CN106920957A - A kind of molybdenum dioxide nano particle for lithium ion battery negative material and preparation method thereof - Google Patents
A kind of molybdenum dioxide nano particle for lithium ion battery negative material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of molybdenum dioxide nano particle for lithium ion battery negative material and preparation method thereof, first reducing sugar solution and molybdenum source solution are well mixed, mixed solution A is obtained, the mol ratio of reducing sugar and molybdenum source is (1~4) in mixed solution A:1；Then the surfactant solution of mixed solution A volume 1%~5% is accounted for addition in mixed solution A, it is well mixed to obtain mixed solution B；The pH value of regulation mixed solution B carries out homogeneous hydro-thermal reaction 1~4 at 180~220 DEG C；Homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains the molybdenum dioxide nano particle for lithium ion battery negative material.The present invention is by the MoO synthesized by hydro-thermal method2Nano particle diameter is small, shortens the lithium ion diffusion path in cyclic process, the bulk effect in cyclic process is reduced, 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 for the two of lithium ion battery negative material
Molybdenum oxide nanoparticles and preparation method thereof.
Background technology
With the continuous advance in epoch and continuing to develop for science and technology, lithium ion battery gradually replaces as a kind of novel energy
The status of traditional energy turns into the inseparable part of the mankind, is widely used in portable type electronic product, electronic traffic
Instrument, 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.]。
Graphite is used as a kind of commercialized lithium ion battery negative material, and its 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) as a kind of transition metal oxide, with metallic conductivity.Additionally, 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.It is relevant with phase in version during Lithium-ion embeding
Volume Changes 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 there is larger volume expansion during Lithium-ion embeding/abjection in it, so as to cause active material particle
Efflorescence, rupture, active material is come off from electrode, cause larger irreversible capacitance loss.At present, there are two methods
This problem can be solved, one is preparing the active material of nanosizing, increases the specific surface area of material, reduce electric charge diffusion road
Footpath.The second is being combined with carbon material, coming off for active material, and the carbon coating layer for being formed so not only is prevented to carry
The electric conductivity of material high；But the capacity for improving is little.
The content of the invention
It is an object of the invention to overcome problems of the prior art, there is provided one kind is used for lithium ion battery negative material
Molybdenum dioxide nano particle of material and preparation method thereof, circulation when improving molybdenum dioxide as lithium ion battery negative material is steady
It is qualitative.
In order to achieve the above object, the present invention is adopted the following technical scheme that：
Comprise the following steps：
(1) reducing sugar solution and molybdenum source solution are well mixed, obtain mixed solution A, reducing sugar in mixed solution A
It is (1~4) with the mol ratio of molybdenum source:1；Then live on the surface for accounting for mixed solution A volume 1%~5% to addition in mixed solution A
Property agent solution, it is well mixed to obtain mixed solution B；
(2) pH value of regulation mixed solution B obtains mixed solution C 1~4；
(3) mixed solution C is carried out into homogeneous hydro-thermal reaction at 180~220 DEG C；
(4) homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains for lithium-ion electric
The molybdenum dioxide nano particle of pond negative 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 is 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 uses NPE.
Further, it is to be well mixed by stirring 10~15min at 25~30 DEG C in step (1).
Further, using the HCl solution regulation pH value 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
Fill than 40%~70%, then sealing polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, be 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 to dry 10~15h in 60~80 DEG C of vacuum drying ovens.
It is a kind of to utilize the obtained molybdenum dioxide for lithium ion battery negative material of preparation method as described above nanometer
Grain, the molybdenum dioxide nano particle is monoclinic phase MoO2, particle diameter is in 10~50nm；500 are circulated under the current density of 100mA/g
Secondary capacity is in 610~650mAh/g.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention is reduced molybdenum source by reducing sugar, and a kind of MoO is provided by hydro-thermal method2The preparation side of nano particle
Method, the MoO2Nano particle has metallic conductivity, at room temperature resistivity very little, can be used in lithium ion battery negative material,
Product crystal property is good obtained in the inventive method, and size belongs to Nano grade, with excellent physical and chemical performance；Prepare letter
Single, cost is relatively low, is conducive to extensive 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 during as lithium ion battery negative material, has in 10~50nm
There is a good cycling stability, long service life, the advantages of specific capacity is big.It is circulated 500 times under the current density of 100mA/g, is held
Amount is up to 650mAh/g.
