CN108987126B - A kind of Ti3C2/Ni composite electrode material and preparation method thereof - Google Patents
A kind of Ti3C2/Ni composite electrode material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910009819 Ti3C2 Inorganic materials 0.000 title claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000002135 nanosheet Substances 0.000 claims abstract description 34
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- 239000006260 foam Substances 0.000 claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 12
- 238000011068 loading method Methods 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- -1 octadecyldimethylbenzyl quaternary ammonium chloride Chemical compound 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 4
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 4
- 239000011165 3D composite Substances 0.000 claims 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000000707 layer-by-layer assembly Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 3
- 239000006262 metallic foam Substances 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002525 ultrasonication Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- XWMGYUIDSBAERU-UHFFFAOYSA-N [Cl-].C(CCCCCCCCCCC)C([NH+](C)C)CCCCCCCCCCCC Chemical compound [Cl-].C(CCCCCCCCCCC)C([NH+](C)C)CCCCCCCCCCCC XWMGYUIDSBAERU-UHFFFAOYSA-N 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本发明属于材料技术领域，公开了一种Ti3C2/Ni复合电极材料及其制备方法。将Ti3AlC2经过氢氟酸刻蚀得到二维结构的Ti3C2；将二维结构的Ti3C2经过二甲基亚砜插层及超声剥离得到表面带负电荷的Ti3C2纳米片；通过阳离子表面活性剂与Ti3C2纳米片正负电荷静电自组装方法将Ti3C2纳米片负载在泡沫镍的表面而得到Ti3C2/Ni复合电极材料。本发明制备工艺流程快速简单，成本低，复合电极材料具有优异的电化学性能，可以作超级电容器的电极材料，同时为Ti3C2纳米片与其他金属泡沫的复合物在超级电容器电极材料研究方面提供了一定的理论研究基础。
The invention belongs to the technical field of materials, and discloses a Ti 3 C 2 /Ni composite electrode material and a preparation method thereof. Ti 3 AlC 2 is etched with hydrofluoric acid to obtain two-dimensional Ti 3 C 2 ; Ti 3 C 2 with two-dimensional structure is intercalated with dimethyl sulfoxide and ultrasonically stripped to obtain negatively charged Ti 3 C on the surface 2 nanosheets; Ti 3 C 2 /Ni composite electrode material is obtained by loading Ti 3 C 2 nano sheets on the surface of nickel foam by electrostatic self-assembly method of cationic surfactant and Ti 3 C 2 nano sheets with positive and negative charges. The preparation process of the invention is fast and simple, the cost is low, the composite electrode material has excellent electrochemical performance, and can be used as the electrode material of the supercapacitor. It provides a certain theoretical basis for research.
Description
技术领域technical field
本发明属于材料技术领域，在于公开一种Ti3C2/Ni复合电极材料及其制备方法。The invention belongs to the technical field of materials, and discloses a Ti 3 C 2 /Ni composite electrode material and a preparation method thereof.
背景技术Background technique
伴随着煤、化石燃料等不可再生能源的过渡开采以及环境严重污染，绿色能源的开发及其可持续发展问题日益备受关注，研发一种高效环保，低成本的能源储存与转换系统已经迫在眉睫。超级电容器作为一种高效储能装置，因其具有功率密度高，充放电速率快，循环寿命长以及环境友好等特点而引起广泛关注。目前，超级电容器已经成功应用于便携式消费类电子产品等领域，具有广泛的市场发展前景。With the over-exploitation of non-renewable energy sources such as coal and fossil fuels and the serious environmental pollution, the development of green energy and its sustainable development have attracted increasing attention. It is urgent to develop an efficient, environmentally friendly and low-cost energy storage and conversion system. As an efficient energy storage device, supercapacitors have attracted extensive attention due to their high power density, fast charge-discharge rate, long cycle life, and environmental friendliness. At present, supercapacitors have been successfully used in portable consumer electronic products and other fields, and have broad market development prospects.
