CN108218408B - 一种Al4SiC4结合Al2O3-SiC复合材料的制备方法 - Google Patents
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种Al4SiC4结合Al2O3‑SiC复合材料的制备方法，属于耐火材料领域。该复合材料按重量百分比计的原料组成为：45%‑86%的高铝矾土，10‑25%的碳化硅，5‑15%的活性氧化铝，1‑15%的金属铝，0‑5%炭黑或石墨，外加上述原料总量2‑6%的酚醛树脂结合剂。生产时按配比称取各种原料，混合均匀，经混炼得到泥料，然后压制成型，先在120‑250℃下烘干10‑25 h，然后在1300℃‑1700℃埋炭气氛下烧结5‑12 h。本发明产品高温烧成过程中原位合成了Al4SiC4为结合相，其具有高熔点、高强度、高耐磨性、高化学稳定性、低热膨胀系数以及优异的抗氧化性和抗水化性能，是一种高温结构材料和高性能耐火材料。
Description
技术领域
本发明涉及一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，属于耐火材料领域。
背景技术
随着水泥回转窑生产越来越大型化，窑的转速加快，窑径加大，对耐火材料的要求越来越高。尤其是回转窑窑口耐火衬是窑衬的薄弱环节，需要承受急冷、急热气流冲击，高温水泥熟料磨损和高温有害气体碱腐蚀等，使用条件十分苛刻。要求耐火材料必须具有良好的抗热震性、耐磨性和耐碱性。
干熄焦炉冷却室主要完成干熄炉内焦炭冷却作用，底部的冷却气流沿向上与自上而下的焦炭层对流换热，焦炭沿干熄炉冷却室壁向下运动的过程中与工作面耐火砖形成挤压和剧烈磨擦以及化学侵蚀，并且耐火砖每年要经受数万余次的温度变化，要求耐火材料具有优异的耐磨性、热震稳定性和抗侵蚀性。
用于连接与调控炼铁和炼钢之间的铁水输送、储存缓冲和预处理设备如混铁车（鱼雷罐）、混铁炉、铁水罐等用的耐火材料普遍存在抗冲刷性不好、抗渣侵蚀和渗透性差、炉衬材料中的C易被氧化等原因而造成炉衬使用寿命低、易结渣等问题。
洪彦若等在研究非氧化物复合材料时，提出了金属塑性相复合耐火材料的理论及实现该材料的工艺，即过渡塑性相工艺。在刚性的无机氧化物中加入一定量的金属，金属的大部分为过渡塑性相，少部分为金属塑性相。两者初始时均起塑性成型作用，在常温压制成型时金属的塑性使刚性成型转变为塑性成型，提高制坯的密度和降低气孔率；在烧结过程，金属液化或软化，充填空隙，起助烧剂作用，提高制品致密度。区别之处在于烧结过程，过渡塑性相的金属与环境气氛及材料发生了反应，生成了非金属增强相，提高材料的高温强度和抗热震性。
Al4SiC4具有高熔点（大约2037 ℃）、高强度、高化学稳定性、低热膨胀系数以及优异的抗氧化和抗水化性能，是一种高温结构材料和高性能耐火材料，也是含碳材料和非氧化物使用的抗氧化剂。并且Al4SiC4难以被铁及氧化物基熔渣润湿, 因而具有优良的抗渣侵蚀性和抗渣渗透性。
发明内容
本发明旨在制备出一种Al4SiC4结合Al2O3-SiC复合材料，具有气孔率低、强度高、耐磨性好、热震稳定性好、抗侵蚀性好等优良的性能指标，可广泛用于水泥回转窑、干熄焦炉、铁水罐和鱼雷罐等。
为了达到以上目的，本发明采用如下技术方案：
一种Al4SiC4结合Al2O3-SiC复合材料，各物质含量按重量百分比计算为45%-86%的高铝矾土，10-25%的碳化硅，5-15%的活性氧化铝，1-15%的金属铝，0-5%炭黑或石墨，外加上述原料总量2-6%的酚醛树脂。
以上述复合材料中酚醛树脂为结合剂，所述高铝矾土有3-1 mm、1-0 mm或小于0.088 mm三种粒度，所述碳化硅的粒度为1-0 mm或小于0.088 mm，所述活性氧化铝的粒度为小于0.088 mm，所述金属铝的粒度为小于0.088 mm，所述炭黑或石墨的粒度为小于0.088mm，所述高铝矾土的氧化铝质量百分比大于80%，，所述碳化硅的纯度大于97%。不同粒度的比例为：1≤粒度≤3mm，44-66%；0≤粒度≤1mm，18-30%；0≤粒度≤0.088mm，17-30%。
以上述Al4SiC4结合Al2O3-SiC复合材料的制备方法，其特征在于：按配比称取各种原料，混合均匀，经混炼得到泥料，然后加压成型，先在120-250 ℃下烘干10-25 h，然后在1300 ℃-1700 ℃埋炭气氛下烧结5-12 h。
本发明的有益效果为：
