CN108821774A - 多孔氮化硅-碳化硅复合陶瓷的制备方法 - Google Patents

多孔氮化硅-碳化硅复合陶瓷的制备方法 Download PDF

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CN108821774A
CN108821774A CN201810699803.9A CN201810699803A CN108821774A CN 108821774 A CN108821774 A CN 108821774A CN 201810699803 A CN201810699803 A CN 201810699803A CN 108821774 A CN108821774 A CN 108821774A
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silicon nitride
titanium dioxide
composite ceramic
porous silicon
carbide composite
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CN108821774B (zh
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章波
郭元
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LINSHU DONGSHENG ABRASIVE Co.,Ltd.
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Wuhu Corey Yuen New Mstar Technology Ltd
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Abstract

本发明提出了一种多孔氮化硅‑碳化硅复合陶瓷的制备方法，包括以下步骤：1)按照重量百分数计算，称取氮化硅粉体30～60％、碳化硅粉体15～40％、改性二氧化钛6～15％、稀土氧化物2～5％及结合剂3～6％备用；2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与稀土氧化物混合后，再加入结合剂混合均匀，干压成型得到素坯；3)将素坯在氮气气氛下以1～10℃/min的升温速度升温到1500～1650℃，保温2～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅‑碳化硅复合陶瓷；其中，改性二氧化钛主要由二氧化钛、椰壳粉与羟甲基纤维素制备得到。该制备方法烧结温度较低，获得的多孔氮化硅‑碳化硅复合陶瓷气孔率高且断裂韧性高。

Description

多孔氮化硅-碳化硅复合陶瓷的制备方法
技术领域
本发明属于陶瓷制备技术领域，具体涉及一种多孔氮化硅-碳化硅复合陶瓷的制备方法。
背景技术
多孔陶瓷普遍具有轻质、隔热、耐热、耐蚀的特点，广泛地应用于过滤、催化、吸音、气敏及人工骨等领域。与氧化物基多孔陶瓷相比，多孔Si3N4陶瓷强度高、介电常数低且稳定，在军事电子工业方面作为一种新型的“结构-功能”一体化材料有应用前景，引起了广泛的研究。
多孔陶瓷的制备有添加造孔剂法、模板复制法、发泡法、颗粒堆积法、溶胶凝胶法等。其中添加造孔剂法、模板复制法、发泡法、溶胶凝胶法均需要另外添加造孔剂、模板、发泡剂、引发剂、催化剂等有机试剂使成型工艺复杂，需要考虑的影响因素增多，增加了生产成本。采用现有方法制备的多孔氮化硅-碳化硅复合陶瓷均存在一些缺陷，有些由于产品中存在未反应的硅粉导致陶瓷的耐蚀性及耐热性较差，有些产品抗弯强度较低，有些存在烧结温度较高、制备工艺复杂及生产成本较高的缺陷。
发明内容
本发明提出一种多孔氮化硅-碳化硅复合陶瓷的制备方法，该制备方法烧结温度较低，获得的多孔氮化硅-碳化硅复合陶瓷气孔率高且断裂韧性高。
本发明的技术方案是这样实现的：
一种多孔氮化硅-碳化硅复合陶瓷的制备方法，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体30～60％、碳化硅粉体15～40％、改性二氧化钛6～15％、稀土氧化物2～5％及结合剂3～6％备用；
2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与稀土氧化物混合后，再加入结合剂混合均匀，干压成型得到素坯；
3)将素坯在氮气气氛下以1～10℃/min的升温速度升温到1500～1650℃，保温2～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅-碳化硅复合陶瓷；
其中，所述改性二氧化钛主要由二氧化钛、椰壳粉与羟甲基纤维素制备得到。
作为优选，所述改性二氧化钛的制备方法包括以下步骤：
1)将二氧化钛与羟甲基纤维素溶于醇溶剂中，然后加热至40～50℃搅拌混合均匀，即可获得混合液；
2)将椰壳粉加入到步骤1)的混合液搅拌混合后干燥，再在氮气气氛下450～650℃进行焙烧3～5h，冷却至室温，粉磨即可。
作为优选，所述二氧化钛与所述羟甲基纤维素的质量之比为1:0.03～0.06，所述二氧化钛与所述椰壳粉的质量之比为1:0.1～0.3。
作为优选，所述醇溶剂选自乙醇、丙醇与丁二醇中的一种或者多种。
作为优选，稀土氧化物为氧化钇。
作为优选，所述结合剂为树脂或者聚乙二醇。
作为优选，干压成型压力为6～18MPa。
本发明的有益效果：
本发明采用主要由二氧化钛、椰壳粉与羟甲基纤维素制备得到的改性二氧化钛作为烧结助剂，能够有效地降低陶瓷材料的烧结温度,制备出断裂韧性高的氮化硅陶瓷材料。
本发明中的改性二氧化钛中以椰壳粉参与作为改性剂，其能够显著减少晶界氧化物含量，还提高陶瓷气孔的开孔率。
本发明制备的多孔氮化硅-碳化硅复合陶瓷的开孔率为52～60％，断裂韧性为12.1～13.6MPa·m1/2,抗弯强度达到52.5～65.1MPa。
具体实施方式
实施例1
改性二氧化钛的制备方法包括以下步骤：
1)将二氧化钛与羟甲基纤维素溶于乙醇中，然后加热至40℃搅拌混合均匀，即可获得混合液；
2)将椰壳粉加入到步骤1)的混合液搅拌混合后干燥，再在氮气气氛下650℃进行焙烧3h，冷却至室温，粉磨即可。二氧化钛与羟甲基纤维素的质量之比为1:0.03，二氧化钛与椰壳粉的质量之比为1:0.1。
实施例2
改性二氧化钛的制备方法包括以下步骤：
1)将二氧化钛与羟甲基纤维素溶于丁二醇中，然后加热至50℃搅拌混合均匀，即可获得混合液；
2)将椰壳粉加入到步骤1)的混合液搅拌混合后干燥，再在氮气气氛下450℃进行焙烧5h，冷却至室温，粉磨即可。二氧化钛与羟甲基纤维素的质量之比为1:0.06，二氧化钛与椰壳粉的质量之比为1:0.3。
实施例3
一种多孔氮化硅-碳化硅复合陶瓷的制备方法，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体40％、碳化硅粉体35％、实施例1的改性二氧化钛15％、氧化钇4％及聚乙二醇6％备用；
2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与氧化钇混合后，再加入聚乙二醇混合均匀，干压成型得到素坯；
3)将素坯在氮气气氛下以5℃/min的升温速度升温到1600℃，保温8小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅-碳化硅复合陶瓷。
本实施例制备的多孔氮化硅-碳化硅复合陶瓷的开孔率为60％，断裂韧性为12.1MPa·m1/2,抗弯强度达到65.1MPa。
实施例4
一种多孔氮化硅-碳化硅复合陶瓷的制备方法，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体60％、碳化硅粉体29％、改性二氧化钛6％、氧化钇2％及树脂3％备用；
2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与氧化钇混合后，再加入树脂混合均匀，干压成型得到素坯；
3)将素坯在氮气气氛下以1℃/min的升温速度升温到1500℃，保温10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅-碳化硅复合陶瓷。
本实施例制备的多孔氮化硅-碳化硅复合陶瓷的开孔率为52％，断裂韧性为12.1MPa·m1/2,抗弯强度达到52.5MPa。
实施例5
一种多孔氮化硅-碳化硅复合陶瓷的制备方法，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体40％、碳化硅粉体40％、实施例2的改性二氧化钛9％、氧化钇5％及聚乙二醇6％备用；
2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与氧化钇混合后，再加入聚乙二醇混合均匀，干压成型得到素坯；
3)将素坯在氮气气氛下以10℃/min的升温速度升温到1650℃，保温2小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅-碳化硅复合陶瓷。
本实施例制备的多孔氮化硅-碳化硅复合陶瓷的开孔率为57％，断裂韧性为12.9MPa·m1/2,抗弯强度达到62.1MPa。
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 (6)

