CN114014685A - 一种抗氧化多孔碳陶复合材料及其制备方法 - Google Patents
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Abstract
本发明涉及一种抗氧化多孔碳陶复合材料及其制备方法。该抗氧化多孔碳陶复合材料由碳纤维隔热材料和抗氧化陶瓷相组成,制备的关键在于陶瓷相可被均匀引入碳纤维隔热材料的孔隙中,且陶瓷相与碳纤维表面有一定结合力,包覆效果优异。陶瓷相对碳纤维的均匀包覆可明显提高碳纤维隔热材料的力学强度和高温抗氧化能力。同时,复合材料可保持较低的密度。本发明对碳基隔热材料的性能提升有重要意义。
Description
技术领域
本发明属于防隔热材料制备领域,具体涉及一种多孔抗氧化碳陶复合材料及其制备方法。
背景技术
在恶劣的气动环境下仍能具备优异的耐温性,并能够起到抗冲刷和隔热作用的材料是保障飞行器速度不断提升的关键因素之一。碳基隔热材料具备优异的耐温性和较低的密度,目前在航天热防护材料领域受到了广泛的研究。然而在有氧环境中碳基材料耐温性显著降低,限制了其在航天热防护材料领域的应用。因此,利用陶瓷相对碳纤维进行表面改性,制备抗氧化碳陶隔热材料对于提升热防护材料耐温性和防护性能均有重要意义。
发明内容
本发明的技术解决问题是:克服多孔纤维状碳基隔热材料高温抗氧化性不足的问题,利用水与正硅酸甲酯或正硅酸乙酯的反应,在碳纤维表面形成凝胶,高温裂解后在碳纤维表面生成抗氧化陶瓷相。由于水与正硅酸甲酯或正硅酸乙酯的溶解性较差,但与碳纤维表面浸润性较好,反应过程中首先在碳纤维表面形成凝胶,随后向孔隙中生长。因此,生成的陶瓷相能够对碳纤维进行较好的包覆,制备的碳陶复合材料兼具低密度和抗氧化的特性。
本发明的技术方案为:
第一方面,本发明提供一种低密度抗氧化多孔碳陶复合材料的制备方法,包括以下步骤:
(1)将多孔碳纤维隔热材料在陶瓷前驱体中进行真空浸渍;
(2)将浸渍陶瓷前驱体后的碳纤维隔热材料浸入去离子水中,并加入催化剂,静置一定时间;
(3)将步骤(2)处理后的碳纤维隔热材料取出,并进行干燥处理;
(4)将步骤(3)干燥后的碳纤维隔热材料于高纯氮气中升温进行高温裂解,裂解完毕后在惰性气氛中降至室温;
(5)重复步骤(1)-(4),得到多孔抗氧化陶瓷基复合材料。
进一步地,步骤(1)中陶瓷前驱体为正硅酸甲酯或正硅酸乙酯。
进一步地,步骤(1)所述真空浸渍的时间为20-40min。
进一步地,步骤(2)中使用1M盐酸或1M氨水作为催化剂,配制成水溶液,催化剂为水质量的2-6%。将浸渍了陶瓷前驱体的碳纤维隔热材料从前驱体液体中取出后,即可浸入水溶液中,例如可以将模具中的陶瓷前驱体倒出,倒入去离子水,加入催化剂,需静置24-48小时。
进一步地,步骤(2)利用水与碳纤维表面的浸润性及水与正硅酸甲酯或正硅酸乙酯较差的相溶性,首先在碳纤维表面形成溶胶凝胶,随后向孔隙中继续生长。
进一步地,步骤(3)中,将(2)中的碳纤维隔热材料从溶液中取出,在鼓风干燥箱中干燥24-48小时。
进一步地,步骤(4)中,将步骤(3)干燥后的碳纤维隔热材料于高纯氮气中以3-6℃/min 的升温速率升温至1000-1200℃,高温裂解60-120min,即需在1000-1200℃惰性气氛中进行高温裂解,在碳纤维表面形成陶瓷相。
进一步地,步骤(5)中,为得到轻质抗氧化碳陶复合材料,前驱体浸渍-裂解过程需重复2-4次。
进一步地,步骤(5)形成的抗氧化多孔碳陶复合材料的密度为0.35-0.55g/cm3。
第二方面,本发明提供一种采用上述方法制备的低密度抗氧化多孔碳陶复合材料。
本发明的抗氧化多孔碳陶复合材料由碳纤维隔热材料和抗氧化陶瓷相组成,制备的关键在于陶瓷相可被均匀引入碳纤维隔热材料孔隙中,且陶瓷相与碳纤维表面有一定结合力,包覆效果优异。陶瓷相对碳纤维的均匀包覆可明显提高碳纤维隔热材料的力学强度和高温抗氧化能力。同时,复合材料可保持较低的密度。本发明对碳基隔热材料的性能提升有重要意义。
本发明的有益效果是:
(1)利用水与正硅酸甲酯或正硅酸乙酯的溶解性较差,但与碳纤维表面浸润性较好的特性,反应过程中首先在碳纤维表面形成凝胶,随后向孔隙中生长。因此,生成的陶瓷相能够对碳纤维进行较好的包覆。
(2)制备工艺简单易操作。
(3)制备的碳陶复合材料兼具低密度和抗氧化的优异特性。
具体实施方式
下面通过具体实施例,对本发明做进一步详细说明。
实施例1
(1)将多孔碳纤维隔热材料(本实施例采用多孔碳纤维隔热瓦)在正硅酸甲酯中真空浸渍20min;
(2)将浸满正硅酸甲酯的碳纤维隔热材料从溶液中取出,以1M的氨水作为催化剂,氨水与去离子水的质量比1:49,配制水溶液,将浸满正硅酸甲酯的碳纤维隔热材料置于水溶液中,静置24小时;
