CN102716700B - 一种高强度耐高温块状C-AlN复合气凝胶的制备方法 - Google Patents
一种高强度耐高温块状C-AlN复合气凝胶的制备方法 Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 63
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 46
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 42
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 23
- 238000000352 supercritical drying Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 46
- 230000032683 aging Effects 0.000 claims description 30
- 239000000499 gel Substances 0.000 claims description 30
- 239000011240 wet gel Substances 0.000 claims description 27
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000001294 propane Substances 0.000 claims description 12
- 238000005352 clarification Methods 0.000 claims description 10
- 238000006073 displacement reaction Methods 0.000 claims description 10
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 9
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000011810 insulating material Substances 0.000 abstract description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- 229910017083 AlN Inorganic materials 0.000 description 32
- 235000019441 ethanol Nutrition 0.000 description 13
- 239000007787 solid Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
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- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
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Abstract
本发明涉及高强度耐高温块状C-AlN复合气凝胶的制备方法,通过将氯化铝结晶体、水、乙醇、环氧丙烷均匀搅拌,得到澄清的氧化铝溶胶溶液,再向溶液中加入甲醛、间苯二酚,搅拌均匀,得到RF/Al2O3复合气凝胶溶胶溶液,静置凝胶。再利用CO2超临界干燥法对样品进行处理,最后对样品进行氮气条件下高温热处理,最终得到高强度耐高温块状C-AlN复合气凝胶。本发明制备工艺过程简单,制备出的复合气凝胶具有高完整性、高比表面积、结构完整、低热导率、低密度、高强度等优点,该体系在1500℃以上高温隔热材料方面将具有很好的应用价值。
Description
技术领域
本发明属于具有高温隔热特征无机纳米材料制备的技术领域,涉及一种高强度块状C-AlN复合气凝胶的制备方法,尤其采用一种CO2超临界法制备高强度块状C-AlN复合气凝胶的方法。
背景技术
气凝胶是由胶体粒子或高聚物分子相互聚结构成的一种纳米孔网络结构,是一种新型的多孔材料。气凝胶材料具有高的比表面积、高孔隙率、低折射率、低密度、强吸附性,而且在热学、光学、电学、声学等方面都表现出独特的性质。尤其,在热学方面,气凝胶的纳米多孔结构能够有效抑制固态热传导和气体传热,具有优异的隔热特性,是目前公认热导率最低的固态材料,因此,气凝胶作为一种轻质保温隔热材料在航天航空、化工、冶金、节能建筑等领域具有广阔的应用前景。
虽然气凝胶材料具有诸多的优良性能,但本身的脆性问题以及耐高温性能(大于1000℃)大大限制了其工作条件。氮化铝(AlN)类属金刚石氮化物,最高可稳定在2200℃,室温强度高,而且随温度的升高强度下降较慢。AlN材料还是电绝缘体,介电性能良好,用作电器元件也很有希望。C-AlN复合气凝胶保持了气凝胶原有的优良特性,而且AlN材料的参杂大大提高了整体气凝胶的强度和耐高温性能,进一步提高了气凝胶材料的应用领域。