根据不同的储能机制，超级电容器可分为双电层电容器和赝电容器。双电层电容器是在电极/溶液界面通过电子或离子的定向排列造成电荷的对峙而进行充放电过程；赝电容器则是通过电活性物质发生高度可逆的化学吸脱附和氧化还原反应而进行充放电工作的。赝电容器的电极材料通常过渡金属氧化物、氢氧化物等以及聚合物，但由于其导电性及稳定性差等缺点而应用受到限制。因此开发一种新型且具有优异电化学性能的超级电容器电极材料成为一个关键问题。本文研究的Ti3C2/Ni复合材料首次正极材料而应用于超级电容器，为制备新型超级电容器电极材料的发展提供了崭新的研究方向。According to different energy storage mechanisms, supercapacitors can be divided into electric double-layer capacitors and pseudocapacitors. Electric double layer capacitors are charged and discharged through the confrontation of charges caused by the directional arrangement of electrons or ions at the electrode/solution interface; pseudocapacitors are charged and discharged through highly reversible chemical adsorption, desorption and redox reactions of electroactive substances. work. The electrode materials of pseudocapacitors are usually transition metal oxides, hydroxides, and polymers, but their applications are limited due to their poor electrical conductivity and stability. Therefore, the development of a new type of supercapacitor electrode material with excellent electrochemical performance has become a key issue. The Ti 3 C 2 /Ni composite material studied in this paper is the first cathode material to be used in supercapacitors, which provides a new research direction for the development of the preparation of new supercapacitor electrode materials.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于公开一种Ti3C2/Ni复合电极材料及其制备方法。基于 Ti3C2纳米片的优异导电性、具有负电位以及表面具有大量含氧官能团等特点，通过正负电荷静电自组装法将Ti3C2纳米片负载在具有三维多孔结构且具有高电导率的泡沫镍表面，通过Ti3C2纳米片与泡沫镍的接触而充分发挥两者的优势而表现出良好的电化学性能。The purpose of the present invention is to disclose a Ti 3 C 2 /Ni composite electrode material and a preparation method thereof. Based on the excellent electrical conductivity, negative potential and a large number of oxygen-containing functional groups on the surface of Ti3C2 nanosheets, Ti3C2 nanosheets were supported on a three - dimensional porous structure with high electrical conductivity by electrostatic self-assembly of positive and negative charges. The surface of nickel foam with high rate, through the contact between Ti 3 C 2 nanosheets and nickel foam, gives full play to the advantages of both and shows good electrochemical performance.
本发明的技术方案：Technical scheme of the present invention:
一种Ti3C2/Ni复合电极材料充分结合Ti3C2纳米片和泡沫镍的优点，基于二维Ti3C2纳米片电导率高(1～3×106S/m)、亲水性、表面带负电以及具有大量含氧官能团的特点，泡沫镍具有高比表面积、高电导率、低密度以及三维多孔结构等特点，以泡沫镍为基底，阳离子表面活性剂作为桥连剂，通过正负电荷静电自组装的方式将Ti3C2纳米片负载在泡沫镍表面，制备出具有优异的电化学性能且作为超级电容器正极材料的Ti3C2/Ni复合电极材料。所述Ti3C2纳米片在泡沫镍表面负载质量为0.2～0.6毫克/平方厘米。 A Ti 3 C 2 /Ni composite electrode material fully combines the advantages of Ti 3 C 2 nanosheets and nickel foam. It is water-based, negatively charged on the surface and has a large number of oxygen-containing functional groups. Nickel foam has the characteristics of high specific surface area, high electrical conductivity, low density and three-dimensional porous structure. It is based on nickel foam and cationic surfactant as a bridge agent. Ti 3 C 2 nanosheets were loaded on the surface of nickel foam by electrostatic self-assembly of positive and negative charges, and a Ti 3 C 2 /Ni composite electrode material with excellent electrochemical performance was prepared as a positive electrode material for supercapacitors. The loading mass of the Ti 3 C 2 nanosheets on the surface of the nickel foam is 0.2-0.6 mg/cm 2 .
