CN109301233A - A kind of the porous carbon anode and preparation method of water system Zinc ion battery - Google Patents
A kind of the porous carbon anode and preparation method of water system Zinc ion battery Download PDFInfo
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- CN109301233A CN109301233A CN201811186457.0A CN201811186457A CN109301233A CN 109301233 A CN109301233 A CN 109301233A CN 201811186457 A CN201811186457 A CN 201811186457A CN 109301233 A CN109301233 A CN 109301233A
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/42—Alloys based on zinc
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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Abstract
The invention discloses a kind of porous carbon of water system Zinc ion battery anode and preparation methods, first, dried lychee exocarp is placed in tube furnace, roasting is carbonized 3 ~ 4 hours in advance to 250 ~ 300 DEG C, obtains the lychee exocarp of pre- carbonization, and then carbonization lychee exocarp and activator will be scattered in deionized water according to certain mass ratio in advance, it is then placed into tube furnace, roasting keeps the temperature 3 ~ 4 hours, obtains porous carbon materials to 500 ~ 850 DEG C.Method is relatively easy in this preparation process, low production cost, abundant raw material, and material has more micropore, and obtained porosity positive electrode has good chemical property, and the Zinc ion battery assembled has a good application prospect.
Description
Technical field
The invention belongs to battery technology fields, the specially preparation method of water system zinc ion secondary battery positive electrode material.
Background technique
Zinc ion battery has the characteristics that at low cost, highly-safe, environmental-friendly, it is considered to be substitution lithium ion battery is made
It is preferably selected for electrical source of power.Research in relation to zinc battery positive electrode is relatively fewer, and its positive electrode is optional remaining
Ground is smaller, therefore positive electrode is the critical issue for restricting Zinc ion battery development.Porous carbon has large specific surface area, electric conductivity
Good, the advantages that chemical stability is high, in recent years because gas separation, Water warfare, battery, supercapacitor and in terms of
Extensive use and receive much attention.If preparing carbon material using biomass, as agricultural wastes, wood type raw material, bamboo class are planted
The renewable resources such as object and lignin make carbon source, not only its abundance, but also meet circular economy and sustainable development
National policy.Recently, researcher uses in N2 800 DEG C of directly thermal decomposition acetate fibers usually prepare porous carbon in atmosphere
(Chemistry Materials, 2002,14:2940-2945.).Sun Li uses chemical impregnation oxy-carbo method with pine
Wood saw end is the nanometer porous carbon that raw material is prepared for N doping, and specific surface area and Kong Rong respectively reach 2153m2/ g and
1.37cm3/ g(Ph.D. Dissertation, Dalian University of Technology, 2013.).Kurosaki etc. has been obtained more by sharply heating sawdust
The porous carbon of layer hierarchical structure, specific surface area 372m2/ g(Carbon, 2008,46 (6): 850-857).As it can be seen that sharp
Porous carbon materials, cheap and easy to get and function admirable are prepared with biomass, while realizing the cycling and reutilization and carbon of waste
The sustainable development of material, therefore there is extensive Prospect of R & D.
Summary of the invention
Object of the present invention is to mix according to a certain percentage after lychee exocarp is carbonized in advance with activating agent, finally activation is obtained porous
Carbon material.The chemical property of Zinc ion battery positive electrode is improved using the porous performance of porous carbon.This method raw material reserves
Abundant, renewable, cheap, environmental sound, preparation process is relatively easy, and prepared porosity positive electrode has good
Stability and chemical property.
To achieve the purpose of the present invention, the following technical schemes are provided:
(1) lychee exocarp and a certain amount of deionized water are washed 1 ~ 2 hour under ultrasonic wave effect, then in 80 ~ 90 DEG C of vacuum
It is 10 ~ 18 hours dry in baking oven；
(2) it takes lychee exocarp dried in step (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere,
250 ~ 300 DEG C are warming up to 2 ~ 3 DEG C/min of rates, keeps the temperature 3 hours, cooled to room temperature, grinding is uniformly；
(3) by the pre- carbonization lychee exocarp powder of gained in step (2) and KOH, NaOH or ZnCl21:0 ~ 5 in mass ratio are added to one
In quantitative deionized water, disperse 1 ~ 2 hour under the action of ultrasonic wave, the forced air drying by gained mixture at 45 ~ 60 DEG C
It is 12 ~ 16 hours dry in case；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, with 5 ~ 10 DEG C/minute
Clock rate rate is warming up to 500 ~ 850 DEG C, keeps the temperature 3 ~ 4 hours, cooled to room temperature, and it is uniform will to obtain black solid grinding；
(5) it takes porous carbon materials, conductive agent and binder in above-mentioned steps (4) to mix according to mass ratio 8:1:1, and is added dropwise suitable
Mixed slurry is coated on stainless steel foil by amount N-Methyl pyrrolidone after ball mill ball milling 4 hours, at 110 ~ 120 DEG C
Vacuum drying 10 ~ 12 hours, obtains positive electrode.
