CN111732438B - SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法 - Google Patents
SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。其技术方案是：将装有Al4SiC4坯体的坩埚置于高温气压炉内，真空条件下加热至1150～1250℃，充氮气至0.1～5MPa，保压条件下升温至1600～1800℃，保温保压10～300min，制得制品。或将装有Al4SiC4坯体的坩埚置于高温气压炉内，在真空条件下加热至1150～1250℃，用5～10min充氮气至0.1～1MPa，保压条件下加热至1500～1600℃，保温保压10～300min；再用5～10min充氮气至1.2～7MPa，保压条件下继续加热至1600～1800℃，保温保压10～60min，制得制品。所述坯体是将Al4SiC4粉体模压成型或将Al4SiC4粉体模压成型后再等静压成型。本发明所制制品抗氧化性能优异、致密度高且力学性能好。
Description
技术领域
本发明属于非氧化物陶瓷结合碳复合耐火材料技术领域。具体涉及一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。
背景技术
碳材料具有质量轻、热膨胀系数低、高温力学性能优异、导电及导热性能好、耐腐蚀和抗渣性能强的特点，广泛应用于航空航天、国防、体育和医学等领域。但由于碳材料在400℃时就发生氧化且强度低，难以与其他物质形成化学结合，限制其在高温行业中的应用。为使碳材料能应用于高温结构部件，目前最有效的方法是将陶瓷材料引入碳材料中，制备陶瓷-碳复合材料，结果表明该种方式可以有效提高单相碳材料的强度和抗氧化等性能。
氧化物陶瓷-碳复合材料在现有耐火材料的广泛应用已经相对成熟，例如铝碳(Al2O3-C)耐火材料(J.Ding,C.Yu,J.P.Liu,et al.Effects of silicon powder contenton the properties and interfacebonding of nitrided Al2O3-C refractories[J].Materials Chemistry and Physics,206,2018,193-203)应用于钢铁行业中的堵头、包盖或浸入式喷嘴器件，这种材料虽对液体炉渣的润湿性差和耐腐蚀性好，但在高温下易被氧化，使用寿命低。非氧化物陶瓷-碳复合材料作为一种新型耐火材料具有轻质、高强的特点，且能够应用于超高温极端环境中，近年来受到越来越多学者关注，如S.B.Zhou等人(S.B.Zhou,Z.Wang,W.Zhang,Effect of graphite flake orientation onmicrostructure and mechanical properties of ZrB2-SiC-graphite composite,Journal of Alloys and Compounds,485,2009,181-185.)采用粒径为2μm的ZrB2细粉、粒径为2μm的SiC细粉与粒径为15μm且厚度为2μm的鳞片石墨为原料，通过球磨湿混干燥等步骤，采用热压烧结的方法，在30MPa单向压力下，1900℃保温1h氩气气氛下烧结制得ZrB2-SiC-graphite复合材料。采用此种制备方法的材料容易存在原料混合不充分、产物化学成分分布不均匀、制备过程需要高温高压的环境、条件苛刻和成本高等缺陷，且该类材料通常采用细粉为原料，没有现有耐火材料粗颗粒骨料构筑的骨架结构，其中的陶瓷和碳颗粒之间通过简单的物理堆积的方式结合，亦无法形成强化学键结合，因此材料的力学性能差。Chen等人(W.W.Chen,Y.Miyamoto,T.Tojo,M.Naito,Densification and properties ofAlN ceramic bonded carbon,Journal of the European Ceramic Society,32,2012,245-250.)通过结合凝胶注模和放电等离子烧结技术制备出AlN陶瓷结合C材料，虽然该材料中AlN陶瓷相形成了连续的网络状骨架结构，碳聚集体被包覆在连续的陶瓷骨架中，但该法制备工艺复杂，陶瓷相与碳聚集体之间的结合弱，断裂极易发生在陶瓷-碳界面结合处和碳聚集体中，影响材料的致密性和机械性能。
发明内容
本发明旨在克服现有技术缺陷，目的在于是提供一种工艺简单、成本低的SiC晶须增强AlN陶瓷结合C复合耐火材料的制备方法，用该方法制备的SiC晶须增强AlN陶瓷结合C复合耐火材料力学性能优异、高温抗氧化性能优异和致密性高。
为实现上述目的，本发明采用的技术方案是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150～1250℃；再用5～10min充氮气至0.1～5MPa，保压条件下升温至1600～1800℃，保温保压10～300min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
或将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150～1250℃，用5～10min充氮气至0.1～1MPa，保压条件下再加热至1500～1600℃，保温保压10～300min；再用5～10min充氮气至1.2～7MPa，保压条件下继续加热至1600～1800℃，保温保压10～60min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体为坯体I或为坯体II：坯体I是将Al4SiC4粉体在5～50MPa条件下模压成型，即得Al4SiC4坯体I；坯体II是将Al4SiC4粉体在5～50MPa条件下模压成型，再于100～200MPa条件下等静压成型，即得Al4SiC4坯体II。
