CN105585001A - Preparation technique of three-dimensional porous carbon and application of three-dimensional porous carbon in sodium-ion batteries - Google Patents
Preparation technique of three-dimensional porous carbon and application of three-dimensional porous carbon in sodium-ion batteries Download PDFInfo
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- CN105585001A CN105585001A CN201610117428.3A CN201610117428A CN105585001A CN 105585001 A CN105585001 A CN 105585001A CN 201610117428 A CN201610117428 A CN 201610117428A CN 105585001 A CN105585001 A CN 105585001A
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- dimensional porous
- porous carbon
- black powder
- sodium
- deionized water
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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 relates to a preparation technique of three-dimensional porous carbon. The specific preparation method comprises the following steps: adding a carbon source and a soluble ion salt into a container according to a certain mass ratio, adding a right amount of deionized water, and stirring to obtain a homogeneous solution; drying the obtained homogeneous solution, sintering at 500-800 DEG C under nitrogen conditions for 5-10 hours, and naturally cooling to obtain a black powder sample; adding the black powder sample into deionized water, carrying out ultrasonic treatment and stirring to obtain a suspension, and centrifuging the suspension many times to remove the soluble ion salt in the black powder; and drying the obtained product to obtain three-dimensional porous carbon nanosheets. The three-dimensional porous carbon nanosheets are applied to a sodium-ion battery negative pole material. The sample prepared by the technique has a three-dimensional porous structure, and is composed of abundant nanosheets. The three-dimensional porous carbon has higher charge/discharge capacity and stable cycle performance when being used as a sodium-ion battery negative pole material.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of novel anode material of lithium-ion battery, belong to energy storage material and electrificationLearn field of power supplies.
Technical background
Renewable Energy Development is the effective way that solution energy crisis is improved environmental pollution. But regenerative resource has notContinuously, unsettled feature, need energy storage device to store and change. Operating voltage is high, ratio because having for lithium ion batteryEnergy is large, advantages of environment protection and become a kind of desirable energy storage device, has broad application prospects. But the earthUpper lithium reserves are limited, and the large-scale exploitation of lithium ion battery highlights lithium resource shortage problem gradually, and lithium salts cost more and moreHeight, will certainly limit the development of extensive accumulation power supply. Therefore, development resource is abundant, advanced battery system with low costIt is the effective way that solves following energy-storage battery.
Sodium aboundresources, with low cost, there is similar physical property to lithium, sodium-ion battery has similar to lithium ion batteryElectrochemical properties, in recent years obtained widely and to have paid close attention to. At present, the performance of sodium-ion battery still can not show a candle to lithium ion battery,The principal element that restricts its development is electrode material. Main cause is: sodium ion is larger than lithium ion radius, many canThe electrode material that embeds/deviate from as lithium ion can not be analogized as sodium-ion battery electrode material. Up to the present, closeResearch in sodium-ion battery positive electrode has obtained greater advance, has derived many on anode material for lithium-ion batteries basisIndividual potential material system, and the progress of anode material of lithium-ion battery is slower, material system is also relatively single. Development letterFolk prescription method is prepared on a large scale anode material of lithium-ion battery and is had very important meaning for the research of sodium-ion battery with applicationJustice. Based on above background, this patent is invented the three-dimensional porous carbon of the extensive preparation of a kind of straightforward procedure, using it as sodium ion electricityPond negative pole demonstrates higher specific capacity and excellent cyclical stability. At present, correlative study there is not yet report.
