CN109360987A - A kind of preparation method of high-tap density anode material of lithium-ion battery - Google Patents
A kind of preparation method of high-tap density anode material of lithium-ion battery Download PDFInfo
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- CN109360987A CN109360987A CN201811266656.2A CN201811266656A CN109360987A CN 109360987 A CN109360987 A CN 109360987A CN 201811266656 A CN201811266656 A CN 201811266656A CN 109360987 A CN109360987 A CN 109360987A
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- lithium
- tap density
- ion battery
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- anode material
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
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- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A kind of preparation method of high-tap density anode material of lithium-ion battery, comprising steps of molybdenum source and sulphur source are distributed in organic solution；The method of material solvent heat carries out the synthesis of material；MoS will be obtained after substance cleaning after reaction2Material；In order to further increase the crystallinity of material, high-temperature heat treatment is carried out to material under certain atmosphere.Solvent-thermal process technology is utilized in a kind of preparation method of high-tap density anode material of lithium-ion battery of the invention, has constructed the MoS with excellent tap density by regulating and controlling synthesis condition2Material has excellent chemical property as anode material of lithium-ion battery；Preparation method is simple, environmental-friendly, and can be realized to MoS2Tap density carry out finely regulating, the production of scale easy to accomplish.
Description
Technical field
The present invention relates to cell negative electrode material more particularly to a kind of preparations of high-tap density anode material of lithium-ion battery
Method.
Background technique
Lithium ion battery is the energy storage being most widely used at present and conversion equipment, but elemental lithium is rich in the earth's crust
Degree is only 0.006%, and not only reserves are rare, but also are unevenly distributed in the world, therefore be difficult to realize extensive, sustainable
Development and utilization.To be widely applied secondary cell more, it is especially applied to extensive green network energy storage side
Face needs to develop a kind of excellent new battery energy storage system of comprehensive effectiveness.For lithium, content of the sodium element in the earth's crust
Want far richer, abundance is up to 2.64%, is in metallic element reserves are ranked in the earth's crust the 4th, while containing big in ocean
The sodium of amount extracts also very simple.Chemically from the point of view of angle, lithium and sodium are in same main group, and chemical property is extremely close；Separately
Outside, correlative study discovery sodium-ion battery is usually expressed as chemical property similar with lithium ion battery, thus carry out sodium from
Sub- battery related work be it is practicable, this to maintain the energy sustainable development have practical significance.
Currently, sodium-ion battery generallys use the compound of some stratiforms or olivine structural as positive electrode, this
A little materials are evolved by anode material for lithium-ion batteries mostly, and chemical property is rather ideal.Compared to positive electrode, sodium from
The research and development of sub- cell negative electrode material is faced with bigger difficulty and challenge.Graphite is in lithium ion battery using the widest
General negative electrode material, but the interlamellar spacing of researcher discovery graphite is insufficient to allow sodium ion to be stablized in the research of early period
Deintercalation.Seek suitable negative electrode material and also faces huge challenge.
A series of transient metal sulfides with layer structure, MoS2、WS2、SnS、SnS2Deng being proven to have certain
Storage sodium ability.Wherein, there is the MoS of high reversible theoretical specific capacity2(670mA h g-1) it is considered a kind of very promising
Anode material of lithium-ion battery.Currently, researcher passes through regulation MoS2Pattern, can effectively improve MoS2Storage
Sodium ability.But it is current research shows that: to obtain high chemical property, material, which needs to have, carries out nanosizing processing.It receives
Meter Hua Neng reduces the transmission path of sodium ion and electronics, improves the chemical property of material.But the material of nanosizing have compared with
Low tap density, this is highly detrimental to practical application.Therefore, high-performance/high-tap density MoS is obtained2Material is also faced with
Very big challenge.
Summary of the invention
The purpose of the present invention is to provide a kind of with high-tap density/high electrochemical sodium-ion battery MoS2Cathode material
The preparation method of material.
For achieving the above object, technical scheme is as follows:
A kind of preparation method of high-tap density anode material of lithium-ion battery, comprising steps of
S1: molybdenum source and sulphur source are distributed in organic solvent and obtain mixed liquor；
S2: the mixed liquor in step S1 is packed into reaction kettle, carries out solvent thermal reaction；
S3: being cleaned the mixed liquor after reacting in step S2 and dried, and MoS is obtained2Material.
The technical solution further preferred as the present invention, the step S3 further include later step S4: step S3 is obtained
The MoS obtained2Material is heat-treated in sintering atmosphere.
As further preferred technical solution of the invention, the sintering temperature in the step S4 is 800 DEG C, sintering time
For 2h.
As further preferred technical solution of the invention, the sintering atmosphere in the step S4 is nitrogen, argon gas, argon gas
At least one of with hydrogen mixed gas atmosphere.
As further preferred technical solution of the invention, the molybdenum source in the step S1 is ammonium molybdate, sodium molybdate, six carbonyls
At least one of base molybdenum, phosphomolybdic acid, acetyl acetone, potassium molybdate.
As further preferred technical solution of the invention, the sulphur source in the step S1 is sulphur powder, thiocarbamide, thioacetyl
At least one of amine, thiosemicarbazide, thioglycolic acid.
As further preferred technical solution of the invention, the organic solvent in the step S1 is methanol, ethyl alcohol, isopropyl
At least one of alcohol, glycerine, acetone, toluene, dimethylbenzene.
As the further preferred technical solution of the present invention, the reaction temperature of the step S2 is 200 DEG C, and the reaction time is
12h。
Compared with prior art, beneficial effects of the present invention:
Solvent-thermal process skill is utilized in a kind of preparation method of high-tap density anode material of lithium-ion battery of the invention
Art has constructed the MoS with excellent tap density by regulating and controlling synthesis condition2Material, as anode material of lithium-ion battery, tool
There is excellent chemical property；Preparation method is simple, environmental-friendly, and can be realized to MoS2Tap density carry out
Finely regulating, the production of scale easy to accomplish.