一种Ti3C2/Ni复合电极材料及其制备方法，步骤如下：A Ti 3 C 2 /Ni composite electrode material and a preparation method thereof, the steps are as follows:
第一步，将Ti3AlC2加入到氢氟酸中，在室温均匀搅拌的条件下，反应20-26 小时，经过离心、水洗及真空干燥，得到具有二维层状结构的Ti3C2；In the first step, Ti 3 AlC 2 was added to hydrofluoric acid, and the reaction was carried out for 20-26 hours under the condition of uniform stirring at room temperature. After centrifugation, water washing and vacuum drying, Ti 3 C 2 with a two-dimensional layered structure was obtained. ;
氢氟酸的质量分数为40％～50％；The mass fraction of hydrofluoric acid is 40% to 50%;
Ti3AlC2与氢氟酸的质量比为1:30～1:50；The mass ratio of Ti 3 AlC 2 to hydrofluoric acid is 1:30～1:50;
第二步，将第一步得到的二维层状结构的Ti3C2加入到二甲基亚砜，在室温下搅拌22-27小时，经过离心、水洗后，再将Ti3C2分散在去离子水中进行超声，离心1小时得到Ti3C2纳米片的悬浮液；In the second step, the two-dimensional layered Ti 3 C 2 obtained in the first step was added to dimethyl sulfoxide, stirred at room temperature for 22-27 hours, centrifuged and washed with water, and then the Ti 3 C 2 was dispersed Sonicate in deionized water and centrifuge for 1 hour to obtain a suspension of Ti 3 C 2 nanosheets;
二维层状结构的Ti3C2与二甲基亚砜的质量比为1:40～1:60；The mass ratio of Ti 3 C 2 in the two-dimensional layered structure to dimethyl sulfoxide is 1:40～1:60;
Ti3C2与去离子水的质量比为1:30～1:70；The mass ratio of Ti 3 C 2 to deionized water is 1:30～1:70;
超声时间为1-5小时；Ultrasound time is 1-5 hours;
第三步，配制阳离子表面活性剂的水溶液The third step is to prepare an aqueous solution of cationic surfactant
阳离子表面活性剂为十二烷基三甲基氯(溴)化铵，十四烷基三甲基氯(溴) 化铵，十六烷基三甲基氯(溴)化铵，双十二烷基三甲基氯(溴)化铵，十八烷基二甲基苄基季铵氯(溴)化物中的一种或两种以上混合。Cationic surfactants are dodecyl trimethyl ammonium chloride (bromide), tetradecyl trimethyl ammonium chloride (bromide), hexadecyl trimethyl ammonium chloride (bromide), didodecyl trimethyl ammonium chloride (bromide) One or more mixtures of alkyl trimethyl ammonium chloride (bromide) and octadecyldimethylbenzyl quaternary ammonium chloride (bromide).
阳离子表面活性剂的水溶液浓度为1-4mg/ml；The aqueous solution concentration of cationic surfactant is 1-4mg/ml;
第四步，将表面处理干净的泡沫镍分别交替浸渍在阳离子表面活性剂的水溶液与Ti3C2纳米片的悬浮液中，每次浸渍时间为2-5分钟，共交替浸渍5-8次；将剩余的Ti3C2纳米片的悬浮液通过真空抽滤的方法负载在泡沫镍表面，即得到 Ti3C2/泡沫镍复合电极材料。In the fourth step, the surface-treated clean nickel foam is alternately immersed in the aqueous solution of cationic surfactant and the suspension of Ti3C2 nanosheets, each immersion time is 2-5 minutes, and a total of 5-8 times of alternating ; Load the remaining suspension of Ti 3 C 2 nanosheets on the surface of the nickel foam by vacuum filtration to obtain the Ti 3 C 2 /nickel foam composite electrode material.
所述泡沫镍的面积为1-8cm2，具有高比表面积(28.5cm2/g)，高电导率，低密度(350g/m2)以及三维多孔结构。The nickel foam has an area of 1-8 cm 2 , high specific surface area (28.5 cm 2 /g), high electrical conductivity, low density (350 g/m 2 ) and a three-dimensional porous structure.
所述的Ti3C2纳米片具有二维结构，厚度在8～15纳米，直径在1～2微米，电导率1～3×106S/m，亲水性强，表面带负电且具有70％含氧官能团。The Ti 3 C 2 nanosheet has a two-dimensional structure, a thickness of 8-15 nanometers, a diameter of 1-2 microns, an electrical conductivity of 1-3×10 6 S/m, strong hydrophilicity, a negatively charged surface and a 70% oxygen-containing functional groups.
