CN106588022B - 一种利用模板法制备碳化硅泡沫陶瓷的工艺 - Google Patents

一种利用模板法制备碳化硅泡沫陶瓷的工艺 Download PDF

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CN106588022B
CN106588022B CN201611172913.7A CN201611172913A CN106588022B CN 106588022 B CN106588022 B CN 106588022B CN 201611172913 A CN201611172913 A CN 201611172913A CN 106588022 B CN106588022 B CN 106588022B
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吴德炳
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Qingdao Dong Tong refractory material Co., Ltd.
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Abstract

本发明涉及一种利用模板法制备碳化硅泡沫陶瓷的工艺，属于多孔材料技术领域。本发明采用有机物模板法制备碳化硅泡沫陶瓷，主要是利用在碳化硅颗粒上先包覆一层有机物模板，再将其与无机纤维进行混合并形成泡沫原料，利用模板剂防止无机纤维陷入碳化硅颗粒的表面微孔中，烧结之后去除模板，利用无机纤维与颗粒物的紧固实现了提高泡沫陶瓷的机械强度的效果。

Description

一种利用模板法制备碳化硅泡沫陶瓷的工艺
技术领域
本发明涉及一种利用模板法制备碳化硅泡沫陶瓷的工艺，属于多孔材料技术领域。
背景技术
泡沫陶瓷是一种无机非金属材料，是以陶瓷原矿、页岩、陶瓷工业废渣、粉煤灰、煤矸石、大理石尾矿、炉渣等等无机材料作为主要原料．掺加一定比例的发泡剂、助溶剂等经混合、制粉、填料工艺，再经高温焙烧而成的高气孔率的陶瓷材料。泡沫陶瓷采用的是低值低质的页岩、工业废渣，对环境的保护和降低能耗有更大的优势。在同等导热系数值时，泡沫陶瓷的抗压强度和抗折强度要大于泡沫玻璃。使用更安全。
作为一种新型的无机非金属过滤材料，泡沫陶瓷具有质量轻、强度高、耐高温、耐腐蚀、再生简单、使用寿命长及良好的过滤吸附性等优点，与传统的过滤器如陶瓷颗粒烧结体、玻璃纤维布相比，不仅操作简单，节约能源，成本低，而且过滤效果好。泡沫陶瓷可以广泛地应用于冶金、化工、轻工、食品、环保、节能等领域。
泡沫陶瓷材料的制备方法很多 ，其中应用比较成功的有 :有机物燃烧法、添加造孔剂法、发泡法、有机前驱体浸渍法及溶胶-凝胶方法等。
CN104311136A公开一种氮化硅、碳化硅结合碳化硼泡沫陶瓷的制备方法，将B4C、硅微粉、酚醛树脂外加羟丙基甲基纤维素溶液均匀混合制成陶瓷浆料，然后将陶瓷浆料浸渍在聚氨酯泡沫上，干燥后在氮气气氛中烧制成氮化硅、碳化硅结合碳化硼泡沫陶瓷。CN103641508A公开了一种免烧结地聚合物泡沫陶瓷的制备方法，先将废旧陶瓷研磨成粉末，然后将100份陶瓷粉，30~60份碱激发剂和1~5份发泡剂混合搅拌均匀，倒入模具中，放入60℃混凝土养护箱中养护24h后脱膜，继续养护28d即可得到。
但是上述的技术只关注于泡沫陶瓷的保温性能，其机械强度低的问题没有得到解决。
发明内容
本发明的目的是提供一种具有高强度的碳化硅泡沫陶瓷。
技术方案是：
一种利用模板法制备碳化硅泡沫陶瓷的工艺，包括如下步骤：
第1步，按重量份计，将碳化硅粉体20～30份、碳酸钠10～15份，混合均匀后，放置于石英舟中，加热升温至720～740℃，升温速度是6～10℃/分，保温，保温时间是4～5分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅20～30份、脂肪酸4～10份、有机溶剂10～20份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将的硝酸铝4～6份、5～10wt%的氨水50～100份、阴离子表面活性剂0.5～3份均匀混合，于110℃～130℃密闭保温反应4～6h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在500～550℃下煅烧5～7h，自然冷却至室温，即得氧化铝纳米纤维；
第4步，按重量份计，将包覆有机物模板的碳化硅粉体30～40份、氧化铝纳米纤维4～5份、水200～280份混合均匀，进行球磨，再加入非离子表面活性剂0.5～2份，高速分散后，得到泡沫原料，再经过减压干燥之后，进行烧结后，得到泡沫陶瓷。
所述的第2步中，脂肪酸是含有12～18个碳原子的直链或者带支链的脂肪酸；有机溶剂是酯类或者酮类溶剂。例如：乙酸乙酯或者丙酮等。
所述的第4步中，减压干燥的温度是80～90℃；烧结步骤的程序是：以4～8℃/分的速度升温至1200～1300℃，保持3～6h，再自然冷却。
有益效果
本发明采用有机物模板法制备碳化硅泡沫陶瓷，主要是利用在碳化硅颗粒上先包覆一层有机物模板，再将其与无机纤维进行混合并形成泡沫原料，利用模板剂防止无机纤维陷入碳化硅颗粒的表面微孔中，烧结之后去除模板，利用无机纤维与颗粒物的紧固实现了提高泡沫陶瓷的机械强度的效果。
具体实施方式
实施例1
