CN115028200B - Preparation method of bismuth oxide/bismuth oxycarbonate composite electrode material - Google Patents
Preparation method of bismuth oxide/bismuth oxycarbonate composite electrode material Download PDFInfo
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 56
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000007772 electrode material Substances 0.000 title claims abstract description 34
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- FWIZHMQARNODNX-UHFFFAOYSA-L dibismuth;oxygen(2-);carbonate Chemical compound [O-2].[O-2].[Bi+3].[Bi+3].[O-]C([O-])=O FWIZHMQARNODNX-UHFFFAOYSA-L 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 34
- 229910052802 copper Inorganic materials 0.000 claims description 34
- 239000010949 copper Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000006260 foam Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910052797 bismuth Inorganic materials 0.000 claims description 12
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract description 7
- 229940036358 bismuth subcarbonate Drugs 0.000 abstract description 5
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000010406 cathode material Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 102000020897 Formins Human genes 0.000 description 4
- 108091022623 Formins Proteins 0.000 description 4
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01—INORGANIC CHEMISTRY
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- C01P2006/40—Electric properties
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- 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
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Abstract
The invention belongs to the field of new energy materials, and relates to a preparation method of a bismuth oxide/bismuth oxycarbonate composite electrode material. The bismuth oxide/bismuth oxycarbonate composite electrode material is prepared by taking bismuth nitrate and graphene oxide as raw materials and adopting a three-step method of 'electric replacement-calcination-solvothermal'. The bismuth oxide and the bismuth subcarbonate in the composite material have a synergistic effect, and the capacitance performance of a single material can be improved. The composite material is used as a super capacitor cathode material and has a current density of 40mA cm ‑2 When the specific capacity is measured, the specific capacity is up to 14.1mAhcm ‑2 Much higher than the values reported in the literature, at a current density of 200mA cm ‑2 The specific capacitance of 82% can be still maintained, and the electrochemical performance is extremely excellent. The bismuth oxide/bismuth oxycarbonate composite electrode material with ultrahigh specific capacitance can be expected to be applied to the energy storage field of super capacitors and the like.
Description
Technical Field
The invention belongs to the field of new energy materials, and relates to a preparation method of a bismuth oxide/bismuth oxycarbonate composite electrode material.
Background
In order to solve the ubiquitous problems of energy shortage and environmental pollution, energy storage technologies such as electrochemical energy storage systems including batteries and super capacitors, etc., with low cost and high efficiency are required. The selection and modification of electrode materials as the core part of electrochemical energy storage devices have been the hot topic of research by researchers. During the last few years, researchers have been working on electrode materials that combine the short charging time of supercapacitors with the high energy density of batteries to achieve environmental and economic utilization. Carbon-based materials are widely used as negative electrode materials due to their large specific surface area, good electrical conductivity, and fast charge-discharge kinetics, however, the low specific capacity limits the energy density of their supercapacitors. Therefore, metal oxide-based anode materials such as iron oxide, manganese oxide, bismuth oxide, and the like show good application prospects because of their higher specific capacities than carbon-based materials. Among them, the application research of bismuth oxide in the super capacitor technology is increasing due to its redox performance, energy storage capability and environmental friendliness, however, the volume expansion in the energy storage process destroys its structural integrity, so that its actual specific capacity and stability are yet to be further improved.
Bismuth subcarbonate, also known as bismuth subcarbonate or bismuth subcarbonate, can be widely used in photocatalysis, supercapacitors, health medicines, humidity sensors, nonlinear optical devices and the like due to its special layered structure and low toxicity.