Summary of the invention
The object of the present invention is to provide simple and easy, the extensive preparation side of the three-dimensional porous carbon of a kind of anode material of lithium-ion batteryMethod. Reaction raw materials is citric acid or sucrose, and soluble ionic salt is as template. Its principle is utilized soluble ionic saltThe guiding absorption of crystallization process induction organic carbon source molecule, in sintering process subsequently, high-melting-point soluble ionic salt can be used asTemplate, impels organic carbon source along surperficial carbonization. Finally, by eccentric cleaning, remove soluble ionic salt template, can obtainThree-dimensional porous carbon. Concrete preparation method is as follows:
(1) carbon source and soluble ionic salt are fed intake by certain mass ratio, be positioned over and in container, add appropriate amount of deionized water and stirMix, obtain homogeneous solution;
(2) homogeneous solution step (1) being obtained is placed in baking oven and dries at 60～80 DEG C, will dry subsequently product and exist500～800 DEG C, sintering 5～10 hours under condition of nitrogen gas, the naturally cooling black powder sample that obtains;
(3) the black powder sample in step (2) is added in deionized water, ultrasonic, stirring obtains suspension, subsequentlySuspension is carried out to repeatedly centrifugal treating, remove the soluble ionic salt in black powder in step (1);
(4) product step (3) being obtained is placed in baking oven to dry at 60～80 DEG C and just obtains a kind of three-dimensional porous carbon and receiveRice sheet.
Described carbon source and the mass ratio of soluble ionic salt are 0.05:0.4～0.1:1; Carbon source is citric acid or sucrose; CanDissolubility ion salt is any one in sodium sulphate, potassium chloride, sodium chloride, potassium sulfate.
The present invention is applied to described three-dimensional porous carbon nanosheet on anode material of lithium-ion battery.
The preparation technology of a kind of three-dimensional porous carbon involved in the present invention has following distinguishing feature:
(1) synthetic method is simple, with low cost, is convenient to extensive preparation;
(2) prepared sample presents three-dimensional porous structure, is made up of a large amount of nanometer sheet;
(3) prepared three-dimensional porous carbon, as anode material of lithium-ion battery, has higher charge and discharge capacity and stableCycle performance.
Brief description of the drawings
The SEM figure of Fig. 1 embodiment 1 prepared sample.
The curve of charge and discharge first (a) of Fig. 2 embodiment 1 prepared sample and (b) cycle performance figure.
The curve of charge and discharge first (a) of Fig. 3 embodiment 2 prepared samples and (b) cycle performance figure.
Detailed description of the invention
Embodiment 1
Take 0.1g citric acid, 1g potassium chloride is placed in beaker, add appropriate amount of deionized water and stir, by stir after moltenLiquid is transferred in culture dish, puts into 60 DEG C of baking ovens and dries. Oven dry product is positioned in crucible, at 500 DEG C, nitrogen barSintering 5 hours under part, the naturally cooling black powder sample that obtains. The black powder sample obtaining is added in deionized water,Ultrasonic, stirring obtains suspension, subsequently suspension is carried out to repeatedly centrifugal treating, removes the potassium chloride in black powder. ?After the product of collection is positioned in baking oven at 60～80 DEG C and dries and just obtain a kind of three-dimensional porous carbon. Prepared sample warpSem analysis, is three-dimensional porous structure, is made up of a large amount of nanometer sheet. The material of embodiment 1 gained is made as followsBecome button cell: by the three-dimensional porous carbon nanosheet sample making and acetylene black and Kynoar by weight being 8:1:1'sRatio is mixed, and makes slurry taking N-first class pyrrolidones as solvent, is coated on the Copper Foil of 10 μ m thickness, at 60 DEG CDry, be cut into the disk of 14mm, vacuum drying 12h at 120 DEG C after to be dried. Taking sodium metal sheet as to electrode,Celgard film is barrier film, is dissolved with NaPF6(1mol/L) solution of EC+DEC (volume ratio is 1:1) is electrolyte,In the glove box of argon shield, be assembled into CR2025 type battery. Battery pack installs rear standing 8h, then uses CT2001A electricityPond test macro carries out constant current charge-discharge test, and test voltage is 3～0.02V. Fig. 2 shows, embodiment 1 prepared threeDimension porous carbon nanometer sheet as sodium-ion battery negative pole first charge and discharge capacity be respectively 283 and 360mAh/g, 100 timesAfter circulation, charge and discharge capacity is 250 and 251mAh/g, has shown higher specific capacity and cyclical stability preferably.
