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CN105565812A - 一种Sialon结合SiC多孔材料的制备方法 - Google Patents

一种Sialon结合SiC多孔材料的制备方法 Download PDF

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CN105565812A
CN105565812A CN201510945685.1A CN201510945685A CN105565812A CN 105565812 A CN105565812 A CN 105565812A CN 201510945685 A CN201510945685 A CN 201510945685A CN 105565812 A CN105565812 A CN 105565812A
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sialon
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张欣
何建
李华臣
陈建章
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Hunan University of Science and Technology
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Abstract

一种Sialon结合SiC多孔材料的制备方法，包括：称取60～80重量份SiC粉、10～20重量份活性氧化铝粉和5～15重量份金属硅粉，入球磨机研磨3h制得原料粉体；称取40～60重量份坯体增强剂，0.1～1.0质量份分散调凝剂，0.1～1.0质量份硅烷偶联剂与原料粉体搅拌均匀制得原料浆料；称取25重量份1wt％三萜皂甙植物发泡剂溶液高速搅拌制得泡沫；将泡沫与原料浆料搅拌均匀制得泡沫浆料；泡沫浆料注模成型、干燥、1400℃下氮化制得Sialon结合SiC多孔材料。其中，SiC粉粒度325目及以下，金属Si粉粒度200目及以下，活性氧化铝粉为ρ-Al2O3，坯体增强剂为聚乙烯醇、木质素磺酸钙和淀粉中的一种或其复合的水溶液，分散调凝剂为碳酸钠、六偏磷酸钠、三聚磷酸钠、碳酸锂中的一种或其复合。

