CN105870435B - A kind of MoO2@CNTs composite material and preparation methods - Google Patents
A kind of MoO2@CNTs composite material and preparation methods Download PDFInfo
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- CN105870435B CN105870435B CN201610243460.6A CN201610243460A CN105870435B CN 105870435 B CN105870435 B CN 105870435B CN 201610243460 A CN201610243460 A CN 201610243460A CN 105870435 B CN105870435 B CN 105870435B
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
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- 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
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- 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 MoO2@CNTs composite material and preparation methods, belong to battery material technical field.Include the following steps：1) ammonium molybdate solution is prepared, stirs, obtains solution A；2) carbon nanotube CNTs is dissolved in deionized water, ultrasonic disperse is uniform, obtains solution B；3) solution B is added dropwise to dropwise in solution A, obtains mixed solution, microwave treatment evaporates solvent to 0.02~0.08 times that volume is initial mixing liquor capacity, obtains suspension C；4) suspension C is freeze-dried, collects desciccate as predecessor D；5) predecessor D is heat-treated, MoO is made2@CNTs preform materials E；6) it repeats step 5) heat treatment operation for several times, MoO is made2@CNTs composite materials.Preparation method is simple for this, reproducible, low for equipment requirements；Through MoO made from this method2@CNTs composite products purity is high, good crystallinity, and binding force is high.
Description
Technical field
The invention belongs to battery material technical fields, are related to a kind of lithium ion battery negative material preparation method, specifically relate to
And a kind of MoO2@CNTs composite material and preparation methods.
Background technology
Lithium ion battery is compared with traditional lead acid batteries, nickel-cadmium cell etc., and energy density is high, self discharge is small, memoryless effect
It answers, have extended cycle life, energy storage efficiency can reach 90% or more, these characteristics determine it in mobile phone, laptop, movement
The application prospect of the portable electronic devices such as power supply, digital camera.At present commercialization graphitic carbon negative electrode intercalation potential it is low, have compared with
High output voltage and stable discharging capacity, but form Li dendrite in charge and discharge process and easily cause battery short circuit, there are huge safety
Hidden danger makes its development be restricted.
Molybdenum dioxide, which is applied to lithium ion battery negative material, has special embedding lithium mechanism, possesses conventional transition metal oxygen
The incomparable advantage of compound：Good conductivity can match in excellence or beauty with metallic conductor, and fusing point is high, stability is good, be ideal lithium
Battery material [Xu Z, Wang H, Li Z, et al.Sulfur refines MoO2 distribution enabling
improved lithium ion battery performance[J].Journal of Physical Chemistry C,
2014,118(32):18387-18396.].But its cyclic process intermediate ion migration rate is low, causes its actual capacity limited
[Auborn J J,Barberio Y L.Lithium intercalation cells without metallic lithium
MoO2/LiCoO2and WO2/LiCoO2[J].Journal of the Electrochemical Society,1987,134
(3):638-641.].In order to overcome its disadvantage, mainly improved by the following aspects：(1) pattern is controlled, nanometer material is prepared
Material, such as nano particle [Sun Y, Hu X, Luo W, et al.Ultrafine MoO2nanoparticles embedded in
a carbon matrix as a high-capacity and long-life anode for lithium-ion
batteries[J].Journal of Materials Chemistry,2011,22(2):425-431.], nanometer rods [Guo
B,Fang X,Li B,et al.Synthesis and Lithium Storage Mechanism of Ultrafine
MoO2Nanorods[J].Chemistry of Materials,2012,24(3):457-463.] etc.；(2) composite conducting carbon materials
Material, such as graphene [Bhaskar A, Deepa M, Rao T N, et al.Enhanced nanoscale conduction
capability of a MoO2 /Graphene composite for high performance anodes in
lithium ion batteries[J]. Journal of Power Sources,2012,216(11):169-178.].Separately
On the one hand, above-mentioned modified technique flow is complicated, and to equipment requirement height, product structure is difficult to control, is unfavorable for realizing industrial metaplasia
Production.
