CN108695500A - The preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material - Google Patents
The preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material Download PDFInfo
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- CN108695500A CN108695500A CN201810495527.4A CN201810495527A CN108695500A CN 108695500 A CN108695500 A CN 108695500A CN 201810495527 A CN201810495527 A CN 201810495527A CN 108695500 A CN108695500 A CN 108695500A
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- molybdenum disulfide
- lithium ion
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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
- H01M4/362—Composites
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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
- H01M4/58—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 kind of preparation methods of carbon pipe modified molybdenum disulfide lithium ion battery negative material, organic sulfur compound, polymolybdote, carbon nanotube are compounded according to a certain percentage, solid product is obtained by hydro-thermal reaction, solid product is washed with deionized water or ethyl alcohol, presoma is obtained after drying, presoma is calcined under an inert atmosphere, calcination temperature is 600~800oC, after soaking time is 2~6h, cool to room temperature with the furnace, obtain molybdenum disulfide-carbon nano tube compound material, by to the sem analysis of composite material, XRD analysis, loop test and conducting performance test, it obtains one-dimensional rod-like pattern nitrogen and is modified molybdenum trioxide anode material for lithium-ion batteries, not only increase the electric conductivity of electrode material, enhance the stability of embedding de- lithium active site in crystal structure, improve lithium ion in the insertion of interlayer or abjection ability, to obtain high specific capacity, good cycle performance and electric conductivity.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparing technical fields, it particularly relates to which a kind of carbon pipe is modified two
The preparation method of molybdenum sulfide lithium ion battery negative material.
Background technology
The lithium ion battery energy storage material one of most potential as 21 century, it is the hot spot side studied at present to be increasingly becoming
To.Traditional lithium ion battery usually selects carbon as negative material, carbon material have price it is excellent it is honest and clean, a system such as have extended cycle life
Row advantage, but its specific capacity is smaller, it is difficult to industrially be promoted and applied on a large scale.Molybdenum disulfide is as novel lithium
Ion battery cathode material has the layer structure similar with graphite-phase:Mo-S-Mo, Mo-S in layer, Mo-Mo is respectively with ion
Key is mutually tied and is combined between layers by faint Van der Waals force.Electrochemical research finds that lithium ion insertion interlayer causes to lead
Body material is expanded along C crystallographic directions, and the Van der Waals force of interlayer is replaced by Coulomb force, is conducive to the insertion of lithium ion and is taken off
Go out, to show higher specific discharge capacity.
But molybdenum disulfide, in cyclic process, there are bulk effects during poorly conductive, lithium ion insertion and abjection
The shortcomings of big;Meanwhile the low activity molybdenum simple substance of de-/embedding generation of electrochemistry reduces structural stability, and reversible capacity is caused to decay
Rapidly, these problems make it cannot be satisfied the requirement of commercial Application.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Invention content
For above-mentioned technical problem in the related technology, the present invention proposes a kind of carbon pipe modified molybdenum disulfide lithium ion battery
The preparation method of negative material can improve the electric conductivity of electrode material, improve structural stability, specific capacity height, cyclicity
It can be good.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way:
A kind of preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material, includes the following steps:
S1. presoma is prepared:Weigh following raw material:Organic sulfur compound, polymolybdote and carbon nanotube, wherein according to rubbing
That concentration ratio meter, organic sulfur compound:Polymolybdote:Carbon nanotube is 5:9:27-1:1:1, the above raw material are added go from
In sub- water, after being uniformly mixed, be added N-Methyl pyrrolidone, the N-Methyl pyrrolidone and the deionized water according to
Volume ratio 1:1-2.5:Solution obtained as above is carried out hydro-thermal reaction by 1 addition, and heating temperature is 150~250oC, heated at constant temperature
12~for 24 hours, solid product is obtained, solid product is washed with deionized water or ethyl alcohol, presoma is obtained after dry;
S2. presoma prepared by step S1 is calcined under an inert atmosphere, calcination temperature is 600~800oC, soaking time 2
~6h;
S3. it cools to room temperature with the furnace, obtains molybdenum disulfide-carbon nano tube compound material.
Further, hydro-thermal reaction described in step S1 carries out heating reaction using polytetrafluoroethylene (PTFE) water heating kettle.
Further, solution heat temperature raising speed described in step S1 is 1-10oC/ minutes.