The research finds that the bismuth oxycarbonate can improve the cycling stability of the electrode material and improve the specific capacity of the electrode material. However, no studies have been reported on the bismuth oxide/bismuth oxycarbonate composite electrode material.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a bismuth oxide/bismuth oxycarbonate composite electrode material by taking bismuth nitrate and graphene oxide as raw materials and adopting an electro-displacement-calcination-solvothermal three-step method. Bi directly grows on the copper substrate in a replacement way to obtain a subsequent composite material, so that the contact between the active material and the current collector can be greatly enhanced, the overall resistance of the electrode is reduced, and the ultrahigh load (13.2 mg cm) -2 ) (ii) a The bismuth oxide and the bismuth subcarbonate in the composite electrode material have a synergistic effect, and the capacitance performance of a single material can be improved. The material is used as a super capacitor cathode material, and the current density is 40mA cm -2 When the specific capacity is measured, the specific capacity is up to 14.1mAhcm -2 At a current density of 200mA cm -2 The specific capacitance of 82% can be still maintained, and the electrochemical performance is extremely excellent.
The technical scheme of the invention is as follows:
a preparation method of a bismuth oxide/bismuth oxycarbonate composite electrode material comprises the following specific steps:
(1) Dissolving bismuth nitrate and nitric acid in an acetonitrile water solution to obtain a mixed solution, immersing the foam copper into the mixed solution, and forming a bismuth simple substance on the surface of the foam copper.
(2) The foam copper sheet with the bismuth elementary substance formed on the surface obtained in the step (1) is processed for 1-5 ℃ min under the air atmosphere -1 The temperature rising rate is increased to 100-500 ℃, and then the bismuth oxide is formed on the surface of the foam copper sheet after the foam copper sheet is calcined for 10-15 hours.
(3) Soaking the foam copper sheet with the surface formed with the bismuth oxide obtained in the step (2) into a graphene oxide aqueous solution, and heating and reacting for 10-15 hours at 100-200 ℃; and cooling to obtain the bismuth oxide/bismuth oxycarbonate composite electrode material.
In the step (1), the foam copper sheet is obtained by pretreatment and ultrasonic cleaning, and the method specifically comprises the following steps: and respectively soaking the foamed copper sheet into a hydrochloric acid solution and absolute ethyl alcohol for ultrasonic treatment, and drying in vacuum to obtain the treated foamed copper sheet.
In the step (1), the molar ratio of bismuth nitrate to nitric acid is 1: (10-20).
In the step (3), the graphene oxide aqueous solution is obtained by ultrasonic dispersion treatment, and the concentration of the graphene oxide in the solution is 0.1-1g L -1 。
The invention has the beneficial effects that:
(1) The preparation method provided by the invention has the advantages of simple and feasible operation process, cheap raw materials, mild reaction, green and environment-friendly whole process, effective reduction of product cost, easy industrial implementation and very high use value.
(2) The bismuth oxide/bismuth oxycarbonate composite electrode material prepared by the invention shows excellent electrochemical properties, including good cycling stability, excellent rate capability and ultrahigh specific capacity. The performance of the bismuth oxide/bismuth oxycarbonate composite electrode material prepared by the invention is superior to that of the previously reported bismuth oxide/bismuth oxycarbonate electrode material, and the bismuth oxide/bismuth oxycarbonate composite electrode material has good application prospect.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) photograph of the bismuth oxide material prepared in example 1 of the present invention.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the bismuth oxide/bismuth oxycarbonate composite electrode material prepared in example 1 of the present invention.
Fig. 3 is a cyclic voltammogram obtained at different scanning rates for the bismuth oxide/bismuth oxycarbonate composite electrode material prepared in example 1 of the present invention.
Fig. 4 is a charge-discharge curve diagram obtained by the bismuth oxide/bismuth oxycarbonate composite electrode material prepared in example 1 of the present invention under different current densities.
Fig. 5 is a graph of rate performance of the bismuth oxide/bismuth oxycarbonate composite electrode material prepared in example 1 of the present invention at different current densities.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the drawings, but the scope of the present invention is not limited to these embodiments.
Example 1:
the copper foam was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate and nitric acid in an acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1. And immersing the foamy copper into the mixed solution to form a bismuth simple substance on the surface of the foamy copper.
The bismuth is obtained at 2 deg.C for min under air atmosphere -1 After the temperature rise rate of the bismuth oxide is increased to 200 ℃ and the bismuth oxide is calcined for 12 hours, the bismuth oxide material is obtained, and the morphology of the bismuth oxide is a rough particle structure, as shown in figure 1.
