CN107579230A - The preparation method of zinc oxide/carbon composite and the application on lithium ion battery - Google Patents
The preparation method of zinc oxide/carbon composite and the application on lithium ion battery Download PDFInfo
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- CN107579230A CN107579230A CN201710801440.0A CN201710801440A CN107579230A CN 107579230 A CN107579230 A CN 107579230A CN 201710801440 A CN201710801440 A CN 201710801440A CN 107579230 A CN107579230 A CN 107579230A
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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 present invention discloses the preparation method of zinc oxide/carbon composite and the application on lithium ion battery, including step：1) it is (3~17) to weigh mass ratio：1 carbon source and zinc source, the addition zinc source into appropriate amount of deionized water, wiring solution-forming, then carbon source is added into above solution, stirring obtains white powder to white gum thing is formed after freeze-drying；2) white powder for obtaining step 1) is moved in vacuum tube furnace, under inert gas shielding at a temperature of 400~950 DEG C, after calcining 3 20h; cool to room temperature with the furnace; black powder, through repeatedly washing, separating-purifying, it is final it is freeze-dried after target product.Zinc oxide/carbon composite is prepared using the inventive method, raw material used is common, prepares simply, and products obtained therefrom impurity is few, and specific surface area is big, even aperture distribution, is easy to large-scale industrial production；It shows good chemical property as lithium ion battery negative material.
Description
Technical field
Application the present invention relates to the preparation method of zinc oxide/carbon composite and on lithium ion battery, belong to lithium from
Sub- cell negative electrode material technical field.
Background technology
Lithium ion battery is wide because having the performances such as voltage is high, self-discharge rate is low, small volume, in light weight, memory-less effect
It is general to be applied in portable electronics and electric automobile.But negative material is nearly all used by current commercial Li-ion battery
It is graphite material, but the theoretical capacity of graphite only has 370 MAhs/g, it is difficult to meet that growing great-power electronic is set
The standby and long range of electric automobile traveling demand, and the electrode potential of carbon and the current potential of lithium are very close to golden when over-charging of battery
Category lithium may separate out in carbon electrodes, form dendrite and trigger safety problem.
As transition metal oxide, zinc oxide is a kind of conventional chemical addition agent, is widely used in plastics, silicon
In the making of the products such as hydrochlorate product, synthetic rubber, lubricating oil, paint, ointment.Its theoretical capacity is up to 978 milliamperes
When/gram `, there is high chemical stability and environment friendly, make it be expected to be used as lithium ion battery negative material.But aoxidize
Zinc can form ZnLi alloys in charge and discharge process, cause serious bulk effect, make its capacity rapid attenuation.
Porous carbon is a kind of carbon material with uniform developed pore structure, has larger specific surface area, good conduction
Property and structural stability.By coating zinc oxide particle, it can not only improve zinc oxide electric conductivity, improve its volumetric expansion effect
Should, while carbon material also has good storage lithium ability, therefore the cyclical stability of zinc oxide material can greatly be improved, have
There is good application prospect.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of preparation method of zinc oxide/carbon composite,
Raw material used is common, and preparation process is simple and controllability is high.Present invention also offers the zinc oxide/carbon composite lithium from
Application on sub- battery.
To achieve these goals, the preparation method for zinc oxide/carbon composite that the present invention uses, including following step
Suddenly：
1) it is (3~17) to weigh mass ratio：1 carbon source and zinc source, zinc source is added into appropriate amount of deionized water, is made into molten
Liquid, then carbon source is added into above solution, stirring obtains white powder to white gum thing is formed after freeze-drying；
2) white powder for obtaining step 1) is moved in vacuum tube furnace, in 400~950 DEG C under inert gas shielding
At a temperature of, after calcining 3-20h, cool to room temperature with the furnace, obtain black powder, it is final chilled through repeatedly washing, separating-purifying
Target product is obtained after drying.
As an improvement, the zinc source is divalent zinc salt, selected from white vitriol, anhydrous zinc chloride, zinc nitrate hexahydrate or water
Close any of zinc acetate.
As an improvement, the carbon source uses high water soluble polymer, selected from Sodium Polyacrylate, polyacrylic acid potassium, poly- third
Any of olefin(e) acid.
