CN112299871A - 一种含碳化硅膜的多孔陶瓷的制备方法 - Google Patents
一种含碳化硅膜的多孔陶瓷的制备方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 94
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229910001868 water Inorganic materials 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000012454 non-polar solvent Substances 0.000 claims abstract description 5
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011812 mixed powder Substances 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- RVDLHGSZWAELAU-UHFFFAOYSA-N 5-tert-butylthiophene-2-carbonyl chloride Chemical compound CC(C)(C)C1=CC=C(C(Cl)=O)S1 RVDLHGSZWAELAU-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- ORPJQHHQRCLVIC-UHFFFAOYSA-N magnesium;propan-2-olate Chemical compound CC(C)O[Mg]OC(C)C ORPJQHHQRCLVIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910002800 Si–O–Al Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
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Abstract
一种含碳化硅膜的多孔陶瓷的制备方法,它涉及碳化硅膜的制备方法。它是要解决现有的碳化硅薄膜的制备方法碳化硅薄膜厚薄不均的技术问题。本方法:将粗、细两种碳化硅粉末混合后,加入到加入到无水非极性溶剂中,再加二三价金属醇盐,搅拌混合得到碳化硅分散液Ⅰ;将水与正丁醇的混合液滴入碳化硅分散液Ⅰ中,混合均匀得到碳化硅分散液Ⅱ,干燥得到处理过的碳化硅粉末;用处理过的碳化硅粉末、分散剂和烧结助剂加水制备浆液;多孔陶瓷支撑体浸入浆液、干燥后烧结,得到含碳化硅膜的多孔陶瓷。该碳化硅膜厚度均匀、致密、裂痕少,机械强度高。可用强酸强碱强氧化条件下的污水净化。
Description
技术领域
本发明涉及碳化硅膜的制备方法。
背景技术
无机陶瓷膜作为膜材料中独特的一类,相比于有机膜,具有机械强度高、抗腐蚀、耐高温、寿命长等特点,其被广范用于化学工业的各个领域。目前常用的无机陶瓷膜材料有二氧化硅、氧化铝等,这些材料在强酸、强碱、高温的特殊条件下,由于其本身固有化学性质的缺陷,会导致其使用寿命与应用效果的下降。
碳化硅的化学性质极为稳定,耐强酸、强碱,且强度较高耐冲击,是制备无机陶瓷膜的一种理想材料,具有很高的应用前景。现有的含碳化硅膜的多孔陶瓷的制备方法有两种:一是将聚碳硅烷等前驱体沉积在多孔陶瓷支撑体上,然后通过高温热解生成碳化硅薄膜。二是将碳化硅颗粒分散到溶液中,然后将多孔陶瓷支撑体放入该溶液中放置一段时间后取出,在多孔陶瓷支撑体表面与内部孔道内附着上一层溶液,之后风干,再进行高温烧结形成碳化硅薄膜。其中第二种方法的效率更高,成本更低,也更具有市场前景。但是这种方法由于碳化硅为原子晶体,且碳与硅的极性相差较小,导致碳化硅颗粒与极性溶剂亲和力相对较差,同时目前也缺少合适的分散剂,使得在使用水等极性做溶剂进行分散时,碳化硅颗粒分布不均匀。这种不均匀会使烧结生成的碳化硅薄膜厚薄不均,机械强度下降,从而使用寿命相对减少。