Bismuth oxide was immersed in 0.5g L -1 Placing the graphene oxide dispersion liquid in a reaction kettle, and heating and reacting for 12 hours at 120 ℃; after the reaction is finished and the electrode is cooled, the bismuth oxide/bismuth oxycarbonate composite electrode material is obtained, as shown in figure 2.
And (3) carrying out electrochemical performance test on the electrode slice of the super capacitor by a three-electrode system, wherein the prepared electrode material of the super capacitor is used as a working electrode, a platinum electrode is used as a counter electrode, an Hg/HgO electrode is used as a reference electrode, and 6mol/L KOH aqueous solution is used as electrolyte.
The obtained bismuth oxide material is at 40mA cm -2 Has a specific capacity of 10.1mAhcm at a current density of -2 . At a current density of 200mA cm -2 The retention of capacitance was 10%.
Fig. 3 shows that ions from the electrolyte can completely enter the electrode material by diffusion at a low scanning rate to perform a complete redox reaction, so that the electrode material has a high specific capacitance, and the cycling curve substantially maintains the original shape with the increase of the scanning rate, thereby showing that the electrode sheet of the present invention has a high specific capacity.
As can be seen from FIGS. 4 and 5, the bismuth oxide/bismuth oxycarbonate composite electrode of the present invention has small charge-discharge variation range and small capacitance loss under different current densities; the capacity of the electrode has smaller change amplitude under different current densities, so the bismuth oxide/bismuth oxycarbonate composite electrode has higher specific capacity and rate discharge performance. At 40mA cm -2 Has a specific capacity of up to 14.1mAhcm at a current density of -2 . At a current density of 200mA cm -2 The specific capacitance of 82% can be still maintained, and the high-power-factor performance is achieved.
Example 2:
the copper foam was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate and nitric acid in an acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1. And immersing the foamy copper into the mixed solution to form a bismuth simple substance on the surface of the foamy copper.
The bismuth simple substance is prepared at 1 deg.C for min under air atmosphere -1 The temperature rise rate of (2) is increased to 100 ℃ and calcined for 10 hours to obtain the bismuth oxide. Bismuth oxide was immersed in 0.1g L -1 Placing the graphene oxide dispersion liquid in a reaction kettle, and heating and reacting for 15 hours at 100 ℃; and after the reaction is finished, cooling to obtain the bismuth oxide/bismuth oxycarbonate composite electrode material.
Example 3:
the copper foam was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate and nitric acid in an acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1. And immersing the foamy copper into the mixed solution to form a bismuth simple substance on the surface of the foamy copper.
The bismuth is obtained at 5 deg.C for min under air atmosphere -1 After the temperature rise rate of (2) is increased to 200 ℃ and calcined for 15 hoursObtaining bismuth oxide. Immersing bismuth oxide in 1g L -1 Placing the graphene oxide dispersion liquid in a reaction kettle, and heating and reacting for 10 hours at 200 ℃; and after the reaction is finished, cooling to obtain the bismuth oxide/bismuth oxycarbonate composite electrode material.
Comparative example 4:
the foamy copper was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate containing 0.1M into ethanol and ethylene glycol solution according to the proportion of 2, uniformly stirring, immersing the treated copper foam into the solution, and placing the solution in a reaction kettle at 160 ℃ for heating reaction for 5 hours to obtain bismuth oxide on the surface of the copper foam. Due to the lack of an "electrometathesis" reaction, the bismuth oxide material prepared was inferior to the material in example 1.
The electrochemical test method of example 1 was used, and the bismuth oxide electrode of this comparative example was used as a working electrode and tested at 40mA cm -2 Specific capacity of 2.4mAhcm at current density of (2) -2 . At a current density of 200mA cm -2 The specific capacitance retention rate was 54%.