As an improvement, separating-purifying in the step 2) is filtered using centrifugation or Buchner funnel, then with deionized water or
Absolute ethyl alcohol washs repeatedly.
Present invention also offers application of the above-mentioned zinc oxide/carbon composite on lithium ion battery, specifically include following
Step：
1) in mass ratio it is X:(9-X):1 ratio weighs zinc oxide/carbon composite, carbon black and polyvinylidene fluoride respectively
Alkene, Kynoar is added in 1-METHYLPYRROLIDONE solution be made into concentration be 5% binder solution, by 120min~
200min magnetic agitations, obtain colourless transparent solution；
2) zinc oxide/carbon composite and carbon black are mixed again, after 60~180min of mechanical ball mill, adds the nothing of step 1)
Color clear solution, continue 60~180min of ball milling, obtain pasty mixture；
3) step 2) is made into pasty mixture to be uniformly coated on clean electrode slice copper foil；
4) after electrode slice made from dries 4-5h at 50~70 DEG C, obtained disk is cut, and suppressed with powder compressing machine
Afterwards, 6~20h is dried in 110~130 DEG C of vacuum drying ovens, is moved into standby in glove box.
As an improvement, 5≤X≤7 in the step 1).
Compared with prior art, the beneficial effects of the invention are as follows：
1) zinc oxide/carbon composite has been prepared using the inventive method, raw material used is common, prepares simply, and
Products obtained therefrom impurity is few, and specific surface area is big, even aperture distribution, is easy to large-scale industrial production.
2) using the zinc oxide/carbon composite porous material as lithium ion battery negative material, good electrification is shown
Learn performance.Both overcome commercialization high-capacity lithium ion cell with traditional carbon negative pole material specific capacity it is low the shortcomings that, but also with
The excellent cycling stability that conventional transition metal oxide negative material does not possess, exploitation new type lithium ion battery is provided newly
Thinking.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction figure that zinc oxide/carbon composite is made in the embodiment of the present invention 1, wherein ordinate
For relative intensity (Intensity), abscissa is angle of diffraction (2 θ)；
Fig. 2 is the electron scanning micrograph that zinc oxide/carbon composite is made in the embodiment of the present invention 1；
Fig. 3 is the charge and discharge cycles figure that zinc oxide/carbon composite is made in the embodiment of the present invention 1.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, below by drawings and Examples, to this
Invention is further elaborated.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention,
The scope being not intended to limit the invention.
Unless otherwise defined, all technical terms and scientific terminology used herein are led with belonging to the technology of the present invention
The implication that the technical staff in domain is generally understood that is identical, and used term is intended merely to retouch in the description of the invention herein
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) it is (3~17) to weigh mass ratio：1 carbon source and zinc source, zinc source is added into appropriate amount of deionized water, is made into molten
Liquid, then carbon source is added into above solution, stirring obtains white powder to white gum thing is formed after freeze-drying；
2) white powder for obtaining step 1) is moved in vacuum tube furnace, in 400~950 DEG C under inert gas shielding
At a temperature of, after calcining 3-20h, cool to room temperature with the furnace, obtain black powder, it is final chilled through repeatedly washing, separating-purifying
Target product is obtained after drying.
As an improvement, the zinc source is divalent zinc salt, selected from white vitriol (ZnSO4·7H2O), anhydrous zinc chloride
(ZnCl2), zinc nitrate hexahydrate (Zn (NO3)2·6(H2)) or acetate hydrate zinc ((CH O3COO)2Zn·2H2Any of O).
As an improvement, the carbon source uses high water soluble polymer, selected from Sodium Polyacrylate, polyacrylic acid potassium, poly- third
Any of olefin(e) acid.
As an improvement, separating-purifying in the step 2) is filtered using centrifugation or Buchner funnel, then with deionized water or
Absolute ethyl alcohol washs repeatedly.
