CN106129393A - A kind of ZnMoO40.8H2o lithium ion battery negative material and preparation method thereof - Google Patents
A kind of ZnMoO40.8H2o lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN106129393A CN106129393A CN201610767658.4A CN201610767658A CN106129393A CN 106129393 A CN106129393 A CN 106129393A CN 201610767658 A CN201610767658 A CN 201610767658A CN 106129393 A CN106129393 A CN 106129393A
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- lithium ion
- ion battery
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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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- 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 invention discloses a kind of ZnMoO4·0.8H2O lithium ion battery negative material and preparation method thereof, is first dissolved in distilled water respectively by zinc salt and molybdate that mol ratio is 1:1, and stirring makes it fully dissolve；In above-mentioned solution, add surfactant the most respectively, and stir；Then molybdate solution is added dropwise in zinc solution, at room temperature stratification after stirring；After the lower floor's powder body centrifugation that finally will obtain in step 3, with distilled water and absolute ethanol washing, then drying is to ZnMoO4·0.8H2O lithium ion battery negative material.The present invention is easy and simple to handle, low cost, the ZnMoO for preparing4·0.8H2O purity is high, excellent performance, can synthesize in a large number, is suitable for industrialized production, and by ZnMoO4·0.8H2O is used as lithium ion battery negative material, makes this lithium battery have the highest specific capacity.
Description
Technical field
The present invention relates to the preparation method of a kind of lithium ion battery negative material, be specifically related to a kind of ZnMoO4·0.8H2O
Lithium ion battery negative material and preparation method thereof.
Background technology
Lithium rechargeable battery is considered as power vehicle of future generation and hybrid vehicle thereof due to the performance of its excellence
The major impetus energy.At present, the negative material that business-like lithium ion battery is used is all carbon materials, such as graphite, soft
Carbon, hard carbon etc., but the theoretical specific capacity ratio of carbon materials is relatively low, only 372mAhg-1, cannot meet growing
Demand to high-capacity lithium ion cell, therefore needs the novel negative pole of high-capacity lithium ion cell developing a kind of alternative graphite badly
Material.
Zinc molybdate is a kind of important inorganic salt product, and the crystal structure special due to it and the characteristics of luminescence are widely applied
With industries such as optics, electronics, biology, coating, medicine, buildings.The pattern of zinc molybdate micro crystal material to it on photoelectric device
Serviceability aspect has a very big impact.
Summary of the invention
It is an object of the invention to provide a kind of ZnMoO4·0.8H2O lithium ion battery negative material and preparation method thereof,
With the defect overcoming above-mentioned prior art to exist, the present invention is easy and simple to handle, low cost, the ZnMoO for preparing4·0.8H2O purity
High, excellent performance, can synthesize in a large number, is suitable for industrialized production, and by ZnMoO4·0.8H2O is used as lithium ion battery negative
Material, makes this lithium battery have the highest specific capacity.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of ZnMoO4·0.8H2The preparation method of O lithium ion battery negative material, comprises the following steps:
Step one: zinc salt and molybdate that mol ratio is 1:1 are dissolved in respectively in distilled water, stirring makes it fully dissolve；
Step 2: add surfactant respectively in above-mentioned solution, and stir；
Step 3: molybdate solution is added dropwise in zinc solution, at room temperature stratification after stirring；
Step 4: after the lower floor's powder body centrifugation that will obtain in step 3, with distilled water and absolute ethanol washing, then
Drying is to ZnMoO4·0.8H2O lithium ion battery negative material.
Further, described molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or zinc chloride.
Further, in step one and step 2, alr mode is magnetic agitation, and mixing time is 10min.
Further, in step 2, surfactant is SDS, wherein adds 0.1～1g surface activity in every 100mL solution
Agent.
Further, the rate of addition in step 3 is 1～3mL/min.
Further, in step 3, mixing time is 0.5～3h, and the standing and reacting time is 1～5d.
Further, in step 4, centrifugal speed is 8000～9000r/min, and centrifugation time is 10～15min.
Further, in step 4, during washing, dehydrated alcohol and distilled water alternately rinse 3～6 times totally.
Further, drying temperature in step 4 is 60 DEG C.
A kind of ZnMoO4·0.8H2O lithium ion battery negative material, uses above-mentioned ZnMoO4·0.8H2O lithium-ion electric
The preparation method of pond negative material prepares.