Brief description of the drawings
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 multiplication factors.
Specific embodiment
The present invention is described in further details below in conjunction with the accompanying drawings.
1) C of 0.5~1M is prepared6H12O6·H2O distilled water solutions, the Na of 0.5~1M2MoO4·2H2O distilled water solutions with
And the NPE 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 to the NPE that addition volume ratio in resulting solution is 1%~5%
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) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
40%~70%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 180~220 DEG C to set temperature parameter, reaction
Time is 18~25h.
6) reaction terminate after be cooled to room temperature, by end reaction thing centrifugation after, respectively with deionized water and anhydrous second
Alcohol respectively washing 3 times.To be centrifuged, the powder material after washing is put into 60~80 DEG C of vacuum drying ovens and dries 10~15h, that is, obtain final
Product.
Embodiment 1
1) C of 0.5M is prepared6H12O6·H2O distilled water solutions, the Na of 0.5M2MoO4·2H2O distilled water solutions and
The NPE distilled water solution of 0.01M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2O=2:1 ratio mixing, stirs at 30 DEG C
Mix 10min.Then to the NPE distilled water solution that volume ratio is 1% is added in resulting solution, stirred under 30
Mix 10min.
3) pH=1 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 2M.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
40%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 180 DEG C to set temperature parameter, and the reaction time is
25h。
6) reaction terminate after be cooled to room temperature, by end reaction thing centrifugation after, respectively with deionized water and anhydrous second
Alcohol respectively washing 3 times.To be centrifuged, the powder material after washing is put into 60 DEG C of vacuum drying ovens and dries 15h, that is, obtain final product.
Circulated 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 is obtained2It is the particle diameter about nutty structure of 15nm.
Embodiment 2
1) C of 1M is prepared6H12O6·H2O distilled water solutions, the Na of 1M2MoO4·2H2O distilled water solutions and 0.03M's
NPE distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2O=1:1 ratio mixing, stirs at 25 DEG C
Mix 15min.Then to the NPE distilled water solution that volume ratio is 5% is added in resulting solution, at 25 DEG C
Stirring 15min.
3) pH=4 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 3M.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
70%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 220 DEG C to set temperature parameter, and the reaction time is
18h。
6) reaction terminate after be cooled to room temperature, by end reaction thing centrifugation after, it is each with deionized water and absolute ethyl alcohol
Washing 3 times.To be centrifuged, the powder material after washing is put into 80 DEG C of vacuum drying ovens and dries 10h, that is, obtain final product.
Circulated 500 times under the current density of 100mA/g, capacity is up to 637mAh/g.
The MoO that the present invention is obtained2It is the particle diameter about nutty structure of 10nm.
Embodiment 3
1) C of 0.8M is prepared6H12O6·H2O distilled water solutions, the Na of 0.6M2MoO4·2H2O distilled water solutions and
The NPE distilled water solution of 0.02M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2O=3:1 ratio mixing, stirs at 28 DEG C
Mix 13min.Then to the NPE distilled water solution that volume ratio is 3% is added in resulting solution, at 28 DEG C
Stirring 13min.
3) pH=2.5 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 2M.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
55%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 200 DEG C to set temperature parameter, and the reaction time is
22h。
6) reaction terminate after be cooled to room temperature, by end reaction thing centrifugation after, it is each with deionized water and absolute ethyl alcohol
Washing 3 times.To be centrifuged, the powder material after washing is put into 70 DEG C of vacuum drying ovens or freeze drying box and dries 13h, that is, obtain
Final product.
Circulated 500 times under the current density of 100mA/g, capacity is up to 614mAh/g.
The MoO that the present invention is obtained2It is the particle diameter about nutty structure of 25nm.
