CN106866168A - 一种α相微孔氧化铝陶瓷的制备方法 - Google Patents

一种α相微孔氧化铝陶瓷的制备方法 Download PDF

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CN106866168A
CN106866168A CN201710224817.0A CN201710224817A CN106866168A CN 106866168 A CN106866168 A CN 106866168A CN 201710224817 A CN201710224817 A CN 201710224817A CN 106866168 A CN106866168 A CN 106866168A
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刘波波
张伟
杨晓青
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Mingke Microelectronic Material Co Ltd Xi'an City
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Abstract

一种α相微孔氧化铝陶瓷的制备方法，氧化铝80～100％,氮化硼粉0～20％，混合均匀。将混合粉料装入石墨坩埚内。将装有粉料的石墨坩埚装入中频感应烧结炉中，在坩埚顶部盖上石墨纸盖和石墨毡。炉内抽真空至炉内压力小于103Pa，充入氩气至炉内压力大于4×103Pa。将石墨坩埚加热1900‑2100℃，石墨纸处的温度为1700‑1900℃，抽气至气压在1×103～2×103Pa，保温0.5～4h，使BN掺杂的氧化铝粉料在坩埚顶部石墨纸盖上通过固‑气‑固机理进行形核生长。后再将气压充至0.6×105～1×105Pa，随炉冷却至室温，打开炉盖，会在石墨纸盖上得到α相微孔氧化铝陶瓷材料。本发明的微孔Al2O3陶瓷材料可以作为过滤器应用于尾气处理，污水处理等环保领域。

