CN107673760B - 一种梯度结构多孔陶瓷材料的制备方法 - Google Patents

一种梯度结构多孔陶瓷材料的制备方法 Download PDF

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CN107673760B
CN107673760B CN201710942378.7A CN201710942378A CN107673760B CN 107673760 B CN107673760 B CN 107673760B CN 201710942378 A CN201710942378 A CN 201710942378A CN 107673760 B CN107673760 B CN 107673760B
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焦春荣
刘晓丽
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AVIC BASIC TECHNOLOGY RESEARCH INSTITUTE
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Abstract

本发明属于多孔陶瓷制备技术领域，涉及一种梯度结构多孔陶瓷材料的制备方法。本发明以不同粒径单分散聚合物微球作为模板，按照一定比例加入陶瓷粉体、粘结剂、塑型剂、分散剂，使用挤出成型工艺分别制备出不同孔结构的陶瓷薄膜，将陶瓷薄膜在模具中按照设计的梯度结构进行叠层后热压成型，脱模后进一步高温烧结得到结构梯度变化的多孔陶瓷材料。利用该方法将陶瓷薄膜在模具中按照设计的梯度结构进行叠层后热压成型、排胶，制备得到孔径和孔隙率可控的多孔陶瓷材料；二次热压成型增强了不同孔结构的多孔陶瓷薄膜之间的结合；梯度结构避免了后续烧结过程中由于收缩不同有可能引发的层间开裂。

