CN106478132A - 氮化硅多孔陶瓷材料及其制备方法 - Google Patents

氮化硅多孔陶瓷材料及其制备方法 Download PDF

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CN106478132A
CN106478132A CN201610826904.9A CN201610826904A CN106478132A CN 106478132 A CN106478132 A CN 106478132A CN 201610826904 A CN201610826904 A CN 201610826904A CN 106478132 A CN106478132 A CN 106478132A
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silicon nitride
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李洋洋
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Zhengzhou Foamtech Nano Material Co Ltd
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Abstract

本发明提出了一种氮化硅多孔陶瓷材料及其制备方法，包括以下原料：陶瓷粉末30～60wt％，水玻璃1～3wt％，分散剂0.5～1.5wt％，余量为水；将原料制成浆料以软质有机泡沫塑料为载体，经浸渍料浆、挤压制成坯体后烧结制成即可；其中，陶瓷粉末由氮化硅70～80wt％、高岭土10～20wt％、氧化石墨烯5～10wt％、氧化铝1～5wt％与黄砂1～5wt％组成。该陶瓷材料孔隙均匀，且孔隙率＞80％，热化学稳定性好，陶瓷筋强度高。

Description

氮化硅多孔陶瓷材料及其制备方法
技术领域
本发明属于功能陶瓷技术领域，具体涉及一种氮化硅多孔陶瓷材料及其制备方法。
背景技术
氮化硅陶瓷具有耐高温、耐腐蚀、抗热震、抗氧化、耐磨损等良好的高低温综合性能，广泛应用在航天航空、汽车发动机、机械、化工、石油等领域。利用其优良的高温性能、高的热导率、良好的抗热震性能和化学稳定性，以及不被铝、铅、锡、银、黄铜、镍等很多种熔融金属或合金所浸润或腐蚀的特性，可用于上述金属的冶炼及熔融金属的过滤。
泡沫陶瓷材料始于20世纪70年代，是一种具有高温特性的多孔材料，我国在20世纪80年代初开展泡沫陶瓷研究工作，近20年来，先后有十几家科研机构和厂家报道了泡沫陶瓷制备的研究。泡沫陶瓷由于具有气孔率高、比表面积大、抗热震、耐高温、耐化学腐蚀及良好的机械强度和过滤吸附性能，广泛应用于热交换材料、布气材料，汽车尾气装置，净化冶金工业过滤熔融态金属，热能回收，轻工喷涂行业，工业污水处理，隔热隔音材料，用作化学催化剂载体，电解隔膜及分类分散元件等。因此，制备高强度、孔径均匀、性能稳定的泡沫陶瓷体，拓宽和开发泡沫陶瓷在国内外多个行业中的应用十分必要。
泡沫陶瓷采用聚氨酯泡沫塑料为载体，将其浸入由陶瓷粉末、粘结剂、助烧结剂、悬浮剂等制成的料浆中，然后挤掉多余料浆，使陶瓷浆料均匀涂覆于载体骨架成为坯体，再将坯体干燥并经高温烧结而成。泡沫陶瓷具有与泡沫塑料相似的孔隙结构，通孔率达85～90％。国内外已根据不同合金的特点，发展了多种不同材质的泡沫陶瓷，如美国专利3893917、3962081、4024056、4075303，中国国家专利87101800.4、92102883.0、200710139286.1、200710139289.5等，这些泡沫陶瓷由氧化铝、氧化硅、氧化锆、氮化硅等材料制成，可用于过滤一般的铝合金、铜合金、铸钢、铸铁等。
发明内容
本发明提出一种氮化硅多孔陶瓷材料，该陶瓷材料孔隙均匀，且孔隙率＞80％，热化学稳定性好，陶瓷筋强度高。
本发明的技术方案是这样实现的：
一种氮化硅多孔陶瓷材料，包括以下原料：