Compared with prior art, the present invention has a following useful technique effect:
The inventive method has at room temperature synthesized ZnMoO4·0.8H2O nanometer rods, diameter 300-400nm, it is about several micro-
Rice, the method is easy and simple to handle, low cost, and the present invention is by the ZnMoO of preparation4·0.8H2O nanometer rods is as lithium ion battery negative
Material has the highest specific capacity, ZnMoO4·0.8H2The charge and discharge potential of the electrode that O negative material prepares is 0.01～3.0V,
It is 100mAg in electric current density-1Time first discharge specific capacity reach 890mAhg-1, coulombic efficiency is up to 89.1% first, even if
It is 500mAg in electric current density-1Time specific discharge capacity still be up to 280mAhg-1, the ZnMoO for preparing4·0.8H2O nanometer rods is pure
Degree is high, excellent performance, can synthesize in a large number, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the ZnMoO of embodiment 1 preparation4·0.8H2The XRD figure of O lithium ion battery negative material；
Fig. 2 is the ZnMoO of embodiment 1 preparation4·0.8H2The SEM figure of O lithium ion battery negative material；
Fig. 3 is the ZnMoO of embodiment 1 preparation4·0.8H2The TEM figure of O lithium ion battery negative material；
Fig. 4 is to use the prepared material of embodiment 1 for the charge-discharge performance figure of simulated battery；
Fig. 5 is to use the prepared material of embodiment 1 for the high rate performance figure of simulated battery；
Fig. 6 is to use the prepared material of embodiment 1 for the cyclic voltammogram of simulated battery.
Detailed description of the invention
Below embodiments of the present invention are described in further detail:
A kind of ZnMoO4·0.8H2The preparation method of O lithium ion battery negative material, comprises the following steps:
Step one: zinc salt and molybdate that mol ratio is 1:1 being dissolved in respectively in distilled water, magnetic agitation 10min makes it
Fully dissolving, wherein, molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or zinc chloride；
Step 2: add surfactant SDS respectively in above-mentioned solution, wherein add 0.1～1g in every 100mL solution
Surfactant, continues magnetic agitation 10min；
Step 3: molybdate solution is added dropwise in zinc solution with the speed of 1～3mL/min, stirring 30min～
3h, at normal temperatures standing and reacting 1～5d；
Step 4: after the powder body obtained in step 3 is centrifuged 10～15min with 8000～9000r/min, dehydrated alcohol
Alternately rinse totally 3～6 times with distilled water, the most in an oven with 60 DEG C of drying to ZnMoO4·0.8H2O lithium ion battery
Negative material.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
Step one: zinc nitrate and ammonium molybdate that mol ratio is 1:1 being dissolved in respectively in distilled water, magnetic agitation 10min makes
It fully dissolves；
Step 2: add surfactant SDS respectively in above-mentioned solution, wherein add 0.5g table in every 100mL solution
Face activating agent, continues magnetic agitation 10min；
Step 3: be added dropwise in zinc nitrate solution with the speed of 1mL/min by ammonium molybdate solution, stirs 30min, often
Lower standing and reacting 5d of temperature；
Step 4: after the powder body obtained in step 3 is centrifuged 10min with 8000r/min, dehydrated alcohol and distilled water are handed over
For rinsing 4 times, the most in an oven with 60 DEG C of drying to ZnMoO4·0.8H2O。
ZnMoO by preparation4·0.8H2O powder body is with conductive agent acetylene black, sodium carboxymethyl cellulose, polyacrylic acid by weight
Mixing than 80:10:5:5, grind uniformly through agate mortar, be coated on Copper Foil after furnishing slurry, coating thickness is 15～20 μm,
