CN113593925A - Preparation method of copper sulfide/carbon composite material used as electrode material - Google Patents
Preparation method of copper sulfide/carbon composite material used as electrode material Download PDFInfo
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- CN113593925A CN113593925A CN202110986811.3A CN202110986811A CN113593925A CN 113593925 A CN113593925 A CN 113593925A CN 202110986811 A CN202110986811 A CN 202110986811A CN 113593925 A CN113593925 A CN 113593925A
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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
- H01G11/32—Carbon-based
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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
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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
- H01G11/84—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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- 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
- Y02E60/10—Energy storage using batteries
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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
Abstract
The invention provides a preparation method of a copper sulfide/carbon composite material used as an electrode material, which comprises the following steps of (a) polymerizing m-aminophenol and formaldehyde, stirring, filtering, washing and drying to obtain APF; (b) dispersing APF into aqueous solution containing copper ions, stirring, filtering, washing and drying to obtain APF/Cu2+A complex; (c) the APF/Cu obtained in the step (b)2+Roasting the compound in a tubular furnace to obtain a CuO/C compound; (d) and (C) dispersing the CuO/C composite obtained in the step (C) into a sulfur-containing solution, carrying out hydrothermal reaction in a reaction kettle, and then filtering, washing and drying to obtain the CuS/C composite material. The method has simple process and low cost, and the prepared composite material is nano-scale, has higher conductivity, and can be used as an electrode material of a super capacitor or lithium ionsAn electrode material for a battery.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to a preparation method of a copper sulfide/carbon composite material used as an electrode material.
Background
The rapid consumption of fossil fuels and environmental crisis has raised a great deal of interest in developing clean and renewable energy storage devices. In the competition for energy in this development, supercapacitors, batteries and fuel cells are the most important competitors in recent times. The super capacitor mainly comprises a Faraday quasi-capacitor super capacitor, a double-point layer super capacitor and a hybrid super capacitor. The double-electric-layer super capacitor realizes energy storage through reversible absorption and desorption of charges on the surface of the material, and the electrode material of the double-electric-layer super capacitor mainly comprises a carbon material with a high specific surface area, including activated carbon, graphene, carbon nanotubes, carbon fibers, carbon aerogel and the like.
Copper sulfide is a typical example of a transition metal chalcogenide, and has wide application in various fields such as electrochemical energy storage devices, super-ionic materials, photocatalysts, enzyme-free sensors and the like. Wherein, in the aspect of electrochemical performance, the theoretical capacity of copper sulfide (CuS) is up to 560mAhg-1And has good conductivity.
At present, the research on the copper sulfide @ carbon compound mainly focuses on the aspects of lithium ion batteries, biological probes and photocatalysis. In the aspect of lithium ion batteries, as graphene has the characteristics of high electronic conductivity, large specific surface area, strong toughness and the like, the cycle performance and the rate performance of the compounded copper sulfide/graphene electrode material are obviously enhanced. The method for preparing the CuS/RGO composite material with the double-layer sandwich structure by the Ren Yurong et al hydrothermal method indicates that the graphene improves the conductivity and the electrode stability of the material, and the capacity is 710.7mAh g after 100 cycles of circulation at 0.2 DEG C-1The special structure of the material greatly reduces Li+Diffusion distance, and Li formed2S can be oxidized again. CuS/RGO is synthesized by Tao group one-pot method, the compound shows good lithium storage performance, and the excellent conductivity of RGO enables the material to have good electrochemical performance. As a photocatalyst, the introduction of graphene can improve the electron transfer rate, increase the specific surface area of the material and improve the light absorption rate, thereby improving the catalytic efficiency of the copper sulfide/graphene composite material. Shi Jingzing et al by a one pot methodThe CuS/rGO compound with the specific surface area of 993.5m2g-1The photocatalytic performance is remarkable. The copper sulfide modified carbon nanotube/paraffin/expanded graphite phase-change energy storage composite material prepared by the slow bin and the like has high thermal conductivity and light absorption, and is an excellent phase-change energy storage composite material. The copper sulfide graphene nanocomposite prepared by the WangYongbin through a hydrothermal one-pot method is superior to copper sulfide in degrading methylene blue, and the catalytic activity is obviously improved.
