CN109979759B - Zn2SnO4Preparation method of active carbon electrode material - Google Patents

Zn2SnO4Preparation method of active carbon electrode material Download PDF

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CN109979759B
CN109979759B CN201910204941.XA CN201910204941A CN109979759B CN 109979759 B CN109979759 B CN 109979759B CN 201910204941 A CN201910204941 A CN 201910204941A CN 109979759 B CN109979759 B CN 109979759B
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hours
electrode material
carbon electrode
active carbon
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CN109979759A (en
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徐靖才
洪波
王新庆
彭晓领
金红晓
金顶峰
葛洪良
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China Jiliang University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

Zn2SnO4The preparation method of the activated carbon electrode material comprises the following steps: first, SnCl4、ZnCl2、C4O6HKAN and active carbon are added into diethylene glycol (DEG) according to a certain proportion and stirred for 24 hours to form a mixed solution A; secondly, preparing a DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 50-80 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml of DEG, then transferring the substance into a reaction kettle for reaction for 8-24 hours at the temperature of 150-220 ℃, washing the product to be neutral by using ethanol and distilled water, and drying the product at the temperature of 80 ℃ to obtain Zn2SnO4Active carbon electrode material. The method has the advantages of simple operation, environmental protection, low energy consumption and the like; zn obtained2SnO4The activated carbon electrode material has higher specific capacitance value and good electrochemical performance stability when being used for the electrode of the super capacitor.