Further, drying condition described in step S1 is:Drying temperature 60~80oC, 6~12 hours drying times.
Further, it is 1-10 that heating rate is calcined described in step S2oC/ minutes.
Further, organic sulfur compound described in step S1 selects L-cysteine or thiocarbamide, the polymolybdote to select
Na2MoO4Or (NH4)2MoO4, the carbon nanotube selects multi-walled carbon nanotube or single-walled carbon nanotube.
Further, inert atmosphere described in step S2 is N2Or Ar.
A kind of carbon pipe modified molybdenum disulfide lithium ion battery negative material comprising molybdenum disulfide and carbon nanotube compound electric
Pole material, the molybdenum disulfide are by using polymolybdote as presoma, utilizing hydro-thermal original with carbon nano-tube combination electrode material
Position self assembly makes nanometer MOS 2 particle be made in carbon nano tube surface homoepitaxial.
Further, the polymolybdote presoma is made of following material, according to molar concentration rate meter, organic sulfide
Object:Polymolybdote:Carbon nanotube is 5:9:27-1:1:1.
Beneficial effects of the present invention:By hydro-thermal reaction, nanometer MOS 2 particle is made uniformly to be given birth in carbon nano tube surface
It is long, not only improve material conductivity, the growth in situ of molybdenum disulfide can also improve structure of the material in de- or process of intercalation
Stability promotes its cycle performance.This method is simple for process, at low cost, and product obtained has specific capacity height, good cycle
Characteristic.
Description of the drawings
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the SEM figures of the according to embodiments of the present invention 1 molybdenum disulfide/carbon nano tube compound material prepared.
Fig. 2 is the XRD spectra of the according to embodiments of the present invention 2 molybdenum disulfide/carbon nano tube compound materials prepared.
Fig. 3 is the cycle performance test knot of the according to embodiments of the present invention 3 molybdenum disulfide/carbon nano tube compound materials prepared
Fruit.
Fig. 4 is the AC impedance spectroscopy of the according to embodiments of the present invention 4 molybdenum disulfide/carbon nano tube compound materials prepared.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained belong to what the present invention protected
Range.
Embodiment 1:
1)Prepare presoma:According to molar concentration rate, L-cysteine:(NH4)2MoO4=5, (NH4)2MoO4:Multi-walled carbon nanotube
=1.5 weigh respective material, i.e. L-cysteine, (NH4)2MoO4And multi-walled carbon nanotube, by L-cysteine, (NH4)2MoO4
It is added in deionized water with multi-walled carbon nanotube, after being uniformly mixed, N-Methyl pyrrolidone, the N- methyl pyrroles of addition is added
Pyrrolidone is 1.5 additions according to volume ratio with deionized water.Acquired solution is transferred to polytetrafluoroethylene (PTFE) water heating kettle, and 5oC/ minutes
Rate be warming up to 200oC, isothermal reaction 12h, obtains solid product, after, it is washed and is consolidated with deionized water or ethyl alcohol
Body product, solid product is 60oIt is 6 hours dry under C, obtain presoma.
2)Above-mentioned presoma is transferred in quartz boat, is placed in tubular heater, under nitrogen atmosphere cycle, 5oC/ points
The rate of clock is warming up to 600oC is calcined, and soaking time 4h cools to room temperature with the furnace and both obtain MoS after reaction2-CNT
Composite material.
As shown in Figure 1, SEM observes that homoepitaxial molybdenum disulfide particles in carbon nanotube, the two are closely compound.
Embodiment 2:
1)Prepare presoma:According to molar concentration rate, thiocarbamide:Na2MoO4=7, Na2MoO4:Multi-walled carbon nanotube=1 weighs accordingly
Material, can thiocarbamide, Na2MoO4Deionized water is added with multi-walled carbon nanotube, after being uniformly mixed, N- methylpyrroles are added
The N-Methyl pyrrolidone of alkanone, addition is added according to volume ratio for 1 with deionized water, and acquired solution is transferred to polytetrafluoroethylene (PTFE)
Water heating kettle, 6oC/ minutes rates are warming up to 180oC, isothermal reaction 18h, obtains solid product, after, use deionized water
Or the solid product that ethyl alcohol washs, solid product is 60oIt is 10 hours dry under C, obtain presoma.