本发明的有益效果：Beneficial effects of the present invention:
1)本发明充分利用二维Ti3C2纳米片电导率高(1～3×106S/cm)，亲水性，表面带负电以及具有大量含氧官能团的特点，泡沫镍具有高比表面积，高电导率以及三维多孔结构等优点，通过正负电荷静电自组装法将Ti3C2纳米片负载在泡沫镍表面而制备具有优异的电化学性能Ti3C2/Ni复合材料，可以作为超级电容器的正极材料，同时为Ti3C2与其他过渡金属泡沫骨架结构的复合物在超级电容器电极材料研究方面提供了理论基础。1) The present invention makes full use of the characteristics of two-dimensional Ti 3 C 2 nanosheets with high electrical conductivity (1-3×10 6 S/cm), hydrophilicity, negative surface charge and a large number of oxygen-containing functional groups, and the foamed nickel has a high specificity. Due to the advantages of surface area, high electrical conductivity and three-dimensional porous structure, Ti 3 C 2 /Ni composites with excellent electrochemical performance were prepared by loading Ti 3 C 2 nanosheets on the surface of nickel foam by electrostatic self-assembly of positive and negative charges. As a positive electrode material for supercapacitors, it also provides a theoretical basis for the research of supercapacitor electrode materials for the composites of Ti3C2 and other transition metal foam framework structures.
2)本发明利用正负电荷静电自组装的方法制备Ti3C2/Ni复合电极材料，制备过程简单，能量消耗较少且易于工业化推广。通过利用阳离子表面活性剂与带负电荷的Ti3C2纳米片静电吸引而负载在泡沫镍表面，使得Ti3C2纳米片表面的含氧官能团暴露在其表面，更多的活性位点进行氧化还原反应而具有更优异的电化学性能，具有较高的比容量。2) The present invention utilizes the method of electrostatic self-assembly of positive and negative charges to prepare the Ti 3 C 2 /Ni composite electrode material, the preparation process is simple, the energy consumption is less, and the industrialization is easy to popularize. By utilizing the electrostatic attraction between cationic surfactants and negatively charged Ti3C2 nanosheets, they are loaded on the surface of nickel foam, so that the oxygen-containing functional groups on the surface of Ti3C2 nanosheets are exposed on the surface, and more active sites can be Redox reaction and have more excellent electrochemical performance, with higher specific capacity.
3)本发明得到的Ti3C2/Ni复合电极材料一种应用于超级电容器电极材料的新型复合电极材料，这种将Ti3C2纳米片与金属泡沫镍复合作为超级电容器正极材料为制备Ti3C2与其他金属泡沫基底的新型复合物提供了一定的技术依据。3) The Ti 3 C 2 /Ni composite electrode material obtained by the present invention is a new type of composite electrode material applied to the supercapacitor electrode material, which is prepared by compounding Ti 3 C 2 nanosheets and metal foam nickel as the supercapacitor positive electrode material. The new composites of Ti 3 C 2 and other metal foam substrates provide a certain technical basis.
附图说明Description of drawings
图1为Ti3C2/Ni复合材料的循环伏安特性曲线图。FIG. 1 is a graph showing the cyclic voltammetry characteristic of the Ti 3 C 2 /Ni composite material.
图2为Ti3C2/Ni复合材料的恒流充放电曲线图。FIG. 2 is a constant current charge-discharge curve diagram of the Ti 3 C 2 /Ni composite material.
图3为Ti3C2/Ni复合材料的扫描电镜图。FIG. 3 is a scanning electron microscope image of the Ti 3 C 2 /Ni composite material.
具体实施方式Detailed ways
下面结合具体实施例，进一步阐述本发明。应理解，以下所有实施例仅用于说明本发明而不用于限制本发明的范围。The present invention will be further described below in conjunction with specific embodiments. It should be understood that all the following examples are only used to illustrate the present invention and not to limit the scope of the present invention.
实施例1Example 1
一种Ti3C2/Ni复合材料的制备方法，包括以下步骤：A preparation method of Ti 3 C 2 /Ni composite material, comprising the following steps:
A.将1.0克Ti3AlC2与35克质量分数为40％的氢氟酸放入100毫升的塑料烧杯中，并在室温下以一定转速均匀搅拌24小时，经过离心、水洗及真空干燥，得到具有二维层状结构的Ti3C2。A. Put 1.0 g of Ti 3 AlC 2 and 35 g of hydrofluoric acid with a mass fraction of 40% into a 100-ml plastic beaker, and stir at room temperature at a certain speed for 24 hours. After centrifugation, washing and vacuum drying, Ti 3 C 2 with a two-dimensional layered structure is obtained.
