CN106920957B - A kind of molybdenum dioxide nano particle and preparation method thereof for lithium ion battery negative material - Google Patents
A kind of molybdenum dioxide nano particle and preparation method thereof for lithium ion battery negative material Download PDFInfo
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- CN106920957B CN106920957B CN201710272339.0A CN201710272339A CN106920957B CN 106920957 B CN106920957 B CN 106920957B CN 201710272339 A CN201710272339 A CN 201710272339A CN 106920957 B CN106920957 B CN 106920957B
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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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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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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- 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 molybdenum dioxide nano particle and preparation method thereof that the present invention relates to a kind of for lithium ion battery negative material, first reducing sugar solution and molybdenum source solution are uniformly mixed, mixed solution A is obtained, the molar ratio of reducing sugar and molybdenum source is (1~4) in mixed solution A: 1；Then the surfactant solution for accounting for mixed solution A volume 1%~5% is added into mixed solution A, is uniformly mixed and obtains mixed solution B；The pH value of mixed solution B is adjusted 1~4, carries out homogeneous hydro-thermal reaction at 180~220 DEG C；It is cooled to room temperature after homogeneous hydro-thermal reaction, isolates product and wash drying, obtain the molybdenum dioxide nano particle for lithium ion battery negative material.The present invention passes through MoO synthesized by hydro-thermal method2Nano particle diameter is small, shortens the lithium ion diffusion path in cyclic process, reduces the bulk effect in cyclic process, so that high rate performance is improved with cyclical stability.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of two for lithium ion battery negative material
Molybdenum oxide nanoparticles and preparation method thereof.
Background technique
With the continuous continuous development advanced with science and technology in epoch, lithium ion battery is gradually replaced as a kind of new energy
The status of traditional energy becomes a part of mankind's interwoveness, is widely used in portable electronic product, electronic traffic
Tool, large-sized power power supply and recharging and energy storage field [Ying Sun, Wei Wang, Jinwen Qin, et
al.Oxygen vacancy-rich mesoporous W18O49nanobelts with ultrahigh initial
Coulombic efficiency toward high-performance lithium storage[J]
.Electrochimica Acta,2016,187:329-339.]。
For graphite as a kind of commercialized lithium ion battery negative material, theoretical capacity only has 372mAh/g, very big
Limit its application in terms of lithium ion battery.In order to meet mankind itself's increasing demand, people begin one's study energy
Replace lithium ion battery negative material [Hao Li, Ming Liang, Weiwei Sun, the et al.Bimetal- of graphite
Organic Framework:One-Step Homogenous Formation and its Derived Mesoporous
Ternary Metal Oxide Nanorod for High-Capacity,High-Rate,and LongCycle-Life
Lithium Storage[J].Advanced Functional Materials,2016,26:1098-1103.].Molybdenum dioxide
(MoO2) it is used as a kind of transition metal oxide, there is metallic conductivity.In addition, when it is as lithium ion battery negative material,
Theoretical capacity is up to 838mAh/g, hence it is evident that higher than the theoretical capacity of graphite.During the process of lithium ion insertion, related with phase transition
Volume change it is smaller, can be used for lithium ion battery negative material [Jianfeng Huang, Zhanwei Xu, Liyun Cao,
et al.Tailoring MoO2/Graphene Oxide Nanostructures for Stable,High-Density
Sodium-Ion Battery Anodes[J].Advanced Functional Materials,2016,26:1098-
1103.], but it is during lithium ion intercalation/deintercalation that there are biggish volume expansions, to cause active material particle
Dusting, rupture, so that active material is fallen off from electrode, lead to biggish irreversible capacitance loss.Currently, there are two methods
It can solve this problem, one is the active material of preparation nanosizing, increases the specific surface area of material, reduce charge and spread road
Diameter.The second is it is compound with carbon material progress, falling off for active material is not only prevented in this way, but also the carbon coating layer formed can mention
The electric conductivity of high material；But the capacity improved is little.
Summary of the invention
It is an object of the invention to overcome problems of the prior art, provide a kind of for negative electrode of lithium ion battery material
It is steady to improve circulation of the molybdenum dioxide as lithium ion battery negative material when for molybdenum dioxide nano particle of material and preparation method thereof
It is qualitative.
