CN111960846A - 一种纳米多孔材料及其制备方法 - Google Patents
一种纳米多孔材料及其制备方法 Download PDFInfo
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- 239000007783 nanoporous material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 22
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 25
- 239000011148 porous material Substances 0.000 claims abstract description 23
- 229910021426 porous silicon Inorganic materials 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 17
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000003431 cross linking reagent Substances 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 11
- 239000005543 nano-size silicon particle Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 125000005587 carbonate group Chemical group 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 238000009472 formulation Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 12
- 239000001569 carbon dioxide Substances 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 9
- 238000000748 compression moulding Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005554 pickling Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229920003257 polycarbosilane Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- MWRWFPQBGSZWNV-UHFFFAOYSA-N Dinitrosopentamethylenetetramine Chemical compound C1N2CN(N=O)CN1CN(N=O)C2 MWRWFPQBGSZWNV-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 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 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000013370 mesoporous silicon carbide Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- XUIMIQQOPSSXEZ-IGMARMGPSA-N silicon-28 atom Chemical compound [28Si] XUIMIQQOPSSXEZ-IGMARMGPSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
本发明属于材料制备领域,具体涉及一种纳米多孔碳化硅陶瓷材料及其制备方法。本发明所述纳米多孔材料是以碳酸盐为造孔剂,利用碳酸盐的分解温度,在碳化硅陶瓷的烧结过程中,随着温度的升高而使碳酸盐分解产生并释放二氧化碳,实现碳化硅陶瓷中产生纳米级孔隙的效果,最终制备得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为20‑300nm,孔隙率为50%‑80%,维氏硬度为650‑950,韧性为10‑25MPa/m1/2,具有高孔隙率和机械性能强的优势,且纳米多孔材料的制备方法简单易操作、绿色环保,适合工业规模化生产。