Description

一种梯度结构多孔陶瓷材料的制备方法
技术领域
本发明属于多孔陶瓷制备技术领域，涉及一种梯度结构多孔陶瓷材料的制备方法。
背景技术
多孔陶瓷材料具有较高的气孔率、较大的比表面积以及可以调节的气孔形状、孔径和气孔分布等特点，是一类环保型绿色材料和结构功能材料，可作为保温隔热材料、过滤器材料、催化剂载体、吸音和透波材料等在在生物医学、石油化工、航空航天、国防军工等领域具有广阔的发展和应用前景，目前大多研究集中于单一孔径、孔隙率的无序多孔陶瓷材料的研制，但无法满足对具有梯度可变性孔结构的陶瓷材料的需求，梯度结构的多孔陶瓷是多孔陶瓷的制造难点。
比如在功能材料领域，多孔陶瓷将雷达吸波材料与微观结构设计相结合，不但可大大减轻材料的质量，而且利用多孔特性可以进行电磁波的散射。如果能将具有电磁损耗功能的电子陶瓷粉体制备成为梯度多孔陶瓷，渐变的孔结构可实现不同波段电磁波的吸收，从而可大大提高结构吸波的效率和可控性。然而目前有关梯度结构多孔陶瓷用于吸波材料的报道基本没有。
以聚合物微球为模板制备多孔陶瓷通常采用干压成型的方法，具体操作步骤为：将微球涂敷料浆后置于模具内干压成型，干燥后再烧结成陶瓷。这种工艺涂敷量不连续的话，容易造成多孔陶瓷的缺陷，干压法可以制备均质多孔陶瓷，对于梯度结构可控的多孔陶瓷的制备有一定难度。
发明内容
本发明的目的是，提出一种孔结构有序渐变，质量更加稳定的梯度结构多孔陶瓷材料的制备方法。
本发明的技术解决方案是，
以不同粒径单分散聚合物微球作为模板，按照比例加入陶瓷粉体、粘结剂、塑型剂、分散剂，使用挤出成型工艺分别制备出不同孔结构的多孔陶瓷薄膜，将陶瓷薄膜在模具中按照设计的梯度结构进行叠层后热压成型，脱模后进行高温烧结得到结构梯度变化的多孔陶瓷材料，具体的制备步骤如下：
(1)选用单分散聚苯乙烯微球或酚醛微球作为模板，按照设计要求与陶瓷粉体按照比例混合均匀；
(2)按照挤出成型工艺配方向挤出机内加入粘结剂、塑型剂以及分散剂，温度升至180-220℃，混炼均匀后加入步骤(1)中的混合粉料，充分混炼均匀后挤出成型陶瓷薄膜，薄膜厚度在0.1-0.3mm之间。其中，粘结剂为甲基纤维素，加入量为粉体质量的16-20％，塑形剂为甘油，加入量为粉体质量的1-1.4％，分散剂为油酸，加入量为粉体质量的0.6-1％；
(3)按照设计要求更换单分散微球的粒径或体积比例，重复步骤(1)-(2)制备其它不同孔结构的陶瓷薄膜；
(4)将不同孔结构的陶瓷薄膜按照设计要求的梯度在模具内进行叠层，升温至150-200℃，压力0.5-2MPa，保温保压2-5h，热压成型多孔陶瓷素坯，冷却后脱模干燥；
(5)将多孔陶瓷素坯置于高温马弗炉内按照1℃/min的升温速率缓慢升至600℃，保温3h进行排胶，再将材料转移至高温石墨化炉内，升温至多孔陶瓷材料的烧结温度，保温3-6h，得到梯度结构多孔陶瓷。
所述的单分散聚苯乙烯微球或酚醛微球模板为实心球，粒径在50μm-650μm之间。
挤出成型用的粘结剂为甲基纤维素，加入量为粉体质量的18％，塑形剂为甘油，加入量为粉体质量的1.2％，分散剂为油酸，加入量为粉体质量的0.8％。
本发明的优点和特点：
(1)本发明以单分散微球为模板，采用挤出成型制备的多孔陶瓷薄膜孔结构及厚度精确可控，便于电结构的设计和实现。
(2)本发明通过电子陶瓷粉体在结构上的梯度渐变进行吸波，实现了功能和结构的一体化。
(3)挤出成型制备多孔陶瓷薄膜生产连续、质量稳定、自动化程度高，适于批量生产。
具体实施方式
梯度结构多孔陶瓷材料的具体实施方案如下：
以不同粒径单分散聚合物微球作为模板，按照比例加入陶瓷粉体、粘结剂、塑型剂、分散剂，使用挤出成型工艺分别制备出不同孔结构的多孔陶瓷薄膜，将陶瓷薄膜在模具中按照设计的梯度结构进行叠层后热压成型，脱模后进行高温烧结得到结构梯度变化的多孔陶瓷材料，具体的制备步骤如下：
(1)选用单分散聚苯乙烯微球或酚醛微球作为模板，按照设计要求与陶瓷粉体按照比例混合均匀；
(2)按照挤出成型工艺配方向挤出机内加入粘结剂、塑型剂以及分散剂，温度升至180-220℃，混炼均匀后加入步骤(1)中的混合粉料，充分混炼均匀后挤出成型陶瓷薄膜，薄膜厚度在0.1-0.3mm之间。其中，粘结剂为甲基纤维素，加入量为粉体质量的16-20％，塑形剂为甘油，加入量为粉体质量的1-1.4％，分散剂为油酸，加入量为粉体质量的0.6-1％；
(3)按照设计要求更换单分散微球的粒径或体积比例，重复步骤(1)-(2)制备其它不同孔结构的陶瓷薄膜；
(4)将不同孔结构的陶瓷薄膜按照设计要求的梯度在模具内进行叠层，升温至150-200℃，压力0.5-2MPa，保温保压2-5h，热压成型多孔陶瓷素坯，冷却后脱模干燥；
(5)将多孔陶瓷素坯置于高温马弗炉内按照1℃/min的升温速率缓慢升至600℃，保温3h进行排胶，再将材料转移至高温石墨化炉内，升温至多孔陶瓷材料的烧结温度，保温3-6h，得到梯度结构多孔陶瓷。
为了更好的理解本发明，下面结合具体的实施例进一步阐述本发明的内容，但本发明的内容不仅仅局限于下面的实施例：
实施例1
(1)选用中位径为0.5μm单分散聚苯乙烯微球作为模板，与1Kg纳米SiC粉体按照1:2的体积比例混合均匀；
(2)按照挤出工艺配方向挤出机内加入甲基纤维素180g，甘油12g，油酸8g，温度升至180℃，混炼均匀后加入(1)中的混合粉料，充分混炼均匀后挤出成型法制备厚度在0.1mm的SiC多孔陶瓷薄膜；
(3)分别按照聚苯乙烯微球与纳米SiC粉体1:3、1:4、1:5的体积比例，按照上述(1)-(2)步骤挤出成型法制备不同孔结构的，厚度在0.1mm的SiC多孔陶瓷薄膜；
(4)将不同孔结构的陶瓷薄膜在模具内按设计要求顺序叠层，在压机上热压成型孔结构梯度渐变的陶瓷素坯，保持温度150℃，压力0.5MPa，5h后冷却、脱模、干燥；
(5)将多孔陶瓷素坯置于高温马弗炉内按照1℃/min的升温速率缓慢升至600℃，保温3h进行排胶，再将材料转移至高温石墨化炉内按照100℃/h的速率升温至1700℃，高温烧结3h得到梯度结构的SiC多孔陶瓷。
实施例2
(1)选用中位径为50nm单分散酚醛微球作为模板，与1Kg纳米TiB2粉体按照1:1的体积比例混合均匀；
(2)按照挤出成型工艺配方向挤出机内加入甲基纤维素200g，加入甘油14g，加入油酸10g，温度升至220℃，混炼均匀后加入步骤(1)中的混合粉料，充分混炼均匀后挤出厚度为0.2mm的陶瓷薄膜；
(3)分别将微球模版更换为中位径为100nm、150nm的单分散酚醛微球，重复步骤(1)-(2)制备其它不同孔结构的厚度为0.2mm的陶瓷薄膜；
(4)将不同孔结构的陶瓷薄膜按照设计要求的梯度在模具内进行叠层，升温至180℃，压力2MPa，保温保压3h，热压成型多孔陶瓷素坯，冷却后脱模干燥；
(5)将多孔陶瓷素坯置于高温马弗炉内按照1℃/min的升温速率缓慢升至600℃，保温3h进行排胶，再将材料转移至高温石墨化炉内按照100℃/min速度升温至2500℃，保温4h，得到梯度结构TiB2多孔陶瓷。