In order to achieve the above object, the present invention adopts the following technical scheme:
The following steps are included:
(1) reducing sugar solution and molybdenum source solution are uniformly mixed, obtain mixed solution A, reducing sugar in mixed solution A
Molar ratio with molybdenum source is (1~4): 1；Then it lives on the surface that addition accounts for mixed solution A volume 1%~5% into mixed solution A
Property agent solution, be uniformly mixed obtain mixed solution B；
(2) pH value of mixed solution B is adjusted 1~4, obtains mixed solution C；
(3) mixed solution C is subjected to homogeneous hydro-thermal reaction at 180~220 DEG C；
(4) it is cooled to room temperature after homogeneous hydro-thermal reaction, isolates product and wash drying, obtain for lithium-ion electric
The molybdenum dioxide nano particle of pond negative electrode material.
Further, the concentration of reducing sugar solution is 0.5~1mol/L in step (1), and the concentration of molybdenum source solution is 0.5
~1mol/L, the concentration of surfactant solution are 0.01~0.03mol/L.
Further, reducing sugar uses C in step (1)6H12O6·H2O。
Further, molybdenum source uses Na in step (1)2WO4·2H2O, surfactant use nonylphenol polyoxyethylene ether.
It further, is uniformly mixed by stirring 10~15min at 25~30 DEG C in step (1).
Further, pH value is adjusted using the HCl solution of 2~3mol/L in step (2).
Further, mixed solution C is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle in step (3), and volume is filled out
It fills than then sealing polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle 40%~70%, is put into homogeneous hydro-thermal reaction instrument
Carry out homogeneous hydro-thermal reaction.
Further, in step (3) homogeneous hydro-thermal reaction 18~25h of time.
Further, the drying in step (4) is in the dry 10~15h of 60~80 DEG C of vacuum drying ovens.
It is a kind of to utilize the molybdenum dioxide nanometer that lithium ion battery negative material is used for made from preparation method as described above
Grain, the molybdenum dioxide nano particle are monoclinic phase MoO2, partial size is in 10~50nm；500 are recycled under the current density of 100mA/g
Secondary capacity is in 610~650mAh/g.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is restored molybdenum source by reducing sugar, provides a kind of MoO by hydro-thermal method2The preparation side of nano particle
Method, the MoO2Nano particle has metallic conductivity, and resistivity very little, can be used in lithium ion battery negative material at room temperature,
Product crystal property made from the method for the present invention is good, and size belongs to Nano grade, has excellent physical and chemical performance；Preparation letter
Single, cost is relatively low, is conducive to large scale preparation.MoO synthesized by the present invention2Nano particle diameter is small, shortens cyclic process
In lithium ion diffusion path, the bulk effect in cyclic process is reduced, so that high rate performance is obtained with cyclical stability
To raising.
MoO synthesized by the present invention2Nano particle diameter is in 10~50nm, when being used as lithium ion battery negative material, tool
There is the advantages that good cycling stability, long service life, specific capacity is big.It is recycled 500 times under the current density of 100mA/g, is held
Amount is up to 650mAh/g.
Detailed description of the invention
Fig. 1 is MoO prepared by the embodiment of the present invention 12XRD spectrum.
Fig. 2 is Nanoparticulate MoO prepared by the embodiment of the present invention 12SEM photograph under 50k amplification factor.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawing.
1) C of 0.5~1M is prepared6H12O6·H2O distilled water solution, the Na of 0.5~1M2MoO4·2H2O distilled water solution with
And the nonylphenol polyoxyethylene ether distilled water solution of 0.01~0.03M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2O=(1~4): 1 ratio mixing, 25
10~15min is stirred at~30 DEG C.Then the nonylphenol polyoxyethylene ether that volume ratio is 1%~5% is added into acquired solution
Distilled water solution stirs 10~15min at 25~30 DEG C.
3) pH=1~4 of above-mentioned mixed solution are adjusted with the HCl solution that concentration is 2~3M.
4) uniformly mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, volume packing ratio is kept to exist
40%~70%.
5) reaction kettle being sealed is put into homogeneous hydro-thermal reaction instrument, setting temperature parameter is 180~220 DEG C, reaction
Time is 18~25h.