B.将步骤A所得到的1克二维层状结构的Ti3C2与50克二甲基亚砜放入100 毫升的烧杯中，在室温下均匀搅拌24小时，经过离心、水洗之后，再将Ti3C2分散在45克去离子水中进行超声，在3500转/分钟的转速下离心1小时得到Ti3C2纳米片的悬浮液。B. Put 1 gram of Ti 3 C 2 with a two-dimensional layered structure obtained in step A and 50 grams of dimethyl sulfoxide into a 100-mL beaker, and uniformly stir at room temperature for 24 hours. After centrifugation and water washing, The Ti 3 C 2 was then dispersed in 45 g of deionized water for ultrasonication, and centrifuged at 3500 rpm for 1 hour to obtain a suspension of Ti 3 C 2 nanosheets.
C.配制质量浓度为2毫克/毫升十二烷基三甲基氯化铵水溶液。C. The preparation mass concentration is 2 mg/ml dodecyl trimethyl ammonium chloride aqueous solution.
D.将表面处理干净的面积为4平方厘米的泡沫镍分别交替浸渍在十二烷基三甲基氯化铵水溶液与Ti3C2纳米片的悬浮液中，每次浸渍时间为3分钟，共浸渍7次；将剩余的Ti3C2纳米片的悬浮液通过真空抽滤的方法负载在泡沫镍表面，即得到Ti3C2/Ni复合电极材料。D. The nickel foam with an area of 4 square centimeters after surface treatment was alternately immersed in the suspension of dodecyltrimethylammonium chloride aqueous solution and Ti3C2 nanosheets, and the immersion time was 3 minutes each time. A total of 7 times of impregnation; the remaining suspension of Ti 3 C 2 nanosheets is supported on the surface of the nickel foam by vacuum filtration, namely the Ti 3 C 2 /Ni composite electrode material is obtained.
本实施例得到的超级电容器电极材料Ti3C2/Ni复合材料循环伏安特性测试图如图1所示，由图可以看出一对明显的氧化还原峰位，可说明Ti3C2/Ni复合物存在着赝电容现象。The test chart of the cyclic voltammetry characteristics of the supercapacitor electrode material Ti 3 C 2 /Ni composite material obtained in this example is shown in Figure 1. From the figure, a pair of obvious redox peaks can be seen, which can indicate that Ti 3 C 2 / There is a pseudocapacitance phenomenon in Ni composites.
本实施例得到的超级电容器电极材料Ti3C2/Ni复合材料恒流充放电曲线图如图2所示，在1A/g的电流密度下容量为618F/g。The constant current charge-discharge curve of the supercapacitor electrode material Ti 3 C 2 /Ni composite material obtained in this example is shown in FIG. 2 , and the capacity is 618 F/g at a current density of 1 A/g.
本实施例得到的Ti3C2/Ni复合材料扫描电镜图如图3所示。由图3可以看出：二维层状结构的Ti3C2经过二甲基亚砜插层及超声剥离得到的Ti3C2纳米片，并且Ti3C2纳米片层层负载在三维多孔结构的泡沫镍表面。本发明为新型超级电容器电极材料的研究提供了一定的理论基础。The SEM image of the Ti 3 C 2 /Ni composite material obtained in this example is shown in FIG. 3 . It can be seen from Fig. 3: Ti 3 C 2 nanosheets obtained by dimethyl sulfoxide intercalation and ultrasonic exfoliation of Ti 3 C 2 with two-dimensional layered structure, and Ti 3 C 2 nanosheets are supported in three-dimensional porous layers. Structural nickel foam surface. The present invention provides a certain theoretical basis for the research of new type supercapacitor electrode materials.
实施例2Example 2
一种Ti3C2/Ni复合材料的制备方法，包括以下步骤：A preparation method of Ti 3 C 2 /Ni composite material, comprising the following steps:
A.将1.0克Ti3AlC2与33克质量分数为40％的氢氟酸放入100毫升的塑料烧杯中，并在室温下以一定转速均匀搅拌22小时，经过离心、水洗及真空干燥，得到具有二维层状结构的Ti3C2。A. Put 1.0 g of Ti 3 AlC 2 and 33 g of hydrofluoric acid with a mass fraction of 40% into a 100-ml plastic beaker, and stir evenly at room temperature for 22 hours at a certain speed. After centrifugation, washing and vacuum drying, Ti 3 C 2 with a two-dimensional layered structure is obtained.