所述Al4SiC4粉体的纯度≥98.0wt％，粒度≤74μm。
所述氮气纯度为≥99.999％。
由于采用上述技术方案，本发明与现有技术相比的有益效果在于：
本发明仅采用单一的Al4SiC4粉体为原料，产物化学成分分布和微观结构均匀；本发明制得的SiC晶须增强AlN陶瓷结合C复合耐火材料，先采用模压或者模压与等静压结合的方法制坯体，然后直接置于高温气压炉内用气压烧结的方法在氮气气氛下烧成，工艺简单，可制得复杂形状的制品；采用模压与等静压结合的方法，坯体的密度更加均匀一致，制品缺陷少。
本发明采用两步气压烧结法制的SiC晶须增强AlN陶瓷结合C复合耐火材料，与一步气压烧结法相比，所制制品致密度更高和机械性能更加优异；本发明制备的SiC晶须增强AlN陶瓷结合C复合耐火材料在1600～1800℃和0.1～7MPa条件下烧成，制备温度低、压强小和条件简单，能显著降低生产成本。
本发明制得的SiC晶须增强AlN陶瓷结合C复合耐火材料，形成了AlN包裹SiC晶须和C的网络状结构，其中原位形成的SiC晶须均匀分散在在C聚集体之间，形成连续的SiC晶须网络，使被分散包裹的碳聚集体变成由晶须网络骨架来加固，而AlN和SiC的结构相似，更容易形成有效的化学结合，因而SiC晶须网络与AlN陶瓷骨架可形成紧密的化学结合，使原本AlN陶瓷与碳聚集体之间的弱结合通过SiC晶须网络加固，因此所制备的SiC晶须增强AlN陶瓷结合C复合耐火材料的力学性能好、抗氧化性能优异且致密性高。
本发明制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测，相对密度为75.8～90％，抗折强度为106.9～200MPa。
因此，本发明制备工艺简单和成本低，所制备的SiC晶须增强AlN陶瓷结合C复合耐火材料不仅化学成分分布和微观结构均匀，且高温抗氧化性能优异、致密度高和力学性能好。
附图说明
图1是本发明制备的一种SiC晶须增强AlN陶瓷结合C复合耐火材料的XRD图；
图2是图1所示SiC晶须增强AlN陶瓷结合C复合耐火材料的TEM图。
具体实施方式
现结合附图和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。
本具体实施方式中：
所述Al4SiC4粉体的纯度≥98.0wt％，粒度≤74μm。
所述氮气纯度为≥99.999％。
实施例中不再赘述。
实施例1
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150℃；再用5min充氮气至0.1MPa，保压条件下升温至1600℃，保温保压300min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在5MPa条件下模压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测，相对密度为75.9％，抗折强度为107MPa。
实施例2
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1180℃；再用7min充氮气至1MPa，保压条件下升温至1680℃，保温保压200min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在20MPa条件下模压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测，相对密度为77.8％，抗折强度为120MPa。
实施例3
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1220℃；再用8min充氮气至3MPa，保压条件下升温至1750℃，保温保压100min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在35MPa条件下模压成型，再于170MPa条件下等静压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测，相对密度为81.2％，抗折强度为141MPa。
实施例4
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1250℃；再用10min充氮气至5MPa，保压条件下升温至1800℃，保温保压10min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在50MPa条件下模压成型，再于200MPa条件下等静压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测，相对密度为86.8％，抗折强度为186MPa。
实施例5
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150℃，用5min充氮气至0.1MPa，保压条件下再加热至1500℃，保温保压300min；再用5min充氮气至1.2MPa，保压条件下继续加热至1600℃，保温保压60min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在5MPa条件下模压成型，再于100MPa条件下等静压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测：相对密度为79.4％；抗折强度为129MPa。
实施例6
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1180℃，用7min充氮气至0.3MPa，保压条件下再加热至1530℃，保温保压200min；再用7min充氮气至3MPa，保压条件下继续加热至1680℃，保温保压45min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在20MPa条件下模压成型，再于130MPa条件下等静压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测：相对密度为82.9％；抗折强度为154MPa。