1.一种多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体30～60％、碳化硅粉体15～40％、改性二氧化钛6～15％、稀土氧化物2～5％及结合剂3～6％备用；
2)先将氮化硅粉体、碳化硅粉体、改性二氧化钛与稀土氧化物混合后，再加入结合剂混合均匀，干压成型得到素坯；
3)将素坯在氮气气氛下以1～10℃/min的升温速度升温到1500～1650℃，保温2～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅-碳化硅复合陶瓷；
其中，所述改性二氧化钛主要由二氧化钛、椰壳粉与羟甲基纤维素制备得到。
2.根据权利要求1所述的多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，所述改性二氧化钛的制备方法包括以下步骤：
1)将二氧化钛与羟甲基纤维素溶于醇溶剂中，然后加热至40～50℃搅拌混合均匀，即可获得混合液；
2)将椰壳粉加入到步骤1)的混合液搅拌混合后干燥，再在氮气气氛下450～650℃进行焙烧3～5h，冷却至室温，粉磨即可。
3.根据权利要求2所述的多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，所述二氧化钛与所述羟甲基纤维素的质量之比为1:0.03～0.06，所述二氧化钛与所述椰壳粉的质量之比为1:0.1～0.3。
4.根据权利要求2所述的多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，所述醇溶剂选自乙醇、丙醇与丁二醇中的一种或者多种。
5.根据权利要求1所述的多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，稀土氧化物为氧化钇。
6.根据权利要求1所述的多孔氮化硅-碳化硅复合陶瓷的制备方法，其特征在于，所述结合剂为树脂或者聚乙二醇。
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