CN105261744A - Preparation method of porous vanadium manganese oxide anode material - Google Patents
Preparation method of porous vanadium manganese oxide anode material Download PDFInfo
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- CN105261744A CN105261744A CN201510605995.9A CN201510605995A CN105261744A CN 105261744 A CN105261744 A CN 105261744A CN 201510605995 A CN201510605995 A CN 201510605995A CN 105261744 A CN105261744 A CN 105261744A
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- vanadium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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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
Abstract
The invention discloses a preparation method of a porous vanadium manganese oxide anode material. The method comprises the following steps: (1) adding a vanadium source, a manganese source, oxalate dihydrate and citric acid to deionized water to form a solution at the molar ratio of a vanadium element to a manganese element to the oxalate dihydrate to the citric acid being 1 to 1 to 2 to (1-3) and controlling the concentration of manganese ions in the solution to be 0.5-1mol/L; (2) putting the obtained solution into a water bath kettle with an ultrasonic stirring device, and carrying out an ultrasonic stirring reaction for 3-6 hours to form sol; (3) putting the obtained sol into a drying oven at 80-120 DEG C and drying the sol for 2-6 hours to obtain gel; and (4) roasting the obtained gel in a protective atmosphere for 2-10 hours at 200-500 DEG C, and cooling the gel to a room temperature along with a furnace, so as to form the porous vanadium manganese oxide anode material. The preparation method is simple in reaction process; industrial control is facilitated; the prepared vanadium manganese oxide has a porous structure and has good gram volume and cycle performance; and intercalation and deintercalation of lithium ions are facilitated.
Description
Technical field
The present invention relates to a kind of preparation method being used as the porous vanadium Mn oxide negative material of lithium ion battery negative material.
Background technology
Lithium ion battery is expected to replace traditional fossil energy in various fields with its significant advantage, is applied in large-sized power battery, energy-storage battery, thus alleviates the global energy and environment problem of puzzlement at present.Research and develop high performance lithium ion battery electrode material and become one of vital task meeting growing lithium ion battery with high energy density demand.
Lithium-ion negative pole is the chief component of lithium ion battery, at present business-like mainly graphite cathode, but its theoretical specific capacity low (372mAh/g).Although it has the advantages such as cheapness, abundance, safety, along with improving constantly of anode capacity, graphite can not meet the needs of negative pole.
Current common metal negative pole all has crystal structure, the easy variable effect circulation of structure after circulation.
CN103864045A discloses a kind of method that freeze-drying prepares duct shape lithium ion battery negative material vanadium phosphate, specifically comprises the following steps: by soluble in water to mole vanadium source that metering ratio is 1:1:3, phosphorus source and reducing agent, stir and obtain homogeneous solution; Obtained solution is transferred in vacuum freezing drying oven by solution homogeneous for gained ,-40 DEG C, 15Pa freeze drying is to the presoma dry powder obtaining vanadium phosphate.Through grinding, compressing tablet, presoma is placed in pipe type sintering furnace, in the lower 750 DEG C of sintering 6h of nonoxidizing atmosphere, cool to room temperature obtains vanadium phosphate negative material.The method freeze drying power consumption is higher, and gram volume is lower first.
CN103972506A discloses a kind of preparation method of nano-sheet lithium ion battery negative material vanadyl phosphate, comprise the following steps: (1) with vanadium source, phosphorus source and reducing agent for raw material, according to mol ratio 1:1:1 ~ 5 of phosphate anion and reducing agent in vanadium ion, phosphorus source in vanadium source, be dissolved in deionized water; (2) stirred in water bath 1 ~ 6h gained mixed solution in step (1) being placed in 70 ~ 90 DEG C obtains uniform solution; (3) solution of gained in step (2), colloidal sol or suspension-turbid liquid are regulated pH to 6 ~ 9; (4) solution of gained in step (3), colloidal sol or suspension-turbid liquid are placed in pyrolytic tank, pyrolysis 10 ~ 30h at 150 ~ 350 DEG C; (5) step (4) products therefrom is filtered, obtain vanadyl phosphate presoma in 80 ~ 120 DEG C of dryings; (6) by step (5) gained vanadyl phosphate presoma 100 ~ 400 DEG C of sintering 1 ~ 10h under non-reducing atmosphere, be cooled to room temperature, obtain vanadyl phosphate.This negative pole preparation process is complicated, and capacity is close with metavanadic acid manganese, and sintering temperature is higher.