（1）本发明提供了一种Al4SiC4结合Al2O3-SiC复合材料，本发明产品以过渡塑性理论为基础，材料在高温烧成过程中原位生成高温结合相Al4SiC4，Al4SiC4具有高熔点（大约2037 ℃）、高强度、高耐磨性、高化学稳定性、低热膨胀系数以及优异的抗氧化、抗水化和抗侵蚀和抗渣渗透性能，未参与反应的金属铝，高温下为球状液体，可以很好的缓冲热应力，使得材料具有优异的热震稳定性；
（2）本发明产品具有强度高、耐磨性好、热震稳定性好、抗侵蚀和抗渗透性好，可以应用于水泥回转窑、干熄焦炉、铁水罐和鱼雷罐等，该复合材料以非氧化物Al4SiC4为结合相，并有少量金属塑性相的存在，具有金属-非金属结合的结构，有优良的物理性能指标：显气孔率3-10%、体积密度2.90-3.40 g/cm3、常温耐压强度150-250 MPa、高温抗折强度20-70Mpa，热震稳定性大于20次，耐磨性1.0-3.0 cc以及优异的抗侵蚀和抗渗透性；
（3）本发明以过渡塑性理论为基础，材料在高温烧成过程中原位生成高温结合相Al4SiC4，并且少量塑性相金属Al的存在，使得复合材料具有优良的抗热震性，能够满足上述窑炉对使用要求。
附图说明：
图1为碳化铝-碳化硅的二元相图。
具体实施方式：
实施例1：一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，
按重量百分比计，原料组成为：65%的83高铝矾土、20%的SiC、12%的活性氧化铝、3%的金属铝粉，外加3%的酚醛树脂为结合剂。
生产时，先按配比称取各种原料，混合均匀，经混炼得到泥料，然后经摩擦压力机压制成型，先在120-250℃下烘干10-25h，然后在1300℃-1700℃埋炭气氛下烧结5-12h。
所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1 mm、1-0 mm的83高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率6.5%，体积密度3.10 g/cm3，常温耐压强度185MPa，热震稳定性（1100 ℃，水冷）25次，高温抗折强度45 MPa，耐磨性2.4 cc，其抗侵蚀性和渗透均较好。
Al4SiC4的反应过程为：
4Al(l)+3C(s)=Al4C3(s)
6Al(l)+3CO(g)=Al4C3(s)+Al2O3(s)
Al4C3(s)+SiC(s)=Al4SiC4(s)
Al4C3(s)+Al2O3(s)=Al4O4C(s)
Al4O4C(s)+SiC(s)+6C(s)=Al4SiC4(s)+4CO(g)
Al4O4C与Al4SiC4相同，均为性能优异的非氧化物材料。
实施例2：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：70%的83高铝矾土、15%的SiC、10%的活性氧化铝、5%的金属铝粉，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1mm、1-0 mm的83高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率5.8%，体积密度3.13 g/cm3，常温耐压强度196MPa，热震稳定性（1100℃，水冷）28次，高温抗折强度50 MPa，耐磨性2.1 cc，其抗侵蚀性和渗透均较好。
实施例3：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：61%的83高铝矾土、15%的SiC、15%的活性氧化铝、7%的金属铝粉、炭黑2%，，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1mm、1-0mm的83高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率5.3%，体积密度3.16 g/cm3，常温耐压强度208MPa，热震稳定性（1100℃，水冷）32次，高温抗折强度59 MPa，耐磨性1.8 cc，其抗侵蚀性和渗透均较好。
