CN105006376B - 一种碳纳米管与氧化镍复合材料的制备方法 - Google Patents
一种碳纳米管与氧化镍复合材料的制备方法 Download PDFInfo
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 29
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 20
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 21
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- 238000010792 warming Methods 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract 1
- 239000005977 Ethylene Substances 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 3
- 239000003708 ampul Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
本发明公开了一种碳纳米管与氧化镍复合材料的制备方法,属于纳米材料技术领域。本发明首先通过水热法,利用Ni(NO3)2·6H2O和D‑葡萄糖混合溶液制备出了氢氧化镍球形结构。将制得的球形结构氢氧化镍放在硅基板上,在化学气相沉积系统(CVD)中,通氩气,然后加热,使得氢氧化镍转变成氧化镍;再同时通氢气,将氧化镍球部分还原成镍单质,然后通乙烯气体,在部分还原的氧化镍球表面原位催化生长碳纳米管。通过这种方法,可以简单高效地一步制备氧化镍与碳管的复合材料。相比于传统复合方法而言,这种方法还能使氧化镍与碳管结合得更加紧密,导电性更好,更加稳定,从而能更有效地提高该复合材料的性能。该复合材料在制备超级电容器和锂电池等电化学器件上有广泛的应用前景。
Description
技术领域
本发明属于纳米材料技术领域,特别涉及一种碳纳米管与氧化镍复合材料的制备方法,该材料可作为催化剂应用于超级电容器和锂电池等电化学设备。
背景技术
碳纳米管作为一种新型的纳米材料,由于其独特的中空结构和纳米尺寸,以及其高比表面积、高导电性等特点,使其在复合材料增强、催化剂场发射等领域具有潜在的价值,由于其高表面积和良好导电性,碳纳米管被认为是超级电容器的理想材料。尽管碳纳米管表面积较高、导电性好,但其仍存在电容量小的缺点。将碳纳米管与过渡金属氧化物复合,可以有效地克服此缺点。氧化镍的易制备、低成本、环境友好及高电容量的优点,使其成为金属氧化物电容器的重要选择。NiO/CNTs的核壳结构,充分发挥碳纳米管导电性的同时,能有效缓解充放电过程中体积的膨胀。
发明内容
本发明的目的是提出一种制备碳纳米管与氧化镍复合材料的的方法。本发明提供的方法,先利用水热法制备氧化镍球。然后利用CVD,将氧化镍球表面还原成镍,采用简单的一步水热合成方法制备松塔状TiO2纳米结构。具体的制备方法包括如下步骤:
1、将0.7~0.9gNi(NO3)2·6H2O、0.8~1.1g D-葡萄糖和20ml去离子水,放入50ml烧杯中,磁力搅拌30min;
2、将溶液转移至内衬为聚四氟乙烯的高压反应釜中在130~140℃条件下反应16~18小时,然后自然冷却至室温;
3、将所得固体产物用去离子水洗涤、抽滤,至滤液为中性后,在50℃~60℃下干燥一段时间后获得氢氧化镍球;
4、将0.1~0.3g所制得的氢氧化镍球均匀铺洒于硅片基板上,然后将样品放置于石英管内。抽真空,同时引入氩气。升温至500℃,保持3小时,得到氧化镍球样品;
5、同时引入氢气和氩气,调节它们的流量比例为1:3。升温至650℃后,保持0.5小时;
6、升温至750~770℃,引入甲烷并保持30~40分钟。三种气源的流量比例控制为甲烷:氢气:氩气等于1:(4~5):(8~10);
7、在Ar氛围下自然降温至室温后,取出样品,可得到碳纳米管与氧化镍复合材料。
所述步骤1中,所用的Ni(NO3)2·6H2O为0.7~0.9g、所用D-葡萄糖为0.8~1.1g,所用水为20ml;
所述步骤2中,反应温度为130~140℃,反应时间为16~18小时;