Claims (1)

1.一种梯度结构多孔陶瓷材料的制备方法，其特征在于，具体的制备步骤如下：
(1)选用中位径为0.5μm单分散聚苯乙烯微球作为模板，与1Kg纳米SiC粉体按照1:2的体积比例混合均匀；
(2)按照挤出工艺配方向挤出机内加入甲基纤维素180g，甘油12g，油酸8g，温度升至180℃，混炼均匀后加入(1)中的混合粉料，充分混炼均匀后挤出成型法制备厚度在0.1mm的SiC多孔陶瓷薄膜；
(3)分别按照聚苯乙烯微球与纳米SiC粉体1:3、1:4、1:5的体积比例，按照上述(1)-(2)步骤挤出成型法制备不同孔结构的，厚度在0.1mm的SiC多孔陶瓷薄膜；
(4)将不同孔结构的陶瓷薄膜在模具内按设计要求顺序叠层，在压机上热压成型孔结构梯度渐变的陶瓷素坯，保持温度150℃，压力0.5MPa，5h后冷却、脱模、干燥；
(5)将多孔陶瓷素坯置于高温马弗炉内按照1℃/min的升温速率缓慢升至600℃，保温3h进行排胶，再将材料转移至高温石墨化炉内按照100℃/h的速率升温至1700℃，高温烧结3h得到梯度结构的SiC多孔陶瓷；
所述梯度结构多孔陶瓷材料的制备方法，通过结构上的梯度渐变进行吸波，实现了功能和结构的一体化。
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