CN114368194A - 一种耐高温隔热陶瓷复合材料及其制备方法 - Google Patents
一种耐高温隔热陶瓷复合材料及其制备方法 Download PDFInfo
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Abstract
本发明提出了一种耐高温隔热陶瓷复合材料及其制备方法，包括质量比为1：0.05‑0.07：0.04‑0.06的陶瓷材料纤维增韧层、多孔薄膜层和粘连层的结构。陶瓷材料纤维增韧层是将多孔陶瓷浆料注入表面修饰纤维编织体，高温热压烧结，制成的表面修饰纤维织物陶瓷材料，多孔薄膜层为泡沫金属制得的多孔薄膜材料，粘连层为环氧胶。本发明采用特定比例构成陶瓷材料纤维增韧层、多孔薄膜层和粘连层的多层结构，使获得的耐高温隔热陶瓷复合材料显气孔率可达86.8％、导热系数可达0.010W·m‑1·k‑1、软化系数达1.05，实验条件下对甲苯的吸附率为72.8％，表现出优异的综合性能，可应用于高温环境的废气吸附，效果保持好。
Description
技术领域
本发明涉及陶瓷材料领域，特别涉及一种耐高温隔热陶瓷复合材料及其制备方法。
背景技术
各类生产如化工、炼油和制药等工业的生产，易伴随着大量的工业废气的产生，而这些废气是大气污染物的重要来源。国家对各类厂矿排放的废气制定了排放标准，降低工业废气中的有毒有害物质。通常高分子材料具有高的气孔率，并具有良好的强度和一定的耐火性，但在较高温度的环境下，由于其隔热效果不佳，易在使用过程出现瓦解而破坏了多孔结构，导致吸附效果变差；或是材料间的热膨胀系数相差较大，在高温下容易发生脱落的情况，也对多孔结构造成了影响。
耐高温隔热陶瓷材料是一种新型环保材料，具有耐高温性能的同时，可使材料保持良好的隔热性能，在承受高温情况下依旧保持不变形，隔热效果不衰减。因陶瓷具有较大的脆性，往往出现较小的裂纹或裂缝就可导致其破碎，通常会加入纤维提升陶瓷材料的断裂韧性。但纤维吸收断裂能的能力有限，且在烧结过程中烧结助剂易于纤维发生化学反应，造成陶瓷材料在使用时纤维和基体的界面力减弱，反而降低了陶瓷的力学性能，进而影响吸附能力。
发明内容
鉴于此，本发明的目的在于提出一种耐高温隔热陶瓷复合材料及其制备方法，解决上述问题。
本发明的技术方案是这样实现的：
一种耐高温隔热陶瓷复合材料，包括质量比为1：0.05-0.07：0.04-0.06的陶瓷材料纤维增韧层、多孔薄膜层和粘连层的结构；
其中，粘连层的一面为陶瓷基复合材料纤维增韧层，而粘连层的另一面为多孔薄膜层。
进一步说明，上述陶瓷材料纤维增韧层为将多孔陶瓷浆料注入表面修饰纤维编织体，高温热压烧结，制成的表面修饰纤维织物陶瓷材料；
上述多孔薄膜层为泡沫金属制得的多孔薄膜材料；
上述粘连层为环氧胶。
进一步说明，该耐高温隔热陶瓷复合材料的制备方法，包括如下步骤：将表面修饰纤维织物陶瓷材料放入模具，依次加入环氧胶和多孔薄膜材料，150-200℃处理10-15min，趁热施加电场，电场强度为200-300V/mm，冷却，得耐高温隔热陶瓷复合材料；热熔状态下外加电场，可在磁场作用下细化金属材料的晶粒，降低材料间的内应力，促进多孔薄膜材料附着于环氧胶表面，使环氧胶下沉，提高耐高温隔热陶瓷复合材料的致密性和融合性，否则，易增加材料的不稳定性。
进一步说明，上述多孔陶瓷浆料是由氧化铝和氧化锆纤维，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，球磨，喷雾干燥，烧结，研磨，无水乙醇溶解而得；
进一步说明，上述表面修饰纤维编织体为由纤维编织混合物与四氯化碳气相沉积反应，经聚吡咯-丙酮溶液超声反应，烧结，冷却，清洗，干燥后制得。