Description

Zn2SnO4Preparation method of active carbon electrode material
Technical Field
The invention relates to the field of composite materials, in particular to Zn2SnO4A preparation method of loaded activated carbon.
Background
With the deterioration of the environment and the exhaustion of conventional non-renewable energy sources such as coal, oil and natural gas, a flexible, light and environmentally friendly renewable energy storage apparatus is popularized. The super capacitor is a candidate product of next-generation power equipment, and is widely applied to the fields of electric automobiles, wind power generation, mobile power supplies, military, aerospace and the like due to the advantages of high power density, quick charging capacity, excellent cycle stability, long cycle life, wide working temperature range, green and environmental protection and the like.
Carbon-based materials, metal oxides, metal sulfides, and conductive polymers may be used as supercapacitor electrode materials. Ternary metal oxides, e.g. MMo2O4(M=Zn，Ni)，MFe2O4(M = Zn, Co, Ni) and M2SnO4(M = Mg, Zn, Co), because of the high theoretical specific capacitance, plays an important role in supercapacitor electrode materials. Among them, cobalt oxide is considered as the most excellent electrochemical material. However, due to the rarity and high cost of Co element, many researchers have attempted to replace Co element with a more widely available and less expensive element. Zinc and tin are one of the ideal elements due to wide sources and low price. Thus, Zn2SnO4Is considered to be an important ternary electrode material because of high electron mobility (10-15 cm)2V-1S-1) Excellent adsorption and chemical stability. However, Zn as an electrode material2SnO4Will cause a large volume expansion during the electrochemical reaction (>200%) results in a rapid specific capacity decay, which hinders Zn2SnO4The commercialization of electrode materials has progressed.
Recently, researchers have discovered that nanocrystallization, doping, and Zn recombination2SnO4Volume expansion can be avoided and electrochemical performance improved. abalone-Lei et al manufacturing of Flexible Zn2SnO4/MnO2Core/shell nanocarbon microfiber composites to improve electrochemical performance of supercapacitor electrodes (Nano lett. 2011, 11, 1215). Chelidan et al demonstrate Zn2SnO4The nanowires show a specific Zn ratio2SnO4Nanoplates have a more stable capacity (ACS appl. mater. interfaces. 2013, 5, 6054). Wangkai et al utilizes polypyrrole doped hollow Zn2SnO4To overcome the swelling problem and improve the cycle performance (center. int. 2014, 40, 2359). Furthermore, Zn is exposed2SnO4Relatively poor conductivity also leads to non-ideal electrochemical performance. Great efforts have been made to introduce the carbon-based material Zn2SnO4In combination to improve electrochemical performance. Such a composite material can take advantage of the advantages of both components: high conductivity and large volume change of carbon-based material and Zn2SnO4High specific capacity of (2). The nano carbon-based Zn is synthesized2SnO4Such as Zn2SnO4Composite material such as graphene, Zn2SnO4/CNTs、Zn2SnO4/MnO2Carbon microfiber, Zn2SnO4/C, etc., have been successfully synthesized, and the specific capacity and the cycling stability have been proved to be higher than those of bare Zn2SnO4. Although nanocarbon materials such as CNTs and graphene bind Zn2SnO4Composite materials exhibit high specific capacity and cycling stability, but these nanocarbon materials are expensive and difficult to prepare and commercially produce. For applications, activated carbon-based supercapacitors are more suitable due to their high surface area, electrical conductivity, chemical stability and low cost.
Disclosure of Invention
The invention aims to provide Zn2SnO4Preparation method of active carbon electrode material, and Zn prepared by method2SnO4The composite electrode material filled with the activated carbon pore channels is loaded, so that the specific capacitance and the cyclic charge and discharge stability of the electrode material of the super capacitor can be improved.
In order to achieve the above object, the present invention provides Zn2SnO4The preparation method of the activated carbon electrode material is characterized by comprising the following steps: first, SnCl4、ZnCl2、C4O6HKAN and active carbon are added into diethylene glycol (DEG) according to a certain proportion and stirred for 24 hours to form a mixed solution A; secondly, preparing a DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 50-80 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml of DEG, then transferring the substance into a reaction kettle for reaction for 8-24 hours at the temperature of 150-220 ℃, washing the product to be neutral by using ethanol and distilled water, and drying the product at the temperature of 80 ℃ to obtain Zn2SnO4Active carbon electrode material。
The invention has the advantages that: the method has the advantages of simple operation, environmental protection, low energy consumption and the like; zn obtained2SnO4The activated carbon electrode material has higher specific capacitance value and good electrochemical performance stability when being used for the electrode of the super capacitor.
The invention adopts a Scanning Electron Microscope (SEM) to characterize Zn prepared by the invention2SnO4The microstructure of the active carbon electrode material adopts X-ray diffraction technology (XRD) to analyze Zn prepared by the invention2SnO4Phase of activated carbon electrode material, testing Zn prepared according to the invention using an electrochemical workstation2SnO4The electrochemical performance of the active carbon electrode material proves that Zn with higher specific capacitance and good electrochemical performance stability is successfully prepared by the invention2SnO4Active carbon electrode material.
Drawings
FIG. 1 is Zn prepared in accordance with embodiment one2SnO4SEM image of/active carbon electrode material, and Zn prepared by the invention can be known from FIG. 12SnO4Activated carbon electrode material forming Zn2SnO4Loading and filling the structure of the active carbon pore canal.
FIG. 2 is Zn prepared in accordance with embodiment one2SnO4XRD (X-ray diffraction) graph of/active carbon electrode material and confirmation of prepared Zn2SnO4Active carbon electrode material containing Zn2SnO4Phase and activated carbon phase.
FIG. 3 is Zn prepared in accordance with embodiment one2SnO4Circulation stability performance diagram of/active carbon electrode material, and the Zn prepared by the invention can be known from the diagram of fig. 32SnO4The specific capacitance value of 91.2 percent of the activated carbon electrode material is still maintained after 3000 cycles under the current density of 2A/g.
Detailed Description
The invention is further illustrated below with reference to specific examples. These examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
Detailed description of the inventionThe method comprises the following steps: firstly, 0.005mol of SnCl4、0.01mol ZnCl2、0.002 mol C4O6HKAN and 1g activated carbon are added into 100ml diethylene glycol (DEG) and stirred for 24h to form a mixed solution A; secondly, preparing a DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 70 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml DEG, then transferring into a reaction kettle for reaction at 200 ℃ for 10 hours, washing the obtained product to be neutral by using ethanol and distilled water, and drying at 80 ℃ to obtain Zn2SnO4Active carbon electrode material.
The second embodiment is as follows: firstly, 0.005mol of SnCl4、0.01mol ZnCl2、0.002 mol C4O6HKAN and 0.5g activated carbon are added into 100ml diethylene glycol (DEG) and stirred for 24h to form a mixed solution A; secondly, preparing DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 50 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml DEG, then transferring into a reaction kettle for reacting for 8 hours at 220 ℃, washing the obtained product to be neutral by using ethanol and distilled water, and drying at 80 ℃ to obtain Zn2SnO4Active carbon electrode material.
The third concrete implementation mode: firstly, 0.005mol of SnCl4、0.01mol ZnCl2、0.002 mol C4O6HKAN and 1g activated carbon are added into 100ml diethylene glycol (DEG) and stirred for 24h to form a mixed solution A; secondly, preparing DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 80 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml DEG, then transferring into a reaction kettle for reaction for 24 hours at 150 ℃, washing the obtained product to be neutral by using ethanol and distilled water, and drying at 80 ℃ to obtain Zn2SnO4Active carbon electrode material.
The fourth concrete implementation mode: firstly, 0.005mol of SnCl4、0.01mol ZnCl2、0.002 mol C4O6HKAN and 2g activated carbon are added into 100ml diethylene glycol (DEG) and stirred for 24h to form a mixed solution A; secondly, preparing DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 60 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml DEG, then transferring the substance into a reaction kettle for reacting for 18 hours at 180 ℃, washing the obtained product to be neutral by using ethanol and distilled water, and drying the product at 80 ℃ to obtain Zn2SnO4Active carbon electrode material.