Description

一种Sialon结合SiC多孔材料的制备方法
技术领域
本发明属于多孔材料技术领域，具体涉及一种Sialon结合SiC多孔材料的制备方法。
背景技术
SiC材料机械性能优异，化学稳定性好，耐腐蚀、抗侵蚀，热震稳定性好，是极为重要的高温结构材料。SiC的Si-C键为键力极强的共价键，常规方法极难烧结，通常添加烧结助剂或采用反应烧结方法制备SiC材料，由此而得硅酸盐结合SiC、氧化物结合SiC、莫来石结合SiC、Si3N4结合SiC等各种SiC制品，其中Sialon结合SiC性能最好，高温强度高，抗热冲击性好，抗氧化性、耐熔体与酸碱侵蚀性强等。
SiC多孔材料气孔率高，渗透性好，隔音隔热性能好，在工业与高科技领域有着广泛应用，遍及冶金、化工、电子、能源、航空、环保、生物等多个领域。例如，可用作高温气体净化器、固体颗粒与熔融金属过滤器、热交换器、传感器、保温隔热材料，以及汽车尾气的催化剂载体等。
多孔材料的制备方法有添加造孔剂法、有机泡沫浸渍法(复制法)和发泡法等。关于SiC多孔材料的制备已有一些研究论文和专利，如：
期刊《硅酸盐学报》2004年第34卷第2期第107页至第112页公开了刘岩等撰写的“金属过滤器用高性能SiC泡沫陶瓷的制备”的文章，以Al2O3、膨润土和硅溶胶为烧结助剂，聚氨酯泡沫为模板，D50分别为15.8μm和7.4μm的SiC粉体为原料，经2次挂浆制得抗弯强度达2.87MPa、平均孔径约3mm、抗热震性良好的SiC泡沫陶瓷。
期刊《中国陶瓷工业》2013年第20卷第1期第9页至第11页公开了郭兴忠等撰写的“淀粉为造孔剂制备SiC多孔材料”的论文，报道了以微米SiC为基体，氧化铝和氧化钇为烧结助剂，淀粉为造孔剂，采用无压烧结技术制备SiC多孔材料。
“高温除尘用复合SiC多孔材料制备及性能研究”(白成英，海南大学硕士学位论文，2014年)，利用原位反应结合技术分别制备并研宄了二氧化硅、莫来石、堇青石结合SiC多孔复合陶瓷。
专利(公开号：CN103058708A)报道了一种低热导率氮化硅结合SiC多孔材料的制备方法，其制备工艺是：1)将SiC细粉、水、分散剂和用于凝胶注模成型的单体、交联剂球磨混合得到均匀的浆料；2)在浆料中加入适量发泡剂，将浆料机械搅拌得到泡沫浆料，向泡沫浆料中依次加入适量引发剂和催化剂，并快速浇注于模具中；3)浆料固化后，脱模得到坯体，坯体先后在恒温恒湿箱和普通烘箱中干燥；4)干燥后的坯体先在空气气氛炉内进行排胶，然后在氮气气氛炉内进行烧结，最终得到Si3N4结合SiC多孔材料，可用于铝电解槽外围保温材料。
但是，迄今尚未见关于Sialon结合SiC多孔材料的研究报道。
发明内容
本发明为一种Sialon结合SiC多孔材料的制备方法，工艺简单，操作方便，所制得的Sialon结合SiC多孔材料体积密度小(不大于0.5g/cm3)，导热系数低(1000℃的导热系数不大于0.25w/(m·k))，气孔呈球形，独立、封闭态，分布均匀，大小约0.5～1mm，主要用于高温与腐蚀性气氛的保温隔热。
为实现上述目的，本发明所采用的技术方案是：以65～85质量份的SiC粉、5～15质量份的金属Si粉和10～20质量份的活性氧化铝粉为原料，刚玉球为研磨介质球磨1～5h，混合均匀，制得原料粉体，然后加入40～60质量份的坯体增强剂，0.1～1.0质量份的分散调凝剂，0.1～1.0质量份的硅烷偶联剂，搅拌均匀，制得粘稠度适中的原料浆料，再与三萜皂甙植物发泡剂制得的泡沫混合均匀，制得碳化硅泡沫浆料，经注模成型、干燥、工业氮化炉中1400℃氮化，制得Sialon结合SiC多孔材料。
上述技术方案中：SiC粉的碳化硅含量大于97％，粒度为325目及以下，金属Si粉粒度为200目及以下，活性氧化铝粉为ρ-Al2O3，坯体增强剂为质量浓度1～5％的聚乙烯醇、木质素磺酸钙和淀粉中的一种或其复合的水溶液，分散调凝剂为碳酸钠、六偏磷酸钠、三聚磷酸钠、碳酸锂中的一种或其复合。
采用上述技术方案，活性氧化铝粉(ρ-Al2O3)水化后形成水合物，使泡沫浆料稠化而起到固泡效果，并赋予多孔坯体一定的干燥强度，500℃左右水合物分解生成极其微细的氧化铝粒子；金属硅粉在氮气气氛中氮化生成极其微细的氮化硅粒子，极微细的氮化硅粒子与氧化铝粒子在高温下反应生成Sialon，将碳化硅颗粒结合起来，由此制得Sialon结合SiC多孔材料。添加分散调凝剂分散碳化硅粒子并调节ρ-Al2O3的水化进程，添加硅烷偶联剂改善泡沫与SiC颗粒的界面结合性能。为增强多孔坯体的烘干强度，采用质量浓度为1～5％的聚乙烯醇、木质素磺酸钙和淀粉中的一种或其复合的水溶液作为坯体增强剂。调节泡沫量可制得体积密度低至0.4g/cm3的Sialon结合SiC多孔材料。
经测定，本发明制备的体积密度为0.5g/cm3的Sialon结合SiC多孔材料，常温耐压强度1.5MPa，1000℃导热系数为0.243w/(m.k)，XRD结果分析表明，主晶相为α-SiC和β-Sialon。
具体实施方式
下面结合具体实例对本发明作进一步详细的描述。
本发明不受下述实施例的限制，可根据本发明的技术方案与实际情况来确定具体的实施方式。
实施例1：
一种Sialon结合SiC多孔材料的制备方法。以
A、称取80重量份325目SiC粉、12.5重量份ρ-Al2O3和7.5重量份200目金属Si粉，加入到刚玉球为研磨介质的球磨机中研磨3h，制得原料粉体，备用。
B、称取45～50重量份质量浓度为2％的坯体增强剂，0.1～0.4重量份分散调凝剂，0.2～0.5重量份硅烷偶联剂KH-550，加入到A步骤经均匀混合的原料粉体中，充分搅拌制得粘稠度适中的原料浆体。
C、称取25重量份质量浓度为1％的发泡剂溶液，使用高速搅拌机以2500r.p.m机械搅拌发泡剂溶液3min，制得泡沫；
D、将适量泡沫加入到原料浆体中，搅拌，使浆料与泡沫混合均匀，制得泡沫浆料。
E、将泡沫浆料注模，空气环境下静置一天，使泡沫浆料固化成型，制得湿坯。
F、将湿坯放入烘箱中干燥，室温到60℃缓慢干燥，升温速度不大于2.5℃/h，60℃干燥24h后脱模，然后以5℃/h的速度升至110℃，保温24h，制得干坯。
G、干坯在1400℃下工业氮化炉中氮化，由此制得体积密度约0.6g/cm3的Sialon结合SiC多孔材料。
实施例2：
一种Sialon结合SiC多孔材料的制备方法。以
A、称取75重量份325目SiC粉、15重量份的ρ-Al2O3和10重量份200目金属Si粉，加入到刚玉球为研磨介质的球磨机中研磨3h，制得原料粉体，备用。
B、称取50～55重量份质量浓度为2％的坯体增强剂，0.1～0.4重量份分散调凝剂，0.2～0.5重量份硅烷偶联剂KH-550，加入到A步骤经均匀混合的原料粉体中，充分搅拌制备粘稠度适中的原料浆体。
C、称取25重量份质量浓度为1％的发泡剂溶液，使用高速搅拌机以2500r.p.m的转速机械搅拌发泡剂溶液3min，制得泡沫。
D、将适量泡沫加入到原料浆体中，搅拌，使浆料与泡沫混合均匀，制得泡沫浆料。
E、将泡沫浆料注模，空气环境下静置一天，使泡沫浆料固化成型，制得湿坯。
F、将湿坯放入烘箱中干燥，室温到60℃缓慢干燥，升温速度不大于2.5℃/h，60℃干燥24h后脱模，然后以5℃/h的速度升至110℃，保温24h，制得干坯。
G、干坯在1400℃下工业氮化炉中氮化，由此制得体积密度约0.5g/cm3的Sialon结合SiC多孔材料。
实施例3：
一种Sialon结合SiC多孔材料的制备方法。以
A、称取70重量份d50＝1.5μm的SiC粉、20重量份的ρ-Al2O3和10重量份325目金属Si粉，加入到刚玉球为研磨介质的球磨机中研磨3h，制得原料粉体，备用。
B、称取55～60重量份质量浓度为2％的坯体增强剂，0.2～0.5重量份分散调凝剂，0.2～0.5重量份硅烷偶联剂KH-550，加入到A步骤经均匀混合的原料粉体中，充分搅拌制备粘稠度适中的原料浆体。
C、称取25重量份质量浓度为1％的发泡剂溶液，使用高速搅拌机以2500r.p.m的转速机械搅拌发泡剂溶液3min，制得泡沫。
D、将适量泡沫加入到原料浆体中，搅拌，使浆料与泡沫混合均匀，制得泡沫浆料。
E、将泡沫浆料注模，空气环境下静置一天，使泡沫浆料固化成型，制得湿坯。
F、将湿坯放入烘箱中干燥，室温到60℃缓慢干燥，升温速度不大于2.5℃/h，60℃干燥24h后脱模，然后以5℃/h的速度升至110℃，保温24h，制得干坯。
G、干坯在1400℃下工业氮化炉中氮化，由此制得体积密度约0.4g/cm3的Sialon结合SiC多孔材料。
上述实施例具有较强的适应性和较佳的实施效果，具体实施中可根据实际需要增减非必要的技术特征，来满足不同情况的需求。
上述实施例与现有技术的对比如下：
本发明使用高纯原料，不引入有害成分，材料的高温性能得到保证。ρ-Al2O3具有很高的活性，极易水化形成一定强度的胶结体，利用这一特性固化泡沫浆料。
本发明中ρ-Al2O3的水化产物500℃左右分解生成极微细的氧化铝粒子，与硅粉氮化形成的极微细氮化硅粒子在高温下反应生成Sialon，将碳化硅颗粒结合起来，由此制得Sialon结合SiC多孔材料。
本发明使用泡沫作为气孔来源，通过改变泡沫加入量，可较准确调节制品的体积密度、气孔率和孔径。
本发明的整个工艺过程不会对环境造成污染，是一种环境友好的工艺，且操作简单。
以上所述，仅为本发明较佳的具体实施方案，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。

