CN105280887A - Preparation method for negative electrode of lithium-ion battery - Google Patents
Preparation method for negative electrode of lithium-ion battery Download PDFInfo
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- CN105280887A CN105280887A CN201510583283.1A CN201510583283A CN105280887A CN 105280887 A CN105280887 A CN 105280887A CN 201510583283 A CN201510583283 A CN 201510583283A CN 105280887 A CN105280887 A CN 105280887A
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- molybdenum
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- molybdenum disulfide
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
-
- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- 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 method for a negative electrode of a lithium-ion battery. The method comprises the following steps: with one or a mixture of two of ammonium molybdate and sodium molybdate as a molybdenum source and thiourea as a sulfur source, dissolving the molybdenum source, the sulfur source and NaCl according to the molar ratio of molybdenum in the molybdenum source to sulfur in the sulfur source being 1 to (1.8-2.5) and the molar ratio of the molybdenum in the molybdenum source to the NaCl being 1 to (150-600); carrying out freezing and vacuum drying to obtain a mixture; grinding the prepared mixture into powder, and carrying out burning and chemical vapor deposition in a tube furnace constant temperature zone to obtain a product A; and washing the product A, and carrying out vacuum drying to obtain a molybdenum disulfide nanosheet. The molybdenum disulfide nanosheet is prepared from cheap and available raw materials, so that the method is low in cost, simple in reaction process and high in controllability; and the molybdenum disulfide nanosheet has certain specific capacity and cycle performance when applied to the negative electrode of the lithium-ion battery.
Description
Technical field
The present invention relates to a kind of method making lithium ion battery negative.
Background technology
Along with 21 century is scientific and technological and industrial development, World Economics has marched toward a brand-new epoch, but along with the consumption of resource and the pollution of environment, in the stem reality nowadays but having occurred disruption of ecological balance, lack of energy of human material, cultural life extreme enrichment, we be badly in need of exploitation a kind of not only clean but also efficiently the energy carry out the non-renewable resource such as petroleum replacing, colliery.And lithium ion battery is as a kind of emerging chemical energy source,, the advantage such as operating voltage high, specific energy high, self-discharge rate low, conversion efficiency high, have extended cycle life, environmental friendliness with low cost with it, has received the extensive research of people and has been applied in the various equipment of productive life.
Although the business development of lithium ion battery has tended to ripe, but in some high-grade, precision and advanced fields, as electric automobile, military project, Aero-Space etc., it to be but far from reaching desirable level with the energy-storage property that energy density and power density are representative, and therefore the tip application of lithium electricity is subject to larger restriction.Improving one of Main Means of lithium ion battery chemical property is exactly find new electrode materials, makes battery have higher lithium embedded quantity and outstanding lithium deintercalation invertibity.At present, the negative material that commercial is maximum is graphite-like material with carbon element, its theoretical reversible specific capacity is only 372mAh/g, far can not meet modern needs, and in fast charging and discharging process destructible layer structure, cyclical stability is poor, simultaneously also with problems such as compatibility of electrolyte, electrode fail safes.Molybdenum bisuphide is as the typical transition metal dichalcogenide of one, have the close-packed hexagonal structure and lamella way of stacking that are similar to Graphene, broader (002) interplanar distance makes it have larger storage lithium space, and the theoretical specific capacity calculating gained can reach 669mAh/g; Moreover, in first circle discharge process, MoS
2react with electrolyte that to form SEI film also more limited to the consumption of active material itself, make it have higher coulombic efficiency first.Therefore, MoS
2be used for preparing lithium ion battery negative as a kind of active material and have much application prospect for the capacity improving current commercial Li-ion battery negative pole.
Summary of the invention
The object of this invention is to provide a kind of molybdenum disulfide nano sheet that utilizes and make the method becoming lithium ion battery negative.The present invention utilizes NaCl to make template, in conjunction with a step chemical vapour deposition (CVD), the molybdenum disulfide nano sheet with features such as quality are high, size uniformity, the number of plies are relatively controlled, output is higher, preparation cost is relatively low can be obtained after freeze-drying, calcining, suction filtration, drying, again using prepared molybdenum disulfide nano sheet as active material, add conductive carbon black, PVDF and NMP, stirring is made homogenate and is coated on Copper Foil, namely obtains with the lithium ion battery negative of this molybdenum disulfide nano sheet for storage lithium active material after drying.