发明内容
本发明是要解决现有的碳化硅薄膜的制备方法碳化硅薄膜厚薄不均的技术问题,而提供一种含碳化硅膜的多孔陶瓷的制备方法。
本发明的一种含碳化硅膜的多孔陶瓷的制备方法,按以下步骤进行:
一、将粗、细两种碳化硅粉末按质量比为1:(0.2~2)混合均匀,得到碳化硅混合粉末;按碳化硅混合粉末的质量百分浓度为10%~30%将碳化硅混合粉末加入到无水非极性溶剂中,混合均匀后,再按二三价金属醇盐的质量百分浓度为0.1%~0.3%加入二三价金属醇盐,搅拌反应30~60min,得到碳化硅分散液Ⅰ;
二、按水与正丁醇的混合溶液的质量百分浓度为1%~3%,将水与正丁醇的混合溶液滴加到碳化硅分散液Ⅰ中,搅拌反应30~60min,得到碳化硅分散液Ⅱ;
三、将碳化硅分散液Ⅱ在高于所使用有机溶剂沸点的条件下干燥12h~24h,得到处理过的碳化硅粉末;
四、按分散剂的质量百分比浓度为1%~10%、处理过的碳化硅粉的质量百分比浓度为10%~30%、烧结助剂的质量百分浓度为1%~10%称取分散剂、处理过的碳化硅粉和烧结助剂;先将分散剂加入到去离子水中,搅拌均匀后再加入处理过的碳化硅粉,搅拌分散2~5min后再加入烧结助剂,持续搅拌5~10min,得到浆液;
五、将多孔陶瓷支撑体浸入到浆液中保持1~5min后取出,在温度为40~80℃的条件下干燥8~24h,得到预制体;
六、将预制体放在烧结炉中,将烧结炉腔内先抽真空至10-4-10-6Pa,然后充入氩气至5~10个大气压,然后以1000~1500℃/h的升温速度加热到1500~2000℃保持4~5h,降温,得到含碳化硅膜的多孔陶瓷。
更进一步地,步骤一中所述的无水非极性溶剂为正己烷、环己烷、石油醚或二氧六环;
更进一步地,步骤一中所述的二三价金属醇盐为三异丙醇铝、三乙醇铝、乙醇镁或异丙醇镁;
更进一步地,步骤二中所述的水与正丁醇的混合溶液中,水与正丁醇的摩尔比为1:(4~5);
更进一步地,步骤四中所述的分散剂为聚乙二醇、聚丙烯酰胺或羧甲基纤维素;
更进一步地,步骤四中所述的分烧结助剂为氧化铝、氧化钇或硼;
更进一步地,步骤五中所述的多孔陶瓷支撑体的孔径范围1~1000μm,孔隙率为20%~90%;
更进一步地,步骤五中所述的多孔陶瓷支撑体为氧化铝或碳化硅;它们是耐高温材料;
碳化硅表面存在一层由于氧化形成的二氧化硅薄膜,二氧化硅薄膜在空气中会与水发生一定程度的反应,从而形成一些硅羟基基团。本发明利用二三价金属的醇盐与这些基团进行反应,形成硅-氧-金属化学键,使醇盐结合到碳化硅粉末表面。之后再通过水解使结合的醇盐中醇分子脱去,并在碳化硅粉末的表面形成一层金属氢氧化物层。由于金属氢氧化物的极性相对于碳化硅更强,处理过后碳化硅粉末可以更好的在水溶液中分散。在该过程中的反应式如下:
≡Si-OH+RO-Al(OR)2→≡Si-O-Al(OR)2+H20
≡Si-O-Al(OR)2+2H20→≡Si-O-Al(OH)2+ROH
通过本发明的方法在多孔陶瓷表面制备的碳化硅膜厚度均匀、致密、裂痕少,机械强度高。可用强酸强碱强氧化条件下的污水净化。
附图说明
图1是实施例1在多孔陶瓷表面制备的碳化硅膜的扫描电镜照片;
图2是对比实施例1在多孔陶瓷表面制备的碳化硅膜的扫描电镜照片。
具体实施方式
用下面的实施例验证本发明的有益效果。
实施例1:本实施例的一种含碳化硅膜的多孔陶瓷的制备方法,按以下步骤进行:
一、将粒径为0.5~0.6μm的粗碳化硅粉末和粒径为0.1~0.2μm的细碳化硅粉末按质量比为1:1混合均匀,得到碳化硅混合粉末;按碳化硅混合粉末的质量百分浓度为25%将碳化硅混合粉末加入到正己烷中,混合均匀后,再按三异丙醇铝的质量百分浓度为0.1%加入三异丙醇铝,搅拌反应45min,得到碳化硅分散液Ⅰ;
