CN111099912A - 耐高温隔热透波一体化气凝胶复合材料及其制备工艺 - Google Patents
耐高温隔热透波一体化气凝胶复合材料及其制备工艺 Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 86
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 239000000463 material Substances 0.000 claims abstract description 64
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- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 24
- 239000003292 glue Substances 0.000 claims description 20
- 239000004965 Silica aerogel Substances 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 12
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- 239000010453 quartz Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
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- 230000032683 aging Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
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- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 4
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229920002748 Basalt fiber Polymers 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002168 alkylating agent Substances 0.000 claims description 2
- 229940100198 alkylating agent Drugs 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
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- 239000000919 ceramic Substances 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- 239000001913 cellulose Substances 0.000 claims 1
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- 238000002834 transmittance Methods 0.000 abstract description 4
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- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 239000002657 fibrous material Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
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Abstract
本发明公开了一种耐高温隔热透波一体化气凝胶复合材料及其制备工艺,该工艺是采用硅溶胶为原料,在酸、碱催化剂的作用下直接形成凝胶,经过老化、超临界CO2干燥、空气热处理和疏水改性,从而获得热导率低、透波性好、耐高温的SiO2气凝胶复合材料。与现有技术相比,本发明采用一步溶胶‑凝胶法,并通过加入无机耐高温透波纤维,无需引入任何分散剂或表面活性剂,最终制得耐高温隔热透波一体化气凝胶复合材料,适合工业化大批量生产。而且制备的材料具备轻质、耐高温、低密度、低热导率、高透波率等特点。
