CN109979759B - Zn2SnO4Preparation method of active carbon electrode material - Google Patents
Zn2SnO4Preparation method of active carbon electrode material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000007772 electrode material Substances 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title abstract description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910003107 Zn2SnO4 Inorganic materials 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 3
- 239000011592 zinc chloride Substances 0.000 claims abstract description 3
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000003990 capacitor Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 19
- 239000002131 composite material Substances 0.000 description 6
- 229910021392 nanocarbon Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 229920001410 Microfiber Polymers 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003658 microfiber Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910000708 MFe2O4 Inorganic materials 0.000 description 1
- -1 MMo2O4(M=Zn Chemical class 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000008961 swelling Effects 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
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- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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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
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)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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Publication number | Priority date | Publication date | Assignee | Title |
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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)
Title |
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"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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