陶瓷粉末30～60wt％，水玻璃1～3wt％，分散剂0.5～1.5wt％，余量为水；将原料制成浆料以软质有机泡沫塑料为载体，经浸渍料浆、挤压制成坯体后烧结制成即可；其中，陶瓷粉末由氮化硅70～80wt％、高岭土10～20wt％、氧化石墨烯5～10wt％、氧化铝1～5wt％与黄砂1～5wt％组成。
进一步，软质聚氨酯泡沫塑料是在50～60℃温度的pH值为9～11的碱溶液中浸泡20～30min，然后先用3.0～6.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.5～1.5wt％的磺酸盐做表面活性处理。
进一步，所述分散剂为羧甲基纤维素钠。
本发明的另一个目的是提供一种氮化硅多孔陶瓷材料的制备方法，包括以下步骤：
1)浆料制备：向陶瓷粉末中加入水玻璃、分散剂与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在100℃～120℃干燥硬化；
4)干燥后的坯料装入烧结炉，在氮气气氛下，升温至900℃～1150℃烧结即可。
进一步，软质聚氨酯泡沫塑料是在50～60℃温度的pH值为9～11的碱溶液中浸泡20～30min，然后先用3.0～6.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.5～1.5wt％的磺酸盐做表面活性处理。具有网状结构、有弹性且能恢复原来形状的可燃性有机泡沫塑料，由很多互联空隙组成泡沫结构，并能在较低温度下以氧化等方式转化成气态排出。采用高浓度的聚乙烯亚胺溶液活化聚氨酯泡沫塑料然后用磺酸盐做表面活性处理，不仅能够提高陶瓷材料的强度，还能克服由于浓度过高聚乙烯亚胺在烧结过程中抑制陶瓷材料强度。
进一步，磺酸盐为木质素磺酸钠或者十二烷基磺酸钠。
进一步，软质聚氨酯泡沫塑料的孔径为40～10PPI。
本发明有益效果：
1、本发明陶瓷粉末采用高岭土、氧化石墨烯、氧化铝与黄砂作为烧结助剂，一方面可以降低烧结温度，另一方面有利于形成更多的气泡，促进陶瓷内部形成三维网状结构，大大提高了陶瓷筋的强度。
2、本发明氮化硅多孔陶瓷材料，配料科学合理，采用的软质聚氨酯泡沫塑料孔径适宜，制得的氮化硅泡沫陶瓷成空间网状结构，孔洞互联，孔隙率可达80～96％，抗压强度达到10MPa，并且热化学稳定性好。
具体实施方式
实施例1
陶瓷粉末由氮化硅70wt％、高岭土10wt％、氧化石墨烯10wt％、氧化铝5wt％与黄砂5wt％组成。
原料配比为：陶瓷粉末60wt％，水玻璃3wt％，羧甲基纤维素钠1.5wt％，余量为水。
选用40PPI的软质聚氨酯泡沫塑料，在50℃温度的pH值为9的碱溶液中浸泡30min，然后先用3.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.5wt％的木质素磺酸钠做表面活性处理。
制备方法：
1)浆料制备：向陶瓷粉末中加入水玻璃、羧甲基纤维素钠与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在100℃干燥硬化，然后在氧化气氛下从室温以40℃/h的速率升温500℃排塑，使泡沫塑料完全挥发，然后以150℃/h的升温速度升温至800℃下保温1h，使素坯具有一定强度；
4)然后将素坯，转移到气氛压力烧结炉内，升温至1150℃保温2h，自然冷去至室温，即可获得氮化硅多孔陶瓷材料。
实施例2
陶瓷粉末由氮化硅75wt％、高岭土15wt％、氧化石墨烯5wt％、氧化铝2wt％与黄砂3wt％组成。
原料配比为：陶瓷粉末50wt％，水玻璃2wt％，羧甲基纤维素钠1wt％，余量为水。
选用30PPI的软质聚氨酯泡沫塑料，在55℃温度的pH值为10的碱溶液中浸泡25min，然后先用4.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.8wt％的木质素磺酸钠做表面活性处理。
制备方法：
1)浆料制备：向陶瓷粉末中加入水玻璃、羧甲基纤维素钠与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在110℃干燥硬化，然后在氧化气氛下从室温以50℃/h的速率升温500℃排塑，使泡沫塑料完全挥发，然后以150℃/h的升温速度升温至800℃下保温1h，使素坯具有一定强度；