Description
技术领域
本发明涉及一种耐高温隔热透波一体化气凝胶复合材料及其制备工艺,属于化工材料技术领域。
背景技术
气凝胶是一种具有三维网络结构的介孔材料,孔隙尺寸在1-100nm之间,骨架尺寸为十几纳米,极低密度,比表面积大,孔隙率最高可达99.8%;热导率为静止空气的一半,仅为0.013W/(m.k)。迄今为止,已经研制出的气凝胶有无机气凝胶(如SiO2、Al2O3、ZrO2等),有机气凝胶(如RF、MF等)和炭气凝胶。然而,气凝胶独特的网络结构及高孔隙率和低密度等特点导致了气凝胶本身具有很大的脆性,并且在温度较高的环境中,半透明的气凝胶材料很难阻抗辐射热导率的影响,因此,在很多领域中,气凝胶很难作为隔热材料单独进行使用,需要与其他材料复合才能达到实际的使用效果。通常解决上述问题的方法是将气凝胶与纤维增强材料复合形成复合材料,以此改善气凝胶材料的强度。
高超声速飞行器长时间在大气层内高速飞行,气动加热严重,飞行器外表面温度达1200K,局部温度可达1400K。由于热量长时间向舱内传递的特性,加之飞行器本身空间狭小等特点,要求在有限空间和重量约束条件下实现对内部设备的有效热防护。上述约束条件对热防护系统提出了很高的要求。气凝胶隔热材料是目前隔热性能最优异的固体材料,已经成为高超声速飞行器热防护系统的首选隔热材料。但通常方法制备的气凝胶隔热材料无法满足高温稳定性好、隔热性能优异的要求。
现有技术中,有通过溶剂交换进行表面修饰并结合常压干燥技术来制备气凝胶纤维毡复合材料的,然而,气凝胶与纤维基体的成分及结构差别较大,这种制备方法并不能很好的平衡二者的性能,所得复合材料的强度性能虽得到改善,但是其导热系数却是纯气凝胶的数倍,较大地损失了气凝胶本身的隔热性能。
发明内容
本发明的目的在于提供一种耐高温隔热透波一体化气凝胶复合材料及其制备工艺,该方法用料和工艺简单,微观结构可控性好,制备出的气凝胶材料具备耐高温、低密度、低热导率、低介电常数、低介质损耗等特性,在保留气凝胶优异隔热性能的同时改善了机械性能,以期达到显著降低雷达天线罩的尺寸和重量,提高雷达的隔热效果和透波性能的效果,从而满足高超声速可重复使用飞行器、防空、潜地、巡航导弹等武器装备雷达天线罩中透波隔热一体化材料的迫切需求。
本发明的技术方案是这样实现的:
本发明的一种耐高温隔热透波一体化气凝胶复合材料及其制备工艺,该工艺是采用硅溶胶为原料,在酸、碱催化剂的作用下直接形成凝胶,经过老化、超临界CO2干燥、空气热处理和疏水改性,从而获得热导率低、透波性好、耐高温的SiO2气凝胶复合材料。包括以下步骤:
1)二氧化硅气凝胶胶液的配制;
2)二氧化硅气凝胶胶液与纤维模具的复合成型;
3)气凝胶湿材料的老化;
4)气凝胶湿材料的超临界CO2干燥;
5)纤维增强气凝胶材料在马弗炉中进行空气热处理;
6)耐高温隔热透波一体化气凝胶复合材料的疏水改性。
前述方法中,所述二氧化硅气凝胶胶液的原料包括硅溶胶、酸性催化剂、碱性催化剂。
前述方法中,所述硅溶胶包括硅溶胶、硅溶胶的稀释液,硅溶胶的浓度要求为15%~35%。
前述方法中,所述酸性催化剂包括草酸、盐酸、硝酸、硫酸、醋酸中的一种或两种以上的混合物。
前述方法中,所述碱性催化剂包括氨水、氢氧化钠、氟化铵、碳酸铵、碳酸氢铵、乙二胺中的一种或两种以上的混合物。
前述方法中,所述纤维模具是以直径为纳米级的纤维丝制成的,密度不大于240kg/m3,包括高纯石英纤维、超细高硅氧纤维、硅酸铝陶瓷纤维、多晶莫来石纤维、玄武岩纤维或多晶氧化铝纤维中的一种。
前述方法中,所述二氧化硅气凝胶胶液由如下摩尔比的组分配制而成:硅溶胶:酸性催化剂:碱性催化剂=(80~120):(1~10):(1~10)。
前述方法中,所述二氧化硅气凝胶胶液与纤维模具的复合成型是先将二氧化硅气凝胶胶液与碱性催化剂通过在线混合的方式混合均匀,然后采用真空注胶的方式将其与纤维模具深度复合,反应至凝胶,室温条件下静置6~24h形成气凝胶湿材料。
前述方法中,所述老化是将气凝胶湿材料表面洒上少量水,放入80±5℃的烘箱中烘24~48h。
前述方法中,所述气凝胶湿材料的表面溶剂置换是将气凝胶湿材料置于50±5℃的溶剂中溶剂置换24~72h,每隔8h更换一次溶剂。所述溶剂包括乙醇、甲醇、丙醇、乙醚、烷基化试剂或直链醇中的一种或两种混合以上。