Claims (8)

1.一种Sialon结合SiC多孔材料的制备方法，其特征在于：以65～85质量份的SiC粉、5～15质量份的金属Si粉和10～20质量份的活性氧化铝粉为原料，刚玉球为研磨介质球磨1～5h，混合均匀制得原料粉体，然后加入40～60质量份坯体增强剂，0.1～1.0质量份分散调凝剂，0.1～1.0质量份硅烷偶联剂，搅拌均匀制得粘稠度适中的原料浆料，再与三萜皂甙植物发泡剂制得的泡沫混合均匀制得碳化硅泡沫浆料，经注模成型、干燥、工业氮化炉中1400℃氮化制得Sialon结合SiC多孔材料。
2.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述的SiC粉碳化硅含量大于97％，粒度为325目及以下。
3.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述的金属Si粉粒度为200目及以下。
4.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述的活性氧化铝粉为ρ-Al2O3。
5.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述坯体增强剂为质量浓度1～5％的聚乙烯醇、木质素磺酸钙和淀粉中的一种或其复合的水溶液。
6.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述的分散调凝剂为碳酸钠、六偏磷酸钠、三聚磷酸钠、碳酸锂中的一种或其复合。
7.根据权利要求1所述的Sialon结合SiC多孔材料的制备方法，其特征在于：所述的硅烷偶联剂为KH-550。
8.一种Sialon结合SiC多孔材料，由根据权利要求1～7项中任一项所述的Sialon结合SiC多孔材料的制备方法所制备得到。
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