Description

一种α相微孔氧化铝陶瓷的制备方法
技术领域
本发明属于微孔陶瓷技术领域，特别涉及一种α相微孔氧化铝陶瓷的制备方法。
背景技术
氧化铝微孔陶瓷在微孔陶瓷中非常具有吸引力,它具有密度低、热膨胀系数小、强度高、耐高温、耐腐蚀、抗氧化和使用寿命长等优点,在冶金、化工、环保和能源等领域有广阔的应用前景。目前，氧化铝微孔陶瓷的制备存在烧结温度相对较高、孔隙度较低、孔隙形状不易控制和比表面积小等问题。开发新的制备工艺以满足高孔隙度、高强度、孔径均匀且可控、性能稳定的氧化铝微孔陶瓷并拓宽其应用领域有十分重要的意义。本工艺制备的氧化铝陶瓷不仅具有较高的开孔孔隙率及较低的体积密度，使其表现出更高的过滤、吸附能力，而且具有较高的机械强度，使其力学性能显著提高。
发明内容
本发明的目的在于提供一种α相微孔氧化铝陶瓷的制备方法，以解决现有技术中氧化铝微孔陶瓷的制备存在烧结温度相对较高、孔隙度较低、孔隙形状不易控制和比表面积小的问题。
为实现上述目的，本发明采用以下技术方案：
一种α相微孔氧化铝陶瓷的制备方法，包括以下步骤：
1)取质量分数大于等于80％且小于100％的氧化铝和质量分数大于0％且小于等于20％的氮化硼粉，用行星式球磨机将氧化铝和氮化硼球磨2小时混合均匀，氧化铝和氮化硼的组份总和为100％；
2)将混合粉料装入石墨坩埚内；
3)将装有混合粉料的石墨坩埚装入中频感应烧结炉，在坩埚顶部依次盖上石墨纸盖和石墨毡；
4)盖上中频感应烧结炉的炉盖，并对炉内抽真空处理，接着充入氩气至炉内；
5)将石墨坩埚加热至1700℃-2000℃，抽气至气压在1×103Pa～2×103Pa，保温0.5h～4h，使BN掺杂的氧化铝粉料在石墨坩埚顶部石墨纸盖上通过固-气-固机理和氧化铝生长螺旋位错机理进行形核生长；
6)将中频感应烧结炉内气压充至0.6×105Pa～1×105Pa，随炉冷却至室温，打开中频感应烧结炉的炉盖，在石墨纸盖上得到α相微孔氧化铝陶瓷。
进一步的，在氧化铝和氮化硼的混合蒸气凝结过程中，氮化硼在晶体中形成排列规律的颗粒，当氧化铝生长台阶接近颗粒时，生长台阶正前方总的吸附原子数量减少，导致正对着颗粒的生长台阶生长速率降低，而远离颗粒的生长台阶由于其正前方吸附有原子的有效面积没有变化而保持平直推进；生长台阶会从颗粒两侧绕过，而形成了以颗粒为中心向内缩小的生长台阶环，形成微孔。
进一步的，混合粉料在石墨坩埚内的添料高度小于坩埚深度的2/3。
进一步的，步骤四中频感应烧结炉抽真空处理至炉内压力小于103Pa，冲入氩气至炉内压力大于4×103Pa。
5、根据权利要求1所述的一种α相微孔氧化铝陶瓷的制备方法，其特征在于，当石墨坩埚加热至1700℃-2000℃时，石墨纸盖处的温度为1700℃-1900℃。
与现有技术相比，本发明有以下技术效果：
本发明得到α相微孔氧化铝陶瓷材料，具有较高的开孔孔隙率及较低的体积密度，使其表现出更高的过滤、吸附能力，而且具有较高的机械强度，使其力学性能显著提高，为进一步开发α相微孔氧化铝陶瓷材料在尾气处理，污水处理等环保领域提供基础。
具体实施方式
实施例1：
一种α相微孔氧化铝陶瓷的制备方法，包括以下步骤：
1)取质量分数为85％的氧化铝粉末和质量分数为15％的氮化硼粉，氧化铝和氮化硼的组份总和为100％，用行星式球磨机球磨2小时混合均匀；
2)将混合粉料装入石墨坩埚内，添料高度小于坩埚深度的2/3；
3)将装有混合粉料的石墨坩埚装入中频感应烧结炉，在坩埚顶部依次盖上石墨纸盖和石墨毡；
4)盖上中频感应烧结炉的炉盖，抽真空至炉内压力小于103Pa，充入氩气至炉内压力大于4×103Pa；
5)将石墨坩埚加热至1800℃，石墨纸盖处的温度为1800℃，抽气至气压在1.5×103Pa，保温2h，使BN掺杂的氧化铝粉料在石墨坩埚顶部石墨纸盖上通过固-气-固机理和氧化铝生长螺旋位错机理进行形核生长；
6)将中频感应烧结炉的气压充至0.8×105Pa，随炉冷却至室温，打开中频感应烧结炉的炉盖，在石墨纸盖上得到α相微孔氧化铝陶瓷。
实施例2：
1)取质量分数为90％的氧化铝粉末和质量分数为10％的氮化硼粉，氧化铝和氮化硼的组份总和为100％，用行星式球磨机球磨2小时混合均匀；
2)将混合粉料装入石墨坩埚内，添料高度小于坩埚深度的2/3；
3)将装有混合粉料的石墨坩埚装入中频感应烧结炉，在坩埚顶部依次盖上石墨纸盖和石墨毡；
4)盖上中频感应烧结炉的炉盖，抽真空至炉内压力小于103Pa，充入氩气至炉内压力大于4×103Pa；
5)将石墨坩埚加热至2000℃，石墨纸盖处的温度为1900℃，抽气至气压在2×103Pa，保温4h，使BN掺杂的氧化铝粉料在石墨坩埚顶部石墨纸盖上通过固-气-固机理和氧化铝生长螺旋位错机理进行形核生长；
6)将中频感应烧结炉的气压充至1×105Pa，随炉冷却至室温，打开中频感应烧结炉的炉盖，在石墨纸盖上得到α相微孔氧化铝陶瓷。
实施例3：
1)取质量分数为95％的氧化铝粉末和质量分数为5％的氮化硼粉，氧化铝和氮化硼的组份总和为100％，用行星式球磨机球磨2小时混合均匀；
2)将混合粉料装入石墨坩埚内，添料高度小于坩埚深度的2/3；
3)将装有混合粉料的石墨坩埚装入中频感应烧结炉，在坩埚顶部依次盖上石墨纸盖和石墨毡；
4)盖上中频感应烧结炉的炉盖，抽真空至炉内压力小于103Pa，充入氩气至炉内压力大于4×103Pa；
5)将石墨坩埚加热至1700℃，石墨纸盖处的温度为1700℃，抽气至气压在1×103Pa，保温0.5h，使BN掺杂的氧化铝粉料在石墨坩埚顶部石墨纸盖上通过固-气-固机理和氧化铝生长螺旋位错机理进行形核生长；
6)将中频感应烧结炉的气压充至0.6×105Pa，随炉冷却至室温，打开中频感应烧结炉的炉盖，在石墨纸盖上得到α相微孔氧化铝陶瓷。
在氧化铝和氮化硼的混合蒸气凝结过程中，氮化硼在晶体中形成排列规律的颗粒，当氧化铝生长台阶接近颗粒时，生长台阶正前方总的吸附原子数量减少，导致正对着颗粒的生长台阶生长速率降低，而远离颗粒的生长台阶由于其正前方吸附有原子的有效面积没有变化而保持平直推进；生长台阶会从颗粒两侧绕过，而形成了以颗粒为中心向内缩小的生长台阶环，形成微孔。