前述方法中,所述超临界CO2干燥是将经过表面溶剂置换的气凝胶湿材料放入萃取釜中,将CO2流体注入萃取釜,调节萃取釜内温度和压力在CO2流体的超临界状态下与材料接触,使材料中的溶剂溶解于超临界流体之中,从而达到干燥的效果。
前述方法中,所述二氧化碳气体的超临界状态温度为50~60℃,压力为12~16MPa;二氧化碳气体通过萃取釜的流量为250~350kg/h,干燥时间为3~8h。
前述方法中,所述的空气热处理是将经过超临界干燥的纤维增强气凝胶材料置于高温马弗炉中,100℃~600℃,处理5~8h。然后自然降温至室温。
前述方法中,所述耐高温隔热透波一体化气凝胶复合材料的疏水改性是将经过空气热处理后的耐高温隔热透波一体化气凝胶复合材料连同模具放入100℃烘箱中加热2h后,称取一定量的疏水改性剂,通过模具使疏水改性剂抽入模具内,材料在改性剂气氛中反应24~72h。所述疏水改性剂包括三甲基氯硅烷、甲基三乙氧基硅烷、甲基三甲氧基硅烷或乙基三乙氧基硅烷中的一种或两种以上的组合。
前述方法中,所述检测步骤是将最佳工艺条件下萃出材料随机选取三点(三点应尽量能反映整卷材料的性能),取300×300mm材料各两块,测量其最高耐受温度、体积密度、导热系数、憎水性和光学透过率。
与现有技术相比,本发明具有以下突出的实质性特点和显著的进步:纤维基材用做二氧化硅气凝胶的复合基材,制备出的耐高温隔热透波一体化气凝胶复合材料导热系数低;抗压性、抗曲性高;介电常数、节电损耗低,使用温度范围为室温~1000℃,常温下导热系数为0.0180~0.0230W/m·K,1000℃导热系数为0.0610~0.0690W/m·K,憎水率≥99%。
本发明方法以及由该方法制备的一种耐高温隔热透波一体化气凝胶复合材料还具有如下特点:
(1)工艺简单。采用一步溶胶-凝胶法,并通过加入无机耐高温透波纤维,无需引入任何分散剂或表面活性剂,最终制得耐高温隔热透波一体化气凝胶复合材料,适合工业化大批量生产。
(2)制备的材料具备轻质、耐高温、低密度、低热导率、高透波率等特点,可为其工程化应用奠定材料和工艺技术基础,有望应用于重复使用飞行器天线罩或窗口,对于保障国家安全具有重大社会效益。
具体实施方式
下面将结合本发明的实施例,对本发明的技术方案进行清楚、完整地描述:
实施例1:
耐高温隔热透波一体化气凝胶复合材料的制备工艺包括以下步骤:二氧化硅胶液配制→二氧化硅气凝胶胶液与纤维模具的复合成型→老化→超临界CO2干燥→空气热处理→疏水改性→检测。配制如下摩尔比的二氧化硅气凝胶胶液:硅溶胶:酸性催化剂:碱性催化剂=95:4:4。酸性催化剂为1mol/L盐酸溶液,碱性催化剂为4mol/L氟化铵水溶液。通过在线混合的方式将酸性硅溶胶与氟化铵水溶液混合均匀,然后采用真空注胶的方式将其与石英纤维模具深度复合,反应至凝胶,室温条件下静置6h形成气凝胶湿材料。表面洒上少量水,放入80℃的烘箱中烘48h。将经过老化的石英纤维气凝胶湿材料放入乙醇溶液中55℃浸泡72h,每隔8h换一次乙醇溶液,并检测溶剂置换后的乙醇溶液的浓度直至乙醇浓度≥90%。将溶剂置换充分后的石英纤维气凝胶湿材料放入萃取釜的物料桶中,将二氧化碳气体注入萃取釜,保持萃取釜内温度和压力在二氧化碳气体的超临界状态与材料接触,使材料中的溶剂溶解于超临界流体之中,超临界温度为55℃,压力为14MPa,萃取时间为5.5h;二氧化碳气体通过萃取釜的流量为270kg/h,从萃取釜的萃取出口收集流体至无溶液排出,停机取出材料。经过超临界CO2干燥的石英纤维增强气凝胶材料置于高温马弗炉中,50℃开始升温,60min升到200℃保温2h,然后再90min升温至600℃,保温2h。然后自然降温至室温。将经过空气热处理后的石英纤维增强气凝胶材料连同模具放入100℃烘箱中加热2h后,称取一定量的疏水改性剂三甲基甲氧基硅烷,通过模具使疏水改性剂抽入模具内,材料在改性剂气氛中反应48h。将经过疏水改性的石英纤维增强气凝胶材料取300×300mm材料各两块,测量密度、导热系数、憎水性、机械强度。测其相关数据:材料厚度10mm,体积密度185kg/m3,常温导热系数0.0217W/m·K,1000℃导热系数为0.0659W/m·K,憎水性为99.5%,光学透过率(85.7%,550nm)。
尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,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)