Embodiment 2
Take 0.2g sucrose, 1.85g potassium chloride is placed in beaker, add appropriate amount of deionized water and stir, by stir after solutionBe transferred in culture dish, put into 60 DEG C of baking ovens and dry. Oven dry product is positioned in crucible, at 500 DEG C, condition of nitrogen gasLower sintering 5 hours, the naturally cooling black powder sample that obtains. The black powder sample obtaining is added in deionized water, superSound, stirring obtain suspension, subsequently suspension are carried out to repeatedly centrifugal treating, remove the sodium sulphate in black powder. FinallyThe product of collection is positioned in baking oven and dries and just obtain a kind of three-dimensional porous carbon at 60～80 DEG C. Taking prepared sample asNegative pole, is prepared into button cell and its chemical property is analyzed by step in embodiment 1. As shown in Figure 3, implementExample 2 prepared three-dimensional porous carbon nanosheet as sodium-ion battery negative pole first charge and discharge capacity be respectively 286 Hes381mAh/g, after 100 circulations, charge and discharge capacity is respectively 255 and 258mAh/g, has shown higher specific volumeAmount and preferably cyclical stability.
Claims (3)
1. a preparation technology for three-dimensional porous carbon, is characterized in that the concrete preparation method of described material is:
(1) carbon source and soluble ionic salt are fed intake by certain mass ratio, are positioned over and in container, add appropriate amount of deionized water and stir,Obtain homogeneous solution;
(2) homogeneous solution step (1) being obtained is placed in baking oven and dries at 60～80 DEG C, will dry subsequently product and exist500～800 DEG C, sintering 5～10 hours under condition of nitrogen gas, the naturally cooling black powder sample that obtains;
(3) the black powder sample in step (2) is added in deionized water, ultrasonic, stirring obtains suspension, right subsequentlySuspension carries out repeatedly centrifugal treating, removes the soluble ionic salt in black powder in step (1);
(4) product step (3) being obtained is placed in baking oven and dries and just obtain a kind of three-dimensional porous carbon nanosheet at 60～80 DEG C.
2. the preparation technology of three-dimensional porous carbon nanosheet according to claim 1, its sign is, carbon source and solubility fromThe mass ratio of alite is 0.05:0.4～0.1:1; Carbon source is citric acid or sucrose; Soluble ionic salt be sodium sulphate, potassium chloride,Any one in sodium chloride, potassium sulfate.
3. the application of the three-dimensional porous carbon nanosheet described in claim 1-2 any one on anode material of lithium-ion battery.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107331836A (en) * | 2017-06-09 | 2017-11-07 | 天津大学 | The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application |
| CN110065934A (en) * | 2019-03-28 | 2019-07-30 | 华南农业大学 | A kind of Specific surface area Carbon Materials and its preparation method and application for kalium ion battery |
| CN110078051A (en) * | 2019-04-30 | 2019-08-02 | 济宁学院 | The preparation method of nano cages material |
| CN111344254A (en) * | 2018-06-29 | 2020-06-26 | 东洋炭素株式会社 | Method for producing porous carbon, and electrode and catalyst carrier comprising porous carbon produced by the production method |
| CN112736261A (en) * | 2021-01-07 | 2021-04-30 | 天津大学 | Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof |
| CN115477548A (en) * | 2022-09-01 | 2022-12-16 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107331836A (en) * | 2017-06-09 | 2017-11-07 | 天津大学 | The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application |
| CN111344254A (en) * | 2018-06-29 | 2020-06-26 | 东洋炭素株式会社 | Method for producing porous carbon, and electrode and catalyst carrier comprising porous carbon produced by the production method |
| CN110065934A (en) * | 2019-03-28 | 2019-07-30 | 华南农业大学 | A kind of Specific surface area Carbon Materials and its preparation method and application for kalium ion battery |
| CN110078051A (en) * | 2019-04-30 | 2019-08-02 | 济宁学院 | The preparation method of nano cages material |
| WO2020220591A1 (en) * | 2019-04-30 | 2020-11-05 | 济宁学院 | Preparation method for carbon nanocage material |
| CN112736261A (en) * | 2021-01-07 | 2021-04-30 | 天津大学 | Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof |
| CN115477548A (en) * | 2022-09-01 | 2022-12-16 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
| CN115477548B (en) * | 2022-09-01 | 2023-11-17 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
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