CN108558412B - 多孔氮化硅陶瓷材料的制备方法 - Google Patents

多孔氮化硅陶瓷材料的制备方法 Download PDF

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CN108558412B
CN108558412B CN201810701180.4A CN201810701180A CN108558412B CN 108558412 B CN108558412 B CN 108558412B CN 201810701180 A CN201810701180 A CN 201810701180A CN 108558412 B CN108558412 B CN 108558412B
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silicon nitride
titanium dioxide
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章波
郭元
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Yangzhou Aisipai Electric Appliance Co ltd
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Abstract

本发明提出了一种多孔氮化硅陶瓷材料的制备方法，包括以下步骤：1)按照重量百分数计算，称取氮化硅粉体60～90％、改性二氧化钛1～20％与纳米氧化镁2～6％，混合均匀得到混合料；2)将步骤1)的混合料加入到质量浓度为0.5％～10％聚乙二醇溶液中，进行球磨，球磨时间为2～24h，浆料烘干、过筛，然后模压成型为坯件；3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以1℃/min的升温速度升温到1500～1650℃，保温1～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即可；其中，改性二氧化钛主要由二氧化钛、秸秆粉与羟甲基纤维素制备得到。该制备方法烧结温度较低，获得的多孔氮化硅陶瓷材料气孔率高且断裂韧性高。