2)Above-mentioned presoma is transferred in quartz boat, is placed in tubular heater, under argon gas atmosphere cycle, 10oC/ points
The rate of clock is warming up to 750oC is calcined, and soaking time 4h cools to room temperature with the furnace and both obtain MoS after reaction2- CNT is multiple
Condensation material.
As shown in Fig. 2, the molybdenum disulfide grown in carbon nanotube has good crystallinity.
Embodiment 3:
1)Prepare presoma:According to molar concentration rate, thiocarbamide:(NH4)2MoO4=6, (NH4)2MoO4:Single-walled carbon nanotube=1.5 claim
Take respective material.By thiocarbamide, (NH4)2MoO4Deionized water is added with single-walled carbon nanotube, after being uniformly mixed, N- first is added
The N-Methyl pyrrolidone of base pyrrolidones, addition is added according to volume ratio for 2 with deionized water, and acquired solution is transferred to poly- four
Vinyl fluoride water heating kettle, 3oC/ minutes rates are warming up to 250oC, isothermal reaction 12h, obtains solid product, after, it spends
The solid product that ionized water or ethyl alcohol wash, solid product is 80oIt is 6 hours dry under C, obtain presoma.
2)Above-mentioned presoma, which is transferred in quartz boat, to be placed in tubular heater, under argon gas atmosphere cycle, 3oC/ points
The rate of clock is warming up to 800oC is calcined, and soaking time 3h cools to room temperature with the furnace and both obtain MoS after reaction2-CNT
Composite material.
As shown in figure 3, loop test is the result shows that cycle after 500 weeks, remains to obtain high power capacity.
Embodiment 4:
1)Prepare presoma:According to molar concentration rate, L-cysteine:Na2MoO4=6, Na2MoO4:Single-walled carbon nanotube=2 claim
Respective material is taken, by L-cysteine, Na2MoO4Deionized water is added with single-walled carbon nanotube, after being uniformly mixed, is added
The N-Methyl pyrrolidone of N-Methyl pyrrolidone, addition is added according to volume ratio for 1 with deionized water, and acquired solution is transferred to
Polytetrafluoroethylene (PTFE) water heating kettle, 5oC/ minutes rates are warming up to 200oC, isothermal reaction 20h, obtains solid product, after,
The solid product washed with deionized water or ethyl alcohol, solid product is 65oIt is 10 hours dry under C, obtain presoma.
2)Above-mentioned presoma, which is transferred in quartz boat, to be placed in tubular heater, under nitrogen atmosphere cycle, 8oC/ points
The rate of clock is warming up to 700oC is calcined, and soaking time 4h cools to room temperature with the furnace and both obtain MoS after reaction2-CNT
Composite material.
Fig. 4 test results show with carbon nanotube it is compound after, materials conductive performance is obviously improved.
Homoepitaxial molybdenum disulfide particles in carbon nanotube, the two are observed by the SEM figures of the product to embodiment 1-4
Close compound, XRD spectrum shows that the molybdenum disulfide grown in carbon nanotube has good crystallinity, by loop test and leads
Electric performance test, the results showed that cycle remains to obtain high power capacity, materials conductive performance is obviously improved after 500 weeks.
The present invention prepares one-dimensional rod-like pattern nitrogen by polymolybdote hydridization presoma pyrolysis and is modified molybdenum trioxide lithium ion
Cell negative electrode material not only increases the electric conductivity of electrode material, enhances the stabilization of embedding de- lithium active site in crystal structure
Property, improve lithium ion interlayer intercalation/deintercalation ability, to obtain high specific capacity, good cycle performance and conduction
Performance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (9)
1. a kind of preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material, which is characterized in that including following step
Suddenly:
S1. presoma is prepared:Weigh following raw material:Organic sulfur compound, polymolybdote and carbon nanotube, wherein according to rubbing
That concentration ratio meter, organic sulfur compound:Polymolybdote:Carbon nanotube is 5:9:27-1:1:1, the above raw material are added go from
In sub- water, after being uniformly mixed, be added N-Methyl pyrrolidone, the N-Methyl pyrrolidone and the deionized water according to
Volume ratio 1:1-2.5:Solution obtained as above is carried out hydro-thermal reaction by 1 addition, and heating temperature is 150~250oC, heated at constant temperature
12~for 24 hours, solid product is obtained, solid product is washed with deionized water or ethyl alcohol, presoma is obtained after dry;
S2. presoma prepared by step S1 is calcined under an inert atmosphere, calcination temperature is 600~800oC, soaking time 2
~6h;
S3. it cools to room temperature with the furnace, obtains molybdenum disulfide-carbon nano tube compound material.
2. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1, feature
It is, hydro-thermal reaction described in step S1 is heated using polytetrafluoroethylene (PTFE) water heating kettle.
3. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1 or 2, special
Sign is that solution heat temperature raising speed described in step S1 is 1-10oC/ minutes.
4. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1, feature
It is, drying condition is described in step S1:Drying temperature 60~80oC, 6~12 hours drying times.
5. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1, feature
It is, it is 1-10 that heating rate is calcined described in step S2oC/ minutes.
6. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1, feature
It is, organic sulfur compound described in step S1 selects L-cysteine or thiocarbamide, the polymolybdote to select Na2MoO4Or (NH4)2MoO4, the carbon nanotube selects multi-walled carbon nanotube or single-walled carbon nanotube.
7. the preparation method of carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 1, feature
It is, inert atmosphere described in step S2 is N2Or Ar.
8. a kind of carbon pipe modified molybdenum disulfide lithium ion battery negative material, which is characterized in that it includes that molybdenum disulfide is received with carbon
Mitron combination electrode material, the molybdenum disulfide and carbon nano-tube combination electrode material be by using polymolybdote as presoma,
Nanometer MOS 2 particle is set to be made in carbon nano tube surface homoepitaxial using hydro-thermal primary reconstruction.
9. carbon pipe modified molybdenum disulfide lithium ion battery negative material according to claim 8, which is characterized in that described more
Molybdate presoma is made of following material, according to molar concentration rate meter, organic sulfur compound:Polymolybdote:Carbon nanotube is 5:
9:27-1:1:1。
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Cited By (8)
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| CN110270305A (en) * | 2019-05-08 | 2019-09-24 | 北京化工大学 | A kind of application of fish scale-shaped transient metal sulfide carbon nanomaterial |
| CN111106319A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped molybdenum disulfide/carbon nanotube composite material |
| CN111106318A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped molybdenum disulfide/C/carbon nanotube composite material |
| CN111992228A (en) * | 2020-09-02 | 2020-11-27 | 大连工业大学 | Molybdenum disulfide and carbon nanotube composite material catalyst, and preparation and application thereof |
| CN112216840A (en) * | 2020-10-13 | 2021-01-12 | 陕西科技大学 | Molybdenum disulfide/molybdenum nitride heterostructure composite material for lithium-sulfur battery electrode and preparation method thereof |
| CN113258046A (en) * | 2021-05-19 | 2021-08-13 | 郑州航空工业管理学院 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
| CN114214659A (en) * | 2022-01-12 | 2022-03-22 | 安徽大学 | Electrocatalytic material and preparation method and application thereof |
| CN115058056A (en) * | 2022-07-05 | 2022-09-16 | 江苏安纳泰环保科技有限公司 | Preparation method and application of molybdenum disulfide carbon nanotube polyvinyl alcohol-based photo-thermal material |
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| CN111106319A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped molybdenum disulfide/carbon nanotube composite material |
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| CN110270305A (en) * | 2019-05-08 | 2019-09-24 | 北京化工大学 | A kind of application of fish scale-shaped transient metal sulfide carbon nanomaterial |
| CN111992228A (en) * | 2020-09-02 | 2020-11-27 | 大连工业大学 | Molybdenum disulfide and carbon nanotube composite material catalyst, and preparation and application thereof |
| CN112216840A (en) * | 2020-10-13 | 2021-01-12 | 陕西科技大学 | Molybdenum disulfide/molybdenum nitride heterostructure composite material for lithium-sulfur battery electrode and preparation method thereof |
| CN113258046A (en) * | 2021-05-19 | 2021-08-13 | 郑州航空工业管理学院 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
| CN113258046B (en) * | 2021-05-19 | 2022-06-14 | 郑州航空工业管理学院 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
| CN114214659A (en) * | 2022-01-12 | 2022-03-22 | 安徽大学 | Electrocatalytic material and preparation method and application thereof |
| CN115058056A (en) * | 2022-07-05 | 2022-09-16 | 江苏安纳泰环保科技有限公司 | Preparation method and application of molybdenum disulfide carbon nanotube polyvinyl alcohol-based photo-thermal material |
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Application publication date: 20181023 |