Further, pre- carburizing temperature is 300 DEG C in step (2) according to claim 1, and the time is 3 hours.
Further, be carbonized in step (3) lychee exocarp powder and KOH, NaOH or ZnCl in advance according to claim 12
Optimum quality ratio 1:4.
Further, activation temperature is 800 DEG C in step (3) according to claim 1, and the time is 3 hours.
Further, conductive agent is acetylene black, conductive carbon black, graphene or carbon in step (5) according to claim 1
At least one of nanotube.
Further, binder is Vingon, acrylonitrile multi-component copolymer in step (5) according to claim 1
One of object or butadiene-styrene rubber.
The features of the present invention
This method preparation process is simple, low raw-material cost, pollution-free, and the electrode obtained material specific surface area is big, good conductivity.
Specific embodiment
Embodiment 1:
(1) lychee exocarp is cleaned up, takes the lower washing 1 of ultrasonic wave effect at room temperature of the deionized water of 3g lychee exocarp and 500ml
Hour, then it is dried in vacuo 12 hours at 80 DEG C；
(2) it takes the dried lychee exocarp in above-mentioned steps (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar
Atmosphere, 300 DEG C, keep the temperature 3 hours, heating rate be 3 DEG C/min, take out crucible, obtained black solid using mortar grinder at
Powder；
(3) by pre- carbonization lychee exocarp powder obtained by step (2) and KOH by pre- carbonization lychee exocarp: the mass ratio 1:3 of KOH is added to
In the deionized water of 10ml, washed 1 hour under the action of ultrasonic wave, gained mixture is dry with 45 DEG C in air dry oven
Dry 12 hours；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, 800 DEG C, heat preservation 3
Hour, heating rate is 5 DEG C/min, takes out crucible, obtained black solid is ground uniform；
(5) porous carbon materials 0.16g, acetylene black 0.02g and the Kynoar 0.02g in above-mentioned steps (4) are taken, is added dropwise appropriate
Mixed slurry is coated on stainless steel foil by N-Methyl pyrrolidone after ball mill grinding 4 hours, is dried in vacuo at 110 DEG C
10 hours, obtain positive electrode.
Embodiment 2:
(1) lychee exocarp is cleaned up, takes the lower washing 1 of ultrasonic wave effect at room temperature of the deionized water of 3g lychee exocarp and 500ml
Hour, then it is dried in vacuo 12 hours at 80 DEG C；
(2) it takes the dried lychee exocarp in above-mentioned steps (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar
Atmosphere, 300 DEG C, keep the temperature 3 hours, heating rate be 3 DEG C/min, take out crucible, obtained black solid using mortar grinder at
Powder；
(3) by pre- carbonization lychee exocarp powder obtained by step (2) and NaOH by pre- carbonization lychee exocarp: the mass ratio 1:4 of NaOH adds
Enter into the deionized water of 10ml, is washed 1 hour under the action of ultrasonic wave, by gained mixture with 45 in air dry oven
DEG C dry 12 hours；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, 800 DEG C, heat preservation 3
Hour, heating rate is 5 DEG C/min, takes out crucible, and it is uniform will to obtain black solid grinding；
(5) porous carbon materials 0.24g, conductive carbon black 0.03g and the acrylonitrile-methylacrylate in above-mentioned steps (4) are taken
Appropriate N-Methyl pyrrolidone is added dropwise in 0.03g, and after ball mill grinding 4 hours, mixed slurry is coated on stainless steel foil,
It is dried in vacuo 12 hours at 110 DEG C, obtains positive electrode.