Claims (5)

1.一种α相微孔氧化铝陶瓷的制备方法，其特征在于，包括以下步骤：
1)取质量分数大于等于80％且小于100％的氧化铝和质量分数大于0％且小于等于20％的氮化硼粉，用行星式球磨机将氧化铝和氮化硼球磨2小时混合均匀，氧化铝和氮化硼的组份总和为100％；
2)将混合粉料装入石墨坩埚内；
3)将装有混合粉料的石墨坩埚装入中频感应烧结炉，在坩埚顶部依次盖上石墨纸盖和石墨毡；
4)盖上中频感应烧结炉的炉盖，并对炉内抽真空处理，接着充入氩气至炉内；
5)将石墨坩埚加热至1700℃-2000℃，抽气至气压在1×103Pa～2×103Pa，保温0.5h～4h，使BN掺杂的氧化铝粉料在石墨坩埚顶部石墨纸盖上通过固-气-固机理和氧化铝生长螺旋位错机理进行形核生长；
6)将中频感应烧结炉内气压充至0.6×105Pa～1×105Pa，随炉冷却至室温，打开中频感应烧结炉的炉盖，在石墨纸盖上得到α相微孔氧化铝陶瓷。
2.根据权利要求1所述的一种α相微孔氧化铝陶瓷的制备方法，其特征在于，在氧化铝和氮化硼的混合蒸气凝结过程中，氮化硼在晶体中形成排列规律的颗粒，当氧化铝生长台阶接近颗粒时，生长台阶正前方总的吸附原子数量减少，导致正对着颗粒的生长台阶生长速率降低，而远离颗粒的生长台阶由于其正前方吸附有原子的有效面积没有变化而保持平直推进；生长台阶会从颗粒两侧绕过，而形成了以颗粒为中心向内缩小的生长台阶环，形成微孔。
3.根据权利要求1所述的一种α相微孔氧化铝陶瓷的制备方法，其特征在于，混合粉料在石墨坩埚内的添料高度小于坩埚深度的2/3。
4.根据权利要求1所述的一种α相微孔氧化铝陶瓷的制备方法，其特征在于，步骤四中频感应烧结炉抽真空处理至炉内压力小于103Pa，冲入氩气至炉内压力大于4×103Pa。
5.根据权利要求1所述的一种α相微孔氧化铝陶瓷的制备方法，其特征在于，当石墨坩埚加热至1700℃-2000℃时，石墨纸盖处的温度为1700℃-1900℃。
CN201710224817.0A 2017-04-07 2017-04-07 一种α相微孔氧化铝陶瓷的制备方法 Active CN106866168B (zh)

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