CN110002881B - 一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法 - Google Patents

一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法 Download PDF

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CN110002881B
CN110002881B CN201910328228.6A CN201910328228A CN110002881B CN 110002881 B CN110002881 B CN 110002881B CN 201910328228 A CN201910328228 A CN 201910328228A CN 110002881 B CN110002881 B CN 110002881B
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张东生
姚栋嘉
吴恒
刘喜宗
方璐
牛利伟
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Abstract

本发明属于多孔二硅化钼陶瓷材料的制备领域，公开一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法。将液态酚醛树脂加入无水乙醇中，保证所得溶液中酚醛树脂的含量为8~15 wt%；按碳纤维粉与酚醛树脂的质量比为（2~8）∶100、二氧化硅气凝胶粉与无水乙醇的质量比为（100~130）∶100、钼粉与二氧化硅气凝胶粉的质量比为（155~165）∶100计，加入碳纤维粉、二氧化硅气凝胶粉、加入钼粉，继续搅拌10~16 h；60~75℃加热搅拌，直至不能搅拌为止；烘干，造粒过筛，压制成型；在氩气气氛保护、1650~1750℃、0.2~0.5 Mpa下烧结1~3 h。本发明制备的碳纤维粉增强多孔二硅化钼使陶瓷材料同时具备两者优异的性能，在电催化、煤气和汽车尾气净化、热交换、燃料电池等方向具有强大的实用价值。

Description

一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法
技术领域
本发明属于多孔二硅化钼陶瓷材料的制备领域，具体涉及一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法。
背景技术
多孔二硅化钼陶瓷具有低密度、耐腐蚀、耐高温、比表面积大、导电性优良等优点，已普遍应用于能源化学工业、新型燃料电池、环保、航空航天、催化等领域，受到越来越广泛的关注。但是，多孔二硅化钼陶瓷存在强度低、质脆等缺陷。碳纤维具有低密度、高比强度、高比模量、耐高温等一系列的优异性能，它的重要应用之一就是作为复合材料的增强体承载负荷。如能利用碳纤维增强多孔二硅化钼陶瓷材料，该复合材料将同时具有碳纤维和多孔二硅化钼的优点，在电催化、煤气和汽车尾气净化、热交换、燃料电池等方向具有强大的实用价值。
发明内容
本发明的目的旨在提供一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法。
为实现上述目的，本发明采取的技术方案如下：
一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，步骤如下：
（1）、将液态酚醛树脂加入无水乙醇中，保证所得溶液中酚醛树脂的含量为8~15wt%，搅拌均匀；
（2）、按碳纤维粉与酚醛树脂的质量比为（2~8）∶100计，将碳纤维粉加入步骤（1）所得溶液中，搅拌均匀；
（3）、按二氧化硅气凝胶粉与无水乙醇的质量比为（100~130）∶100计，将二氧化硅气凝胶粉加入步骤（2）所得溶液中，搅拌均匀；
（4）、按钼粉与二氧化硅气凝胶粉的质量比为（155~165）∶100计，将钼粉加入步骤（3）所得溶液中，继续搅拌10~16 h；
（5）、60~75 ℃加热搅拌，直至浆料粘稠至不能搅拌为止；
（6）、将粘稠浆料烘干，造粒过筛，将所得颗粒粉置于模具中，压制成型，得到坯体；
（7）、将坯体在氩气气氛保护、1650~1750 ℃、0.2~0.5 Mpa下烧结1~3 h，即得到碳纤维增强多孔二硅化钼陶瓷材料。
较好地，所述液态酚醛树脂中固含量≥50 wt%。
较好地，所述碳纤维粉的目数≥300。
较好地，所述二氧化硅气凝胶粉的粒径为0.3~0.6 μm。
较好地，所述钼粉的粒径为3~5 μm。
较好地，所述烘干的温度为80~100 ℃。
较好地，所述压制成型的压力控制在120~150 Mpa。
有益效果：本发明提供一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，工艺简单，操作方便，采用Mo粉与二氧化硅气凝胶粉反应生成多孔状的二硅化钼，同时碳纤维粉增强多孔二硅化钼使陶瓷材料同时具备两者优异的性能，较高的力学强度和刚度，耐高温、耐腐蚀、比表面积高、气孔率高且孔径结构分布均匀、尺寸可控及导电性优良等特性；碳纤维的加入更是弥补了多孔二硅化钼强度低、质脆的缺陷，使其具有较高力学强度和刚度；在电催化、煤气和汽车尾气净化、热交换、燃料电池等方向具有强大的实用价值，特别在电催化和燃料电池方面，碳纤维增强多孔二硅化钼陶瓷材料具备化学稳定好、导电性能突出、比表面积高、孔隙率高等特点，同时由于碳纤维纤维增强提高了多孔二硅化钼的机械强度，从而大幅度地延长了多孔二硅化钼的使用寿命，因此碳纤维增强多孔二硅化钼陶瓷材料的应用将受到越来越广泛的关注。
具体实施方式
下面结合具体实施例对本发明的技术方案做进一步详细、清楚地描述，但本发明的保护范围并不局限于此。
以下实施例1-3中，液态酚醛树脂中固含量为50 wt%，碳纤维粉的目数为300目，二氧化硅气凝胶超细粉的粒径为0.4 μm，所述钼粉的粒径为3 μm。
实施例1
一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，步骤如下：
（1）将液态酚醛树脂加入无水乙醇中，保证所得溶液中酚醛树脂的含量为15 wt%，搅拌均匀；
（2）按碳纤维粉与酚醛树脂的质量比为8∶100计，将碳纤维粉加入步骤（1）所得溶液中，搅拌均匀；
（3）按二氧化硅气凝胶超细粉与无水乙醇的质量比为130∶100计，将二氧化硅气凝胶超细粉加入步骤（2）所得溶液中，搅拌均匀；
（4）按钼粉与二氧化硅气凝胶超细粉的质量比为160∶100计，将钼粉加入步骤（3）所得溶液中，继续搅拌16 h；
（5）60 ℃加热搅拌，直至浆料粘稠至不能搅拌为止；
（6）将粘稠浆料在80 ℃烘干，造粒，过100目筛，将所得颗粒粉置于模具中，140MPa压制成型，得到坯体；
（7）将坯体置于石墨坩埚中，在烧结炉中，1650 ℃、氩气气氛保护、0.4 MPa烧结3h，即得到碳纤维增强多孔二硅化钼陶瓷材料。
相关结果：材料的抗弯强度为88.9 MPa，压缩强度为106.4 MPa，孔径约为8 μm，孔隙率约为75%，比表面积约为30.5 m2/g。
实施例2
一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，步骤如下：
（1）将液态酚醛树脂加入于无水乙醇中，保证所得溶液中酚醛树脂的含量为9wt%，搅拌均匀；
（2）按碳纤维粉与酚醛树脂的质量比为4∶100计，将碳纤维粉加入步骤（1）所得溶液中，搅拌均匀；
（3）按二氧化硅气凝胶超细粉与无水乙醇的质量比为100∶100计，将二氧化硅气凝胶超细粉加入步骤（2）所得溶液中，搅拌均匀；
（4）按钼粉与二氧化硅气凝胶超细粉的质量比为155∶100计，将钼粉加入步骤（3）所得溶液中，继续搅拌10 h；
（5）70 ℃加热搅拌，直至浆料粘稠不能搅拌为止；
（6）将粘稠浆料在90 ℃烘干，造粒，过100目筛，将所得颗粒粉置于模具中，150MPa压制成型，得到坯体；
（7）将坯体置于石墨坩埚中，在烧结炉中，1700 ℃、氩气气氛保护、0.2 MPa烧结2h，即得到碳纤维增强多孔二硅化钼陶瓷材料。
相关结果：材料的抗弯强度为39.6 MPa，压缩强度为58.7 MPa，孔径约为34 μm，孔隙率约为84%，比表面积约为16.2 m2/g。
实施例3
一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，步骤如下：
（1）将液态酚醛树脂加入于无水乙醇中，保证所得溶液中，酚醛树脂的含量为12wt%，搅拌均匀；
（2）按碳纤维粉与酚醛树脂的质量比为5∶100计，将碳纤维粉加入步骤（1）所得溶液中，搅拌均匀；
（3）按二氧化硅气凝胶超细粉与无水乙醇的质量比为115∶100计，将二氧化硅气凝胶超细粉加入步骤（2）所得溶液中，搅拌均匀；
（4）按钼粉与二氧化硅气凝胶超细粉的质量比为165∶100计，将钼粉加入步骤（3）所得溶液中，继续搅拌12 h；
（5）75 ℃加热搅拌，直至浆料粘稠至不能搅拌为止；
（6）将粘稠浆料在100 ℃烘干，造粒100目过筛，将所得颗粒粉置于模具中，120MPa压制成型，得到坯体；
（7）将坯体置于石墨坩埚中，在烧结炉中，1750 ℃、氩气气氛保护、0.5 MPa烧结1h，即得到碳纤维增强多孔二硅化钼陶瓷材料。
相关结果：材料的抗弯强度为50.2 MPa，压缩强度为72.3 MPa，孔径约为21 μm，孔隙率约为78.5%，比表面积约为21.8 m2/g。