Embodiment 3:
(1) lychee exocarp is cleaned up, takes the lower washing 1 of ultrasonic wave effect at room temperature of the deionized water of 3g lychee exocarp and 500ml
Hour, then it is dried in vacuo 12 hours at 80 DEG C；
(2) it takes the dried lychee exocarp in above-mentioned steps (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar
Atmosphere, 300 DEG C, keep the temperature 3 hours, heating rate be 3 DEG C/min, take out crucible, obtained black solid using mortar grinder at
Powder；
(3) by pre- carbonization lychee exocarp powder and ZnCl obtained by step (2)2By pre- carbonization lychee exocarp: ZnCl2Mass ratio 1:5,
Be added in the deionized water of 10ml, washed 1 hour under the action of ultrasonic wave, by gained mixture in air dry oven with
45 DEG C drying 12 hours；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, 800 DEG C, heat preservation 3
Hour, heating rate is 5 DEG C/min, takes out crucible, and it is uniform will to obtain black solid grinding；
(5) porous carbon materials 0.184g, graphene 0.023g and the butadiene-styrene rubber 0.023g in above-mentioned steps (4) are taken, is added dropwise suitable
Mixed slurry is coated on stainless steel foil by amount N-Methyl pyrrolidone after ball mill grinding 4 hours, and vacuum is dry at 110 DEG C
Dry 12 hours, obtain positive electrode.
Embodiment 4:
(1) lychee exocarp is cleaned up, takes the lower washing 1 of ultrasonic wave effect at room temperature of the deionized water of 3g lychee exocarp and 500ml
Hour, then it is dried in vacuo 12 hours at 80 DEG C；
(2) it takes the dried lychee exocarp in above-mentioned steps (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar
Atmosphere, 300 DEG C, keep the temperature 3 hours, heating rate be 3 DEG C/min, take out crucible, obtained black solid using mortar grinder at
Powder；
(3) by pre- carbonization lychee exocarp powder obtained by step (2) and KOH by pre- carbonization lychee exocarp: the mass ratio 1:4 of KOH is added to
In the deionized water of 10ml, washed 1 hour under the action of ultrasonic wave, gained mixture is dry with 45 DEG C in air dry oven
Dry 14 hours；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, 650 DEG C, heat preservation 3
Hour, heating rate is 5 DEG C/min, takes out crucible, and it is uniform will to obtain black solid grinding；
(5) porous carbon materials 0.24g, carbon nanotube 0.03g and the Kynoar 0.03g in above-mentioned steps (4) are taken, is added dropwise suitable
Mixed slurry is coated on stainless steel foil by amount N-Methyl pyrrolidone after ball mill grinding 4 hours, and vacuum is dry at 110 DEG C
Dry 12 hours, obtain positive electrode.
Embodiment 5:
(1) lychee exocarp is cleaned up, taking the deionized water of 3.05g and 500ml, the lower washing 2 of ultrasonic wave effect is small at room temperature
When, then it is dried in vacuo 12 hours at 80 DEG C；
(2) it takes the dried lychee exocarp in above-mentioned steps (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar
Atmosphere, 300 DEG C, keep the temperature 3 hours, heating rate be 3 DEG C/min, take out crucible, obtained black solid using mortar grinder at
Powder；
(3) by pre- carbonization lychee exocarp powder and ZnCl obtained by step (2)2By pre- carbonization lychee exocarp: ZnCl2Mass ratio 1:4,
It is added in the deionized water of 10ml, is washed 1 hour under the action of ultrasonic wave, by gained mixture with 45 in air dry oven
It is DEG C sufficiently dry；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, 700 DEG C, heat preservation 3
Hour, heating rate is 5 DEG C/min, takes out crucible, and it is uniform will to obtain black solid grinding；
(5) porous carbon materials 0.24g, acetylene black 0.03g and the Kynoar 0.03g in above-mentioned steps (4) are taken, is added dropwise appropriate
Mixed slurry is coated on stainless steel foil by N-Methyl pyrrolidone after ball mill grinding 4 hours, is dried in vacuo at 110 DEG C
12 hours, obtain positive electrode.