Description
技术领域
本发明属于材料制备领域,具体涉及一种纳米多孔碳化硅陶瓷材料及其制备方法。
背景技术
多孔材料由于具有良好的选择性渗透传质性能和高的比表面积,在膜过滤、吸附、催化剂制备等领域得到了广泛的应用。无机陶瓷、金属及其氧化物具有优异的化学稳定性、热稳定性或高机械强度等特点,是制备多孔材料的重要原料。多孔碳化硅陶瓷由于具有低密度、透过性好、比表面积大、耐高温、耐腐蚀、化学稳定性好以及抗氧化、抗热震性能好等优良性能,使其在分离装置、各种过滤器、催化剂载体、多孔电极、热交换器等诸多方面具有广泛的应用前景,并逐渐应用于冶金、化工、能源、环保及生物等领域。因此,关于多孔碳化硅陶瓷的制备成为目前多孔陶瓷领域研究的热点之一。
目前,多孔碳化硅陶瓷的研究主要集中在制备方法的改进上,以实现对孔隙率及孔隙结构的控制。目前已开发的方法主要如下:1)添加造孔剂法,如佘继红等人以碳化硅、氧化铝和碳粉为原料,以碳粉为造孔剂,压制成生坯后在空气炉中高温氧化,使碳化硅表面形成氧化硅,氧化硅与氧化铝形成莫来石相连接碳化硅颗粒,制备孔隙率可控的多孔碳化硅(She J H,Yang J F,Naoko kondo,et al.High strength porous silicon carbideceramics.J mater sci,2002,37:3615);2)模板复制法,如朱新文等人以软质聚氨酯海绵为模板,使用碳化硅浆料浸渍模板,养护试样后,在110℃下干燥,然后在600℃下烧掉有机泡沫体,经800℃对素坯预烧,再次用相同组分的低粘度浆料进行浸渍干燥涂覆等处理,最后在高温下烧制得到多孔碳化硅陶瓷(朱新文,江东亮,谭洪寿,张兆泉等,孔结构可控的网眼多孔陶瓷的制备,无机材料学报,2002,17:80);3)发泡法,如Kim等人用聚碳硅烷,物理方法发泡(饱和CO2)制成聚碳硅烷泡沫,然后将聚碳硅烷裂解,烧结制得孔径细小的碳化硅多孔体(Kim Y W,Park C B.Processing of microcellular preceramics using carbondioxide.compos Sci Technol.2003,63:2371);4)颗粒堆积法,如王晓刚等用树脂为粘结剂,将碳素材料和不同粒度的碳化硅级配后,压制成生坯经过干燥,预烧后再2230℃下高温烧结(王晓刚,樊子民.电致发热SiC多孔陶瓷制备工艺与性能研究.硅酸盐通报,2006,No.6:106);5)溶胶凝胶法,如Jin等用正硅酸乙酯加入酚醛树脂中进行水解,硝酸镍作为孔调节剂,形成凝胶后经过碳热还原反应生成孔径微小的介孔SiC材料(Jin G Q,Guo XY.Synthesis and characterization of mesoporous silicon carbide.MicroporMesopor Mat,2003,60:207)。
目前的制备方法得到的多孔碳化硅陶瓷材料的孔径多为微米级大小,纳米孔的多孔碳化硅陶瓷材料尚为少见,而这在一定程度上制约了碳化硅陶瓷的性能和应用。因此,如何制备纳米级的多孔碳化硅陶瓷材料成为研究热点。
发明内容
本发明的目的在于解决现有技术问题的不足,提供一种纳米多孔材料及其制备方法。
本发明的目的之一是提供一种纳米多孔材料,所述纳米多孔材料的配方按质量百分比为:
溶剂 20-50%
纳米颗粒 15-30%
造孔剂 5-30%
交联剂 5-10%
分散剂 1-8%
表面活性剂 1-8%
其中,所述纳米颗粒至少含有纳米碳化硅。
优选的,所述纳米多孔材料的配方按质量百分比为:
溶剂 35%
纳米颗粒 25%
造孔剂 24%
交联剂 8%
分散剂 4%
表面活性剂 4%。
优选的,所述纳米颗粒的组分按质量分数计为50%-70%纳米碳化硅、5%-20%二氧化硅、余量为碳粉的组合,所述纳米碳化硅的粒径为0.1-0.7μm。
优选的,所述造孔剂为碳酸盐。
优选的,所述碳酸盐为碳酸钾、碳酸钙、碳酸镁或碳酸钠的任意一种或多种。
优选的,所述溶剂为水、乙醇或聚乙二醇任意一种或多种。
优选的,所述交联剂为酚醛树脂、聚氨酯树脂、有机硅树脂或环氧树脂的任意一种或多种。
优选的,所述分散剂为羧甲基纤维素、聚丙烯酸钠、焦磷酸钠或六偏磷酸钠。
优选的,所述表面活性剂为十二烷基苯磺酸钠或脂肪醇聚氧乙烯醚。
优选的,所述纳米多孔材料的孔径尺寸为20-300nm,孔隙率为50%-80%。
本发明的另一目的是提供所述纳米多孔材料的制备方法,包括如下步骤:
(1)将配方量的各组分混合均匀后喷雾制粒,得到粒料;