Claims (7)

1.一种碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于，步骤如下：
（1）、将液态酚醛树脂加入无水乙醇中，保证所得溶液中酚醛树脂的含量为8~15 wt%，搅拌均匀；
（2）、按碳纤维粉与酚醛树脂的质量比为（2~8）∶100计，将碳纤维粉加入步骤（1）所得溶液中，搅拌均匀；
（3）、按二氧化硅气凝胶粉与无水乙醇的质量比为（100~130）∶100计，将二氧化硅气凝胶粉加入步骤（2）所得溶液中，搅拌均匀；
（4）、按钼粉与二氧化硅气凝胶粉的质量比为（155~165）∶100计，将钼粉加入步骤（3）所得溶液中，继续搅拌10~16 h；
（5）、60~75 ℃加热搅拌，直至浆料粘稠至不能搅拌为止；
（6）、将粘稠浆料烘干，造粒过筛，将所得颗粒粉置于模具中，压制成型，得到坯体；
（7）、将坯体在氩气气氛保护，在1650~1750 ℃、0.2~0.5 Mpa下烧结1~3 h，即得到碳纤维增强多孔二硅化钼陶瓷材料。
2.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述液态酚醛树脂的固含量≥50 wt%。
3.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述碳纤维粉的目数≥300。
4.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述二氧化硅气凝胶粉的粒径为0.3~0.6 μm。
5.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述钼粉的粒径为3~5 μm。
6.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述烘干的温度为80~100 ℃。
7.如权利要求1所述的碳纤维增强多孔二硅化钼陶瓷材料的制备方法，其特征在于：所述压制成型的压力控制在120~150 Mpa。
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