6) it is cooled to room temperature after reaction, after the centrifuge separation of end reaction object, uses deionized water and anhydrous second respectively
Alcohol respectively washs 3 times.Powder substance after centrifugation, washing is put into the dry 10~15h of 60~80 DEG C of vacuum drying ovens, that is, is obtained final
Product.
Embodiment 1
1) C of 0.5M is prepared6H12O6·H2O distilled water solution, the Na of 0.5M2MoO4·2H2O distilled water solution and
The nonylphenol polyoxyethylene ether distilled water solution of 0.01M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2The ratio of O=2:1 mixes, and stirs at 30 DEG C
Mix 10min.Then the nonylphenol polyoxyethylene ether distilled water solution that volume ratio is 1% is added into acquired solution, is stirred under 30
Mix 10min.
3) pH=1 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 2M.
4) uniformly mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, volume packing ratio is kept to exist
40%.
5) reaction kettle being sealed is put into homogeneous hydro-thermal reaction instrument, setting temperature parameter is 180 DEG C, and the reaction time is
25h。
6) it is cooled to room temperature after reaction, after the centrifuge separation of end reaction object, uses deionized water and anhydrous second respectively
Alcohol respectively washs 3 times.Powder substance after centrifugation, washing is put into 60 DEG C of vacuum drying ovens dry 15h, i.e. acquisition final product.
It is recycled 500 times under the current density of 100mA/g, capacity is up to 650mAh/g.
As seen from Figure 1: product prepared by the present invention is monoclinic phase MoO2。
As seen from Figure 2: the MoO that the present invention obtains2It is the nutty structure that partial size is about 15nm.
Embodiment 2
1) C of 1M is prepared6H12O6·H2O distilled water solution, the Na of 1M2MoO4·2H2O distilled water solution and 0.03M's
Nonylphenol polyoxyethylene ether distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2The ratio of O=1:1 mixes, and stirs at 25 DEG C
Mix 15min.Then the nonylphenol polyoxyethylene ether distilled water solution that volume ratio is 5% is added into acquired solution, at 25 DEG C
Stir 15min.
3) pH=4 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 3M.
4) uniformly mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, volume packing ratio is kept to exist
70%.
5) reaction kettle being sealed is put into homogeneous hydro-thermal reaction instrument, setting temperature parameter is 220 DEG C, and the reaction time is
18h。
6) it is cooled to room temperature after reaction, it is each with deionized water and dehydrated alcohol after the centrifuge separation of end reaction object
Washing 3 times.Powder substance after centrifugation, washing is put into 80 DEG C of vacuum drying ovens dry 10h, i.e. acquisition final product.
It is recycled 500 times under the current density of 100mA/g, capacity is up to 637mAh/g.
The MoO that the present invention obtains2It is the nutty structure that partial size is about 10nm.
Embodiment 3
1) C of 0.8M is prepared6H12O6·H2O distilled water solution, the Na of 0.6M2MoO4·2H2O distilled water solution and
The nonylphenol polyoxyethylene ether distilled water solution of 0.02M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2The ratio of O=3:1 mixes, and stirs at 28 DEG C
Mix 13min.Then the nonylphenol polyoxyethylene ether distilled water solution that volume ratio is 3% is added into acquired solution, at 28 DEG C
Stir 13min.
3) pH=2.5 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 2M.
4) uniformly mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, volume packing ratio is kept to exist
55%.
5) reaction kettle being sealed is put into homogeneous hydro-thermal reaction instrument, setting temperature parameter is 200 DEG C, and the reaction time is
22h。
6) it is cooled to room temperature after reaction, it is each with deionized water and dehydrated alcohol after the centrifuge separation of end reaction object
Washing 3 times.Powder substance after centrifugation, washing is put into 70 DEG C of vacuum drying ovens or freeze drying box dry 13h, that is, is obtained
Final product.
It is recycled 500 times under the current density of 100mA/g, capacity is up to 614mAh/g.
The MoO that the present invention obtains2It is the nutty structure that partial size is about 25nm.
Embodiment 4
1) C of 0.9M is prepared6H12O6·H2O distilled water solution, the Na of 0.9M2MoO4·2H2O distilled water solution and
The nonylphenol polyoxyethylene ether distilled water solution of 0.02M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2The ratio of O=4:1 mixes, and stirs at 26 DEG C
Mix 12min.Then the nonylphenol polyoxyethylene ether distilled water solution that volume ratio is 2% is added into acquired solution, at 26 DEG C
Stir 12min.