实施例7
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1220℃，用8min充氮气至0.7MPa，保压条件下再加热至1570℃，保温保压100min；再用8min充氮气至5MPa，保压条件下继续加热至1750℃，保温保压30min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在35MPa条件下模压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测：相对密度为84.9％；抗折强度为168MPa。
实施例8
一种SiC晶须增强AlN陶瓷结合C复合耐火材料及其制备方法。本实施例所述制备方法是：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1250℃，用10min充氮气至1MPa，保压条件下再加热至1600℃，保温保压100min；再用10min充氮气至7MPa，保压条件下继续加热至1800℃，保温保压10min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料。
所述Al4SiC4坯体是将Al4SiC4粉体在50MPa条件下模压成型，即得Al4SiC4坯体。
本实施例制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测：相对密度为88.7％；抗折强度为198MPa。
本具体实施方式与现有技术相比的有益效果在于：
本具体实施方式仅采用单一的Al4SiC4粉体为原料，所制制品化学成分分布和微观结构均匀；本具体实施方式制得的SiC晶须增强AlN陶瓷结合C复合耐火材料，先采用模压或者模压与等静压结合的方法制坯体，然后直接置于高温气压炉内用气压烧结的方法在氮气气氛下烧成，工艺简单，可制得复杂形状的制品；采用模压与等静压结合的方法，坯体的密度更加均匀一致，制品缺陷少。
本具体实施方式采用两步气压烧结法制的SiC晶须增强AlN陶瓷结合C复合耐火材料，与一步气压烧结法相比，所制制品致密度更高和机械性能更加优异；本具体实施方式制备的SiC晶须增强AlN陶瓷结合C复合耐火材料在1600～1800℃和0.1～7MPa条件下烧成，制备温度低、压强小和条件简单，能显著降低生产成本。
本具体实施方式制得的SiC晶须增强AlN陶瓷结合C复合耐火材料如图1所示，图1是实施例3制备的SiC晶须增强AlN陶瓷结合C复合耐火材料的XRD图；图2是图1所示SiC晶须增强AlN陶瓷结合C复合耐火材料的TEM图。从图1可以看出：所制制品的主要成分为AlN，SiC，C和少量未反应完全的原料Al4SiC4；从图2可以看出：AlN包裹在SiC和C颗粒的周围，其中“蛆状”SiC晶须均匀分布在C聚集体颗粒中。
本具体实施方式的制品形成了AlN包裹SiC晶须和C的网络状结构，其中原位形成的SiC晶须均匀分散在在C聚集体之间，形成连续的SiC晶须网络，使被分散包裹的碳聚集体变成由晶须网络骨架来加固，而AlN和SiC的结构相似，更容易形成有效的化学结合，因而SiC晶须网络与AlN陶瓷骨架可形成紧密的化学结合，使原本AlN陶瓷与碳聚集体之间的弱结合通过SiC晶须网络加固，所制备的SiC晶须增强AlN陶瓷结合C复合耐火材料的力学性能好、抗氧化性能优异且致密性高。
本具体实施方式制得的SiC晶须增强AlN陶瓷结合C复合耐火材料经检测：相对密度为75.8～90％；抗折强度为106.9～200MPa。
因此，本具体实施方式制备工艺简单和成本低，所制备的SiC晶须增强AlN陶瓷结合C复合耐火材料不仅化学成分分布和微观结构均匀，且高温抗氧化性能优异、致密度高和力学性能好。
Claims (2)
1.一种SiC晶须增强AlN陶瓷结合C复合耐火材料的制备方法，其特征在于：
将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150~1250°C；再用5~10min充氮气至0.1~5MPa，保压条件下升温至1600~1800°C，保温保压10~300min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料；
或将Al4SiC4坯体装入石墨坩埚内，然后将所述坩埚置于高温气压炉内，在真空度≤10Pa条件下从室温加热至1150~1250°C，用5~10min充氮气至0.1~1MPa，保压条件下再加热至1500~1600°C，保温保压10~300min；再用5~10min充氮气至1.2~7MPa，保压条件下继续加热至1600~1800°C，保温保压10~60min，冷却至室温，制得SiC晶须增强AlN陶瓷结合C复合耐火材料；
所述Al4SiC4坯体为坯体I或为坯体II：坯体I是将Al4SiC4粉体在5~50MPa条件下模压成型，即得Al4SiC4坯体I；坯体II是将Al4SiC4粉体在5~50MPa条件下模压成型，再于100~200MPa条件下等静压成型，即得Al4SiC4坯体II；
所述Al4SiC4粉体的纯度≥98.0wt%，粒度≤74μm；
所述氮气纯度为≥99.999%。
2.一种SiC晶须增强AlN陶瓷结合C复合耐火材料，其特征在于所述SiC晶须增强AlN陶瓷结合C复合耐火材料是根据权利要求1所述SiC晶须增强AlN陶瓷结合C复合耐火材料的制备方法所制备的SiC晶须增强AlN陶瓷结合C复合耐火材料。
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