第1步，按重量份计，将碳化硅粉体20份、碳酸钠10份，混合均匀后，放置于石英舟中，加热升温至720℃，升温速度是6℃/分，保温，保温时间是4分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅20份、硬脂酸4份、乙酸乙酯10份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将的硝酸铝4份、5wt%的氨水50份、阴离子表面活性剂0.5份均匀混合，于110℃密闭保温反应4h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在500℃下煅烧5h，自然冷却至室温，即得氧化铝纳米纤维；
第4步，按重量份计，将包覆有机物模板的碳化硅粉体30份、氧化铝纳米纤维4份、水200份混合均匀，进行球磨，再加入非离子表面活性剂0.5份，高速分散后，得到泡沫原料，再经过80℃的减压干燥之后，进行烧结，烧结步骤的程序是：以4℃/分的速度升温至1200℃，保持3h，再自然冷却，得到泡沫陶瓷。
实施例2
第1步，按重量份计，将碳化硅粉体30份、碳酸钠15份，混合均匀后，放置于石英舟中，加热升温至740℃，升温速度是10℃/分，保温，保温时间是5分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅30份、硬脂酸10份、乙酸乙酯20份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将的硝酸铝6份、10wt%的氨水100份、阴离子表面活性剂3份均匀混合，于130℃密闭保温反应6h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在550℃下煅烧7h，自然冷却至室温，即得氧化铝纳米纤维；
第4步，按重量份计，将包覆有机物模板的碳化硅粉体40份、氧化铝纳米纤维5份、水280份混合均匀，进行球磨，再加入非离子表面活性剂2份，高速分散后，得到泡沫原料，再经过90℃的减压干燥之后，进行烧结，烧结步骤的程序是：以8℃/分的速度升温至1300℃，保持6h，再自然冷却，得到泡沫陶瓷。
实施例3
第1步，按重量份计，将碳化硅粉体25份、碳酸钠12份，混合均匀后，放置于石英舟中，加热升温至730℃，升温速度是8℃/分，保温，保温时间是4分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅25份、硬脂酸5份、乙酸乙酯15份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将的硝酸铝5份、8wt%的氨水90份、阴离子表面活性剂2份均匀混合，于120℃密闭保温反应5h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在520℃下煅烧6h，自然冷却至室温，即得氧化铝纳米纤维；
第4步，按重量份计，将包覆有机物模板的碳化硅粉体35份、氧化铝纳米纤维4份、水250份混合均匀，进行球磨，再加入非离子表面活性剂1份，高速分散后，得到泡沫原料，再经过85℃的减压干燥之后，进行烧结，烧结步骤的程序是：以6℃/分的速度升温至1250℃，保持5h，再自然冷却，得到泡沫陶瓷。
对照例1
与实施例3的区别在于：未采用模板法加入硬脂酸，直接采用刻蚀碳化硅与氧化铝纤维制备泡沫陶瓷。
第1步，按重量份计，将碳化硅粉体25份、碳酸钠12份，混合均匀后，放置于石英舟中，加热升温至730℃，升温速度是8℃/分，保温，保温时间是4分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将的硝酸铝5份、8wt%的氨水90份、阴离子表面活性剂2份均匀混合，于120℃密闭保温反应5h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在520℃下煅烧6h，自然冷却至室温，即得氧化铝纳米纤维；
第3步，按重量份计，将刻蚀碳化硅35份、氧化铝纳米纤维4份、水250份混合均匀，进行球磨，再加入非离子表面活性剂1份，高速分散后，得到泡沫原料，再经过85℃的减压干燥之后，进行烧结，烧结步骤的程序是：以6℃/分的速度升温至1250℃，保持5h，再自然冷却，得到泡沫陶瓷。
对照例2
与实施例3的区别在于：未加入氧化铝纳米纤维，其重量由碳化硅代替。
第1步，按重量份计，将碳化硅粉体25份、碳酸钠12份，混合均匀后，放置于石英舟中，加热升温至730℃，升温速度是8℃/分，保温，保温时间是4分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅25份、硬脂酸5份、乙酸乙酯15份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将包覆有机物模板的碳化硅粉体39份、水250份混合均匀，进行球磨，再加入非离子表面活性剂1份，高速分散后，得到泡沫原料，再经过85℃的减压干燥之后，进行烧结，烧结步骤的程序是：以6℃/分的速度升温至1250℃，保持5h，再自然冷却，得到泡沫陶瓷。
从上表中可以看出，本发明提供的泡沫陶瓷具有密度小、机械强度高、保温性能好的优点，其导热系数可以在0.035 W/(m·K)以下，抗压强度可以在0.3Mpa以上，抗折强度在0.20Mpa以上 ；实施例3相对于对照例1来说，由于未加入硬脂酸作为模板剂，因此导致了无机纤维会与碳化硅之间的交错性提高，进而导致了闭气孔率明显下降，保温性能也随之下降；而实施例3相对于对照例2来说，通过加入无机纤维作为辅助组分，可以与碳化硅之间在烧结之后形成顶部连接，利用无机纤维提高了整体的陶瓷材料的机械强度。