进一步说明，该多孔陶瓷浆料的具体制备方法，包括如下步骤：在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，球磨24-28h，喷雾干燥，以20-30℃/min升温至500-600℃，保温4-6h，以5-8℃/min升温至1000-1200℃，再冷却至20-25℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；加入特定配比的有机溶液球磨，并结合特定的升温程序，可使多孔陶瓷浆料颗粒分布均匀，有利于使制备成的表面修饰纤维织物陶瓷材料的气孔尺寸进一步缩小，并可调整其气孔的均匀性；
进一步说明，该表面修饰纤维编织体的具体制备方法，包括如下步骤：将纤维编织混合物放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为950-970℃，沉积炉内压力为280-320Pa，浸没至聚吡咯-丙酮溶液，60-70℃超声反应3-4h，600-700℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体。
根据进一步的方案说明，该耐高温隔热陶瓷复合材料中的表面修饰纤维织物陶瓷材料，具体的制备方法包括如下步骤：
(1)将纤维编织混合物放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为950-970℃，沉积炉内压力为280-320Pa，浸没至聚吡咯-丙酮溶液，60-70℃超声反应3-4h，600-700℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体；
(2)在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，球磨24-28h，喷雾干燥，以20-30℃/min升温至500-600℃，保温4-6h，以5-8℃/min升温至1000-1200℃，再冷却至20-25℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
(3)将多孔陶瓷浆料注入表面修饰纤维编织体，边注入边搅拌，得表面修饰纤维织物陶瓷坯体；
(4)将表面修饰纤维织物陶瓷坯体放入高温热压炉中，60-70MPa、1000-1200℃烧结2-4h，得表面修饰纤维织物陶瓷材料。
进一步说明，步骤(1)中，纤维编织混合物为木棉纤维、碳纤维和玻璃纤维组成；聚吡咯-丙酮溶液中聚吡咯和丙酮的质量比为0.2：1。
进一步说明，步骤(2)中，氧化铝粉末、氧化锆纤维、质量浓度75％乙醇溶液、聚乙烯亚胺溶液、聚丙烯酸溶液和无水乙醇的质量比为1：0.6：2：1：1.5：1；步骤(3)中，多孔陶瓷浆料和表面修饰纤维编织体的料液质量比为0.4：1。
根据进一步的方案说明，该耐高温隔热陶瓷复合材料中的多孔薄膜材料，具体的制备方法为采用泡沫金属加入填充液浸泡40-60min，250-350℃热处理20-30min而得。
进一步的方案说明，该多孔薄膜材料，填充液为由质量比为1：1：3的甲基纤维素、聚乙烯醇和聚乙烯吡咯烷酮水溶液混合而成；聚乙烯吡咯烷酮水溶液的质量浓度为10％
与现有技术相比，本发明的有益效果为：
本发明采用特定比例构成陶瓷材料纤维增韧层、多孔薄膜层和粘连层的多层结构，使获得的耐高温隔热陶瓷复合材料显气孔率高、导热系数佳和软化系数好，并对甲苯具有良好的吸附性能，表现出优异的综合性能。
本发明的陶瓷材料纤维增韧层是由多孔陶瓷浆料注入表面修饰纤维编织体，高温热压烧结，制成的表面修饰纤维织物陶瓷材料，孔薄膜层是由泡沫金属制得的多孔薄膜材料，粘连层为环氧胶材料，表面修饰纤维织物陶瓷材料、多孔薄膜材料和环氧胶材料相互协同，从表面修饰纤维织物陶瓷材料内部的细小多孔洞到多孔薄膜材料的表面多孔结构，可对甲苯具有多重的滞留和吸附效应，对高温则具有多重扩散机制。
此外，本发明分别采用聚吡咯-丙酮溶液修饰纤维编织混合物，无水乙醇、聚乙烯亚胺溶液和聚丙烯酸溶液球磨陶瓷粉体，并设定特定的升温程序，充分地提高了表面修饰纤维编织体与多孔陶瓷浆料的混合，进而提升耐高温隔热陶瓷复合材料的隔热性能；采用特定比例的甲基纤维素、聚乙烯醇和聚乙烯吡咯烷酮水溶液处理泡沫金属，有利于提升多孔薄膜材料的组织性能，进而增加耐高温隔热陶瓷复合材料的气孔空隙和软化系数。