3) pH=2 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 3M.
4) uniformly mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, volume packing ratio is kept to exist
60%.
5) reaction kettle being sealed is put into homogeneous hydro-thermal reaction instrument, setting temperature parameter is 190 DEG C, and the reaction time is
24h。
6) it is cooled to room temperature after reaction, it is each with deionized water and dehydrated alcohol after the centrifuge separation of end reaction object
Washing 3 times.Powder substance after centrifugation, washing is put into 65 DEG C of vacuum drying ovens or freeze drying box dry 14h, that is, is obtained
Final product.
It is recycled 500 times under the current density of 100mA/g, capacity is up to 610mAh/g.
The MoO that the present invention obtains2It is the nutty structure that partial size is about 50nm.
Sample crystallization prepared by the present invention is good, and product purity is high, and size is in Nano grade, and yield is big, is conducive to
Factory's large-scale production.In addition, having specific capacity height when it is as lithium ion battery negative material, good cycling stability is used
The advantages that service life is long.
Claims (7)
1. a kind of preparation method of the molybdenum dioxide nano particle for lithium ion battery negative material, it is characterised in that: including
Following steps:
(1) reducing sugar solution and molybdenum source solution are uniformly mixed, obtain mixed solution A, reducing sugar and molybdenum in mixed solution A
The molar ratio in source is (1~4): 1；Then the surfactant for accounting for mixed solution A volume 1%~5% is added into mixed solution A
Solution is uniformly mixed and obtains mixed solution B；
(2) pH value of mixed solution B is adjusted 1~4, obtains mixed solution C；
(3) mixed solution C is subjected to homogeneous hydro-thermal reaction at 180~220 DEG C；
(4) it is cooled to room temperature after homogeneous hydro-thermal reaction, isolates product and wash drying, obtained negative for lithium ion battery
The molybdenum dioxide nano particle of pole material；
The concentration of reducing sugar solution is 0.5~1mol/L in step (1), and the concentration of molybdenum source solution is 0.5~1mol/L, surface
The concentration of activator solution is 0.01~0.03mol/L；
Reducing sugar uses C in step (1)6H12O6·H2O；
Molybdenum source uses Na in step (1)2MoO4·2H2O, surfactant use nonylphenol polyoxyethylene ether.
2. a kind of preparation side of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that: be uniformly mixed by stirring 10~15min at 25~30 DEG C in step (1).
3. a kind of preparation side of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that: pH value is adjusted using the HCl solution of 2~3mol/L in step (2).
4. a kind of preparation side of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that: mixed solution C is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle in step (3), volume packing ratio
40%~70%, then polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle is sealed, is put into homogeneous hydro-thermal reaction instrument and carries out
Homogeneous hydro-thermal reaction.
5. a kind of preparation side of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that: 18~25h of time of homogeneous hydro-thermal reaction in step (3).
6. a kind of preparation side of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that: the drying in step (4) is in the dry 10~15h of 60~80 DEG C of vacuum drying ovens.
7. a kind of utilize the molybdenum dioxide nanometer for being used for lithium ion battery negative material made from preparation method described in claim 1
Particle, it is characterised in that: the molybdenum dioxide nano particle is monoclinic phase MoO2, partial size is in 10~50nm；In the electric current of 100mA/g
500 capacity are recycled under density in 610~650mAh/g.
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| CN112299483B (en) * | 2020-10-29 | 2022-02-01 | 中国科学院过程工程研究所 | Nano molybdenum dioxide and preparation method and application thereof |
| CN113972076A (en) * | 2021-10-26 | 2022-01-25 | 南京信息工程大学 | Molybdenum-based electrode material and preparation method and application thereof |
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| CN102795667A (en) * | 2012-08-29 | 2012-11-28 | 天津大学 | Method for preparing carbon-coated nanometer molybdenum dioxide material |
| CN105977479A (en) * | 2016-05-24 | 2016-09-28 | 中南大学 | Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery |
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| CN102795667A (en) * | 2012-08-29 | 2012-11-28 | 天津大学 | Method for preparing carbon-coated nanometer molybdenum dioxide material |
| CN105977479A (en) * | 2016-05-24 | 2016-09-28 | 中南大学 | Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery |
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