And the sensitivity of the copper sulfide compounded with the graphene is obviously improved by using the copper sulfide as a probe, and the copper sulfide shows excellent stability. The CuS/RGO nano-composite is successfully prepared by Bai sting and Yang Yu Jun through a simple one-pot hydrothermal method and is used for detecting H2O2The sensitivity is greatly improved. The reduced graphene nanocomposite modified by copper sulfide is synthesized by a one-pot method through the coke conservation peak, and the nano composite modified electrode is found to have a good electrocatalytic effect on glucose and is expected to be applied to enzyme-free sensing of glucose.
Disclosure of Invention
The invention aims to provide a preparation method of copper sulfide/carbon used as a composite electrode material, which has the advantages of simple process and low cost, and the prepared composite material is nano-scale, has higher conductivity and can be used as an electrode material of a super capacitor or an electrode material of a lithium ion battery.
The purpose of the invention is realized by the following technical scheme:
a preparation method of copper sulfide/carbon used as a composite electrode material comprises the following steps:
(a) polymerizing M-aminophenol and formaldehyde, stirring, filtering, washing and drying to obtain M-aminophenol formaldehyde resin spheres (APF);
(b) dispersing APF into aqueous solution containing copper ions, stirring, filtering, washing and drying to obtain APF/Cu2+A complex;
(c) the APF/Cu obtained in the step (b)2+Roasting the compound in a tubular furnace to obtain a CuO/C compound;
(d) and (C) dispersing the CuO/C composite obtained in the step (C) into a sulfur-containing solution, heating in a reaction kettle, and then filtering, washing and drying to obtain the CuS/C composite.
Preferably, in step (a), the preparation process of the spherical APF specifically comprises: adding m-aminophenol and formaldehyde into a mixed solution of ethanol, water and ammonia water in sequence, stirring for 10-18h, filtering, washing and drying to obtain spherical APF, wherein the formaldehyde is from a formaldehyde solution, the mass concentration of the formaldehyde in the formaldehyde solution is 35-40%, the ammonia water is from an ammonia water solution, the mass concentration of the ammonia water in the ammonia water solution is 25%, the adding ratio of the m-aminophenol, the formaldehyde solution, the ethanol, the water and the ammonia water solution is 0.6-0.8g, 0.2-2g, 5-15mL, 20-40mL, 1.0-3.0g, the drying temperature is 30-50 ℃, and the drying time is 10-14 h.
More preferably, the pH of the mixed solution of ethanol, water and ammonia water is 9-11, the adding ratio of the m-aminophenol, the formaldehyde solution, the ethanol, the water and the ammonia water solution is 0.71g to 1.034g to 9.6mL to 24mL to 1.956g, the stirring time is 24 hours, the drying temperature is 40 ℃, and the drying time is 12 hours.
Preferably, in the step (a), the stirring time is 10-18h, the drying temperature is 30-50 ℃, and the drying time is 10-14 h. Further preferably, the stirring time is 12 hours, the drying temperature is 40 ℃, and the drying time is 12 hours, and the drying is carried out in an oven.
Preferably, in step (b), the copper ions are selected from one or more of copper acetate or copper chloride. The molar concentration of the copper ions is 0.5-3mol/L, and the mass ratio of the APF to the copper ions is 1 (3.0-6.0).
Preferably, in step (b), the time for the second stirring is 22-26h, the drying temperature is 40-120 ℃, and the drying time is 22-26 h. Further preferably, the stirring time is 24 hours, the drying temperature is 50 ℃, and the drying time is 24 hours, and the drying is carried out in an oven.
Preferably, in the step (c), the roasting temperature is 600-800 ℃, and the roasting time is 2-4 h.
Preferably, the calcination is carried out in step (c) by adopting temperature programming, wherein the temperature raising rate of the temperature programming is 1 ℃/min.
Preferably, in the step (d), the hydrothermal reaction temperature is 100-.
In the invention, m-aminophenol formaldehyde resin spheres are calcined in an inert gas atmosphere to serve as a carbon precursor, the high molecular resin spheres are calcined in a nitrogen atmosphere to become carbon, and a carbon sphere layer is formed, so that a spherical carbon/copper oxide composite material is obtained, wherein in the spherical composite material, the carbon is positioned at the inner layer, and the copper oxide is positioned at the outer layer. In the spherical composite, the metal oxide in the outer layer will cause the difference of ion diffusion speed and conductivity, and thus different electrochemical properties will be obtained. Metal sulfides have a higher specific capacitance than metal oxides. The invention obtains the CuS/C composite material with excellent electrochemical performance by a simple synthesis method.