4)然后将素坯，转移到气氛压力烧结炉内，升温至1100℃保温4h，自然冷去至室温，即可获得氮化硅多孔陶瓷材料。
实施例3
陶瓷粉末由氮化硅80wt％、高岭土10wt％、氧化石墨烯5wt％、氧化铝1wt％与黄砂4wt％组成。
原料配比为：陶瓷粉末40wt％，水玻璃1wt％，羧甲基纤维素钠1wt％，余量为水。
选用20PPI的软质聚氨酯泡沫塑料，在60℃温度的pH值为10.5的碱溶液中浸泡20min，然后先用5.0wt％聚乙烯亚胺溶液做表面活性处理，再用1.2wt％的十二烷基磺酸钠做表面活性处理。
制备方法：
1)浆料制备：向陶瓷粉末中加入水玻璃、羧甲基纤维素钠与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在120℃干燥硬化，然后在氧化气氛下从室温以50℃/h的速率升温500℃排塑，使泡沫塑料完全挥发，然后以150℃/h的升温速度升温至700℃下保温1h，使素坯具有一定强度；
4)然后将素坯，转移到气氛压力烧结炉内，升温至950℃保温5h，自然冷去至室温，即可获得氮化硅多孔陶瓷材料。
实施例4
陶瓷粉末由氮化硅70wt％、高岭土15wt％、氧化石墨烯10wt％、氧化铝4wt％与黄砂1wt％组成。
原料配比为：陶瓷粉末40wt％，水玻璃1wt％，羧甲基纤维素钠0.5wt％，余量为水。
选用10PPI的软质聚氨酯泡沫塑料，在60℃温度的pH值为11的碱溶液中浸泡20min，然后先用6.0wt％聚乙烯亚胺溶液做表面活性处理，再用1.5wt％的十二烷基磺酸钠做表面活性处理。
制备方法：
1)浆料制备：向陶瓷粉末中加入水玻璃、羧甲基纤维素钠与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在120℃干燥硬化，然后在氧化气氛下从室温以20℃/h的速率升温600℃排塑，使泡沫塑料完全挥发，然后以200℃/h的升温速度升温至700℃下保温1h，使素坯具有一定强度；
4)然后将素坯，转移到气氛压力烧结炉内，升温至1100℃保温6h，自然冷去至室温，即可获得氮化硅多孔陶瓷材料。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种氮化硅多孔陶瓷材料，其特征在于，包括以下原料：
陶瓷粉末30～60wt％，水玻璃1～3wt％，分散剂0.5～1.5wt％，余量为水；将原料制成浆料以软质有机泡沫塑料为载体，经浸渍料浆、挤压制成坯体后烧结制成即可；其中，陶瓷粉末由氮化硅70～80wt％、高岭土10～20wt％、氧化石墨烯5～10wt％、氧化铝1～5wt％与黄砂1～5wt％组成。
2.根据权利要求1所述的氮化硅多孔陶瓷材料，其特征在于，软质聚氨酯泡沫塑料是在50～60℃温度的pH值为9～11的碱溶液中浸泡20～30min，然后先用3.0～6.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.5～1.5wt％的磺酸盐做表面活性处理。
3.根据权利要求1所述的氮化硅多孔陶瓷材料，其特征在于，所述分散剂为羧甲基纤维素钠。
4.如权利要求1所述的氮化硅多孔陶瓷材料的制备方法，其特征在于，包括以下步骤：
1)浆料制备：向陶瓷粉末中加入水玻璃、分散剂与水搅拌混合均匀，制成浆料；
2)以软质聚氨酯泡沫塑料为载体，浸渍上述浆料，并挤压制成坯料；
3)坯料放入干燥箱内，在100℃～120℃干燥硬化；
4)干燥后的坯料装入烧结炉，在氮气气氛下，升温至900℃～1150℃烧结即可。
5.根据权利要求4所述的氮化硅多孔陶瓷材料的制备方法，其特征在于，软质聚氨酯泡沫塑料是在50～60℃温度的pH值为9～11的碱溶液中浸泡20～30min，然后先用3.0～6.0wt％聚乙烯亚胺溶液做表面活性处理，再用0.5～1.5wt％的磺酸盐做表面活性处理。
6.根据权利要求5所述的氮化硅多孔陶瓷材料的制备方法，其特征在于，磺酸盐为木质素磺酸钠或者十二烷基磺酸钠。
7.根据权利要求5所述的氮化硅多孔陶瓷材料的制备方法，其特征在于，软质聚氨酯泡沫塑料的孔径为40～10PPI。
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