Description

多孔氮化硅陶瓷材料的制备方法
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陶瓷材料的制备方法。
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。
根据所用起始粉末的不同，现有的多孔氮化硅陶瓷材料的制备方法有以下几种：非全致密烧结留孔法制备多孔Si3N4陶瓷通常以α-Si3N4粉末为原料，同时使用一定量的添加剂，包括Al2O3、Y2O3及纳米氧化镁等，在氮气氛中 1650-2200℃烧结。添加剂与Si3N4原料中混有的SiO2杂质在高温下生成一定量的液相，一方面实现Si3N4的α→β转变和β-Si3N4棒晶的生长，另一方面将β-Si3N4棒晶牢固地结合，提高多孔Si3N4陶瓷力学强度。由于Si3N4陶瓷的致密化程度与液相量密切相关，通过调节添加剂用量和烧结工艺，可达到控制气孔率的目的，但气孔率一般在30％左右，超过60％则烧结困难。碳热还原法，如中国专利200610041867.7中提出了碳热还原法制备多孔氮化硅的方法。在高温下由二氧化硅在氮气中引发3SiO2+6C+2N2→Si3N4+6CO的反应生成氮化硅，利用上述反应也尝试制备了多孔氮化硅陶瓷材料。不足之处是碳热还原法需要少量的氮化硅作为晶种，一定程度上提高了生产成本，由于反应有44％的失重导致烧结过程中产品有较大的收缩，对生产要求形状构件非常不利。
综上，采用现有方法制备的多孔氮化硅陶瓷材料均存在一些缺陷，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陶瓷材料的制备方法，该制备方法烧结温度较低，获得的多孔氮化硅陶瓷材料气孔率高且断裂韧性高。
本发明的技术方案是这样实现的：
一种多孔氮化硅陶瓷材料的制备方法，包括以下步骤：
1)按照重量百分数计算，称取氮化硅粉体60～90％、改性二氧化钛1～20％与纳米氧化镁2～6％，混合均匀得到混合料；
2)将步骤1)的混合料加入到质量浓度为0.5％～10％聚乙二醇溶液中，进行球磨，球磨时间为2～24h，浆料烘干、过筛，然后模压成型为坯件；
3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以1℃/min的升温速度升温到1500～1650℃，保温1～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅陶瓷材料；
其中，所述改性二氧化钛主要由二氧化钛、秸秆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)将秸秆粉加入到步骤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秸秆粉的质量之比为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。
本发明的有益效果：
1、本发明采用主要由二氧化钛、秸秆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。
2、本发明中的改性二氧化钛中以秸秆粉参与作为改性剂，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。
3、本发明制备的多孔氮化硅陶瓷材料的开孔率为51～65％，断裂韧性为 10.2～11.5MPa·m1/2,抗弯强度达到50.4～62.3MPa。
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)将秸秆粉加入到步骤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。二氧化钛与所述羟甲基纤维素的质量之比为1:0.03，所述二氧化钛与所述秸秆粉的质量之比为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)将秸秆粉加入到步骤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。所述二氧化钛与所述羟甲基纤维素的质量之比为1:0.06，所述二氧化钛与所述秸秆粉的质量之比为1:0.3。
实施例3
一种多孔氮化硅陶瓷材料的制备方法，包括以下步骤：
1)按照重量百分数计算，称取粒径为0.1～10μm的氮化硅粉体85％、实施例1的改性二氧化钛10％与纳米氧化镁5％，混合均匀得到混合料；
2)将步骤1)的混合料加入到质量浓度为8％聚乙二醇溶液中，采用氧化锆陶瓷球进行球磨，球料比为4∶1，球磨时间为20h，浆料烘干、过筛，然后模压成型为坯件；
3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以1℃/min的升温速度升温到1580℃，保温6小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅陶瓷材料。
本实施例制备的多孔氮化硅陶瓷材料的开孔率为60％，断裂韧性为 11.1MPa·m1 /2,抗弯强度达到61.6MPa。
实施例4
一种多孔氮化硅陶瓷材料的制备方法，包括以下步骤：
1)按照重量百分数计算，称取粒径为0.1～10μm的氮化硅粉体的氮化硅粉体80％、实施例2的改性二氧化钛18％与纳米氧化镁2％，混合均匀得到混合料；
2)将步骤1)的混合料加入到质量浓度为0.5％聚乙二醇溶液中，采用氧化铝陶瓷球进行球磨，球料比为2∶1，球磨时间为24h，浆料烘干、过筛，然后模压成型为坯件；
3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以1℃/min的升温速度升温到1650℃，保温3小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅陶瓷材料。
本实施例制备的多孔氮化硅陶瓷材料的开孔率为65％，断裂韧性为 11.5MPa·m1 /2,抗弯强度达到62.3MPa。
实施例5
一种多孔氮化硅陶瓷材料的制备方法，包括以下步骤：
1)按照重量百分数计算，称取粒径为0.1～10μm的氮化硅粉体90％、烧实施例1的改性二氧化钛8％与纳米氧化镁2％，混合均匀得到混合料；
2)将步骤1)的混合料加入到质量浓度为10％聚乙二醇溶液中，采用氮化硅陶瓷球进行球磨，球磨时间为24h，浆料烘干、过筛，然后模压成型为坯件；
3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以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，即获得多孔氮化硅陶瓷材料。
本实施例制备的多孔氮化硅陶瓷材料的开孔率为51％，断裂韧性为 10.2MPa·m1 /2,抗弯强度达到50.4MPa。
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 (3)

1.一种多孔氮化硅陶瓷材料的制备方法，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60～90％、改性二氧化钛1～20％与纳米氧化镁2～6％，混合均匀得到混合料；
2)将步骤1)的混合料加入到质量浓度为0.5％～10％聚乙二醇溶液中，进行球磨，球磨时间为2～24h，浆料烘干、过筛，然后模压成型为坯件；
3)将坯件在氮气气氛下快速升温到1100℃，再慢速升温到1400℃，然后以1℃/min的升温速度升温到1500～1650℃，保温1～10小时，烧结过程中始终通入流动氮气，最后随炉冷却，即获得多孔氮化硅陶瓷材料，其中各组分的重量总计为100%；
其中，所述改性二氧化钛主要由二氧化钛、秸秆粉与羟甲基纤维素制备得到；
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)将秸秆粉加入到步骤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。
2.根据权利要求1所述的多孔氮化硅陶瓷材料的制备方法，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秸秆粉的质量之比为1:0.1～0.3。
3.根据权利要求1所述的多孔氮化硅陶瓷材料的制备方法，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。
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