所述步骤3中,干燥温度为50~60℃,煅烧时间为15~17小时;
所述步骤4中,所用氢氧化镍的质量为0.1~0.3g;
所述步骤5中,引入的氢气和氩气比例为(1:10)~(2:7);温度升高到600~650℃,保持时间为0.4~0.5小时;
所述步骤6中,温度升温至750~770℃,保持30~40分钟,三种气源的流量比例控制为甲烷:氢气:氩气等于1:(4~5):(8~10)。
本发明的有益效果是,通过水热法,利用Ni(NO3)2·6H2O和D-葡萄糖混合溶液制备出了球形结构纳米NiO,非常简便。在CVD系统中,分别通氢气,氩气和甲烷,可以将氧化镍球部分还原成镍单质,并原位催化生长碳纳米管。通过这种方法,可以简单高效地一步制备氧化镍与碳管复合材料。相比于传统复合方法而言,这种方法还能使氧化镍与碳管结合得更加紧密,从而更加稳定。
由于该复合材料结合了氧化镍与碳管的优点,在超级电容器、锂离子电池等电化学设备上有广泛的应用前景。
附图说明
图1是本发明实例1中合成的氢氧化镍球。
图2是本发明实例1中经过加热处理得到的氧化镍球。
图3是本发明实例1中碳纳米管与氧化镍复合材料的扫描电镜图。
图4是本发明实例2中碳纳米管与氧化镍复合材料的扫描电镜图。
具体实施方式
本发明提出的一种制备碳纳米管与氧化镍复合材料的方法可通过如下的方法实施,具体的制备方法包括如下步骤:
实施例1
1、将0.7gNi(NO3)2·6H2O、0.9g D-葡萄糖和20ml去离子水,放入50ml烧杯中,磁力搅拌30min;
2、将溶液转移至内衬为聚四氟乙烯的高压反应釜中在140℃条件下反应18小时,然后自然冷却至室温;
3、将所得固体产物用去离子水洗涤、抽滤,至滤液为中性后,在50℃下干燥15小时后获得氢氧化镍球;
4、将0.1g所制得的氢氧化镍球均匀铺洒于硅片基板上,然后将样品放置于石英管内。抽真空,同时引入氩气。升温至500度,保持3小时,得到氧化镍球样品;
5、同时引入氢气和氩气,调节它们的流量比例为1:3。升温至650℃后,保持0.5小时;
6、升温至750℃,引入甲烷并保持30分钟。三种气源的比例控制为甲烷:氢气:氩气等于1:4:8;
7、在Ar氛围下自然降温至室温后,取出样品,可得到碳纳米管与氧化镍的复合结构。
实施例2
1、将0.9gNi(NO3)2·6H2O、1.1g D-葡萄糖和20ml去离子水,放入50ml烧杯中,磁力搅拌30min;
2、将溶液转移至内衬为聚四氟乙烯的高压反应釜中在135℃条件下反应17小时,然后自然冷却至室温;
3、将所得固体产物用去离子水洗涤、抽滤至滤液为中性后,在70℃下干燥24小时。然后利用马弗炉在400℃下锻烧5小时后,获得纳米氧化镍球;
4、将0.25g所制得的氢氧化镍球均匀铺洒于硅片基板上,然后将样品放置于石英管内。抽真空,同时引入氢气和氩气,调节它们的比例为1:8;
5、升温至620℃后,保持0.5小时;
6、升温至760℃,引入甲烷并保持35分钟。三种气源的比例控制为甲烷:氢气:氩气等于1:4:10;
7、在Ar氛围下自然降温至室温后,取出样品,可得到碳纳米管与氧化镍的复合结构。
Claims (1)
1.一种碳纳米管与氧化镍复合材料的制备方法,其特征在于,包括步骤如下:
(1)将0.7~0.9g Ni(NO3)2·6H2O、0.8~1.1g D-葡萄糖和20ml去离子水,放入50ml烧杯中,磁力搅拌30min;
(2)将溶液转移至内衬为聚四氟乙烯的高压反应釜中在120℃~140℃条件下反应10~15小时,然后自然冷却至室温;
(3)将所得固体产物用去离子水洗涤、抽滤至滤液为中性后,在50℃~60℃下干燥15小时后获得氢氧化镍球;
(4)将0.1~0.3g所制得的氢氧化镍球均匀铺洒于硅片基板上,然后将样品放置于石英管内;
抽真空,同时引入氩气;升温至500℃,保持3小时,得到氧化镍球样品;
(5)同时引入氢气和氩气,调节它们的流量比例为1:3;升温至650℃后,保持0.5小时;
(6)升温至750℃~770℃,引入甲烷并保持30~40分钟;三种气源的流量比例控制为甲烷:氢气:氩气等于1:(4~5):(8~10);
(7)在Ar氛围下自然降温至室温后,取出样品,可得到碳纳米管与氧化镍复合材料。
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