Invention content
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of MoO2@CNTs are compound
Material and preparation method thereof, preparation method is simple for this, reproducible, low for equipment requirements；Through MoO made from this method2@
CNTs composite products purity is high, good crystallinity, and binding force is high.
The present invention is to be achieved through the following technical solutions：
The invention discloses a kind of MoO2@CNTs composite material and preparation methods, include the following steps：
1) compound concentration is the ammonium molybdate solution of 1~5mol/L, stirs, obtains solution A；
2) carbon nanotube CNTs is dissolved in deionized water, ultrasonic disperse is uniform, obtains solution B；
3) solution A is pressed：Solution B=1:Solution B is added dropwise in solution A, is mixed by the volume ratio of (1~2) dropwise
Solution, microwave treatment evaporate solvent to 0.02~0.08 times that liquor capacity is initial mixing liquor capacity, obtain suspension C；
4) suspension C is freeze-dried, collects desciccate as predecessor D；
5) under an argon atmosphere by predecessor D, in 400~800 DEG C, it is heat-treated 1~4h, MoO is made2@CNTs precast bodies
Material E；
6) by MoO2For several times by the operation of step 5) heat treatment condition MoO is made in@CNTs preform material E2@CNTs are compound
Material.
Stirred in step 1) is to use 20~40min of magnetic agitation.
Carbon nanotube CNTs and the amount ratio of deionized water are (50~1000) mg in step 2)：(50~80) mL.
Step 3) is that mixed solution is placed in micro-wave oven, microwave treatment evaporate solvent, setting microwave power be 400~
800W。
Step 4) is freeze-dried at -50~-40 DEG C.
It is 100~300sccm that step 5), which controls argon gas flow velocity,.
Step 5) is that predecessor D is placed in rectangular porcelain boat to be heat-treated.
In step 6), operated 3~5 times by step 5) heat treatment condition.
The invention also discloses using MoO made from the above method2@CNTs composite materials.
Compared with prior art, the present invention has technique effect beneficial below：
MoO disclosed by the invention2The preparation method of@CNTs composite materials, can make MoO2It is dispersed in CNTs matrixes
On, CNTs provides more polyion and electron propagation ducts, enhances its migration rate, and inhibit material very well as buffer body
Volume expansion embodies the chemical property being gradually increasing.Meanwhile product is greatly improved using microwave irradiation and repeatedly heat treatment
Circulation volume, effect are fairly obvious.Preparation method is simple for this, reproducible, low for equipment requirements.
Through MoO made from the method for the present invention2@CNTs composite materials, purity is high, good crystallinity, and binding force is high.
Description of the drawings
Fig. 1 is that the present invention prepares MoO2@CNTs composite material XRD diagram.
Fig. 2 is that the present invention prepares MoO2SEM schemes under@CNTs composite material 10.0K multiplying powers.
Fig. 3 is that the present invention prepares MoO2SEM schemes under@CNTs composite material 50.0K multiplying powers.
Fig. 4 is that the present invention prepares MoO2@CNTs combination electrode materials and heat-treated products exist without Overheating Treatment and twice
100mA·g-1Cycle performance comparison diagram under current density.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A kind of MoO2@CNTs composite material and preparation methods, include the following steps：
(1) compound concentration is 1mol/L ammonium molybdate solution 50ml, magnetic agitation 20min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) it weighs 50mg carbon nanotubes to be dissolved in 50ml deionized waters, it is spare to obtain solution B by ultrasonic disperse 4h；
(3) above-mentioned solution B is added dropwise in solution A dropwise, and is transferred to setting microwave power 600W in micro-wave oven, micro-
Amplitude obtains suspension C according to lower gradual evaporation solution to 0.08 times that volume is initial mixing liquor capacity i.e. 8ml；
(4) above-mentioned suspension C is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -45 DEG C,
And desciccate is collected as predecessor D；
(5) above-mentioned predecessor D is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 100sccm
The lower 400 DEG C of reactions 4h of speed, obtains preform material E.