Detailed description of the invention
Fig. 1 is MoS prepared by the embodiment of the present invention 12The SEM photograph of material；
Fig. 2 is MoS prepared by the embodiment of the present invention 12Cycle performance when material is as anode material of lithium-ion battery is surveyed
Test result.
Specific embodiment:
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
A kind of new method of high-tap density anode material of lithium-ion battery molybdenum sulfide preparation, specific steps are as follows:
(1) sulphur powder of the hexacarbonylmolybdenum of 1.5mmol and 4.5mmol is distributed in the ethanol solution of 20ml, quickly by it
Stirring forms uniform solution, is encased in the reaction kettle of 50ml；
(2) reaction kettle in step (1) is put into high temperature oven, 200 DEG C of reaction 12h；
(3) it after taking out reaction kettle in step (2), is cooled to room temperature, reaction kettle is opened, with ethyl alcohol centrifuge washing 3 times, 60
It is dried under DEG C vacuum atmosphere, obtains MoS2Material；
(4) in order to improve MoS2The MoS that the crystallinity of material will obtain in step (3)2It is mixed in argon/hydrogen (volume ratio 95/5)
Lower 800 DEG C of atmosphere are closed to be sintered 2 hours.
Sintered MoS2Material SEM photograph is as shown in Figure 1.By sintered MoS2Material is as sodium-ion battery cathode
Material carries out the test of chemical property, and test is metallic sodium piece to electrode, and electrolyte is 1M NaPF6It is dissolved in carbonic acid second
In enester/dimethyl carbonate (volume ratio 1/1), test results are shown in figure 2.Wherein, using ethyl alcohol as the MoS of solvent2Material
Show optimal cycle performance, high rate performance and high-multiplying power discharge specific capacity.
Embodiment 2
Using the preparation method for the high-tap density molybdenum sulfide being similar in embodiment 1, difference is, in step (1)
Solvent is respectively ethyl alcohol, toluene and acetone.By prepared MoS2Carry out the test of tap density, ethyl alcohol, toluene and acetone system
The tap density of standby material is respectively 0.87,0.44,0.65g cm-3, wherein having by material prepared by solvent of ethyl alcohol
Maximum tap density.
Claims (8)
1. a kind of preparation method of high-tap density anode material of lithium-ion battery, which is characterized in that comprising steps of
S1: molybdenum source and sulphur source are distributed in organic solvent and obtain mixed liquor；
S2: the mixed liquor in step S1 is packed into reaction kettle, carries out solvent thermal reaction；
S3: being cleaned the mixed liquor after reacting in step S2 and dried, and MoS is obtained2Material.
2. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 1, feature exist
In the step S3 further includes later step S4: the MoS that step S3 is obtained2Material is heat-treated in sintering atmosphere.
3. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 2, feature exist
In the sintering temperature in the step S4 is 800 DEG C, sintering time 2h.
4. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 2, feature exist
In the sintering atmosphere in the step S4 is at least one of nitrogen, argon gas, argon gas and hydrogen mixed gas atmosphere.
5. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 1, feature exist
In, molybdenum source in the step S1 be ammonium molybdate, sodium molybdate, hexacarbonylmolybdenum, phosphomolybdic acid, acetyl acetone, in potassium molybdate extremely
Few one kind.
6. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 1, feature exist
In, sulphur source in the step S1 be sulphur powder, thiocarbamide, thioacetamide, thiosemicarbazide, at least one in thioglycolic acid
Kind.
7. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 1, feature exist
In, organic solvent in the step S1 be methanol, ethyl alcohol, isopropanol, glycerine, acetone, toluene, at least one in dimethylbenzene
Kind.
8. a kind of preparation method of high-tap density anode material of lithium-ion battery according to claim 1, feature exist
In the reaction temperature of the step S2 is 200 DEG C, reaction time 12h.
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| CN201811266656.2A CN109360987A (en) | 2018-10-29 | 2018-10-29 | A kind of preparation method of high-tap density anode material of lithium-ion battery |
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| CN201811266656.2A CN109360987A (en) | 2018-10-29 | 2018-10-29 | A kind of preparation method of high-tap density anode material of lithium-ion battery |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140349177A1 (en) * | 2013-05-24 | 2014-11-27 | Korea Institute Of Science And Technology | Magnesium hybrid battery and its fabrication method |
| CN105600824A (en) * | 2016-01-20 | 2016-05-25 | 三峡大学 | High-performance micro-nano multilevel-structure MoS2 material and preparation method and application thereof |
| CN107579248A (en) * | 2017-08-23 | 2018-01-12 | 江汉大学 | The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide |
| CN107732239A (en) * | 2017-11-17 | 2018-02-23 | 东北师范大学 | A kind of preparation method of lithium/sodium ion low temperature battery ferrous sulfide/carbon coating negative material |
-
2018
- 2018-10-29 CN CN201811266656.2A patent/CN109360987A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140349177A1 (en) * | 2013-05-24 | 2014-11-27 | Korea Institute Of Science And Technology | Magnesium hybrid battery and its fabrication method |
| CN105600824A (en) * | 2016-01-20 | 2016-05-25 | 三峡大学 | High-performance micro-nano multilevel-structure MoS2 material and preparation method and application thereof |
| CN107579248A (en) * | 2017-08-23 | 2018-01-12 | 江汉大学 | The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide |
| CN107732239A (en) * | 2017-11-17 | 2018-02-23 | 东北师范大学 | A kind of preparation method of lithium/sodium ion low temperature battery ferrous sulfide/carbon coating negative material |
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