The present invention is realized by the following technical programs,
A manufacture method for lithium ion battery negative, comprises the following steps:
(1) with one or both mixtures in ammonium molybdate, sodium molybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the sulphur mol ratio in the molybdenum in molybdenum source, sulphur source), and be 1:(150 ~ 600 by the mol ratio of the molybdenum in molybdenum source and NaCl), molybdenum source, sulphur source and NaCl are added in deionized water and dissolve, stir wiring solution-forming, more ultrasonic mix after freezing at 0 DEG C, after solution freeze over, carry out vacuumize, obtain mixture;
(2) by the mixture grind into powder that step (1) is obtained, be laid in Noah's ark after crossing 100-300 mesh sieve, be placed in tube furnace flat-temperature zone and calcine: with N
2, a kind of gas of He and Ar or mist as inert gas source, be first that 200-400ml/min passes into inert gas 10-30 minute with deaeration with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 600-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain product A after reaction terminates;
(3) collect the obtained powder product A of step (2), be washed to till there is no NaCl in calcined product, the product after washing is placed in and carries out vacuumize, obtain molybdenum disulfide nano sheet;
(4) be the proportioning of 1285:1338:16 according to mass ratio, by molybdenum disulfide nano sheet, PVDF and conductive carbon black mix after slurry is made in stirring and are applied to copper sheet as negative pole, with LiPF
6as electrolyte, using lithium sheet as positive pole, obtained half-cell.
The present invention has the following advantages: the present invention utilizes raw material cheap and easy to get to prepare molybdenum disulfide nano sheet, with low cost, and course of reaction is simple, controllability is strong.This kind of material crystalline degree is high simultaneously, quality is good, and structure is homogeneous, and pattern is excellent, excellent performance, molybdenum disulfide nano sheet is used for lithium ion battery negative and has certain specific capacity and cycle performance, and circulating under the current density of 100mA/g still to keep the specific capacity of more than 250mAh/g after 50 times.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the pattern and the size that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 2 is the FE-SEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the thickness that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 3 is the TEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the overall structure that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 4 is the TEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the sheet number of layers and the lattice dot matrix that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 5 is the XRD collection of illustrative plates of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.
Fig. 6 is the charge-discharge performance figure of the lithium ion battery negative that the embodiment of the present invention 1 utilizes molybdenum disulfide nano sheet to obtain.
Embodiment
Below in conjunction with specific embodiment, particular content of the present invention is described as follows:
Embodiment 1:
Take 0.3531g ammonium molybdate, 0.3654g thiocarbamide and 35.1g sodium chloride, mixture is dissolved in the deionized water of 200ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-50 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 150 mesh sieves, get 10g powder and be placed in Noah's ark, Noah's ark is put into tube furnace, pass into the Ar inert gas deaeration of 200ml/min, again with the Ar inert gas of 200ml/min, and be warming up to temperature 750 DEG C with the programming rate of 10 DEG C/min, insulation 2h carries out chemical vapour deposition (CVD), under Ar atmosphere protection, room temperature is cooled to after reaction terminates, obtain calcined product A, collect, porphyrize, be washed to till there is no NaCl in product, at-50 DEG C, vacuumize 8h is carried out in freeze drier, obtain molybdenum disulfide nano sheet, the how triangular in shape and hexagon of this molybdenum disulfide nano sheet, the length of single nanometer sheet is 0.1-40um, thickness is 0.6-100.0nm, the molybdenum disulfide nano sheet number of plies is 1-40 layer.
By 0.1285g molybdenum disulfide nano sheet, 0.1338gPVDF (Kynoar), 0.0161g conductive carbon black mixes after slurry is made in stirring and is applied to copper sheet as negative pole, with the LiPF of 1M
6as electrolyte, using lithium sheet as positive pole, obtained half-cell, the specific capacity of more than 250mAh/g still protected by its 50 circles that circulate under the current density of 100mA/g, as shown in Figure 6.