Present invention also offers application of the above-mentioned zinc oxide/carbon composite on lithium ion battery, specifically include following
Step：
1) in mass ratio it is X:(9-X):1 ratio weighs zinc oxide/carbon composite, carbon black and polyvinylidene fluoride respectively
Alkene, Kynoar is added in 1-METHYLPYRROLIDONE solution be made into concentration be 5% binder solution, by 120min~
200min magnetic agitations, obtain colourless transparent solution；
2) zinc oxide/carbon composite and carbon black are mixed again, after 60~180min of mechanical ball mill, adds the nothing of step 1)
Color clear solution, continue 60~180min of ball milling, obtain pasty mixture；
3) step 2) is made into pasty mixture to be uniformly coated on clean electrode slice copper foil；
4) after electrode slice made from dries 4-5h at 50~70 DEG C, obtained disk is cut, and suppressed with powder compressing machine
Afterwards, 6~20h is dried in 110~130 DEG C of vacuum drying ovens, is moved into standby in glove box.
As an improvement, 5≤X≤7 in the step 1).
Embodiment 1
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) 3g white vitriols (ZnSO is slowly added in 5ml deionized waters4·7H2O), solution is configured to, then in solution
Middle addition 20g high water soluble polymer poly PAAs, are during which stirred continuously, while add 300ml deionizations with glass bar
Water, suspension is constantly expanded, ultimately form white gum thing, product through vacuum freeze drying (vacuum is 40~
60Pa, temperature -61~-55 DEG C) take out after 12h, by constantly grinding, obtain white powder；
2) powdered product of step 1) is put into vacuum tube furnace, 5h is incubated in 850 DEG C under atmosphere of inert gases protection
Afterwards, cool to normal temperature with the furnace, and filtered with Buchner funnel, wash to obtain black powder repeatedly with deionized water and absolute ethyl alcohol,
Carry out freeze-drying process and can obtain target product.
Product is made through Bruker D8ADVANCE x-ray powder diffraction instruments with Cu K alpha ray (wavelength
Scanning leg speed is 0.08 °/sec) hexagonal wurtzite structure zinc oxide (such as Fig. 1) is accredited as, with JCPDS card standard values No.89-
0511 matches, and the porous carbon in material exists with amorphous forms, and no other impurities peak occurs.
Using the pattern of JSF-6700 scanning electron microscopic observations zinc oxide/carbon composite, as shown in Fig. 2 zinc oxide/carbon is multiple
Condensation material is mainly made up of nanoporous of the size distribution in 200nm or so.
Electrochemical property test：
1) it is 7 in mass ratio：2：1 ratio weighs zinc oxide/carbon composite, carbon black and Kynoar respectively, first
Kynoar is added in 1-METHYLPYRROLIDONE solution and is made into the binder solution that concentration is 5%, is stirred by 120min magnetic force
Mix, obtain colourless transparent solution；
2) zinc oxide/carbon composite and carbon black are mixed again, after mechanical ball mill 120min, adds the colourless of step 1)
Bright solution, continue ball milling 120min, obtain pasty mixture；
3) step 2) is made into pasty mixture to be uniformly coated on clean electrode slice copper foil；
4) after electrode slice made from dries 4h at 60 DEG C, obtained disk is cut.It is uniform in order to preferably improve electrode slice
Property and intensifier electrode material to the adhesive force of copper foil, after powder compressing machine compacting, moved in vacuum drying oven after 120 DEG C of dry 6h
Enter standby in glove box；In the environment full of argon gas, electrode slice, barrier film and lithium piece are assembled into button cell in conventional manner
And carry out constant current charge-discharge capacity and cycle performance test.Its chemical property is as shown in Figure 3.
Embodiment 2
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) 3g acetate hydrate zinc ((CH is slowly added in 5ml deionized waters3COO)2Zn·2H2O), solution is configured to, then
10g high water soluble polymer poly potassium acrylates are added in the solution, are during which stirred continuously with glass bar, while add 150ml
Deionized water, suspension is constantly expanded, ultimately form white gum thing, (vacuum is product through vacuum freeze drying
40~60Pa, temperature -61~-55 DEG C) take out after 12h, by constantly grinding, obtain white powder；
2) powdered product of step 1) is put into vacuum tube furnace, 5h is incubated in 650 DEG C under atmosphere of inert gases protection
Afterwards, cool to normal temperature with the furnace, and filtered with Buchner funnel, wash to obtain black powder repeatedly with deionized water and absolute ethyl alcohol,
Carry out freeze-drying process and can obtain target product.