(3)将步骤(2)处理后的碳纤维隔热材料取出,鼓风烘箱中干燥24小时;
(4)将步骤(3)干燥后的碳纤维隔热材料于高纯氮气中以3℃/min的升温速率升温至 1200℃,高温裂解120min,裂解完毕后在惰性气氛中降至室温;
(5)重复步骤(1)-(4)4次,得到多孔抗氧化陶瓷基复合材料。
本实施例制备的多孔抗氧化陶瓷基复合材料的材料密度0.5g/cm3,压缩强度3.9MPa。空气气氛1200℃处理0.5小时,材料失重率0.8%;1400℃处理0.5小时,材料失重率7.1%。
实施例2
(1)将多孔碳纤维隔热材料(本实施例采用多孔碳纤维隔热瓦)在正硅酸乙酯中真空浸渍40min;
(2)将浸满正硅酸乙酯的碳纤维隔热材料从溶液中取出,以1M的氨水作为催化剂,氨水与去离子水的质量比1:19,配制水溶液,将浸满正硅酸甲酯的碳纤维隔热材料置于水溶液中,静置48小时;
(3)将步骤(2)处理后的碳纤维隔热材料取出,鼓风烘箱中干燥48小时;
(4)将步骤(3)干燥后的碳纤维隔热材料于高纯氮气中以3℃/min的升温速率升温至 1000℃,高温裂解60min,裂解完毕后在惰性气氛中降至室温;
(5)重复步骤(1)-(4)2次,得到多孔抗氧化陶瓷基复合材料。
本实施例制备的多孔抗氧化陶瓷基复合材料的材料密度0.35g/cm3,压缩强度3.1MPa。空气气氛1200℃处理0.5小时,材料失重率1.3%;1400℃处理0.5小时,材料失重率9.7%。
实施例3
(1)将多孔碳纤维隔热材料在正硅酸乙酯中真空浸渍40min;
(2)将浸满正硅酸乙酯的碳纤维隔热材料从溶液中取出,以1M的盐酸作为催化剂,盐酸与去离子水的质量比1:94,配制水溶液,将浸满正硅酸甲酯的碳纤维隔热材料置于水溶液中,静置4小时,再在溶液中加入1M的氨水,氨水与上述溶液的质量比1:19,混合均匀后,将上述碳纤维隔热材料置于水溶液中,静置48小时;
(3)将步骤(2)处理后的碳纤维隔热材料取出,鼓风烘箱中干燥48小时;
(4)将步骤(3)干燥后的碳纤维隔热材料于高纯氮气中以6℃/min的升温速率升温至 1200℃,高温裂解120min,裂解完毕后在惰性气氛中降至室温;
(5)重复步骤(1)-(4)4次,得到多孔抗氧化陶瓷基复合材料。
本实施例制备的多孔抗氧化陶瓷基复合材料的材料密度0.49g/cm3,压缩强度3.6MPa。空气气氛1200℃处理0.5小时,材料失重率0.9%;1400℃处理0.5小时,材料失重率8.5%。
以上公开的本发明的具体实施例,其目的在于帮助理解本发明的内容并据以实施,本领域的普通技术人员可以理解,在不脱离本发明的精神和范围内,各种替换、变化和修改都是可能的。本发明不应局限于本说明书的实施例所公开的内容,本发明的保护范围以权利要求书界定的范围为准。
Claims (10)
1.一种抗氧化多孔碳陶复合材料的制备方法,其特征在于,包括以下步骤:
(1)将多孔碳纤维隔热材料在陶瓷前驱体中进行真空浸渍;
(2)将浸渍陶瓷前驱体后的碳纤维隔热材料浸入去离子水中,并加入催化剂,静置一定时间;
(3)将步骤(2)处理后的碳纤维隔热材料取出,并进行干燥处理;
(4)将干燥后的碳纤维隔热材料于高纯氮气中升温进行高温裂解,裂解完毕后在惰性气氛中降至室温;
(5)重复步骤(1)-(4),得到抗氧化多孔碳陶复合材料。
2.根据权利要求1所述的方法,其特征在于,步骤(1)所述陶瓷前驱体为正硅酸甲酯或正硅酸乙酯。
3.根据权利要求1所述的方法,其特征在于,步骤(1)所述真空浸渍的时间为20-40min。
4.根据权利要求1所述的方法,其特征在于,步骤(2)所述催化剂为1M盐酸或1M氨水,催化剂质量为去离子水质量的2-6%;步骤(2)所述静置的时间为24-48小时。
5.根据权利要求1所述的方法,其特征在于,步骤(2)利用水与碳纤维表面的浸润性及水与正硅酸甲酯或正硅酸乙酯较差的相溶性,首先在碳纤维表面形成溶胶凝胶,随后向孔隙中继续生长。
6.根据权利要求1所述的方法,其特征在于,步骤(3)所述干燥处理是将碳纤维隔热材料在鼓风干燥箱中干燥24-48小时。
7.根据权利要求1所述的方法,其特征在于,步骤(4)将干燥后的碳纤维隔热材料于高纯氮气中以3-6℃/min的升温速率升温至1000-1200℃,高温裂解60-120min,在碳纤维表面形成陶瓷相。
8.根据权利要求1所述的方法,其特征在于,步骤(5)所述重复步骤(1)-(4),其重复次数为2-4次。
9.根据权利要求1所述方法,其特征在于,步骤(5)形成的抗氧化多孔碳陶复合材料的密度为0.35-0.55g/cm3。
10.根据权利要求1~9中任一权利要求所述方法制备的抗氧化多孔碳陶复合材料。
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