CN113800939B - 一种纳米纤维SiO2多孔陶瓷材料及其制备方法 - Google Patents

一种纳米纤维SiO2多孔陶瓷材料及其制备方法 Download PDF

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CN113800939B
CN113800939B CN202111000881.3A CN202111000881A CN113800939B CN 113800939 B CN113800939 B CN 113800939B CN 202111000881 A CN202111000881 A CN 202111000881A CN 113800939 B CN113800939 B CN 113800939B
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silicon dioxide
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谭划
袁绮
张海波
南博
任勇飞
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Huazhong University of Science and Technology
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Abstract

本发明提供了一种纳米纤维SiO2多孔陶瓷材料及其制备方法。本发明以二氧化硅粉体为原料，通过放电等离子体烧结法，没有添加任何烧结助剂，成功制备出比表面积大、强度高和吸附效率高的纳米纤维SiO2多孔陶瓷材料，还具有使用寿命长和安全性高特点，该纳米纤维SiO2多孔陶瓷材料在过滤器、膜/催化剂载体和反应器床等方面的有着巨大的应用前景。而且本发明方法还具有制备工艺简单、可操控性强、容易实现规模化生产等优点。

Description

一种纳米纤维SiO2多孔陶瓷材料及其制备方法
技术领域
本发明涉及无机多孔分离材料技术领域，尤其涉及一种纳米纤维SiO2多孔陶瓷材料及其制备方法。
背景技术
随着经济全球化的快速发展，人口数量的急剧增加和城市化进程的不断加快，包括石油开采、海洋运输、工业制造、汽车排放和煤炭燃烧等生产活动日益增多，导致环境污染等问题日益严重，严重威胁到水体和大气的生态环境以及公众的身体健康及生活质量。因此,制备高效的过滤材料成为解决当前日益严重的水污染和空气污染问题的有效手段之一。
纳米多孔轻质材料具有良好的稳定性和机械强度，而且孔隙率高、比表面积大、表面易于修饰、成本低廉、原料易得、生物相容性好。纳米纤维多孔陶瓷材料具有微观的纤维结构，相比于常用的颗粒状粉料, 纤维具有更纤细的构型, 还可以搭建3D网络状结构的孔道, 从而可以制备具有低阻力且高孔隙率的多孔陶瓷。
现有技术的纳米多孔陶瓷的制备过程中，容易出现比表面积、强度和吸附效率不能能兼顾的问题，通过合理的设计制备工艺，有希望制备出具有比表面积大、强度高和吸附效率高等高性能的纳米多孔陶瓷。
发明内容
本发明的目的在于，针对现有技术的上述不足，提出一种纳米纤维SiO2多孔陶瓷材料及其制备方法。
为实现上述目的，本发明采用如下的技术方案：
本发明提供的一种纳米纤维SiO2多孔陶瓷材料的制备方法，包括以下步骤：
步骤S1，将二氧化硅原料研磨粉粹，制得二氧化硅粉体；
步骤S2，将步骤S1所得二氧化硅粉体装入石墨模具，并置于放电等离
子体烧结炉内，在真空条件下进行烧结，制得纳米纤维SiO2多孔陶瓷材料。
进一步的，所述二氧化硅粉体的粒径为0.5~10μm。
进一步的，步骤S1中，所述研磨的方式为湿法行星球磨，其球磨介质
为乙醇。
进一步的，步骤S2中，所述真空条件的真空度小于10Pa。
进一步的，步骤S2中，所述烧结的加热升温速率为50℃/min。
进一步的，步骤S2中，所述烧结的过程中真空压力为3 MPa。
进一步的，步骤S2中，所述烧结的保温温度为600~800℃，其保温时
间为10~15min。
本发明还提供一种采用上述制备方法得到的纳米纤维SiO2多孔陶瓷材料，所述纳米纤维SiO2多孔陶瓷材料的孔隙率为50~80%；孔径大小为1~10μm。
本发明提供的技术方案带来的有益效果是：
（1）本发明以二氧化硅粉体为原料，通过放电等离子体烧结法，没有添加任何烧结助剂，成功制备出比表面积大、强度高和吸附效率高的纳米纤维SiO2多孔陶瓷材料，还具有使用寿命长和安全性高特点，该纳米纤维SiO2多孔陶瓷材料在过滤器、膜/催化剂载体和反应器床等方面的有着巨大的应用前景。
（2）本发明方法还具有制备工艺简单、可操控性强、容易实现规模化生产等优点。
附图说明
图1为实施例1制备的纳米纤维SiO2多孔陶瓷材料的断面SEM图；
图2为实施例3制备的纳米纤维SiO2多孔陶瓷材料的断面SEM图；
图3为实施例4制备的纳米纤维SiO2多孔陶瓷材料的断面SEM图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合附图和实施例对本发明实施方式作进一步地描述。
实施例1：
