CN115466129A - 一种石墨烯增韧氧化铝复合陶瓷的制备方法 - Google Patents
一种石墨烯增韧氧化铝复合陶瓷的制备方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000000919 ceramic Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 73
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004729 solvothermal method Methods 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011224 oxide ceramic Substances 0.000 claims description 4
- 239000010410 layer Substances 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000758 substrate Substances 0.000 abstract description 10
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000000725 suspension Substances 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本申请公开了一种石墨烯增韧氧化铝复合陶瓷的制备方法，包括：在蒸馏水或有机溶剂体系内加入氧化石墨烯，配制成均匀的氧化石墨烯分散液，再加入氧化铝陶瓷粉末和少量的烧结助剂，搅拌形成均匀的悬浮分散液体系，将所得的分散液倒入高温反应釜，通过溶剂热反应形成自支撑的三维石墨烯与陶瓷粉体复合材料，再经过移除溶剂，压实和高温烧结处理，得到石墨烯增韧氧化铝复合陶瓷。本发明通过在氧化铝基底中引入三维交联的石墨烯网络，来提高氧化铝陶瓷基底的强度和断裂韧性，三维石墨烯也能够使氧化铝基底的导电率大幅度提高。
Description
技术领域
本申请涉及材料合成领域，具体涉及一种石墨烯增韧氧化铝复合陶瓷的制备方法。
背景技术
传统的陶瓷材料，例如氧化铝、氧化硅等，由于其硬度高，强度大，耐热性好，被广泛应用于结构材料，绝缘材料等领域。但是，传统的陶瓷材料最大的缺点就是其韧性差，耐冲击性能较差，这也对其使用寿命有不利影响。而且大部分的陶瓷材料的导电性较差，极大程度的限制了其在电极材料，催化等领域的应用。
为了改善陶瓷材料固有的韧性差的问题，目前科研工作者们提出了多种增韧的方法，包括引入陶瓷晶须，加入纳米颗粒，引入微裂纹等。而碳材料也被用作改善陶瓷的脆性，包括石墨微粒，碳纳米管，以及石墨烯，都有着不错的增韧效果，而且，碳材料的引入对于改善陶瓷基底的低导电率问题有很大帮助。
目前大部分石墨烯复合陶瓷材料的制备是将陶瓷粉体与石墨烯简单的共混，石墨烯在体系内会发生团聚，造成复合材料的不均匀，且石墨烯难以形成有效的连接，这在一定程度上会阻碍石墨烯本征性质的发挥。
发明内容
本发明的目的在于提供一种石墨烯增韧氧化铝复合陶瓷的制备方法。本发明通过溶剂热法制得自支撑的三维石墨烯包覆陶瓷粉体的块体材料，再通过压实烧结制得三维石墨烯增韧氧化铝陶瓷复合材料，该复合材料在陶瓷基底中引入具有三维交联结构的石墨烯网络，石墨烯分散在氧化铝陶瓷的晶界处，起到增韧的效果，同时三维石墨烯也能够大幅度提高陶瓷基底的导电性能。
石墨烯增韧氧化铝陶瓷复合材料的制备步骤如下：
(1)将氧化石墨烯加入到蒸馏水、有机溶剂或它们的混合物中，搅拌得到氧化石墨烯分散液；
(2)在所述氧化石墨烯分散液中加入氧化铝陶瓷粉末以及少量的烧结助剂，搅拌得到均匀的分散液；
(3)将所述分散液加入到高温反应釜中，进行溶剂热反应，得到自支撑的含有水和/或有机溶剂的三维石墨烯-氧化铝粉体复合材料；
