
实例2
1选取纯度为99.4％以上电熔或者烧结刚玉。分别选取颗粒级配为：5-3mm、3-1mm、1-0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％。
2按质量分数取75％刚玉颗粒和细粉、15％的镁砂细粉和10％的金属铝粉为原料，加入3-5％三聚磷酸钠或者六偏磷酸钠作为结合剂。将原料混合后进行混炼，并在150MPa下压制成型。将压制成型后的试样放入烧结炉中，在1800℃进行氮化20h后自然冷却即可获得一种刚玉质尖晶石固溶体耐火材料。
实例3：
1选取纯度为99.4％以上电熔或者烧结刚玉。分别选取颗粒级配为：5-3mm、3-1mm、1-0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％。
2按质量分数取70％刚玉颗粒和细粉、18％的镁砂细粉和12％的金属铝粉为原料，加入3-5％三聚磷酸钠或者六偏磷酸钠作为结合剂。将原料混合后进行混炼，并在150MPa下压制成型。将压制成型后的试样放入烧结炉中，在1600℃进行氮化24h后自然冷却即可获得一种刚玉质尖晶石固溶体耐火材料。

Claims (1)

1.一种刚玉质尖晶石固溶体耐火材料制备工艺，其特征在于：所述的材料采用刚玉颗粒、镁砂细粉和金属铝粉作为原料氮化而制备；具体制备工艺是取质量分数取60-85％刚玉颗粒、10-20％的镁砂细粉和5-20％的金属铝粉为原料，加入3-5％的结合剂；将原料混合后进行混炼，并在100-160MPa下压制成型；将压制成型后的试样放入烧结炉中，在1600-1900℃进行氮化8-24h后自然冷却；在烧结过程中金属铝粉氮化，在基质中原位生成氮化铝，生成的氮化铝与氧化铝或新生成的尖晶石固溶形成阿隆或者镁阿隆增强相；所制备的材料内部结构为富铝尖晶石固溶体和少量的阿隆、镁阿隆增强相的结合结构；
刚玉颗粒为电熔刚玉或烧结刚玉中的至少一种，所含Al2O3质量百分比≥99.4％，颗粒级配分别有：5-≥3mm，3-≥1mm、1-＞0.088mm和≤0.088mm，分别对应其质量分数：10-30％、20-30％、10-30％和30-50％；
镁砂为烧结镁砂或电熔镁砂中的至少一种，所含MgO质量百分比≥97.3％，以≤0.088mm的细粉存在于基质中，与刚玉颗粒反应生成富铝的尖晶石固溶体；
铝粉中Al质量百分数≥99.3％，以≤0.088mm的细粉存在于基质中；
结合剂是三聚磷酸钠和六偏磷酸钠中的一种或两种。
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