实施例4：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：63%的83高铝矾土、13%的SiC、15%的活性氧化铝、7%的金属铝粉、炭黑2%，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝、金属铝粉和炭黑，所述骨料粒度为3-1 mm、1-0 mm的83高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率8.5%，体积密度3.07 g/cm3，常温耐压强度188MPa，热震稳定性（1100 ℃，水冷）28次，高温抗折强度46 MPa，耐磨性2.2 cc，其抗侵蚀性和渗透均较好。
实施例5：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：68%的88高铝矾土、15%的SiC、10%的活性氧化铝、7%的金属铝粉，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1mm、1-0 mm的88高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率5.0%，体积密度3.20 g/cm3，常温耐压强度223MPa，热震稳定性（1100 ℃，水冷）35次，高温抗折强度63 MPa，耐磨性1.5 cc，其抗侵蚀性和渗透均较好。
实施例6：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：73%的88高铝矾土、12%的SiC、10%的活性氧化铝、5%的金属铝粉，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1mm、1-0 mm的88高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率5.3%，体积密度3.17 g/cm3，常温耐压强度210MPa，热震稳定性（1100 ℃，水冷）31次，高温抗折强度55 MPa，耐磨性1.8 cc，其抗侵蚀性和渗透均较好。
实施例7：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：73%的88高铝矾土、10%的SiC、10%的活性氧化铝、5%的金属铝粉、2%的炭黑，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝和金属铝粉，所述骨料粒度为3-1 mm、1-0 mm的88高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率5.8%，体积密度3.14 g/cm3，常温耐压强度230MPa，热震稳定性（1100 ℃，水冷）29次，高温抗折强度48 MPa，耐磨性2.1 cc，其抗侵蚀性和渗透均较好。
实施例8：生产工艺和实施例1相同，不同之处在于：
一种Al4SiC4结合Al2O3-SiC复合材料的制备方法，按重量百分比计，原料组成为：70%的88高铝矾土、13%的SiC、10%的活性氧化铝、5%的金属铝粉、2%的炭黑，外加3%的酚醛树脂为结合剂。所述粉料为粒度小于0.088 mm的碳化硅、活性氧化铝、金属铝粉和炭黑，所述骨料粒度为3-1 mm、1-0 mm的88高铝矾土和碳化硅。
所得产品的性能指标为：显气孔率7.5%，体积密度3.04 g/cm3，常温耐压强度195MPa，热震稳定性（1100 ℃，水冷）26次，高温抗折强度42 MPa，耐磨性2.2 cc，其抗侵蚀性和渗透均较好。
以上所述仅是本发明的优选实施方式，应当指出对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (1)
1.一种Al4SiC4结合Al2O3-SiC复合材料，其特征在于：各物质含量按重量百分比计算为45%-86%的高铝矾土，10-25%的碳化硅，5-15%的活性氧化铝，1-15%的金属铝，2-5%炭黑或石墨，上述物质的总量为100%，外加上述原料总量2-6%的酚醛树脂为结合剂；按配比称取各种原料，混合均匀，经混炼得到泥料，然后加压成型，先在120-250 ℃下烘干10-25 h，然后在1300℃-1700 ℃埋炭气氛下烧结5-12 h。
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| CN102898157A (zh) * | 2012-10-08 | 2013-01-30 | 北京科技大学 | Al4O4C结合Al-Al2O3复合无碳滑板及制备方法 |
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