Claims (2)
1. a manufacture method for lithium ion battery negative, comprises the following steps:
(1) with one or both mixtures in ammonium molybdate, sodium molybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the sulphur mol ratio in the molybdenum in molybdenum source, sulphur source), and be 1:(150 ~ 600 by the mol ratio of the molybdenum in molybdenum source and NaCl), molybdenum source, sulphur source and NaCl are added in deionized water and dissolve, stir wiring solution-forming, more ultrasonic mix after freezing at 0 DEG C, after solution freeze over, carry out vacuumize, obtain mixture;
(2) by the mixture grind into powder that step (1) is obtained, be laid in Noah's ark after crossing 100-300 mesh sieve, be placed in tube furnace flat-temperature zone and calcine: with N
2, a kind of gas of He and Ar or mist as inert gas source, be first that 200-400ml/min passes into inert gas 10-30 minute with deaeration with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 600-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain product A after reaction terminates;
(3) collect the obtained powder product A of step (2), be washed to till there is no NaCl in calcined product, the product after washing is placed in and carries out vacuumize, obtain molybdenum disulfide nano sheet;
(4) be the proportioning of 1285:1338:16 according to mass ratio, by molybdenum disulfide nano sheet, PVDF and conductive carbon black mix after slurry is made in stirring and are applied to copper sheet as negative pole, with LiPF
6as electrolyte, using lithium sheet as positive pole, obtained half-cell.
2. preparation method according to claim 1, is characterized in that, the product after washing is placed in freeze drier at the temperature of-50 DEG C ~-30 DEG C and carries out vacuumize 8h, obtain molybdenum disulfide nano sheet.
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| CN201510583283.1A CN105280887B (en) | 2015-09-14 | 2015-09-14 | A kind of preparation method of negative electrode of lithium ion battery |
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| CN201510583283.1A CN105280887B (en) | 2015-09-14 | 2015-09-14 | A kind of preparation method of negative electrode of lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058200A (en) * | 2016-07-25 | 2016-10-26 | 天津大学 | Method for modifying titanium-dioxide lithium-ion battery negative pole material simultaneously by using carbon and monolayer molybdenum disulfide |
| WO2020124394A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Transition metal chalcogenide nanosheet material, preparation method thereof, negative electrode material for battery, secondary battery and use thereof |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN112899704A (en) * | 2020-11-25 | 2021-06-04 | 武汉大学 | Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite |
| CN113140803A (en) * | 2021-04-29 | 2021-07-20 | 天能帅福得能源股份有限公司 | Based on lamella MoS2Preparation method of high-rate lithium ion battery as anode |
| CN115092959A (en) * | 2022-06-16 | 2022-09-23 | 西安理工大学 | Manganese/sodium vanadate material prepared by salt template-assisted solid-phase sintering method and preparation method and application thereof |
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| CN104393294A (en) * | 2014-11-27 | 2015-03-04 | 江苏理工学院 | Preparation method of flower-shaped molybdenum disulfide microspheres |
| CN104409706A (en) * | 2014-12-22 | 2015-03-11 | 湖南大学 | Molybdenum disulfide/sulfur-and-nitrogen-doped graphene nanosheet composite material as well as preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103715430A (en) * | 2013-12-23 | 2014-04-09 | 天津大学 | Three-dimensional graphene reticular structure loaded carbon-coated tin nanometer material as well as preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058200A (en) * | 2016-07-25 | 2016-10-26 | 天津大学 | Method for modifying titanium-dioxide lithium-ion battery negative pole material simultaneously by using carbon and monolayer molybdenum disulfide |
| WO2020124394A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Transition metal chalcogenide nanosheet material, preparation method thereof, negative electrode material for battery, secondary battery and use thereof |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN111785928B (en) * | 2019-04-04 | 2021-11-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN112899704A (en) * | 2020-11-25 | 2021-06-04 | 武汉大学 | Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite |
| CN112899704B (en) * | 2020-11-25 | 2022-04-29 | 武汉大学 | Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite |
| CN113140803A (en) * | 2021-04-29 | 2021-07-20 | 天能帅福得能源股份有限公司 | Based on lamella MoS2Preparation method of high-rate lithium ion battery as anode |
| CN115092959A (en) * | 2022-06-16 | 2022-09-23 | 西安理工大学 | Manganese/sodium vanadate material prepared by salt template-assisted solid-phase sintering method and preparation method and application thereof |
| CN115092959B (en) * | 2022-06-16 | 2024-03-26 | 西安理工大学 | Manganese/sodium vanadate material prepared by salt template-assisted solid-phase sintering method, and preparation method and application thereof |
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