发明内容
本发明的目的是为了改善目前所研究的硅、铝等复合体系气凝胶强度较低、高温热稳定性差等缺点而提供一种具有高强度、耐高温1500℃以上的高强度块状C-AlN复合气凝胶的制备方法。
本发明的技术方案为:一种高强度耐高温块状C-AlN复合气凝胶的制备方法,其具体步骤如下:
(1)将结晶氯化铝、蒸馏水、无水乙醇、环氧丙烷均匀搅拌,得到澄清的氧化铝溶胶溶液;
(2)向步骤(1)制得的氧化铝溶胶溶液中加入甲醛,简称R、间苯二酚,简称F,搅拌均匀,得到RF/Al2O3复合气凝胶溶胶溶液;
(3)将步骤(2)中的RF/Al2O3复合气凝胶溶胶溶液倒入模具中反应至凝胶;
(4)向步骤(3)制得的凝胶中加入老化液,进行老化置换处理;
(5)将步骤(4)中老化置换处理好的湿凝胶放置60~75℃烘箱老化5~10d,取出;再进行干燥处理;
(6)将步骤(5)中干燥处理好的样品在氮气条件下进行热处理,得到高强度耐高温块状C-AlN复合气凝胶;
其中:步骤(1)中,结晶氯化铝、蒸馏水、无水乙醇、环氧丙烷摩尔比为=1:(50~70):(20~30):(8~13);步骤(2)中,按结晶氯化铝:间苯二酚:甲醛摩尔比为:(1~5):1:2。
优选步骤(3)中反应至凝胶的时间为2~10h;优选步骤(4)中所述的老化液至少为无水乙醇或去离子水中一种;老化置换处理过程中老化液置换次数为3~5次,每次置换时间为12~24h;优选步骤(5)中所述的干燥处理为CO2超临界干燥法;其中CO2超临界干燥法采用CO2气体保护,反应温度为45~50℃,高压反应釜压力控制在8~12MP,反应时间为2~3d;优选步骤(6)中所述的热处理温度在1500~1700℃之间,热处理时间为1h~10h。
有益效果:
1、本发明采用超临界干燥技术制备出RF/Al2O3复合块状气凝胶,在经过高温热处理得到高强度耐高温块状C-AlN复合气凝胶。首先通过溶胶凝胶法制备出RF/Al2O3复合气凝胶湿凝胶体系,再利用超临界干燥技术制备出孔隙均匀(通过例1所制备的高强度耐高温块状C-AlN复合气凝胶的SEM照片可以看出),再进行样品的高温热处理得到高强度耐高温块状C-AlN复合气凝胶,其比表面积较大(以Al、R摩尔比1:1为例,比表面积为500~600m2/g)、强度高(以Al、C摩尔比1:1为例,热处理时间为2h,密度为0.16g/cm3,压缩强度高达4-6MPa,远远超过了Si、Al体系以及纤维增强气凝胶的压缩强度)。此方法制备的高强度耐高温块状C-AlN复合气凝胶不需要多余的繁琐步骤,制备过程简单容易操作。
2、本发明制备的高强度耐高温块状C-AlN复合气凝胶,采用的是廉价的无机盐作为铝源,再结合碳气凝胶良好的机械性能进行复合制备,目前铝、碳体系复合制备气凝胶国内外还没有相关报道,由于高强度耐高温块状C-AlN复合气凝胶不仅具备气凝胶的所有特征,更重要的是其具有高的强度和良好的高温热稳定性,是传统方法制备的气凝胶无法超越的,所以此发明非常具有意义,将会在各个领域有更好的应用前景。
附图说明
图1是实施例1所制备的高强度耐高温块状C-AlN复合气凝胶的SEM照片。
具体实施方式
实例1
将氯化铝结晶体、间苯二酚、甲醛按摩尔比1:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.1mol的结晶氯化铝倒入500ml烧杯中,再向烧杯中加入151.4ml乙醇(Al/EtOH=1:26),90ml去离子水(Al/H2O=1:50),63ml环氧丙烷(Al/PO=9),充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。,从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约8h,凝胶后,采用乙醇作为老化液,置换湿凝胶中的杂质离子,置换3次,每次24h。最后,再将模具中的湿凝胶放入75℃烘箱进行高温老化10d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在10MPa,控制温度在50℃,超临界干燥时间为48h。最后,对样品进行氮气条件下1500℃高温热处理2h,得到高强度耐高温块状C-AlN复合气凝胶。所制备的高强度耐高温块状C-AlN复合气凝胶的SEM照片;经过表征发现,该气凝胶的比表面积为596m2/g,压缩强度为5.22MPa。
实例2