(4)去除复合材料中的水和/或有机溶剂，再将复合材料置于模具中压坯，最后在氩气气氛下烧结处理，得到三维石墨烯增韧氧化铝复合陶瓷。
优选的，所述有机溶剂选自甲醇、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、异丁醇、叔丁醇、N,N-二甲基甲酰胺、四氢呋喃和丙酮中的一种或两种以上任意比例的混合物。
优选的，用于制备所述氧化石墨烯分散液的氧化石墨烯为单层氧化石墨烯或少层(2-10层)氧化石墨烯，优选为单层氧化石墨烯；所述氧化石墨烯分散液中氧化石墨烯的浓度为0.3mg/mL-10mg/mL，优选1-3mg/mL。
优选的，所述氧化铝陶瓷粉末的粒径尺寸为1nm-50μm，优选100nm-10μm。所述烧结助剂为氧化硅，氧化铜，氧化钛，氧化硼陶瓷粉体的一种或两种以上任意比例的混合物。所述烧结助剂的总质量占氧化铝质量的0.5％-5％，优选 2％-3％。
优选的，所述氧化石墨烯和氧化铝陶瓷粉末及烧结助剂形成的分散液中，氧化石墨烯占总固体质量含量的0.2％-50％，优选0.5％-2％，所有陶瓷粉体共占总固体质量含量的50％-99.8％。
优选的，所述溶剂热反应温度为100℃-200℃，反应时间为8h-24h。
优选的，去除所述复合材料中的水和/或有机溶剂的方法可以使用冷冻干燥或真空干燥，优选冷冻干燥。需要注意的是，如果使用有机溶剂，在冷冻干燥前，需将复合材料中的有机溶剂置换成水。如果使用真空干燥，干燥温度为50-150℃，干燥时间6-48h。
优选的，所述压坯过程的压力在100-500MPa，压制时间30min-3h。
优选的，所述烧结过程在惰性气氛中进行，升温速率1-10℃/min，烧结温度为1200-1800℃，保温时间为1-12h。
本发明的制备方法及所得到的产物具有如下优点及有益效果：
(1)本发明提出的通过溶剂热反应和压实，烧结处理制得的三维石墨烯增韧氧化铝复合陶瓷具有三维交联的石墨烯网络结构，避免了石墨烯片层的堆积，提高了石墨烯的利用率。分散在陶瓷基底晶界处的石墨烯网络可以使裂纹尖端的应力传播方向偏转，起到增韧的作用。
(2)本发明制得的三维石墨烯增韧氧化铝复合陶瓷具有良好的导电性能，三维石墨烯的引入为氧化铝陶瓷基底提供了一个良好的导电网络，能够极大程度的改善陶瓷基底的电绝缘性质。
(3)本发明提出的三维石墨烯增韧氧化铝复合陶瓷的制备方法具有普适性。对于氧化物陶瓷，如Al2O3、TiO2、SiO2等，复合氧化物陶瓷，如BaTiO3、 BaZrO3、MgAl2O4等，以及非氧化物陶瓷，如TiC、SiC、BN、Si3N4等，都有良好的适用性。
附图说明
图1：三维石墨烯增韧氧化铝陶瓷的光学照片。
图2：不同氧化石墨烯含量制得的三维石墨烯增韧氧化铝陶瓷的断裂韧性。
图3：不同氧化石墨烯含量制得的三维石墨烯增韧氧化铝陶瓷的电导率。
实施例
以下实施例仅用于说明而非限制本申请范围的目的。
实施例1：
取60mg氧化石墨烯加入到60mL蒸馏水之中，搅拌均匀，配制成1mg/mL 的分散液。称取11.94g的Al2O3粒子(平均粒径尺寸为200nm),158.4mg的 TiO2粒子，79.2mg的CuO粒子，加入到氧化石墨烯分散液中，机械搅拌5小时混匀。之后，将浆料倒进100ml的水热反应釜之中，加热180℃ 12h。溶剂热之后将成型的复合材料取出，冷冻干燥除去溶剂，在300MPa的压力下维持1小时将材料压实，再在氩气气氛保护下1500℃ 4h烧结处理，升温速率 5℃/min。随炉冷却至室温，最终获得一种三维石墨烯增韧氧化铝陶瓷复合材料。
所制得复合材料如图1所示，由于石墨烯网络的引入，样品呈灰黑色。所制得的复合材料的断裂韧性能够达到4.71MPa m0.5，相比于没有添加石墨烯的空白样品(3.26MPam0.5)提高了44％，如图2所示。同时，三维石墨烯的引入大幅度的提高了陶瓷基底的电导率，如图3所示，随着石墨烯含量的增加，复合材料的电导率也有所提高。