Comparative example 5:
the copper foam was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate, nitric acid and acetonitrile in an aqueous solution respectively, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1. And immersing the foamy copper into the mixed solution to form a bismuth simple substance on the surface of the foamy copper.
The bismuth is obtained at 2 deg.C for min under air atmosphere -1 The temperature rise rate of the bismuth oxide is increased to 200 ℃ and the bismuth oxide is calcined for 12 hours to obtain the bismuth oxide.
Immersing bismuth oxide into a glucose solution containing 0.06M, and placing the bismuth oxide in a reaction kettle to be heated and reacted for 8 hours at 180 ℃; and calcining the mixture for 2 hours at 450 ℃ in an argon environment to obtain the bismuth oxide/glucose carbon composite electrode material.
The electrochemical test method of example 1 was adopted, and the bismuth oxide/glucose carbon composite electrode of the comparative example was used as a working electrode and tested at 40mA cm -2 Specific capacity of 4.6mAhcm at the current density of -2 . The specific capacity retention ratio was 30% at a current density of 200mA cm-2.
According to the comparative example analysis, the bismuth oxide/bismuth oxycarbonate composite electrode material prepared by the invention has ultrahigh specific area capacity and good rate performance, and shows excellent electrochemical performance.
Claims (2)
1. A preparation method of a bismuth oxide/bismuth oxycarbonate composite electrode material is characterized by comprising the following specific steps:
(1) Dissolving bismuth nitrate and nitric acid in an acetonitrile water solution to obtain a mixed solution, immersing the foamy copper into the mixed solution, and forming a bismuth simple substance on the surface of the foamy copper;
(2) The foam copper sheet with the bismuth elementary substance formed on the surface obtained in the step (1) is processed for 1-5 ℃ min under the air atmosphere -1 The temperature rise rate is increased to 100-500 ℃, then the mixture is calcined for 10-15 hours, and bismuth oxide is formed on the surface of the foam copper sheet;
(3) Immersing the foam copper sheet with the surface formed with the bismuth oxide obtained in the step (2) into a graphene oxide aqueous solution, placing the foam copper sheet into a reaction kettle, and heating and reacting for 10-15 hours at the temperature of 100-200 ℃; cooling to obtain the bismuth oxide/bismuth oxycarbonate composite electrode material;
in the step (1), the molar ratio of bismuth nitrate to nitric acid is 1: (10-20);
in the step (3), the graphene oxide aqueous solution is obtained by ultrasonic dispersion treatment, and the concentration of the graphene oxide in the solution is 0.1-1g L -1 。
2. The preparation method of the bismuth oxide/bismuth oxycarbonate composite electrode material according to claim 1, wherein in the step (1), the foam copper sheet is obtained by pretreatment and ultrasonic cleaning, and specifically comprises the following steps: and respectively soaking the foamed copper sheet into a hydrochloric acid solution and absolute ethyl alcohol for ultrasonic treatment, and drying in vacuum to obtain the treated foamed copper sheet.
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| JPH09183620A (en) * | 1995-12-27 | 1997-07-15 | Dowa Mining Co Ltd | Bismuth oxycarbonate powder and its production |
| CN105271405A (en) * | 2015-11-25 | 2016-01-27 | 上海交通大学 | Material based on bismuth oxycarbonate or bismuth oxide nano tube and preparation method thereof |
| CN106158401A (en) * | 2016-07-12 | 2016-11-23 | 昆明理工大学 | There is the new application of the subcarbonate of layer structure |
| CN110227526A (en) * | 2019-06-25 | 2019-09-13 | 延安大学 | Bismuth oxide/bismuthyl carbonate/bismuth molybdate composite photocatalyst material and preparation method thereof |
| CN112774706A (en) * | 2021-01-31 | 2021-05-11 | 湖南科技大学 | Bismuth oxycarbonate/sepiolite composite photocatalyst and preparation method thereof |
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| CN112808287B (en) * | 2021-01-31 | 2023-10-20 | 湖南科技大学 | Magnetic core-shell bismuth oxide carbonate/sepiolite composite photocatalyst and preparation method thereof |
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