Claims (1)

1. Zn2SnO4The preparation method of the activated carbon electrode material is characterized by comprising the following steps: first, SnCl4、ZnCl2、C4O6HKAN and active carbon are added into diethylene glycol (DEG) according to a certain proportion and stirred for 24 hours to form a mixed solution A; secondly, preparing a DEG solution of 2 mol/L NaOH, dropwise adding the DEG solution into the mixed solution A, and stirring for 10 hours at 50-80 ℃; thirdly, putting the mixture obtained in the second step into a muffle furnace, and calcining for 2h at 240 ℃; fourthly, soaking the substance obtained in the third step in distilled water for 2 hours, filtering, then adding 100ml of DEG, then transferring the substance into a reaction kettle for reaction for 8-24 hours at the temperature of 150-220 ℃, washing the product to be neutral by using ethanol and distilled water, and drying the product at the temperature of 80 ℃ to obtain Zn2SnO4Active carbon electrode material.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103137333A (en) * 2013-01-22 2013-06-05 南京大学 Zn2SnO4/SnO2 compound nanometer structure, preparation method and application thereof
CN105405656A (en) * 2015-11-30 2016-03-16 福州大学 Hierarchical structure Zn<2>SnO<4> and application thereof
CN108940326A (en) * 2018-08-14 2018-12-07 洛阳理工学院 A kind of preparation method of visible light-responded zinc stannate/carbon/silver bromide nano composite photo-catalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103137333A (en) * 2013-01-22 2013-06-05 南京大学 Zn2SnO4/SnO2 compound nanometer structure, preparation method and application thereof
CN105405656A (en) * 2015-11-30 2016-03-16 福州大学 Hierarchical structure Zn<2>SnO<4> and application thereof
CN108940326A (en) * 2018-08-14 2018-12-07 洛阳理工学院 A kind of preparation method of visible light-responded zinc stannate/carbon/silver bromide nano composite photo-catalyst

Non-Patent Citations (1)

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Title
"Zn2SnO4/activated carbon composites for high cycle performance supercapacitor electrode";kaile jin,et al.;《Journal of Alloys and Compounds》;20180720;第419-423页 *

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