将二氧化硅原料以乙醇为介质、Si3N4球为磨球，在行星球磨机上以500转/分钟的转速进行球磨粉粹5h，再经旋转蒸发得到干燥的二氧化硅粉体；将所得二氧化硅粉体装入石墨模具，然后置于放电等离子体烧结炉内，在气压低于10Pa的真空中，加热的升温速率为50℃/min，待温度升温至600℃，在600℃、3MPa的烧结条件下，保温15min，制得纳米纤维SiO2多孔陶瓷材料。
经测试分析，所制备的纳米纤维SiO2多孔陶瓷材料的断面SEM照片如图1所示，孔隙率为71.85%，比表面积为469.68 m2/g。
实施例2：
将二氧化硅原料以乙醇为介质、Si3N4球为磨球，在行星球磨机上以500转/分钟的转速进行球磨粉粹5h，再经旋转蒸发得到干燥的二氧化硅粉体；将所得二氧化硅粉体装入石墨模具，然后置于放电等离子体烧结炉内，在气压低于10Pa的真空中，加热的升温速率为50℃/min，待温度升温至650℃，在650℃、3MPa的烧结条件下，保温15min，制得纳米纤维SiO2多孔陶瓷材料。
经测试分析，所制备的纳米纤维SiO2多孔陶瓷材料的孔隙率为70.72%，比表面积为389.95 m2/g。
实施例3：
将二氧化硅原料以乙醇为介质、Si3N4球为磨球，在行星球磨机上以500转/分钟的转速进行球磨粉粹5h，再经旋转蒸发得到干燥的二氧化硅粉体；将所得二氧化硅粉体装入石墨模具，然后置于放电等离子体烧结炉内，在气压低于10Pa的真空中，加热的升温速率为50℃/min，待温度升温至700℃，在700℃、3MPa的烧结条件下，保温13min，制得纳米纤维SiO2多孔陶瓷材料。
经测试分析，所制备的纳米纤维SiO2多孔陶瓷材料的断面SEM照片如图2所示，孔隙率为70.08%，比表面积为361.08 m2/g。
实施例4：
将二氧化硅原料以乙醇为介质、Si3N4球为磨球，在行星球磨机上以500转/分钟的转速进行球磨粉粹5h，再经旋转蒸发得到干燥的二氧化硅粉体；将所得二氧化硅粉体装入石墨模具，然后置于放电等离子体烧结炉内，在气压低于10Pa的真空中，加热的升温速率为50℃/min，待温度升温至750℃，在750℃、3MPa的烧结条件下，保温13min，制得纳米纤维SiO2多孔陶瓷材料。
经测试分析，所制备的纳米纤维SiO2多孔陶瓷材料的断面SEM照片如图3所示，孔隙率为70.74%，比表面积为287.21 m2/g。
实施例5：
将二氧化硅原料以乙醇为介质、Si3N4球为磨球，在行星球磨机上以500转/分钟的转速进行球磨粉粹5h，再经旋转蒸发得到干燥的二氧化硅粉体；将所得二氧化硅粉体装入石墨模具，然后置于放电等离子体烧结炉内，在气压低于10Pa的真空中，加热的升温速率为50℃/min，待温度升温至800℃，在800℃、3MPa的烧结条件下，保温10min，制得纳米纤维SiO2多孔陶瓷材料。
经测试分析，所制备的纳米纤维SiO2多孔陶瓷材料的孔隙率为67.16%，比表面积为139.98 m2/g。
由实施例1-5的测试结果可知，随着烧结温度的升高，纳米纤维SiO2多孔陶瓷材料的孔隙率和比表面积表现减少的趋势，但其孔隙率和比表面积相对于现有技术仍表现出优越的性能，相同过滤效率体积更小，强度更高使应用场景增加，完全可以用于一些液体流速快、冲击力大的场景。这是因为在放电等离子烧结过程中，由于二氧化硅粉体内部的自发热，极大抑制了二氧化硅晶粒的长大，在晶粒空隙处放电时，会产生高达几千度的局部高温，引起晶粒表面的蒸发和熔化，从而促进材料的烧结，此时表观的烧结温度是远远低于局部和瞬时高温的，导致测量得到的温度要比实际的低出许多，从而实现低温快速烧结。低温快速烧结不仅降低生产成本，更有助于材料不宜发生过渡烧结，降低密度，提高孔隙率和比表面积，本发明的使用的二氧化硅粉体的纤维直径为纳米级别，烧结活性高且在较低温度下就能达到较高的强度，相同体积下，比表面积更大，过滤效率更高。
将实施例1制备的纳米纤维SiO2多孔陶瓷材料进行空气过滤试验：
在3.6-3.8L/min流速的空气中，捕获时间为45min-2h，捕获杂质的效率达到99%以上，比现有技术捕获效率高，维持时间长。
在不冲突的情况下，本文中上述实施例及实施例中的特征可以相互结合。
以上所述仅为本发明的较佳实施例，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 (1)

1.一种纳米纤维SiO2多孔陶瓷材料，其特征在于：所述纳米纤维SiO2多孔陶瓷材料的孔隙率为65~72%；孔径大小为1~10μm，所述纳米纤维SiO2多孔陶瓷材料的制备方法包括以下具体步骤：
S1、将二氧化硅原料研磨粉粹，制得二氧化硅粉体，所述二氧化硅粉
体的粒径为0.5~10μm，所述二氧化硅粉体的纤维直径为纳米级别；所述研磨的方式为湿法行星球磨，其球磨介质为乙醇；
S2、将步骤S1所得二氧化硅粉体装入石墨模具，并置于放电等离子体烧结炉内，在真空条件下进行烧结，制得纳米纤维SiO2多孔陶瓷材料，所述真空条件的真空度小于10Pa；真空压力为3 MPa ；所述烧结的加热升温速率为50℃/min；所述烧结的保温温度为600~800℃，其保温时间为10~15min。
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