具体实施方式
图1为本发明实施例4的耐高温隔热陶瓷复合材料的截面示意图，注：1为多孔薄膜层，2为粘连层，3为陶瓷材料纤维增韧层；
图2为本发明实施例4制备的耐高温隔热陶瓷复合材料的光学显微镜图，从图中可知，该材料具有细小的多孔结构，致密化程度好。
具体实施方式
为了更好理解本发明技术内容，下面提供具体实施例，对本发明做进一步的说明。
本发明实施例所用的实验方法如无特殊说明，均为常规方法。
本发明实施例所用的材料、试剂等，如无特殊说明，均可从商业途径得到。
实施例1
如图1所示，一种耐高温隔热陶瓷复合材料，由质量比为1：0.07：0.04的陶瓷材料纤维增韧层[3]、多孔薄膜层[1]和粘连层[2]的结构构成，粘连层[2]的一面为陶瓷基复合材料纤维增韧层[3]，粘连层[2]的另一面为多孔薄膜层[1]；
其中，陶瓷材料纤维增韧层[3]为由将多孔陶瓷浆料注入表面修饰纤维编织体，高温热压烧结，制成的表面修饰纤维织物陶瓷材料；
多孔薄膜层[1]为由泡沫金属制得的多孔薄膜材料；
粘连层[2]为环氧胶。
实施例2
本实施例与实施例1的区别在于，陶瓷材料纤维增韧层[3]、多孔薄膜层[1]和粘连层[2]的质量比为1：0.07：0.06。
上述实施例1-2的耐高温隔热陶瓷复合材料的制备方法，包括如下步骤：将表面修饰纤维织物陶瓷材料放入模具，依次加入环氧胶和多孔薄膜材料，150℃处理15min，趁热施加电场，电场强度为300V/mm，冷却，得耐高温隔热陶瓷复合材料；
其中，原料制备方法如下：
1、表面修饰纤维织物陶瓷材料
(1)将纤维编织混合物(由木棉纤维、碳纤维和玻璃纤维以1：1：1混合而成)放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为970℃，沉积炉内压力为320Pa，浸没至聚吡咯-丙酮溶液(聚吡咯和丙酮的质量比为0.2：1)，70℃超声反应4h，700℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体；
(2)按质量比为1：0.6：2：1：1.5：1，在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，放入陶瓷管中，以刚玉球为球磨介质，进行球磨28h，喷雾干燥，以30℃/min升温至600℃，保温6h，以8℃/min升温至1200℃，再冷却至25℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
(3)按料液质量比为0.4：1，将多孔陶瓷浆料注入表面修饰纤维编织体，边注入边搅拌，得表面修饰纤维织物陶瓷坯体；
(4)将表面修饰纤维织物陶瓷坯体放入高温热压炉中，70MPa、1200℃烧结4h，得表面修饰纤维织物陶瓷材料。
2、多孔薄膜材料
在泡沫金属中加入填充液浸泡50min，300℃热处理25min，得多孔薄膜材料，其中，填充液为由质量比为1：1：3的甲基纤维素、聚乙烯醇和质量浓度10％聚乙烯吡咯烷酮水溶液混合而成。
实施例3
本实施例与实施例1的区别在于，陶瓷材料纤维增韧层[3]原料-表面修饰纤维织物陶瓷材料制备方法的参数进行调整，具体步骤如下：
(1)将纤维编织混合物(由木棉纤维、碳纤维和玻璃纤维以1：1：1混合而成)放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为960℃，沉积炉内压力为300Pa，浸没至聚吡咯-丙酮溶液(聚吡咯和丙酮的质量比为0.2：1)，65℃超声反应3.5h，650℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体；