二、按水与正丁醇的混合溶液的质量百分浓度为1.5%,将水与正丁醇的混合溶液滴加到碳化硅分散液Ⅰ中,搅拌反应30min,得到碳化硅分散液Ⅱ;其中水与正丁醇的混合溶液中,水与正丁醇的摩尔比为1:4;
三、将碳化硅分散液Ⅱ在90℃的条件下干燥12h,得到处理过的碳化硅粉末;
四、按分散剂羧甲基纤维素的质量百分比浓度为2%、处理过的碳化硅粉的质量百分比浓度为20%、烧结助剂氧化铝的质量百分浓度为2%称取羧甲基纤维素、处理过的碳化硅粉和氧化铝;先将羧甲基纤维素加入到去离子水中,搅拌均匀后再加入处理过的碳化硅粉,搅拌分散5min后再加入氧化铝,持续搅拌10min,得到浆液;
五、将孔径分布范围5~800μm之间、孔隙率为42%的碳化硅多孔陶瓷支撑体浸入到浆液中保持3min后取出,在温度为80℃的条件下干燥12h,得到预制体;
六、将预制体放在烧结炉中,将烧结炉腔内先抽真空至10-5Pa,然后充入氩气至5个大气压,然后以1200℃/h的升温速度加热到1800℃保持4h,降温,得到含碳化硅膜的碳化硅多孔陶瓷。
对比实施例1:将碳化硅混合粉末不做处理,直接用于制备多孔陶瓷表面的碳化硅膜,作为对比,具体的步骤如下:
一、取粒径为0.5~0.6μm的粗碳化硅粉末和粒径为0.1~0.2μm的细碳化硅粉末按质量比为1:1混合均匀,得到作为对比的碳化硅混合粉末;
二、按分散剂羧甲基纤维素的质量百分比浓度为2%、作为对比的碳化硅混合粉末的质量百分比浓度为20%、烧结助剂氧化铝的质量百分浓度为2%称取羧甲基纤维素、作为对比的碳化硅混合粉末和氧化铝;先将羧甲基纤维素加入到去离子水中,搅拌均匀后再加入作为对比的碳化硅混合粉末,搅拌分散5min后再加入氧化铝,持续搅拌10min,得到对比浆液;
三、将孔径分布范围5~800μm之间、孔隙率为42%的碳化硅多孔陶瓷支撑体浸入到对比浆液中保持3min后取出,在温度为80℃的条件下干燥12h,得到对比预制体;
四、将对比预制体放在烧结炉中,将烧结炉腔内先抽真空至10-5Pa,然后充入氩气至5个大气压,然后以1200℃/h的升温速度加热到1800℃保持4h,降温,得到作为对比的含碳化硅膜的碳化硅多孔陶瓷。
将对比实施例1中作为对比的碳化硅混合粉末与本实施例1的步骤三中得到的处理过的碳化硅粉末同时进行分散稳定性测试,具体是将作为对比的碳化硅混合粉末和处理过的碳化硅粉末以质量百分浓度为20%分别加入到水中,再加入质量百分浓度为2%的羧甲基纤维素,然后磁力搅拌5min,之后静置5h,将上层溶液倒出,对底层粉末干燥、称重,计算沉淀占原物质的质量分数。结果为处理过的碳化硅粉末的沉淀占原加入量的9.7%,而未处理的作为对比的碳化硅混合粉末的沉淀占原加入量的12.1%。通过对比可知,经过处理后的碳化硅混合粉末的分散稳定性提高。
本实施例1制备的含碳化硅膜的碳化硅多孔陶瓷的扫描电镜照片如图1所示,对比实施例1制备的作为对比的含碳化硅膜的碳化硅多孔陶瓷的扫描电镜照片如图2所示。从图1和图2对比,可以看出,实施例1制备的碳化硅多孔陶瓷表面的碳化硅膜裂痕较少,裂缝较窄,而对比实施例1制备的碳化硅多孔陶瓷表面的含碳化硅膜裂痕较多,裂缝较宽。通过对比可知,实施例1中碳化硅粉末的表面改性提高了其在水中的分散性,这减少了分散剂的使用量,也使其分散的更加均一,减少了因分散不均导致生成的碳化硅薄膜厚薄不均、开裂及机械强度下降现象。
实施例2:本实施例的一种含碳化硅膜的多孔陶瓷的制备方法,按以下步骤进行:
一、将粒径为0.5~0.6μm的粗碳化硅粉末和粒径为0.1~0.2μm的细碳化硅粉末按质量比为1:2混合均匀,得到碳化硅混合粉末;按碳化硅混合粉末的质量百分浓度为30%将碳化硅混合粉末加入到正己烷中,混合均匀后,再按三异丙醇铝的质量百分浓度为0.2%加入三异丙醇铝,搅拌反应45min,得到碳化硅分散液Ⅰ;
二、按水与正丁醇的混合溶液的质量百分浓度为3%,将水与正丁醇的混合溶液滴加到碳化硅分散液Ⅰ中,搅拌反应50min,得到碳化硅分散液Ⅱ;其中水与正丁醇的混合溶液中,水与正丁醇的摩尔比为1:4;
三、将碳化硅分散液Ⅱ在90℃的条件下干燥24h,得到处理过的碳化硅粉末;