Claims (7)
1. the porous carbon anode and preparation method of a kind of water system Zinc ion battery, which comprises the steps of:
(1) lychee exocarp is washed 1 ~ 2 hour under ultrasonic wave effect with a certain amount of deionized water, then in 80 ~ 90 DEG C of vacuum
It is 12 ~ 18 hours dry in baking oven；
(2) it takes lychee exocarp dried in step (1) to be placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere,
250 ~ 350 DEG C are warming up to 2 ~ 3 DEG C/min of rates, keeps the temperature 2 ~ 4 hours, cooled to room temperature, grinding is uniformly；
(3) by the pre- carbonization lychee exocarp powder of gained in step (2) and activator 1:0 ~ 5 in mass ratio, it is added to a certain amount of go
In ionized water, disperse 1 ~ 2 hour under the action of ultrasonic wave, gained mixture is dry in 45 ~ 60 DEG C of air dry oven
12 ~ 16 hours；
(4) step (3) mixture is placed in crucible, is roasted using tube furnace, condition are as follows: Ar atmosphere, with 5 ~ 10 DEG C/minute
Clock rate rate is warming up to 600 ~ 850 DEG C, keeps the temperature 3 ~ 4 hours, cooled to room temperature, and it is uniform will to obtain black solid grinding；
(5) it takes porous carbon materials, conductive agent and binder in above-mentioned steps (4) to mix according to mass ratio 8:1:1, and is added dropwise suitable
Mixed slurry is coated on stainless steel foil by amount N-Methyl pyrrolidone after ball mill ball milling 4 hours, at 100 ~ 120 DEG C
Vacuum drying 10 ~ 12 hours, obtains positive electrode.
2. the porous carbon anode and preparation method of a kind of water system Zinc ion battery according to claim 1, it is characterised in that institute
Stating pre- carburizing temperature in step (2) is 300 DEG C, and the time is 3 hours.
3. a kind of porous carbon anode of water system Zinc ion battery and preparation method are it is characterized in that described according to claim 1
Activator is KOH, NaOH or ZnCl in step (3)2At least one of.
4. a kind of porous carbon anode of water system Zinc ion battery and preparation method are it is characterized in that described according to claim 1
Be carbonized lychee exocarp powder and KOH, NaOH or ZnCl in advance in step (3)2Optimum quality ratio 1:4.
5. a kind of porous carbon anode of water system Zinc ion battery and preparation method are it is characterized in that described according to claim 1
Activation temperature is 800 DEG C in step (4), and the time is 3 hours.
6. the porous carbon anode and preparation method of a kind of water system Zinc ion battery according to claim 1, it is characterised in that institute
Stating conductive agent in step (5) is at least one of acetylene black, conductive carbon black, graphene or carbon nanotube.
7. the porous carbon anode and preparation method of a kind of water system Zinc ion battery according to claim 1, it is characterised in that institute
Stating binder in step (5) is one of Vingon, acrylonitrile multiple copolymer or butadiene-styrene rubber.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111384424A (en) * | 2019-11-05 | 2020-07-07 | 郑州大学 | Lignin-based complex electrolyte for aqueous zinc-ion battery and aqueous zinc-ion battery based on same |
| CN112017871A (en) * | 2020-08-31 | 2020-12-01 | 深圳职业技术学院 | Composite electrode material and preparation method and application thereof |
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| CN104157852A (en) * | 2014-07-18 | 2014-11-19 | 南京大学 | Sulfur positive electrode of lithium sulfur battery and preparation method |
| CN107188171A (en) * | 2017-06-21 | 2017-09-22 | 武汉工程大学 | Porous carbon materials and its preparation method and the porous carbon-based electrode material for ultracapacitor prepared using the porous carbon materials |
| CN107681230A (en) * | 2017-08-18 | 2018-02-09 | 中国科学院合肥物质科学研究院 | A kind of zinc-air battery and its application |
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2018
- 2018-10-12 CN CN201811186457.0A patent/CN109301233A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104157852A (en) * | 2014-07-18 | 2014-11-19 | 南京大学 | Sulfur positive electrode of lithium sulfur battery and preparation method |
| CN107188171A (en) * | 2017-06-21 | 2017-09-22 | 武汉工程大学 | Porous carbon materials and its preparation method and the porous carbon-based electrode material for ultracapacitor prepared using the porous carbon materials |
| CN107681230A (en) * | 2017-08-18 | 2018-02-09 | 中国科学院合肥物质科学研究院 | A kind of zinc-air battery and its application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111384424A (en) * | 2019-11-05 | 2020-07-07 | 郑州大学 | Lignin-based complex electrolyte for aqueous zinc-ion battery and aqueous zinc-ion battery based on same |
| CN112017871A (en) * | 2020-08-31 | 2020-12-01 | 深圳职业技术学院 | Composite electrode material and preparation method and application thereof |
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Application publication date: 20190201 |