Embodiment 4
1) C of 0.9M is prepared6H12O6·H2O distilled water solutions, the Na of 0.9M2MoO4·2H2O distilled water solutions and
The NPE distilled water solution of 0.02M.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2MoO4·2H2O=4:1 ratio mixing, stirs at 26 DEG C
Mix 12min.Then to the NPE distilled water solution that volume ratio is 2% is added in resulting solution, at 26 DEG C
Stirring 12min.
3) pH=2 of above-mentioned mixed solution is adjusted with the HCl solution that concentration is 3M.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
60%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 190 DEG C to set temperature parameter, and the reaction time is
24h。
6) reaction terminate after be cooled to room temperature, by end reaction thing centrifugation after, it is each with deionized water and absolute ethyl alcohol
Washing 3 times.To be centrifuged, the powder material after washing is put into 65 DEG C of vacuum drying ovens or freeze drying box and dries 14h, that is, obtain
Final product.
Circulated 500 times under the current density of 100mA/g, capacity is up to 610mAh/g.
The MoO that the present invention is obtained2It is the particle diameter about nutty structure of 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 mass produces.Additionally, when it is as lithium ion battery negative material, good cycling stability high with specific capacity is used
The advantages of long lifespan.
Claims (10)
1. the preparation method of a kind of 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 well mixed, obtain mixed solution A, reducing sugar and molybdenum in mixed solution A
The mol ratio in source is (1~4):1；Then the surfactant of mixed solution A volume 1%~5% is accounted for addition in mixed solution A
Solution, it is well mixed to obtain mixed solution B；
(2) pH value of regulation mixed solution B obtains mixed solution C 1~4；
(3) mixed solution C is carried out into homogeneous hydro-thermal reaction at 180~220 DEG C；
(4) homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains negative for lithium ion battery
The molybdenum dioxide nano particle of pole material.
2. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：The concentration of reducing sugar solution is 0.5~1mol/L in step (1), the concentration of molybdenum source solution for 0.5~
1mol/L, the concentration of surfactant solution is 0.01~0.03mol/L.
3. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：Reducing sugar uses C in step (1)6H12O6·H2O。
4. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：Molybdenum source uses Na in step (1)2WO4·2H2O, surfactant uses NPE.
5. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：It is to be well mixed by stirring 10~15min at 25~30 DEG C in step (1).
6. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：Using the HCl solution regulation pH value of 2~3mol/L in step (2).
7. the preparation side of a kind 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, being put into homogeneous hydro-thermal reaction instrument is carried out
Homogeneous hydro-thermal reaction.
8. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：18~the 25h of time of homogeneous hydro-thermal reaction in step (3).
9. the preparation side of a kind of molybdenum dioxide nano particle for lithium ion battery negative material according to claim 1
Method, it is characterised in that：Drying in step (4) is to dry 10~15h in 60~80 DEG C of vacuum drying ovens.
10. it is a kind of to utilize the obtained molybdenum dioxide for lithium ion battery negative material of preparation method described in claim 1 to receive
Rice grain, it is characterised in that：The molybdenum dioxide nano particle is monoclinic phase MoO2, particle diameter is in 10~50nm；In the electricity of 100mA/g
500 capacity are circulated under current density in 610~650mAh/g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511756A (en) * | 2019-09-23 | 2019-11-29 | 中国科学技术大学先进技术研究院 | Quantum dot material and preparation method and application thereof |
| CN112299483A (en) * | 2020-10-29 | 2021-02-02 | 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 |
| US20150263335A1 (en) * | 2014-03-11 | 2015-09-17 | Panasonic Corporation | Turbostratic material, active material for electricity storage devices, electrode, and electricity storage device |
| 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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2017
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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 |
| US20150263335A1 (en) * | 2014-03-11 | 2015-09-17 | Panasonic Corporation | Turbostratic material, active material for electricity storage devices, electrode, and electricity storage device |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110511756A (en) * | 2019-09-23 | 2019-11-29 | 中国科学技术大学先进技术研究院 | Quantum dot material and preparation method and application thereof |
| CN110511756B (en) * | 2019-09-23 | 2022-05-13 | 中国科学技术大学先进技术研究院 | Quantum dot material and preparation method and application thereof |
| CN112299483A (en) * | 2020-10-29 | 2021-02-02 | 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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