Gained superfine powder is hexagonal wurtzite structure zinc oxide (JCPDS No.89-0511), zinc oxide/carbon composite
Mainly it is made up of nanoporous of the size distribution in 200nm or so.
Embodiment 3
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) 3g white vitriols (ZnSO is slowly added in 5ml deionized waters4·7H2O), solution is configured to, then in solution
Middle addition 15g high water soluble polymer poly acrylic acid, is during which stirred continuously with glass bar, while adds 230ml deionized waters,
Suspension is constantly expanded, ultimately form white gum thing, product through vacuum freeze drying (vacuum is 40~60Pa,
Temperature -61~-55 DEG C) take out after 12h, by constantly grinding, obtain white powder；
2) powdered product of step 1) is put into vacuum tube furnace, 3h is incubated in 650 DEG C under atmosphere of inert gases protection
Follow-up 850 DEG C of insulation 3h of temperature of continuing rising, cool to normal temperature with the furnace, and are filtered with Buchner funnel, anti-with deionized water and absolute ethyl alcohol
After backwashing washs to obtain black powder, carries out freeze-drying process and can obtain target product.
Gained superfine powder is hexagonal wurtzite structure zinc oxide (JCPDS No.89-0511), zinc oxide/carbon composite
Mainly it is made up of nanoporous of the size distribution in 200nm or so.
Embodiment 4
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) 2g white vitriols (ZnSO is slowly added in 5ml deionized waters4·7H2O), solution is configured to, then in solution
Middle addition 17g high water soluble polymer poly PAAs, are during which stirred continuously, while add 250ml deionizations with glass bar
Water, suspension is constantly expanded, ultimately form white gum thing, product through vacuum freeze drying (vacuum is 40~
60Pa, temperature -61~-55 DEG C) take out after 12h, by constantly grinding, obtain white powder；
2) powdered product of step 1) is put into vacuum tube furnace, 5h is incubated in 550 DEG C under atmosphere of inert gases protection
Afterwards, cool to normal temperature with the furnace, and filtered with Buchner funnel, wash to obtain black powder repeatedly with deionized water and absolute ethyl alcohol,
Carry out freeze-drying process and can obtain target product.
Gained superfine powder is hexagonal wurtzite structure zinc oxide (JCPDS No.89-0511), zinc oxide/carbon composite
Mainly it is made up of nanoporous of the size distribution in 200nm or so.
Embodiment 5
A kind of preparation method of zinc oxide/carbon composite, comprises the following steps：
1) 4g zinc nitrate hexahydrates (Zn (NO are slowly added in 5ml deionized waters3)2·6(H2O)), solution is configured to, then
17g high water soluble polymer poly PAAs are added in the solution, are during which stirred continuously with glass bar, while add 270ml
Deionized water, suspension is constantly expanded, ultimately form white gum thing, (vacuum is product through vacuum freeze drying
40~60Pa, temperature -61~-55 DEG C) take out after 12h, by constantly grinding, obtain white powder；
2) powdered product of step 1) is put into vacuum tube furnace, 3h is incubated in 800 DEG C under atmosphere of inert gases protection
Afterwards, cool to normal temperature with the furnace, and filtered with Buchner funnel, wash to obtain black powder repeatedly with deionized water and absolute ethyl alcohol,
Carry out freeze-drying process and can obtain target product.
Gained superfine powder is hexagonal wurtzite structure zinc oxide (JCPDS No.89-0511), zinc oxide/carbon composite
Mainly it is made up of nanoporous of the size distribution in 200nm or so.
Electrical performance testing：
1) it is 7 in mass ratio：2：1 ratio weighs zinc oxide/carbon composite, carbon black and Kynoar respectively, will
Kynoar adds in 1-METHYLPYRROLIDONE solution the binder solution for being made into that concentration is 5%, is stirred by 200min magnetic force
Mix, obtain colourless transparent solution；
2) zinc oxide/carbon composite and carbon black are mixed again, after mechanical ball mill 180min, adds the colourless of step 1)
Bright solution, continue ball milling 60min, obtain pasty mixture；
3) step 2) is made into pasty mixture to be uniformly coated on clean electrode slice copper foil；
4) after electrode slice made from dries 5h at 50 DEG C, obtained disk is cut, and after being suppressed with powder compressing machine,
20h is dried in 110 DEG C of vacuum drying ovens, is moved into standby in glove box.