(2)所述粒料经压制成型得到生坯;
(3)所述生坯经真空烧结得到预制体;
(4)所述预制体冷却出炉,经酸液腐蚀得到纳米多孔碳化硅陶瓷材料。
优选的,所述步骤(3)中真空烧结分为两步,先在500-800℃下烧结10-500min,后在800-1000℃下烧结10-240min。
优选的,所述步骤(3)中真空烧结的真空度为500Pa及以下。
本发明与现有技术相比,其有益效果主要体现在:本发明提供一种纳米多孔材料,具体为一种纳米多孔碳化硅陶瓷材料,所述材料是以碳酸盐为造孔剂,利用碳酸盐的分解温度,在碳化硅陶瓷的烧结过程中,随着温度的升高而使碳酸盐分解产生并释放二氧化碳,实现碳化硅陶瓷中产生纳米级孔隙的效果,最终制备得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为20-300nm,孔隙率为50%-80%。,维氏硬度为650-950,韧性为10-25MPa/m1/2,具有高孔隙率和机械性能强的优势,且纳米多孔材料的制备方法简单易操作、绿色环保,适合工业规模化生产。
附图说明
图1是纳米多孔碳化硅陶瓷材料的扫描电镜图。
具体实施方式
本发明提供一种纳米多孔材料,所述纳米多孔材料的配方按质量百分比为:
溶剂 20-50%
纳米颗粒 15-30%
造孔剂 5-30%
交联剂 5-10%
分散剂 1-8%
表面活性剂 1-8%
其中,所述纳米颗粒为纳米碳化硅、二氧化硅、金属硅或碳粉的任意组合;所述造孔剂为碳酸盐。
本发明还提供一种所述纳米多孔材料的制备方法,包括如下步骤:
(1)将配方量的各组分混合均匀后喷雾制粒,得到粒料;
(2)所述粒料经压制成型得到生坯;
(3)所述生坯经真空烧结得到预制体;
(4)所述预制体冷却出炉,经酸液腐蚀得到纳米多孔碳化硅陶瓷材料。
本发明中,对所述混合方式没有特殊限制,能够将各组分原料混合均匀即可,具体采用本领域技术人员熟知的混料方式即可,如搅拌、球磨等。将原料混匀后,进行喷雾制粒。本发明中,所述喷雾制粒所得粒料的粒度优选为50-200μm。
本发明中,对粒料压制成型,所述压制成型的压力优选为5-25MPa,保压时长优选为5-30s,从而获得高强度的生坯,适用后续加工需求并满足产品基本性能要求。
本发明中,所述真空烧结分为两步,先在500-800℃下烧结10-500min,使造孔剂碳酸盐在此温度下分解,释放二氧化碳,形成孔隙,后在800-1000℃下烧结10-240min,得到预制体,真空烧结的升温速率优选为1-3℃/min,真空烧结的真空度优选为500Pa及以下是指真空效果优于500Pa的真空度,即真空度数值低于500Pa。
本发明中,酸液优选为盐酸、硫酸、硝酸、乙酸或草酸的任意一种或多种,以除去碳酸盐分解并释放二氧化碳后剩余的氧化物。
本发明中,通过添加碳酸盐作为造孔剂,在烧结过程中,先一步达到碳酸盐的分解温度,释放二氧化碳后产生空隙,后续烧结过程中,碳粉与氧气生成二氧化碳也会造成空隙,并且后续腐蚀步骤去除碳酸盐分解后留下的氧化物也能够造成一定的空隙。
下面通过具体实施例,并结合附图对本发明的技术方案作进一步的具体说明。
实施例1:
一种纳米多孔材料,配方按质量百分比为:
溶剂 35%
纳米颗粒 25%
造孔剂 24%
交联剂 8%
分散剂 4%
表面活性剂 4%,
其中,纳米颗粒为64%纳米碳化硅、18%二氧化硅、18%碳粉组合;造孔剂为碳酸钙,溶剂为水,交联剂为酚醛树脂,分散剂为羧甲基纤维素,表面活性剂为十二烷基苯磺酸钠。
所述纳米多孔材料的制备方法为:将配方量的各组分混合均匀后喷雾制粒,得到粒料,在压力18MPa下保压20s压制成型得到生坯,生坯在80Pa的真空度下以2℃/min的速率升温至680℃烧结340min,继续升温至1000℃烧结180min,得到预制体,后经1mol/L稀盐酸酸洗腐蚀,得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为180nm,孔隙率为78%,扫描电镜图见附图1。
实施例2:
一种纳米多孔材料,配方按质量百分比为:
溶剂 48%
纳米颗粒 24%
造孔剂 8%
交联剂 10%
分散剂 2%
表面活性剂 8%,
其中,纳米颗粒为70%纳米碳化硅、20%二氧化硅、10%碳粉组合;造孔剂为碳酸镁,溶剂为乙醇,交联剂为环氧树脂,分散剂为聚丙烯酸钠,表面活性剂为十二烷基苯磺酸钠。
所述纳米多孔材料的制备方法为:将配方量的各组分混合均匀后喷雾制粒,得到粒料,在压力7MPa下保压30s压制成型得到生坯,生坯在500Pa的真空度下以2℃/min的速率升温至500℃烧结250min,继续升温至1000℃烧结240min,得到预制体,后经1mol/L稀硝酸酸洗腐蚀,得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为270nm,孔隙率为55%。