Use of a copper sulphide/carbon composite material as a supercapacitor. The composite material contains both carbon and metal sulfide, so that the composite material has the conductivity of carbon and the high electrochemical performance of sulfide, such as the specific capacitance applicable to a super capacitor, and is an excellent electrode material. The carbon material with good conductivity and the metal sulfide are combined, and the formed metal sulfide and carbon composite material can be used as an electrode material and further applied to a super capacitor. In addition, composite materials with different morphologies may have different physical and chemical properties. Among them, the spherical composite material has a lower density, a higher specific surface area and a better electron-capturing ability.
The m-aminophenol formaldehyde resin spheres adopted by the invention contain amino with negative charges, and due to the bonding effect between the positive charges and the negative charges, metal ions with positive charges can be combined with the amino with negative charges and firmly adsorbed on the resin spheres, and the content of metal oxides can be quantitatively adjusted by controlling the number of the amino on the resin spheres, so that metal oxide sphere coating structures with different qualities and volumes can be prepared according to requirements.
The composite material prepared by the invention is nano-scale, has high conductivity, can be used in a super capacitor or a lithium ion battery, and has the advantages of simple process, convenient operation and wide raw material source.
Drawings
FIG. 1 is a scanning electron micrograph of the copper sulfide/carbon composite prepared in example 2.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A copper sulfide/carbon composite material used as an electrode material is prepared by the following steps:
(1) preparing polymer spheres: adding 2.0 g of 25% ammonia water solution into 30-degree solution containing 24 g of deionized water and 10 ml of absolute ethyl alcohol, adding 0.71g of m-aminophenol, stirring to dissolve, then adding 1.0 g of 35% formaldehyde solution, continuing stirring for 24 hours, performing centrifugal separation to obtain a crude polymer ball (APF) product, and drying the crude polymer ball (APF) product in a 40-degree oven for 12 hours.
(2) Dispersing APF of the macromolecule ball in (1) into 160 ml of 0.1-2mol/L copper acetate solution. Stirred for 24 hours and then taken out. Placing the mixture into a 40-degree oven and standing for 24 hours. Obtaining APF/Cu2+And (c) a complex.
(3) Mixing APF/Cu2+And (3) programming the temperature of the composite to 600 ℃ under a nitrogen atmosphere, and keeping for 2 hours to obtain the CuO/C composite material.
Grinding the CuO/C composite material, and dispersing into 0.1-1mmol/L sodium sulfide nonahydrate solution. Taking out after hydrothermal for 24 hours at 100 ℃, centrifuging, washing and drying.
Example 2
A copper sulfide/carbon composite material used as a composite electrode material is prepared by the following steps:
(1) preparing polymer spheres: adding 2.0 g of 25% ammonia water solution into 30-degree solution containing 24 g of deionized water and 10 ml of absolute ethyl alcohol, adding 0.71g of m-aminophenol, stirring to dissolve, then adding 1.0 g of 35% formaldehyde solution, continuing stirring for 24 hours, performing centrifugal separation to obtain a crude polymer ball (APF) product, and drying the crude polymer ball (APF) product in a 40-degree oven for 12 hours.
(2) The macromolecular spheres APF in (1) are dispersed in 160 ml of 0.2mol/L copper chloride solution. Stirred for 24 hours and then taken out. Placing the mixture into a 40-degree oven and standing for 24 hours. Obtaining APF/Cu2+And (c) a complex.
(3) Mixing APF/Cu2+And (3) programming the temperature of the composite to 600 ℃ under a nitrogen atmosphere, and keeping for 2 hours to obtain the CuO/C composite material.
Grinding the CuO/C composite material, and dispersing into 0.1-1mmol/L sodium sulfide nonahydrate solution. Taking out after hydrothermal for 24 hours at 100 ℃, centrifuging, washing and drying.
The scanning electron micrograph of the composite material is shown in FIG. 1, and it can be seen that the size of the sample particles is about 500 nm.
Example 3
A copper sulfide/carbon composite material used as an electrode material is prepared by the following steps:
(1) preparing polymer spheres: adding 2.0 g of 25% ammonia water solution into 30-degree solution containing 24 g of deionized water and 10 ml of absolute ethyl alcohol, adding 0.71g of m-aminophenol, stirring to dissolve, then adding 1.0 g of 35% formaldehyde solution, continuing stirring for 24 hours, performing centrifugal separation to obtain a crude polymer ball (APF) product, and drying the crude polymer ball (APF) product in a 40-degree oven for 12 hours.