(6) precast body E is transferred to rectangular porcelain boat to repeat the above steps (5) 3 times, is successfully prepared by being heat-treated three times
MoO2@CNTs composite materials.
Embodiment 2
A kind of MoO2@CNTs composite material and preparation methods, include the following steps：
(1) compound concentration is 2mol/L ammonium molybdate solution 60ml, magnetic agitation 20min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) it weighs 100mg carbon nanotubes to be dissolved in 60ml deionized waters, it is spare to obtain solution B by ultrasonic disperse 3h；
(3) above-mentioned solution B is added dropwise in solution A dropwise, and is transferred to setting microwave power 500W in micro-wave oven, micro-
Amplitude obtains suspension C according to lower gradual evaporation solution to 0.05 times that volume is initial mixing liquor capacity i.e. 7ml；
(4) above-mentioned suspension C is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -40 DEG C,
And desciccate is collected as predecessor D；
(5) above-mentioned predecessor D is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 150sccm
The lower 500 DEG C of reactions 3h of speed, obtains MoO2@CNTs preform materials E.
(6) precast body E is transferred to rectangular porcelain boat to repeat the above steps (5) 4 times, is heat-treated by four times and successfully prepares
MoO2@CNTs composite materials.
Embodiment 3
A kind of MoO2@CNTs composite material and preparation methods, include the following steps：
(1) compound concentration is 4mol/L ammonium molybdate solution 80ml, magnetic agitation 30min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) it weighs 500mg carbon nanotubes to be dissolved in 80ml deionized waters, it is spare to obtain solution B by ultrasonic disperse 3h；
(3) above-mentioned solution B is added dropwise in solution A dropwise, and is transferred to setting microwave power 450W in micro-wave oven, micro-
Amplitude obtains suspension C according to lower gradual evaporation solution to 0.03 times that volume is initial mixing liquor capacity i.e. 6ml；
(4) above-mentioned suspension C is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -40 DEG C,
And desciccate is collected as predecessor D；
(5) above-mentioned predecessor D is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 200sccm
The lower 600 DEG C of reactions 2h of speed, obtains MoO2@CNTs preform materials E.
(6) precast body E is transferred to rectangular porcelain boat to repeat the above steps (5) 3 times, is successfully prepared by being heat-treated three times
MoO2@CNTs composite materials.
Embodiment 4
A kind of MoO2@CNTs composite material and preparation methods, include the following steps：
(1) compound concentration is 5mol/L ammonium molybdate solution 50ml, magnetic agitation 40min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) it weighs 1000mg carbon nanotubes to be dissolved in 80ml deionized waters, it is spare to obtain solution B by ultrasonic disperse 4h；
(3) above-mentioned solution B is added dropwise in solution A dropwise, and is transferred to setting microwave power 800W in micro-wave oven, micro-
Amplitude obtains suspension C according to lower gradual evaporation solution to 0.06 times that volume is initial mixing liquor capacity i.e. 8ml；
(4) above-mentioned suspension C is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -50 DEG C,
And desciccate is collected as predecessor D；
(5) above-mentioned predecessor D is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 300sccm
The lower 700 DEG C of reactions 1h of speed, obtains MoO2@CNTs preform materials E.
(6) precast body E is transferred to rectangular porcelain boat to repeat the above steps (5) 5 times, is heat-treated by five times and successfully prepares
MoO2@CNTs composite materials.
It will be seen from figure 1 that prepared MoO2@CNTs composite materials, good crystallinity, product purity are high.It can from Fig. 2
Go out, prepared MoO2@CNTs composite materials are uniformly dispersed, and do not occur apparent agglomeration, MoO2For size 500nm or so particle.