将氯化铝结晶体、间苯二酚、甲醛按摩尔比2:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.2mol的结晶氯化铝倒入1000ml烧杯中,再向烧杯中加入349.9ml乙醇(Al/EtOH=1:30),252ml去离子水(Al/H2O=1:70),环氧丙烷126ml(Al/PO=9)充分均匀搅拌,直至溶液直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约6h,凝胶后,采用乙醇与去离子水混合溶液作为老化液,置换湿凝胶中的杂质离子,置换5次,每次12h。最后,再将模具中的湿凝胶放入60℃烘箱进行高温老化7d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在12MPa,控制温度在45℃,超临界干燥时间为72h。最后,对样品进行氩气保护1650℃高温热处理1h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶热的比表面积为503m2/g,压缩强度为5.95MPa。
实例3
将氯化铝结晶体、间苯二酚、甲醛按摩尔比5:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.5mol的结晶氯化铝倒入2000ml烧杯中,再向烧杯中加入583.16ml乙醇(Al/EtOH=1:20),450ml去离子水(Al/H2O=1:50),345ml环氧丙烷(Al/PO=1:10)充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约2h,凝胶后,利用去离子水作为老化液,置换湿凝胶中的杂质离子,置换3次,每次18h。最后,再将模具中的湿凝胶放入65℃烘箱进行高温老化5d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在8MPa,控制温度在50℃,超临界干燥时间为60h。最后,对样品进行氮气条件下1550℃高温热处理5h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶的比表面积为526m2/g,压缩强度为4.14MPa。
实例4
将氯化铝结晶体、间苯二酚、甲醛按摩尔比1:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.1mol的结晶氯化铝倒入500ml烧杯中,再向烧杯中加入151ml乙醇(Al/EtOH=1:26),126ml去离子水(Al/H2O=1:70),91ml环氧丙烷(Al/PO=1:13),充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约9h,凝胶后,利用乙醇作为老化液,置换湿凝胶中的杂质离子,置换4次,每次15h。最后,再将模具中的湿凝胶放入70℃烘箱进行高温老化10d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在10MPa,控制温度在45℃,超临界干燥时间为48h。最后,对样品进行氮气条件下1600℃高温热处理3h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶的比表面积为555m2/g,压缩强度为5.17MPa。
实例5
将氯化铝结晶体、间苯二酚、甲醛按摩尔比4:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.4mol的结晶氯化铝倒入2000ml烧杯中,再向烧杯中加入699.8ml乙醇(Al/EtOH=1:30),504ml去离子水(Al/H2O=1:70),307.9ml环氧丙烷(Al/PO=1:11)充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛、,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约7h,凝胶后,利用去离子水作为老化液,置换湿凝胶中的杂质离子,置换4次,每次20h。最后,再将模具中的湿凝胶放入70℃烘箱进行高温老化10d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在11MPa,控制温度在45℃,超临界干燥时间为60h。最后,对样品进行氮气条件下1550℃高温热处理4h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶的比表面积为506m2/g,压缩强度为4.57MPa。
实例6
将氯化铝结晶体、间苯二酚、甲醛按摩尔比2:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.2mol的结晶氯化铝倒入1000ml烧杯中,再向烧杯中加入233.27ml乙醇(Al/EtOH=1:20),216ml去离子水(Al/H2O=1:60),84ml环氧丙烷(Al/PO=1:12)充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),甲醛15ml,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约5h,凝胶后,利用乙醇与去离子水混合溶液作为老化液,置换湿凝胶中的杂质离子,置换4次,每次18h。最后,再将模具中的湿凝胶放入60℃烘箱进行高温老化7d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在10MPa,控制温度在50℃,超临界干燥时间为48h。最后,对样品进行氮气条件下1700℃高温热处理5h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶的比表面积为525m2/g,压缩强度为5.88MPa。