(2) Dispersing the APF of the macromolecule ball in (1) into 160 ml of 0.1-2mol/L copper nitrate solution. Stirred for 24 hours and then taken out. Placing the mixture into a 40-degree oven and standing for 24 hours. Obtaining APF/Cu2+And (c) a complex.
(3) Mixing APF/Cu2+And (3) programming the temperature of the composite to 600 ℃ under a nitrogen atmosphere, and keeping for 2 hours to obtain the CuO/C composite material.
Grinding the CuO/C composite material, and dispersing into 0.1-1mmol/L sodium sulfide nonahydrate solution. Taking out after hydrothermal for 24 hours at 100 ℃, centrifuging, washing and drying.
Example 4
A copper sulfide/carbon composite material used as an electrode material is prepared by the following steps:
(1) preparing polymer spheres: adding 2.0 g of 25% ammonia water solution into 30-degree solution containing 24 g of deionized water and 10 ml of absolute ethyl alcohol, adding 0.71g of m-aminophenol, stirring to dissolve, then adding 1.0 g of 35% formaldehyde solution, continuing stirring for 24 hours, performing centrifugal separation to obtain a crude polymer ball (APF) product, and drying the crude polymer ball (APF) product in a 40-degree oven for 12 hours.
(2) Dispersing the APF of the macromolecule ball in (1) into 160 ml of 0.1-2mol/L copper sulfate solution. Stirred for 24 hours and then taken out. Placing the mixture into a 40-degree oven and standing for 24 hours. Obtaining APF/Cu2+And (c) a complex.
(3) Mixing APF/Cu2+And (3) programming the temperature of the composite to 600 ℃ under a nitrogen atmosphere, and keeping for 2 hours to obtain the CuO/C composite material.
Grinding the CuO/C composite material, and dispersing into 0.1-1mmol/L mixed solution of sodium sulfide nonahydrate and thiourea. Taking out after hydrothermal for 24 hours at 100 ℃, centrifuging, washing and drying.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A method for preparing a copper sulfide/carbon composite material used as an electrode material is characterized by comprising the following steps:
(a) polymerizing m-aminophenol and formaldehyde, stirring, filtering, washing and drying to obtain APF;
(b) dispersing APF into aqueous solution containing copper ions, stirring, filtering, washing and drying to obtain APF/Cu2 +A complex;
(c) the APF/Cu obtained in the step (b)2+Roasting the compound in a tubular furnace to obtain a CuO/C compound;
(d) and (C) dispersing the CuO/C composite obtained in the step (C) into a sulfur-containing solution, carrying out hydrothermal reaction in a reaction kettle, and then filtering, washing and drying to obtain the CuS/C composite material.
2. The method for preparing the copper sulfide/carbon composite material used as the electrode material according to claim 1, wherein in the step (a), the APF is prepared by a specific process comprising: adding m-aminophenol and formaldehyde into a mixed solution of ethanol, water and ammonia water in sequence, stirring, and filtering, washing and drying in sequence to obtain the spherical APF.
3. The method for preparing a copper sulfide/carbon composite material for an electrode material according to claim 2, wherein the addition ratio of m-aminophenol, the formaldehyde solution, the ethanol, the water and the aqueous ammonia solution is 0.6 to 0.8g:0.2-2g:5-15mL:20-40mL:1.0-3.0g, the mass concentration of formaldehyde in the formaldehyde solution is 35-40%, and the mass concentration of ammonia water in the ammonia water solution is 25%.
4. The method according to claim 1, wherein in the step (b), the copper ions are selected from copper acetate and/or copper chloride, the molar concentration of the copper ions is 0.5-3mol/L, and the mass ratio of APF to copper ions is 1 (3.0-6.0).
5. The method of claim 1, wherein in the step (b), the stirring time is 22-26h, the drying temperature is 40-120 ℃, and the drying time is 22-26 h.
6. The method of claim 1, wherein the stirring time is 24 hours, the drying temperature is 50 ℃, and the drying time is 24 hours in the step (b).
7. The method as claimed in claim 1, wherein the step (c) comprises a calcination temperature of 600-.
8. The method of claim 1, wherein in the step (d), the sulfur-containing solution is one or both of sodium sulfide and thiourea, and the concentration is 0.1 to 1 mmol/L.
9. The method as claimed in claim 1, wherein the hydrothermal reaction temperature in step (d) is 100-200 ℃ and the hydrothermal time is 22-26 h.
10. The method of claim 1, wherein the drying temperature is 40-120 ℃ and the drying time is 22-26h in step (d).
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