(2)按质量比为1：0.6：2：1：1.5：1，在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，放入陶瓷管中，以刚玉球为球磨介质，进行球磨26h，喷雾干燥，以25℃/min升温至500℃，保温5h，以6℃/min升温至1000℃，冷却至20℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
(3)按料液质量比为0.4：1，将多孔陶瓷浆料注入表面修饰纤维编织体，边注入边搅拌，得表面修饰纤维织物陶瓷坯体；
(4)将表面修饰纤维织物陶瓷坯体放入高温热压炉中，65MPa、1000℃烧结3h，得表面修饰纤维织物陶瓷材料。
实施例4
本实施例与实施例3的区别在于，耐高温隔热陶瓷复合材料制备方法的参数进行调整，具体步骤如下：
按质量比为1：0.06：0.05，将表面修饰纤维织物陶瓷材料放入模具，依次加入环氧胶和多孔薄膜材料，180℃处理12min，趁热施加电场，电场强度为250V/mm，冷却，得耐高温隔热陶瓷复合材料。
实施例5
本实施例与实施例4的区别在于，陶瓷材料纤维增韧层[3]-表面修饰纤维织物陶瓷材料的制备方法不同，未进行表面修饰，具体步骤如下：
(1)将纤维编织混合物(由木棉纤维、碳纤维和玻璃纤维以1：1：1混合而成)放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为960℃，沉积炉内压力为300Pa，得纤维编织体；
(2)按质量比为1：0.6：2：1：1.5：1，在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，放入陶瓷管中，以刚玉球为球磨介质，进行球磨26h，，喷雾干燥，以25℃/min升温至500℃，保温5h，以6℃/min升温至1000℃，再冷却至20℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
(3)按料液质量比为0.4：1，将多孔陶瓷浆料注入纤维编织体，边注入边搅拌，得纤维织物陶瓷坯体；
(4)将纤维织物陶瓷坯体放入高温热压炉中，65MPa、1000℃烧结3h，得纤维织物陶瓷材料。
实施例6
本实施例与实施例4的区别在于，陶瓷材料纤维增韧层[3]-表面修饰纤维织物陶瓷材料的制备方法不同，步骤(2)不同，具体步骤如下：
(1)将纤维编织混合物(由木棉纤维、碳纤维和玻璃纤维以1：1：1混合而成)放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为960℃，沉积炉内压力为300Pa，浸没至聚吡咯-丙酮溶液(聚吡咯和丙酮的质量比为0.2：1)，65℃超声反应3.5h，650℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体；
(2)按质量比为1：0.6：3：1：1.5，在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，放入陶瓷管中，以刚玉球为球磨介质，进行球磨26h，得陶瓷浆料；
(3)按料液质量比为0.4：1，将陶瓷浆料注入表面修饰纤维编织体，边注入边搅拌，得表面修饰纤维织物陶瓷坯体；
(4)将表面修饰纤维织物陶瓷坯体放入高温热压炉中，65MPa、1000℃烧结3h，得表面修饰纤维织物陶瓷材料。
实施例7
本实施例与实施例4的区别在于，多孔薄膜层[1]中，采用泡沫金属替换多孔薄膜材料。
对比例1
本对比例与实施例4的区别在于，陶瓷材料纤维增韧层[3]、多孔薄膜层[1]和粘连层[2]的质量比为1：0.03：0.04。
对比例2
本对比例与实施例4的区别在于，采用氧化铝陶瓷材料替换陶瓷材料纤维增韧层[3]的表面修饰纤维织物陶瓷材料，氧化铝陶瓷材料的制备步骤如下：
(1)按质量比为1：0.6：3：0.05，在氧化铝粉末中加入碳纳米管、无水乙醇和烧结助剂氧化钇，球磨26h，得陶瓷料浆；
(2)将陶瓷料浆烘干，采用质量浓度5％聚乙烯醇水溶液对陶瓷粉体进行造粒，得陶瓷粉体；