实例7
将氯化铝结晶体、间苯二酚、甲醛按摩尔比3:1:2配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.3mol的结晶氯化铝倒入1000ml烧杯中,再向烧杯中加入454.2ml乙醇(Al/EtOH=1:26),去324ml离子水(Al/H2O=1:60),207ml环氧丙烷(Al/PO=1:10),充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),15ml甲醛,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约6h,凝胶后,利用乙醇作为老化液,置换湿凝胶中的杂质离子,置换5次,每次12h。最后,再将模具中的湿凝胶放入70℃烘箱进行高温老化10d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在8MPa,控制温度在50℃,超临界干燥时间为72h。最后,对样品进行氮气条件下1600℃高温热处理5h,得到块状碳支撑Al2O3-Al4C3复合气凝胶。经过表征发现,该气凝胶的比表面积为508m2/g,压缩强度为5.18MPa。
实例8
将氯化铝结晶体、间苯二酚、甲醛按摩尔比3:1:1配置制备高强度耐高温块状C-AlN复合气凝胶。第一步:称取0.3mol的结晶氯化铝倒入1000ml烧杯中,再向烧杯中加入524.85ml乙醇(Al/EtOH=1:30),270ml去离子水(Al/H2O=1:50),252ml环氧丙烷(Al/PO=1:12),充分均匀搅拌,直至得到澄清的氧化铝溶胶溶液。第二步:再向第一步氧化铝溶胶溶液中加入0.1mol的间苯二酚(白色针状结晶),甲醛15ml,充分均匀搅拌,直至溶液完全呈现浅红色澄清溶胶溶液。从而得到RF/Al2O3复合气凝胶溶胶溶液,倒入模具凝胶。室温凝胶时间大约4h,凝胶后,利用去离子水作为老化液,置换湿凝胶中的杂质离子,置换3次,每次20h。最后,再将模具中的湿凝胶放入75℃烘箱进行高温老化5d,使其充分反应。再将RF/Al2O3复合湿凝胶放入高温高压釜中,利用CO2超临界干燥法对样品进行干燥,其中CO2压力控制在10MPa,控制温度在45℃,超临界干燥时间为60h。最后,对样品进行氮气条件下1650℃高温热处理10h,得到高强度耐高温块状C-AlN复合气凝胶。经过表征发现,该气凝胶热的比表面积为426m2/g,压缩强度为5.31MPa。
Claims (3)
1.一种高强度耐高温块状C-AlN复合气凝胶的制备方法,其具体步骤如下:
(1)将结晶氯化铝、蒸馏水、无水乙醇、环氧丙烷均匀搅拌,得到澄清的氧化铝溶胶溶液;
(2)向步骤(1)制得的氧化铝溶胶溶液中加入甲醛,简称R、间苯二酚,简称F,搅拌均匀,得到RF/Al2O3复合气凝胶溶胶溶液;
(3)将步骤(2)中的RF/Al2O3复合气凝胶溶胶溶液倒入模具中反应至凝胶;
(4)向步骤(3)制得的凝胶中加入老化液,进行老化置换处理;
(5)将步骤(4)中老化置换处理好的湿凝胶放置60~75℃烘箱老化5~10d,取出;再进行干燥处理;其中所述的干燥处理为CO2超临界干燥法;其中CO2超临界干燥法采用CO2气体保护,反应温度为45~50℃,高压反应釜压力控制在8~12MPa,反应时间为2~3d。
(6)将步骤(5)中干燥处理好的样品在氮气条件下进行热处理,得到高强度耐高温块状C-AlN复合气凝胶;所述的热处理温度在1500~1700℃之间,热处理时间为1h~10h;其中:步骤(1)中,结晶氯化铝、蒸馏水、无水乙醇、环氧丙烷摩尔比为=1:(50~70):(20~30):(8~13);步骤(2)中,按结晶氯化铝:间苯二酚:甲醛摩尔比为:(1~5):1:2。
2.根据权利要求1所述的制备方法,其特征在于,步骤(3)中反应至凝胶的时间为2~10h。
3.根据权利要求1所述的制备方法,其特征在于,步骤(4)中所述的老化液至少为无水乙醇或去离子水中一种;老化置换处理过程中老化液置换次数为3~5次,每次置换时间为12~24h。
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US9869422B2 (en) | 2018-01-16 |
US20150108389A1 (en) | 2015-04-23 |
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