Fig. 3 can be seen that the MoO2@CNTs composite material CNTs uniform windings are in MoO2Surface, it is swollen as the fine buffer volumes of matrix
It is swollen.Fig. 4 is the MoO2@CNTs combination electrode materials are with without Overheating Treatment and twice heat-treated products in current density
100mA·g-1Lower cycle performance curve comparison figure, it can be seen that product circulation, which is stablized, after being repeatedly heat-treated is obviously improved,
Never process performance 200mAhg-1, heat treatment performance 250mAhg twice-1Promote product property after being repeatedly heat-treated
900mAh·g-1, thus repeatedly heat treatment process is obviously improved its cycle charge-discharge specific capacity.
Claims (6)
1. a kind of MoO2The preparation method of@CNTs composite materials, which is characterized in that include the following steps：
1) compound concentration is the ammonium molybdate solution of 1~5mol/L, stirs, obtains solution A；
2) carbon nanotube CNTs is dissolved in deionized water, ultrasonic disperse is uniform, obtains solution B；It carbon nanotube CNTs and goes
The amount ratio of ionized water is (50~1000) mg：(50~80) mL；
3) solution A is pressed：Solution B=1:Solution B is added dropwise in solution A, obtains mixed solution by the volume ratio of (1~2) dropwise,
Microwave treatment evaporates solvent to 0.02~0.08 times that liquor capacity is initial mixing liquor capacity, obtains suspension C；
4) suspension C is freeze-dried, collects desciccate as predecessor D；
5) under an argon atmosphere by predecessor D, control argon gas flow velocity is 100~300sccm, in 400~800 DEG C, heat treatment 1~
MoO is made in 4h2@CNTs preform materials E；
6) by MoO2MoO is made by the operation processing 3~5 times of step 5) in@CNTs preform material E2@CNTs composite materials.
2. MoO according to claim 12The preparation method of@CNTs composite materials, which is characterized in that fully stirred in step 1)
Mix is uniformly to use 20~40min of magnetic agitation.
3. MoO according to claim 12The preparation method of@CNTs composite materials, which is characterized in that step 3) is will to mix
Solution is placed in micro-wave oven, and microwave treatment evaporates solvent, and setting microwave power is 400~800W.
4. MoO according to claim 12The preparation method of@CNTs composite materials, which is characterized in that step 4) is -50
It is freeze-dried at~-40 DEG C.
5. MoO according to claim 12The preparation method of@CNTs composite materials, which is characterized in that step 5) is by forerunner
Object D is placed in rectangular porcelain boat and is heat-treated.
6. using MoO made from any one of Claims 1 to 5 the method2@CNTs composite materials.
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| CN108258221B (en) * | 2018-01-17 | 2019-07-09 | 扬州大学 | A kind of spherical S/C@MoO2 composite material and preparation method and application |
| CN109494358B (en) * | 2018-09-28 | 2021-09-07 | 陕西科技大学 | Mo supported by carbon matrix4O11/MoO2Lithium ion battery cathode material and preparation method thereof |
| CN111490235B (en) * | 2019-01-29 | 2021-08-06 | 中国科学院上海硅酸盐研究所 | Micron-particle high-capacity lithium ion battery cathode material based on conversion reaction and preparation method and application thereof |
| CN111933897B (en) * | 2019-05-13 | 2022-03-08 | 北京新能源汽车股份有限公司 | Composite material, preparation method and application thereof |
| CN113582231A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | MoO (MoO)2Preparation method of/carbon composite interlayer |
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| CN103288137A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Method for preparing molybdenum dioxide nanoparticles by microwave hydrothermal process |
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| CN103288137A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Method for preparing molybdenum dioxide nanoparticles by microwave hydrothermal process |
| CN104577072A (en) * | 2015-01-29 | 2015-04-29 | 陕西科技大学 | Preparation method of graphene-oxide-based MoO2 high-performance electrode material of lithium/sodium ion battery |
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