(3)将陶瓷粉体以0.5MPa进行模压成型，烘干，得陶瓷体，以25℃/min速率升温到550℃，再以6℃/min速率升温到1000℃，保温4h，冷却，得氧化铝陶瓷材料。
该耐高温隔热陶瓷复合材料，制备方法如下：
按质量比为1：0.06：0.05，将氧化铝陶瓷材料放入模具，依次加入环氧胶和多孔薄膜材料，180℃处理12min，趁热施加电场，电场强度为250V/mm，冷却，得耐高温隔热陶瓷复合材料。
对比例3
本对比例与实施例4的区别在于，耐高温隔热陶瓷复合材料仅有陶瓷材料纤维增韧层[3]。
试验例1
导热系数的测定：采用激光热导仪测定材料的热扩散系数α(cm2·s-1)和比热容Cp(J·g-1·k-1)，采用堆积密度仪测定材料的堆积密度ρ(g·cm-3)，计算公式：导热系数k(W·m-1·k-1)＝ρCpα。
显气孔率的测定：按照GB/T 2997-2015《致密定形耐火制品体积密度、显气孔率和真气孔率试验方法》进行测定；
软化系数的测定：取20g制备的耐高温隔热陶瓷复合材料，在水中浸泡20h，过滤烘干，计算软化系数S，公式如下：
软化系数S＝F1/F0，式中，F1为浸泡后材料的耐压强度，F0为浸泡前材料的耐压强度，当S>0 85时，可表示材料具备耐水性能，实验结果如下表。
表1
| 项目 | 导热系数 | 显气孔率(％) | 软化系数 |
| 实施例1 | 0.013 | 86.8 | 1.00 |
| 实施例2 | 0.017 | 85.4 | 1.02 |
| 实施例3 | 0.012 | 86.0 | 1.03 |
| 实施例4 | 0.010 | 85.5 | 1.05 |
| 实施例5 | 0.046 | 71.0 | 0.82 |
| 实施例6 | 0.057 | 68.5 | 0.85 |
| 实施例7 | 0.036 | 75.8 | 0.75 |
| 对比例1 | 0.028 | 72.7 | 0.99 |
| 对比例2 | 0.092 | 60.7 | 0.67 |
| 对比例3 | 0.078 | 65.6 | 0.77 |
由上表可知，实施例1-4的导热系数在0.020(W·m-1·k-1)以下，具备优异的隔热性能，显气孔率可达86.8％，软化系数最高可达1.05，实施例4虽然显气孔率稍有降低，但从整体上考虑，其综合性能优良，表明本发明通过采用特定配比的陶瓷材料纤维增韧层、多孔薄膜层和粘连层的结构，构成具有多层的耐高温隔热陶瓷复合材料，可使其具有优良的综合性能；实施例5和6，表明本发明制备的表面修饰纤维织物陶瓷材料对材料的导热性能有较大影响；实施例7表明本发明制备的多孔薄膜材料有助于提升软化系数。
对比例1显气孔率下降较多，表明特定配比的陶瓷材料纤维增韧层、多孔薄膜层和粘连层，有助于调整三层的耐高温隔热陶瓷复合材料的气孔率；对比例2采用普通的氧化铝陶瓷材料，各方面性能都较差；对比例3表明多孔薄膜层和粘连层有利于提高材料的隔热性能。
试验例2
设置实验参数为：入口处甲苯的浓度为1000mg/m3、体积空速为6000h-1、流动时间为4h，吸附温度为400℃，以甲苯的吸附率Y为评价指标，计算公式：吸附率Y＝(1-C1/C0)×100，式中，C0为入口处甲苯的浓度，C1为出口处甲苯的浓度，选用市售沸石分子筛蜂窝陶瓷(型号13X，萍乡市美陶化工填料有限公司)作为对照，实验结果如下表。
表2
由上表可知，本发明实施例1-4制备的耐高温隔热陶瓷复合材料对甲苯具有良好的吸附性能，吸附率可达72.8％，优于市售产品。
以上所述仅为本发明的较佳实施例而已，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 (10)
1.一种耐高温隔热陶瓷复合材料，其特征在于，包括质量比为1：0.05-0.07：0.04-0.06的陶瓷材料纤维增韧层、多孔薄膜层和粘连层的结构；
所述粘连层的一面为陶瓷基复合材料纤维增韧层，所述粘连层的另一面为多孔薄膜层。
2.根据权利要求1的一种耐高温隔热陶瓷复合材料，其特征在于，所述陶瓷材料纤维增韧层为将多孔陶瓷浆料注入表面修饰纤维编织体，高温热压烧结，制成的表面修饰纤维织物陶瓷材料；