B.将步骤A所得到的1克二维层状结构的Ti3C2与55克二甲基亚砜放入100 毫升的烧杯中，在室温下均匀搅拌26小时，经过离心、水洗之后，再将Ti3C2分散在50克去离子水中进行超声，在3500转/分钟的转速下离心1小时得到Ti3C2纳米片的悬浮液。B. Put 1 gram of Ti 3 C 2 with a two-dimensional layered structure obtained in step A and 55 grams of dimethyl sulfoxide into a 100-mL beaker, and uniformly stir at room temperature for 26 hours. After centrifugation and water washing, The Ti 3 C 2 was then dispersed in 50 g of deionized water for ultrasonication, and centrifuged at 3500 rpm for 1 hour to obtain a suspension of Ti 3 C 2 nanosheets.
C.配制质量浓度为3毫克/毫升十六烷基三甲基氯化铵水溶液。C. Prepare an aqueous solution with a mass concentration of 3 mg/ml cetyltrimethylammonium chloride.
D.将表面处理干净的面积为6平方厘米的泡沫镍分别交替浸渍在十二烷基三甲基氯化铵水溶液与Ti3C2纳米片的悬浮液中，每次浸渍时间为2.5分钟，共浸渍8次；将剩余的Ti3C2纳米片的悬浮液通过真空抽滤的方法负载在泡沫镍表面，即得到Ti3C2/Ni复合电极材料。D. The surface-treated nickel foam with an area of 6 square centimeters was alternately dipped in the suspension of dodecyltrimethylammonium chloride aqueous solution and Ti3C2 nanosheets, and the dipping time was 2.5 minutes each time. A total of 8 times of impregnation; the remaining suspension of Ti 3 C 2 nanosheets is supported on the surface of the nickel foam by vacuum filtration, namely, the Ti 3 C 2 /Ni composite electrode material is obtained.
实施例3Example 3
一种Ti3C2/Ni复合材料的制备方法，包括以下步骤：A preparation method of Ti 3 C 2 /Ni composite material, comprising the following steps:
A.将1.0克Ti3AlC2与40克质量分数为49％的氢氟酸放入100毫升的塑料烧杯中，并在室温下以一定转速均匀搅拌26小时，经过离心、水洗及真空干燥，得到具有二维层状结构的Ti3C2。A. Put 1.0 g of Ti 3 AlC 2 and 40 g of hydrofluoric acid with a mass fraction of 49% into a 100-ml plastic beaker, and stir evenly at room temperature for 26 hours at a certain speed. After centrifugation, washing and vacuum drying, Ti 3 C 2 with a two-dimensional layered structure is obtained.
B.将步骤A所得到的1克二维层状结构的Ti3C2与60克二甲基亚砜放入100 毫升的烧杯中，在室温下均匀搅拌22小时，经过离心、水洗之后，再将Ti3C2分散在60克去离子水中进行超声，在3500转/分钟的转速下离心1小时得到Ti3C2纳米片的悬浮液。B. Put 1 gram of Ti 3 C 2 with a two-dimensional layered structure obtained in step A and 60 grams of dimethyl sulfoxide into a 100-mL beaker, and uniformly stir at room temperature for 22 hours. After centrifugation and water washing, The Ti 3 C 2 was then dispersed in 60 g of deionized water for sonication, and centrifuged at 3500 rpm for 1 hour to obtain a suspension of Ti 3 C 2 nanosheets.
C.配制质量浓度为3毫克/毫升十八烷基二甲基苄基季铵氯化物水溶液。C. Prepare an aqueous solution of octadecyldimethylbenzyl quaternary ammonium chloride with a mass concentration of 3 mg/ml.
D.将处理干净的面积为2平方厘米的泡沫镍分别交替浸渍在十二烷基三甲基氯化铵水溶液与Ti3C2纳米片的悬浮液中，每次浸渍时间为4分钟，共浸渍5 次；将剩余的Ti3C2纳米片的悬浮液通过真空抽滤的方法负载在泡沫镍表面，即得到Ti3C2/Ni复合电极材料。D. The cleaned nickel foam with an area of 2 square centimeters was alternately immersed in the suspension of dodecyltrimethylammonium chloride aqueous solution and Ti3C2 nanosheets, and the immersion time was 4 minutes for a total of 4 minutes. Immerse for 5 times; load the remaining suspension of Ti 3 C 2 nanosheets on the surface of the nickel foam by vacuum filtration to obtain the Ti 3 C 2 /Ni composite electrode material.
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