At present, the invention research that relevant amorphous metal oxide makes negative pole is had no.
Summary of the invention
Technical problem to be solved by this invention is, for the deficiencies in the prior art, provide a kind of preparation method of porous vanadium Mn oxide negative material, the material prepared by the method has regular loose structure, can bring good gram volume and cycle performance.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of porous vanadium Mn oxide negative material, comprises the following steps:
(1) be 1:1:2:1 ~ 3 ratio by vanadium source, manganese source and two oxalic acid hydrates, citric acid in v element, manganese element, two oxalic acid hydrates, citric acid mol ratio, add in deionized water and form solution, the concentration controlling manganese ion in solution is 0.5 ~ 1mol/L;
(2) solution of step (1) gained is placed in the water-bath with ultrasonic agitation device, the preferred 4-5h of ultrasonic agitation reaction 3-6h(), form colloidal sol;
(3) colloidal sol of step (2) gained is put into the dry 2 ~ 6h of 80 ~ 120 DEG C of baking ovens, obtain gel;
(4) by the gel of step (3) gained in protective atmosphere, at 200 ~ 500 DEG C, after roasting 2 ~ 10h, cool to room temperature with the furnace, obtain porous vanadium Mn oxide negative material.
Further, in step (1), described vanadium source is ammonium metavanadate, vanadyl oxalate, vanadic oxide or their mixture.The introducing of vanadium root can prevent Mn oxide from forming crystal structure, to improve its performance.
Further, in step (1), described manganese source is the mixture of one or more in four acetate hydrate manganese, Manganous sulfate monohydrate, two oxalic acid hydrate manganese.
Further, in step (2), ultrasonic frequency is 20 ~ 40kHz, and the speed of stirring is 50 ~ 400r/min.
Further, in step (2), the bath temperature of water-bath is 70 ~ 90 DEG C.
Further, in step (4), described protective atmosphere is argon gas, nitrogen, hydrogen, carbon dioxide, carbon monoxide or hydrogen/argon-mixed; The volumetric concentration of described hydrogen/argon-mixed middle hydrogen is 2 ~ 8%.
The present invention utilizes vanadic acid root to mix with manganese ion and forms amorphous metal oxide at a certain temperature, utilizes impalpable structure to improve the cycle performance of material.The negative material of preparation discharges the gram volume 407mAh/g that to discharge first under gram volume 1024mAh/g, 300mA/g electric current first, and the capability retention after 50 times that circulates reaches 100%.
Building-up process of the present invention is simple, and condition is easy to control, and the negative material cycle performance obtained is excellent.
Accompanying drawing explanation
The SEM figure of the porous vanadium manganese negative material of Fig. 1 obtained by embodiment 1;
The porous vanadium manganese negative material discharge curve under different current density of Fig. 2 obtained by embodiment 1;
The porous vanadium manganese negative material cyclic curve under 300mA/g current density of Fig. 3 obtained by embodiment 1.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
embodiment 1
(1) ammonium metavanadate 11.70g(0.1mol is taken), four acetate hydrate manganese 24.51g(0.1mol), two oxalic acid hydrate 25.32g(0.2mol), citric acid 38.42g(0.2mol), join in 150mL deionized water and form solution, in solution, the concentration of manganese ion is 0.67mol/L;
(2) solution of step (1) gained is placed in the water-bath with ultrasonic agitation device, ultrasonic agitation reaction 4.5h, control supersonic frequency is 30kHz, and the speed of stirring is 200r/min, bath temperature 80 DEG C, forms colloidal sol;
(3) colloidal sol of step (2) gained is put into 110 DEG C of dry 5h of baking oven, obtain gel;
(4) by the gel of step (3) gained in argon gas atmosphere, at 400 DEG C, after roasting 6h, cool to room temperature with the furnace, obtain porous vanadium Mn oxide negative material.
As shown in Figure 1, known as shown in Figure 1, material has porous pattern to the SEM figure of the porous vanadium manganese negative material obtained by the present embodiment.
The assembling of battery: the porous vanadium manganese negative material taking 0.40g gained, add 0.05g acetylene black and make conductive agent and 0.05gNMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on Copper Foil and make negative plate, be positive pole with metal lithium sheet in vacuum glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC(volume ratio 1:1) be electrolyte, can be assembled into the button cell of CR2025.