所述多孔薄膜层为泡沫金属制得的多孔薄膜材料；
所述粘连层为环氧胶。
3.根据权利要求1或2的一种耐高温隔热陶瓷复合材料，其特征在于，所述耐高温隔热陶瓷复合材料是采用将表面修饰纤维织物陶瓷材料放入模具，依次加入环氧胶和多孔薄膜材料，150-200℃处理10-15min，趁热施加电场，电场强度为200-300V/mm，冷却后而得。
4.根据权利要求2的一种耐高温隔热陶瓷复合材料，其特征在于，所述多孔陶瓷浆料是由氧化铝和氧化锆纤维，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，球磨，喷雾干燥，烧结，研磨，无水乙醇溶解而得；
所述表面修饰纤维编织体为由纤维编织混合物与四氯化碳气相沉积反应，经聚吡咯-丙酮溶液超声反应，烧结，冷却，清洗，干燥后制得。
5.根据权利要求2或4的一种耐高温隔热陶瓷复合材料，其特征在于，所述多孔陶瓷浆料的制备方法，包括如下步骤：在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，球磨24-28h，喷雾干燥，以20-30℃/min升温至500-600℃，保温4-6h，以5-8℃/min升温至1000-1200℃，再冷却至20-25℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
所述表面修饰纤维编织体的制备方法，包括如下步骤：将纤维编织混合物放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为950-970℃，沉积炉内压力为280-320Pa，浸没至聚吡咯-丙酮溶液，60-70℃超声反应3-4h，600-700℃烧结，冷却，清洗，干燥，得表面修饰纤维编织体。
6.根据权利要求5的一种耐高温隔热陶瓷复合材料，其特征在于，所述表面修饰纤维织物陶瓷材料的制备方法，包括如下步骤：
(1)将纤维编织混合物放入沉积炉中，通入四氯化碳进行气相沉积反应，沉积温度为950-970℃，沉积炉内压力为280-320Pa，浸没至聚吡咯-丙酮溶液，60-70℃超声反应3-4h，600-700℃烧结，冷却、清洗、干燥，得表面修饰纤维编织体；
(2)在氧化铝粉末中加入氧化锆纤维，超声分散，加入质量浓度75％乙醇溶液、聚乙烯亚胺溶液和聚丙烯酸溶液，搅拌，球磨24-28h，喷雾干燥，以20-30℃/min升温至500-600℃，保温4-6h，以5-8℃/min升温至1000-1200℃，再冷却至20-25℃，研磨，加入无水乙醇，搅拌，得多孔陶瓷浆料；
(3)将多孔陶瓷浆料注入表面修饰纤维编织体，边注入边搅拌，得表面修饰纤维织物陶瓷坯体；
(4)将表面修饰纤维织物陶瓷坯体放入高温热压炉中，60-70MPa、1000-1200℃烧结2-4h，得表面修饰纤维织物陶瓷材料。
7.根据权利要求6的一种耐高温隔热陶瓷复合材料，其特征在于，步骤(1)中，所述纤维编织混合物为木棉纤维、碳纤维和玻璃纤维组成；所述聚吡咯-丙酮溶液中聚吡咯和丙酮的质量比为0.2：1。
8.根据权利要求6的一种耐高温隔热陶瓷复合材料，其特征在于，步骤(2)中，所述氧化铝粉末、氧化锆纤维、质量浓度75％乙醇溶液、聚乙烯亚胺溶液、聚丙烯酸溶液和无水乙醇的质量比为1：0.6：2：1：1.5：1；步骤(3)中，所述多孔陶瓷浆料和表面修饰纤维编织体的料液质量比为0.4：1。
9.根据权利要求2的一种耐高温隔热陶瓷复合材料，其特征在于，所述多孔薄膜材料是采用泡沫金属加入填充液浸泡40-60min，250-350℃热处理20-30min而得。
10.根据权利要求9的一种耐高温隔热陶瓷复合材料，其特征在于，所述填充液为由质量比为1：1：3的甲基纤维素、聚乙烯醇和聚乙烯吡咯烷酮水溶液混合而成；所述聚乙烯吡咯烷酮水溶液的质量浓度为10％。
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