1.一种耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于该工艺包括以下步骤:
1)二氧化硅气凝胶胶液的配制;
2)二氧化硅气凝胶胶液与纤维模具的复合成型;
3)气凝胶湿材料的老化;
4)气凝胶湿材料的表面溶剂置换;
5)气凝胶湿材料的超临界CO2干燥;
6)纤维增强气凝胶材料在马弗炉中进行空气热处理;
7)耐高温隔热透波一体化气凝胶复合材料的疏水改性。
2.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述二氧化硅气凝胶胶液由如下摩尔比的组分配制而成:硅溶胶:酸性催化剂:碱性催化剂=80~120:1~10:1~10。
3.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述二氧化硅气凝胶胶液的原料包括硅溶胶、酸性催化剂、碱性催化剂;所述硅溶胶包括硅溶胶、硅溶胶的稀释液,硅溶胶的浓度为15%~35%;所述酸性催化剂包括草酸、盐酸、硝酸、硫酸、醋酸中的一种或两种以上的组合,所述碱性催化剂包括氨水、氢氧化钠、氟化铵、碳酸铵、碳酸氢铵、乙二胺中的一种或两种以上的组合。
4.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述二氧化硅气凝胶胶液与纤维模具的复合成型是先将二氧化硅气凝胶胶液与碱性催化剂通过在线混合的方式混合均匀,然后采用真空注胶的方式将其与纤维模具深度复合,反应至凝胶,室温条件下静置6~24h形成气凝胶湿材料。
5.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述纤维模具是以直径为纳米级的纤维丝为材料制成的,密度不大于240kg/m3,所述纤维素的来源包括高纯石英纤维、超细高硅氧纤维、硅酸铝陶瓷纤维、多晶莫来石纤维、玄武岩纤维或多晶氧化铝纤维中的一种或两种以上的组合。
6.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述气凝胶湿材料的老化是将气凝胶湿材料表面洒上少量水,放入80±5℃的烘箱中烘24~48h。
7.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述气凝胶湿材料的表面溶剂置换是将气凝胶湿材料置于50±5℃的溶剂中进行溶剂置换24~72h,每隔8h更换一次溶剂;所述溶剂包括乙醇、甲醇、丙醇、乙醚、烷基化试剂或直链醇中的一种或两种混合以上。
8.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述气凝胶湿材料的超临界CO2干燥是将经过溶剂置换的气凝胶湿材料放入物料桶中,将CO2流体注入物料桶,调节物料桶内温度和压力在CO2流体的超临界状态下与材料接触,使材料中的溶剂溶解于超临界流体之中,从而达到干燥的效果;超临界干燥介质二氧化碳气体的超临界状态温度为50~60℃,压力为12~16MPa;二氧化碳气体通过萃取釜的流量为2500~3500kg/h,干燥时间为3~8h。
9.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述的空气热处理是将经过超临界干燥的纤维增强气凝胶材料置于高温马弗炉中,100℃~600℃,处理5~8h,然后自然降温至室温。
10.根据权利要求1所述的耐高温隔热透波一体化气凝胶复合材料及其制备工艺,其特征在于:所述疏水改性是将经过空气热处理后的耐高温隔热透波一体化气凝胶复合材料连同模具放入100℃烘箱中加热2h后,称取一定量的疏水改性剂,通过模具使疏水改性剂抽入模具内,材料在改性剂气氛中反应24~72h;所述疏水改性剂包括三甲基甲氧基硅烷、三甲基氯硅烷、甲基三乙氧基硅烷、甲基三乙氧基硅烷或乙基三乙氧基硅烷中的一种或其混合物。
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CN115925435A (zh) * | 2022-11-28 | 2023-04-07 | 湖北三江航天江北机械工程有限公司 | 2.5d石英复合陶瓷天线罩快速复合成型方法 |
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