实施例3:
一种纳米多孔材料,配方按质量百分比为:
溶剂 25%
纳米颗粒 30%
造孔剂 30%
交联剂 5%
分散剂 8%
表面活性剂 2%,
其中,纳米颗粒为58%纳米碳化硅、14%二氧化硅、28%碳粉组合;造孔剂为碳酸钠,溶剂为水,交联剂为聚氨酯树脂,分散剂为焦磷酸钠,表面活性剂为脂肪醇聚氧乙烯醚。
所述纳米多孔材料的制备方法为:将配方量的各组分混合均匀后喷雾制粒,得到粒料,在压力25MPa下保压8s压制成型得到生坯,生坯在500Pa的真空度下以2℃/min的速率升温至800℃烧结20min,继续升温至1000℃烧结50min,得到预制体,后经1mol/L稀盐酸酸洗腐蚀,得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为40nm,孔隙率为76%。
实施例4:
一种纳米多孔材料,配方按质量百分比为:
溶剂 40%
纳米颗粒 18%
造孔剂 18%
交联剂 10%
分散剂 6%
表面活性剂 8%,
其中,纳米颗粒为60%纳米碳化硅、15%二氧化硅、5%金属硅、20%碳粉组合;造孔剂为碳酸钠,溶剂为乙醇,交联剂为环氧树脂,分散剂为羧甲基纤维素,表面活性剂为十二烷基苯磺酸钠。
所述纳米多孔材料的制备方法为:将配方量的各组分混合均匀后喷雾制粒,得到粒料,在压力15MPa下保压20s压制成型得到生坯,生坯在80Pa的真空度下以2℃/min的速率升温至700℃烧结70min,继续升温至1000℃烧结150min,得到预制体,后经1mol/L稀盐酸酸洗腐蚀,得到纳米多孔碳化硅陶瓷材料。所述纳米多孔材料的孔径为220nm,孔隙率为66%。
试验例1:
对实施例1-4所得纳米多孔碳化硅陶瓷材料进行性能检测,检测结果参见表1,其中,维氏硬度利用维氏硬度计进行测试,断裂韧性按照压痕法进行测试。
表1实施例1-4所得纳米多孔材料的性能检测结果
由以上结果可知,本发明制备的多孔材料,不仅孔径为纳米级,同时具有良好的机械性能。
以上所述的实施例只是本发明的较佳方案,并非对本发明作任何形式上的限制,在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (10)
1.一种纳米多孔材料,其特征在于,所述纳米多孔材料的配方按质量百分比为:
溶剂20-50%
纳米颗粒15-30%
造孔剂5-30%
交联剂5-10%
分散剂1-8%
表面活性剂1-8%
其中,所述纳米颗粒至少含有纳米碳化硅。
2.根据权利要求2所述一种纳米多孔材料,其特征在于,所述纳米多孔材料的配方按质量百分比为:
溶剂35%
纳米颗粒25%
造孔剂24%
交联剂8%
分散剂4%
表面活性剂4%。
3.根据权利要求1所述一种纳米多孔材料,其特征在于,所述纳米颗粒的组分按质量分数计为50%-70%纳米碳化硅、5%-20%二氧化硅、余量为碳粉的组合,所述纳米碳化硅的粒径为0.1-0.7μm。
4.根据权利要求1所述一种纳米多孔材料,其特征在于,所述造孔剂为碳酸盐。
5.根据权利要求4所述一种纳米多孔材料,其特征在于,所述碳酸盐为碳酸钾、碳酸钙、碳酸镁或碳酸钠的任意一种或多种。
6.根据权利要求1所述一种纳米多孔材料,其特征在于,所述溶剂为水、乙醇或聚乙二醇任意一种或多种;所述交联剂为酚醛树脂、聚氨酯树脂、有机硅树脂或环氧树脂的任意一种或多种;所述分散剂为羧甲基纤维素、聚丙烯酸钠、焦磷酸钠或六偏磷酸钠;所述表面活性剂为十二烷基苯磺酸钠或脂肪醇聚氧乙烯醚。
7.根据权利要求1所述一种纳米多孔材料,其特征在于,所述纳米多孔材料的孔径尺寸为20-300nm,孔隙率为50%-80%。
8.一种权利要求1-7任一所述纳米多孔材料的制备方法,包括如下步骤:
(1)将配方量的各组分混合均匀后喷雾制粒,得到粒料;
(2)所述粒料经压制成型得到生坯;
(3)所述生坯经真空烧结得到预制体;
(4)所述预制体冷却出炉,经酸液腐蚀得到纳米多孔碳化硅陶瓷材料。
9.根据权利要求8所述的一种纳米多孔材料的制备方法,其特征在于,所述步骤(3)中真空烧结分为两步,先在500-800℃下烧结10-500min,后在800-1000℃下烧结10-240min。
10.根据权利要求8所述的一种纳米多孔材料的制备方法,其特征在于,所述步骤(3)中真空烧结的真空度为500Pa及以下。
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