CN115028200A - 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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- CN115028200A CN115028200A CN202210527003.5A CN202210527003A CN115028200A CN 115028200 A CN115028200 A CN 115028200A CN 202210527003 A CN202210527003 A CN 202210527003A CN 115028200 A CN115028200 A CN 115028200A
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- C—CHEMISTRY; METALLURGY
- 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 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 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 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 Is far higher than the numerical value reported in the literature and has the 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 is expectedThe method is 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 negative electrode materials such as iron oxide, manganese oxide, and bismuth oxide show a promising application prospect because they have higher specific capacities than carbon-based materials. In particular, 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 the structural integrity thereof, so that the actual specific capacity and stability thereof need to be further improved.
Bismuth oxycarbonate, also known as bismuth subcarbonate and bismuth subcarbonate, can be widely used in photocatalysis, supercapacitors, health medicine, humidity sensors, nonlinear optical devices and the like due to its special layered structure and low toxicity.
Research shows 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 uses bismuth nitrate and graphene oxide as raw materials, and prepares the bismuth oxide/bismuth oxycarbonate composite electrode material by a three-step method of 'electric replacement-calcination-solvothermal'. The direct replacement growth of Bi on the copper substrate to obtain the subsequent composite material can greatly enhance the active material and the collectionThe contact between the electric bodies reduces the overall resistance of the electrode and realizes an ultra-high load (13.2mg 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 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 ℃ and 500 ℃, and then the bismuth oxide is formed on the surface of the foam copper sheet after the calcination is carried out for 10 to 15 hours.
(3) Soaking the foamed 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 at 100-200 ℃ for 10-15 hours; 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 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 of the bismuth oxide/bismuth oxycarbonate composite electrode material prepared in example 1 of the present invention at different scanning rates.
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 capability 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 foamy copper was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Dissolving bismuth nitrate and nitric acid in acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1: 10. 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.
Immersing bismuth oxide in 0.5g L -1 Oxygen of (2)Dissolving the graphene dispersion liquid, placing the graphene 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 plate of the super capacitor through a three-electrode system, wherein the prepared super capacitor electrode material 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 The specific capacity of the alloy is 10.1mAhcm at the current density of (A) -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 as the scanning rate increases, so that the electrode sheet of the present invention has a high specific capacity.
As can be seen from fig. 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 The specific capacity of the material is up to 14.1mAhcm at the current density of (2) -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 acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1: 15. 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 1 deg.C for min under air atmosphere -1 After the temperature rise rate of (2) is increased to 100 ℃ and calcined for 10 hoursObtaining bismuth oxide. Immersing bismuth oxide 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 acetonitrile water solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1: 20. 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 The temperature rise rate of the bismuth oxide is increased to 200 ℃ and the bismuth oxide is calcined for 15 hours to obtain the 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 glycol solution with the ratio of 2:1, uniformly stirring, immersing the treated foamy copper into the solution, and placing the foamy copper into a reaction kettle for heating reaction at 160 ℃ for 5 hours to obtain bismuth oxide on the surface of the foamy copper. 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 foamy copper was sonicated in hydrochloric acid solution and ethanol, respectively, and dried under vacuum. Respectively dissolving bismuth nitrate, nitric acid and acetonitrile in an aqueous solution, wherein the molar ratio of the bismuth nitrate to the nitric acid is 1: 10. 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 2 ℃ under air atmospheremin -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 is adopted, the bismuth oxide/glucose carbon composite electrode of the comparative example is taken as a working electrode, and the bismuth oxide/glucose carbon composite electrode is tested to be 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 area specific 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 calcination is carried out 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, and heating and reacting at 100-200 ℃ for 10-15 hours; 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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Citations (6)
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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 |
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| 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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- 2022-05-16 CN CN202210527003.5A patent/CN115028200B/en active Active
Patent Citations (6)
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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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