四、按分散剂聚丙烯酰胺的质量百分比浓度为8%、处理过的碳化硅粉的质量百分比浓度为30%、烧结助剂氧化铝的质量百分浓度为5%称取聚丙烯酰胺、处理过的碳化硅粉和氧化铝;先将聚丙烯酰胺加入到去离子水中,搅拌均匀后再加入处理过的碳化硅粉,搅拌分散5min后再加入氧化铝,持续搅拌10min,得到浆液;
五、将孔径分布范围5~800μm之间、孔隙率为42%的碳化硅多孔陶瓷支撑体浸入到浆液中保持5min后取出,在温度为60℃的条件下干燥12h,得到预制体;
六、将预制体放在烧结炉中,将烧结炉腔内先抽真空至10-5Pa,然后充入氩气至5个大气压,然后以1500℃/h的升温速度加热到2000℃保持4h,降温,得到含碳化硅膜的碳化硅多孔陶瓷。
实施例2制备的碳化硅多孔陶瓷表面的碳化硅膜裂痕较少,碳化硅薄膜厚薄均匀,提高了膜层的机械强度。
Claims (8)
1.一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于该方法按以下步骤进行:
一、将粗、细两种碳化硅粉末按质量比为1:(0.2~2)混合均匀,得到碳化硅混合粉末;按碳化硅混合粉末的质量百分浓度为10%~30%将碳化硅混合粉末加入到无水非极性溶剂中,混合均匀后,再按二三价金属醇盐的质量百分浓度为0.1%~0.3%加入二三价金属醇盐,搅拌反应30~60min,得到碳化硅分散液Ⅰ;
二、按水与正丁醇的混合溶液的质量百分浓度为1%~3%,将水与正丁醇的混合溶液滴加到碳化硅分散液Ⅰ中,搅拌反应30~60min,得到碳化硅分散液Ⅱ;
三、将碳化硅分散液Ⅱ在高于所使用有机溶剂沸点的条件下干燥12h~24h,得到处理过的碳化硅粉末;
四、按分散剂的质量百分比浓度为1%~10%、处理过的碳化硅粉的质量百分比浓度为10%~30%、烧结助剂的质量百分浓度为1%~10%称取分散剂、处理过的碳化硅粉和烧结助剂;先将分散剂加入到去离子水中,搅拌均匀后再加入处理过的碳化硅粉,搅拌分散2~5min后再加入烧结助剂,持续搅拌5~10min,得到浆液;
五、将多孔陶瓷支撑体浸入到浆液中保持1~5min后取出,在温度为40~80℃的条件下干燥8~24h,得到预制体;
六、将预制体放在烧结炉中,将烧结炉腔内先抽真空至10-4-10-6Pa,然后充入氩气至5~10个大气压,然后以1000~1500℃/h的升温速度加热到1500~2000℃保持4~5h,降温,得到含碳化硅膜的多孔陶瓷。
2.根据权利要求1所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤一中所述的无水非极性溶剂为正己烷、环己烷、石油醚或二氧六环。
3.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤一中所述的二三价金属醇盐为三异丙醇铝、三乙醇铝、乙醇镁或异丙醇镁。
4.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤二中所述的水与正丁醇的混合溶液中,水与正丁醇的摩尔比为1:(4~5)。
5.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤四中所述的分散剂为聚乙二醇、聚丙烯酰胺或羧甲基纤维素。
6.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤四中所述的分烧结助剂为氧化铝、氧化钇或硼。
7.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤五中所述的多孔陶瓷支撑体的孔径范围1~1000μm,孔隙率为20%~90%。
8.根据权利要求1或2所述的一种含碳化硅膜的多孔陶瓷的制备方法,其特征在于步骤五中所述的多孔陶瓷支撑体为氧化铝、氮化硼或碳化硅。
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