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
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
1. the preparation method of zinc oxide/carbon composite, it is characterised in that comprise the following steps：
1) it is (3~17) to weigh mass ratio：1 carbon source and zinc source, the addition zinc source into appropriate amount of deionized water, wiring solution-forming, then
Carbon source is added into above solution, stirring obtains white powder to white gum thing is formed after freeze-drying；
2) white powder for obtaining step 1) is moved in vacuum tube furnace, in 400~950 DEG C of temperature under inert gas shielding
Under degree, after calcining 3-20h, cool to room temperature with the furnace, obtain black powder, it is final freeze-dried through repeatedly washing, separating-purifying
Target product is obtained afterwards.
2. the preparation method of zinc oxide/carbon composite according to claim 1, it is characterised in that the zinc source is two
Valency zinc salt, selected from any of white vitriol, anhydrous zinc chloride, zinc nitrate hexahydrate or acetate hydrate zinc.
3. the preparation method of zinc oxide/carbon composite according to claim 1, it is characterised in that the carbon source uses
High water soluble polymer, selected from any of Sodium Polyacrylate, polyacrylic acid potassium, polyacrylic acid.
4. the preparation method of zinc oxide/carbon composite according to claim 1, it is characterised in that in the step 2)
Separating-purifying filtered using centrifugation or Buchner funnel, then washed repeatedly with deionized water or absolute ethyl alcohol.
5. zinc oxide/carbon composite is made on lithium ion battery according to any one of the claim 1-4 preparation methods
Using, it is characterised in that specifically include following steps：
1) in mass ratio it is X:(9-X):1 ratio weighs zinc oxide/carbon composite, carbon black and Kynoar respectively, will
Kynoar adds to 1-METHYLPYRROLIDONE solution and is made into the binder solution that concentration is 5%, by 120min~200min
Magnetic agitation, obtain colourless transparent solution；
2) zinc oxide/carbon composite and carbon black are mixed again, after 60~180min of mechanical ball mill, adds the colourless of step 1)
Bright solution, continue 60~180min of ball milling, obtain pasty mixture；
3) step 2) is made into pasty mixture to be uniformly coated on clean electrode slice copper foil；
4) after electrode slice made from dries 4-5h at 50~70 DEG C, obtained disk is cut, and after being suppressed with powder compressing machine,
6~20h is dried in 110~130 DEG C of vacuum drying ovens, is moved into standby in glove box.
6. application of the zinc oxide/carbon composite on lithium ion battery according to claim 5, it is characterised in that described
5≤X≤7 in step 1).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111554905A (en) * | 2020-05-14 | 2020-08-18 | 云南民族大学 | Preparation method, product and application of zinc oxide-based carbon composite nano material |
| CN112439371A (en) * | 2019-08-31 | 2021-03-05 | 北京化工大学 | Preparation method of submicron copper oxide-polymer carbon skeleton material with core-shell structure |
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| CN107240694A (en) * | 2017-07-05 | 2017-10-10 | 中国矿业大学 | A kind of composite porous method for preparing sodium-ion battery for negative pole of zinc oxide/carbon |
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| CN112439371A (en) * | 2019-08-31 | 2021-03-05 | 北京化工大学 | Preparation method of submicron copper oxide-polymer carbon skeleton material with core-shell structure |
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| CN111554905B (en) * | 2020-05-14 | 2020-12-29 | 云南民族大学 | Preparation method, product and application of zinc oxide-based carbon composite nano material |
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Denomination of invention: Preparation method of zinc oxide/carbon composite material and application in lithium ion battery Effective date of registration: 20220830 Granted publication date: 20200612 Pledgee: Bank of Nanjing Co.,Ltd. Xuzhou Branch Pledgor: JIANGSU FREY BATTERY TECHNOLOGY CO.,LTD. Registration number: Y2022980014175 |