120 DEG C of vacuum drying 24h, obtain anode plate for lithium ionic cell through sheet-punching machine punching.
With the anode plate for lithium ionic cell that obtains as positive pole, with 1mol/L LiPF6Three component mixed solvent (volume ratios
Vinyl carbonate EC: dimethyl carbonate DMC: diethyl carbonate EMC=1:1:1) be electrolyte, microporous polypropylene membrane be every
Film, lithium sheet is that negative plate is assembled into simulated battery, and simulated battery carries out performance test, uses Shenzhen new prestige cell tester pair
Simulated battery carries out charging and discharging capacity cycle performance test, carries out constant current charge-discharge specific capacity with the electric current density of 100mA/g
Loop test is tested, and charging/discharging voltage is limited in 0.01～3.0V, and result shows, embodiment 1 simulated battery prepared is at electricity
Current density is 100mAg-1Time first discharge specific capacity reach 890mAhg-1, coulombic efficiency is up to 89.1% first, even if at electricity
Current density is 500mAg-1Time specific discharge capacity still be up to 280mAhg-1。
Embodiment 2
Step one: zinc chloride and sodium molybdate that mol ratio is 1:1 being dissolved in respectively in distilled water, magnetic agitation 10min makes
It fully dissolves；
Step 2: add surfactant SDS respectively in above-mentioned solution, wherein add 0.1g table in every 100mL solution
Face activating agent, continues magnetic agitation 10min；
Step 3: be added dropwise in liquor zinci chloridi with the speed of 2mL/min by sodium molybdate solution, stirs 1h, at room temperature
Lower standing and reacting 4d；
Step 4: after the powder body obtained in step 3 is centrifuged 12min with 9000r/min, dehydrated alcohol and distilled water are handed over
For rinsing 3 times, the most in an oven with 60 DEG C of drying to ZnMoO4·0.8H2O。
Embodiment 3
Step one: zinc chloride and ammonium molybdate that mol ratio is 1:1 being dissolved in respectively in distilled water, magnetic agitation 10min makes
It fully dissolves；
Step 2: add surfactant SDS respectively in above-mentioned solution, wherein add 1g surface in every 100mL solution
Activating agent, continues magnetic agitation 10min；
Step 3: be added dropwise in liquor zinci chloridi with the speed of 3mL/min by ammonium molybdate solution, stirs 2h, at room temperature
Lower standing and reacting 1d；
Step 4: after the powder body obtained in step 3 is centrifuged 15min with 8500r/min, dehydrated alcohol and distilled water are handed over
For rinsing 6 times, the most in an oven with 60 DEG C of drying to ZnMoO4·0.8H2O。
Embodiment 4
Step one: zinc nitrate and sodium molybdate that mol ratio is 1:1 being dissolved in respectively in distilled water, magnetic agitation 10min makes
It fully dissolves；
Step 2: add surfactant SDS respectively in above-mentioned solution, wherein add 1g surface in every 100mL solution
Activating agent, continues magnetic agitation 10min；
Step 3: be added dropwise in zinc nitrate solution with the speed of 1mL/min by sodium molybdate solution, stirs 3h, at room temperature
Lower standing and reacting 3d；
Step 4: after the powder body obtained in step 3 is centrifuged 10min with 8000r/min, dehydrated alcohol and distilled water are handed over
For rinsing 5 times, the most in an oven with 60 DEG C of drying to ZnMoO4·0.8H2O。
Claims (10)
1. a ZnMoO4·0.8H2The preparation method of O lithium ion battery negative material, it is characterised in that comprise the following steps:
Step one: zinc salt and molybdate that mol ratio is 1:1 are dissolved in respectively in distilled water, stirring makes it fully dissolve；
Step 2: add surfactant respectively in above-mentioned solution, and stir；
Step 3: molybdate solution is added dropwise in zinc solution, at room temperature stratification after stirring；
Step 4: after the lower floor's powder body centrifugation that will obtain in step 3, with distilled water and absolute ethanol washing, then dry
I.e. obtain ZnMoO4·0.8H2O lithium ion battery negative material.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, described molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or zinc chloride.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, in step one and step 2, alr mode is magnetic agitation, and mixing time is 10min.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, in step 2, surfactant is SDS, wherein adds 0.1～1g surfactant in every 100mL solution.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, the rate of addition in step 3 is 1～3mL/min.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, in step 3, mixing time is 0.5～3h, and the standing and reacting time is 1～5d.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, in step 4, centrifugal speed is 8000～9000r/min, and centrifugation time is 10～15min.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, in step 4, during washing, dehydrated alcohol and distilled water alternately rinse 3～6 times totally.
A kind of ZnMoO the most according to claim 14·0.8H2The preparation method of O lithium ion battery negative material, its feature
Being, drying temperature in step 4 is 60 DEG C.
10. a ZnMoO4·0.8H2O lithium ion battery negative material, it is characterised in that use any one of claim 1～9
Described ZnMoO4·0.8H2The preparation method of O lithium ion battery negative material prepares.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106532030A (en) * | 2016-12-26 | 2017-03-22 | 惠州Tcl金能电池有限公司 | Calcium molybdate lithium ion battery negative electrode material and preparation method thereof |
| CN114203983A (en) * | 2021-11-04 | 2022-03-18 | 江苏大学 | Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532030A (en) * | 2016-12-26 | 2017-03-22 | 惠州Tcl金能电池有限公司 | Calcium molybdate lithium ion battery negative electrode material and preparation method thereof |
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| CN114203983A (en) * | 2021-11-04 | 2022-03-18 | 江苏大学 | Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery |
| CN114203983B (en) * | 2021-11-04 | 2022-11-18 | 江苏大学 | Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery |
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Application publication date: 20161116 |