Claims (3)

1.一种利用模板法制备碳化硅泡沫陶瓷的工艺，其特征在于，包括如下步骤：
第1步，按重量份计，将碳化硅粉体20～30份、碳酸钠10～15份，混合均匀后，放置于石英舟中，加热升温至720～740℃，升温速度是6～10℃/分，保温，保温时间是4～5分钟，放冷后，将固体物用稀盐酸洗涤至恒重，得到刻蚀碳化硅；
第2步，按重量份计，将刻蚀碳化硅20～30份、脂肪酸4～10份、有机溶剂10～20份混合均匀，升温回流，放冷后，将固体物滤出，减压蒸出有机溶剂，得到包覆有机物模板的碳化硅粉体；
第3步，按重量份计，将硝酸铝4～6份、5～10wt%的氨水50～100份、阴离子表面活性剂0.5～3份均匀混合，于110℃～130℃密闭保温反应4～6h后自然冷却，对产物进行抽滤、洗涤、干燥，再将得到的产物在500～550℃下煅烧5～7h，自然冷却至室温，即得氧化铝纳米纤维；
第4步，按重量份计，将包覆有机物模板的碳化硅粉体30～40份、氧化铝纳米纤维4～5份、水200～280份混合均匀，进行球磨，再加入非离子表面活性剂0.5～2份，高速分散后，得到泡沫原料，再经过减压干燥之后，进行烧结后，得到泡沫陶瓷。
2.根据权利要求1所述的利用模板法制备碳化硅泡沫陶瓷的工艺，其特征在于，所述的第2步中，脂肪酸是含有12～18个碳原子的直链或者带支链的脂肪酸；有机溶剂是酯类或者酮类溶剂。
3.根据权利要求1所述的利用模板法制备碳化硅泡沫陶瓷的工艺，其特征在于，所述的第4步中，减压干燥的温度是80～90℃；烧结步骤的程序是：以4～8℃/分的速度升温至1200～1300℃，保持3～6h，再自然冷却。
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