By battery in 0.05 ~ 3V voltage range, survey its charge/discharge capacity and high rate performance, the gram volume that discharges first under 30mA/g electric current is the gram volume that discharges first under 1024mAh/g, 300mA/g electric current is 407.3mAh/g, and the capability retention after 50 times that circulates is that 100%(is shown in Fig. 2 and Fig. 3).
embodiment 2
(1) vanadyl oxalate 12.25g(0.05mol is taken), vanadic oxide 9.1g(0.05mol), two oxalic acid hydrate manganese 8.95g(0.05mol), Manganous sulfate monohydrate 8.45g(0.05mol), two oxalic acid hydrate 25.32g(0.2mol), citric acid 19.12g(0.1mol), join in 100mL deionized water and form solution, in solution, the concentration of manganese ion is 1mol/L;
(2) solution of step (1) gained is placed in the water-bath with ultrasonic agitation device, ultrasonic agitation reaction 4h, control supersonic frequency is 20kHz, and the speed of stirring is 50r/min, bath temperature 70 DEG C, forms colloidal sol;
(3) colloidal sol of step (2) gained is put into 80 DEG C of dry 6h of baking oven, obtain gel;
(4) by the gel of step (3) gained in argon gas atmosphere, at 200 DEG C, after roasting 10h, cool to room temperature with the furnace, obtain porous vanadium Mn oxide negative material.
The assembling of battery: the porous vanadium manganese negative material taking 0.40g gained, add 0.05g acetylene black and make conductive agent and 0.05gNMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on Copper Foil and make negative plate, be positive pole with metal lithium sheet in vacuum glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC(volume ratio 1:1) be electrolyte, can be assembled into the button cell of CR2025.
By battery in 0.05 ~ 3V voltage range, survey its charge/discharge capacity and high rate performance, the gram volume that discharges first under 30mA/g electric current is the gram volume that discharges first under 1008.4mAh/g, 300mA/g electric current is 380.3mAh/g, and the capability retention after 50 times that circulates is 98%.
embodiment 3
(1) vanadyl oxalate 24.50g(0.1mol is taken), Manganous sulfate monohydrate 16.90g(0.1mol), two oxalic acid hydrate 25.32g(0.2mol), citric acid 57.36g(0.3mol), join in 200mL deionized water and form solution, in solution, the concentration of manganese ion is 0.5mol/L;
(2) solution of step (1) gained is placed in the water-bath with ultrasonic agitation device, ultrasonic agitation reaction 5h, control supersonic frequency is 40kHz, and the speed of stirring is 400r/min, bath temperature 90 DEG C, forms colloidal sol;
(3) colloidal sol of step (2) gained is put into 120 DEG C of dry 2h of baking oven, obtain gel;
(4) by the gel of step (3) gained in hydrogen/argon-mixed (hydrogen volume concentration is 5%), at 500 DEG C, after roasting 2h, cool to room temperature with the furnace, obtain porous vanadium Mn oxide negative material.
The assembling of battery: the porous vanadium manganese negative material taking 0.40g gained, add 0.05g acetylene black and make conductive agent and 0.05gNMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on Copper Foil and make negative plate, be positive pole with metal lithium sheet in vacuum glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC(volume ratio 1:1) be electrolyte, can be assembled into the button cell of CR2025.
By battery in 0.05 ~ 3V voltage range, survey its charge/discharge capacity and high rate performance, the gram volume that discharges first under 30mA/g electric current is the gram volume that discharges first under 980.5mAh/g, 300mA/g electric current is 353.1mAh/g, and the capability retention after 50 times that circulates is 95%.
Claims (7)
1. a preparation method for porous vanadium Mn oxide negative material, is characterized in that, comprise the following steps:
(1) be 1:1:2:1 ~ 3 ratio by vanadium source, manganese source and two oxalic acid hydrates, citric acid in v element, manganese element, two oxalic acid hydrates, citric acid mol ratio, add in deionized water and form solution, the concentration controlling manganese ion in solution is 0.5 ~ 1mol/L;
(2) solution of step (1) gained is placed in the water-bath with ultrasonic agitation device, ultrasonic agitation reaction 3-6h, forms colloidal sol;
(3) colloidal sol of step (2) gained is put into the dry 2 ~ 6h of 80 ~ 120 DEG C of baking ovens, obtain gel;
(4) by the gel of step (3) gained in protective atmosphere, at 200 ~ 500 DEG C, after roasting 2 ~ 10h, cool to room temperature with the furnace, obtain porous vanadium Mn oxide negative material.