实施例2：
取120mg氧化石墨烯加入到60mL乙醇之中，搅拌均匀，配制成2mg/mL 的分散液。称取5.82g的Al2O3粒子(平均粒径尺寸为200nm),79.2mg的TiO2粒子，39.6mg的CuO粒子，加入到氧化石墨烯分散液中，机械搅拌5小时混匀。之后，将浆料倒进100ml的水热反应釜之中，加热160℃ 12h。溶剂热之后将成型的复合材料取出，冷冻干燥除去溶剂，在200MPa的压力下维持1 小时将材料压实，再在氩气气氛保护下1600℃ 4h烧结处理。升温速率 5℃/min。随炉冷却至室温，最终获得一种三维石墨烯增韧氧化铝陶瓷材料。
实施例3：
取60mg氧化石墨烯加入到60mL乙醇之中，搅拌均匀，配制成1mg/mL 的分散液。称取5.82g的Al2O3粒子(平均粒径尺寸为1μm),110mg的SiO2粒子，加入到氧化石墨烯分散液中，机械搅拌5小时混匀。之后，将浆料倒进100ml的水热反应釜之中，加热160℃ 12h。溶剂热之后将成型的复合材料取出，冷冻干燥除去溶剂，在200MPa的压力下维持1小时将材料压实，再在氩气气氛保护下1400℃ 6h烧结处理。升温速率2℃/min。随炉冷却至室温，最终获得一种三维石墨烯增韧氧化铝陶瓷材料。
以上所述的具体实施方式，对本发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施方式而已，并不用于限定本发明的保护范围，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种石墨烯增韧氧化铝复合陶瓷的制备方法，其特征在于具体步骤如下：
步骤一、将氧化石墨烯加入到蒸馏水、有机溶剂或它们的混合物中，搅拌得到氧化石墨烯分散液；
步骤二、在所述氧化石墨烯分散液中加入氧化铝陶瓷粉末以及少量的烧结助剂，搅拌得到均匀的分散液；
步骤三、将所述分散液加入到高温反应釜中，进行溶剂热反应，得到自支撑的含有水和/或有机溶剂的三维石墨烯-氧化铝粉体复合材料；
步骤四、去除复合材料中的水和/或有机溶剂，再将复合材料置于模具中压坯，最后在氩气气氛下烧结处理，得到三维石墨烯增韧氧化铝复合陶瓷。
2.根据权利要求1所述的制备方法，其特征在于：所述有机溶剂选自甲醇、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、异丁醇、叔丁醇、N,N-二甲基甲酰胺、四氢呋喃和丙酮中的一种或两种以上任意比例的混合物。
3.根据权利要求1所述的制备方法，其特征在于：用于制备所述氧化石墨烯分散液的氧化石墨烯为单层氧化石墨烯或2-10层氧化石墨烯，所述氧化石墨烯分散液中氧化石墨烯的浓度为0.3mg/mL-10mg/mL。
4.根据权利要求1所述的制备方法，其特征在于：所述氧化铝陶瓷粉末的粒径尺寸为1nm-50μm，所述烧结助剂为氧化硅、氧化铜、氧化钛、氧化硼陶瓷粉体的一种或两种以上任意比例的混合物，所述烧结助剂的总质量占氧化铝质量的0.5％-5％。
5.根据权利要求1所述的制备方法，其特征在于：所述氧化石墨烯和氧化铝陶瓷粉末及烧结助剂形成的分散液中，氧化石墨烯占总固体质量含量的0.2％-50％。
6.根据权利要求1所述的制备方法，其特征在于：所述溶剂热反应温度为100℃-200℃，反应时间为8h-24h。
7.根据权利要求1所述的制备方法，其特征在于：去除所述复合材料中的水和/或有机溶剂的方法可以使用冷冻干燥或真空干燥，优选冷冻干燥。
8.根据权利要求1所述的制备方法，其特征在于：所述压坯过程使用的压力在100-500MPa，压制时间30min-3h，所述烧结过程在惰性气氛中进行，升温速率1-10℃/min，烧结温度为1200-1800℃，保温时间为1-12h。
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