2. the preparation method of porous vanadium Mn oxide negative material according to claim 1, is characterized in that, in step (1), described vanadium source is ammonium metavanadate, vanadyl oxalate, vanadic oxide or their mixture.
3. the preparation method of porous vanadium Mn oxide negative material according to claim 1 and 2, is characterized in that, in step (1), described manganese source is the mixture of one or more in four acetate hydrate manganese, Manganous sulfate monohydrate, two oxalic acid hydrate manganese.
4. the preparation method of porous vanadium Mn oxide negative material according to claim 1 and 2, is characterized in that, in step (2), ultrasonic frequency is 20 ~ 40kHz, and the speed of stirring is 50 ~ 400r/min.
5. the preparation method of porous vanadium Mn oxide negative material according to claim 1 and 2, is characterized in that, in step (2), the bath temperature of water-bath is 70 ~ 90 DEG C.
6. the preparation method of porous vanadium Mn oxide negative material according to claim 1 and 2, is characterized in that, in step (4), described protective atmosphere is argon gas, nitrogen, hydrogen, carbon dioxide, carbon monoxide or hydrogen/argon-mixed.
7. the preparation method of porous vanadium Mn oxide negative material according to claim 6, is characterized in that, the volumetric concentration of described hydrogen/argon-mixed middle hydrogen is 2 ~ 8%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106684359A (en) * | 2017-01-19 | 2017-05-17 | 电子科技大学 | Co(VO<3>)<2>-Mn(VO<3>)<2> of different morphologies, and preparation method and application thereof |
| CN107394128A (en) * | 2017-06-19 | 2017-11-24 | 厦门大学 | A kind of novel cathode material for lithium ion battery and preparation method thereof |
| CN111204811A (en) * | 2020-01-13 | 2020-05-29 | 中国科学技术大学 | Preparation method of vanadium-based spinel material and preparation method of battery anode |
| CN112322953A (en) * | 2020-12-07 | 2021-02-05 | 湖南众鑫新材料科技股份有限公司 | Nitrided ferrovanadium alloy and preparation method thereof |
| CN112575239A (en) * | 2020-12-08 | 2021-03-30 | 湖南众鑫新材料科技股份有限公司 | Preparation method of high-quality low-cost nitrided ferrovanadium |
| CN114229901A (en) * | 2021-12-17 | 2022-03-25 | 华南协同创新研究院 | Transition metal vanadate material and preparation method and application thereof |
| CN116060019A (en) * | 2023-03-15 | 2023-05-05 | 天津大学 | Supported multi-metal oxide series catalyst and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684359A (en) * | 2017-01-19 | 2017-05-17 | 电子科技大学 | Co(VO<3>)<2>-Mn(VO<3>)<2> of different morphologies, and preparation method and application thereof |
| CN106684359B (en) * | 2017-01-19 | 2019-05-10 | 电子科技大学 | Different-shape Co (VO3)2-Mn(VO3)2And its preparation method and application |
| CN107394128A (en) * | 2017-06-19 | 2017-11-24 | 厦门大学 | A kind of novel cathode material for lithium ion battery and preparation method thereof |
| CN111204811A (en) * | 2020-01-13 | 2020-05-29 | 中国科学技术大学 | Preparation method of vanadium-based spinel material and preparation method of battery anode |
| CN111204811B (en) * | 2020-01-13 | 2021-05-07 | 中国科学技术大学 | Preparation method of vanadium-based spinel material and preparation method of battery anode |
| CN112322953A (en) * | 2020-12-07 | 2021-02-05 | 湖南众鑫新材料科技股份有限公司 | Nitrided ferrovanadium alloy and preparation method thereof |
| CN112575239A (en) * | 2020-12-08 | 2021-03-30 | 湖南众鑫新材料科技股份有限公司 | Preparation method of high-quality low-cost nitrided ferrovanadium |
| CN114229901A (en) * | 2021-12-17 | 2022-03-25 | 华南协同创新研究院 | Transition metal vanadate material and preparation method and application thereof |
| CN116060019A (en) * | 2023-03-15 | 2023-05-05 | 天津大学 | Supported multi-metal oxide series catalyst and preparation method and application thereof |
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