CN107706405A - A kind of method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano - Google Patents
A kind of method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano Download PDFInfo
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- CN107706405A CN107706405A CN201711178903.9A CN201711178903A CN107706405A CN 107706405 A CN107706405 A CN 107706405A CN 201711178903 A CN201711178903 A CN 201711178903A CN 107706405 A CN107706405 A CN 107706405A
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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
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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 method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano, the manganese dioxide of nano bar-shape is prepared first, then by manganese dioxide, nitrogenous or nitrogen element sulphur conductive high polymer monomer, emulsifying agent is well mixed according to certain ratio, it is then transferred to 12~24h of mechanical agitation in cryostat, wash drying, and then 2~6h is calcined in 200 DEG C~500 DEG C inert gas shielding atmosphere, obtain nitrogen or the bar-shaped composite of nitrogen sulfur doping carbon coating manganese dioxide composite Nano, finally by composite coated into positive electrode.Nitrogen or nitrogen sulfur doping carbon coating manganese dioxide composite material used time prepared by this method are short, yield is high, cost is low and has high electronic conductivity and cycle performance, and its electron transport ability and electrochemistry store up zinc function admirable.
Description
Technical field
The invention belongs to electrochemical field, falls within energy technology field, and in particular to a kind of secondary electricity of water system zinc ion
The preparation method of pond positive electrode.
Background technology
With the increase of environmental pollution, the secondary cell for needing high power and high-energy is used as big to clean energy resource
Type energy storage instrument effectively stores and distributed energy.Secondary water system Zinc ion battery is a kind of new green environment protection being recently proposed
Battery system, using abundant, cheap, less toxic, tractable metallic zinc as negative material, zinc sulfate or zinc acetate it is water-soluble
Liquid can assemble in atmosphere as electrolyte.The emphasis that high performance positive electrode is research is selected, manganese dioxide is because having valency
The advantages of lattice are cheap and environment-friendly is widely used in field of batteries.Xun etc. have studied α-MnO2As secondary water system zinc
The electrochemical properties of ion battery positive electrode, the discharge capacity of zinc-manganese dioxide water system battery first lap is 210 mA h/g
（Angewandte Chemie, 2012,51,933-935）；Alfaruqi etc. uses nano bar-shape α-MnO2As positive pole material
Material, first charge-discharge capacity is 233 mA h/g under 83 mA/g current densities, and macrocyclic coulombic efficiency is close to 100%
（Journal of Power Sources ,2015, 288, 320-327）；The zinc-manganese dioxide water system battery of the preparations such as Pan
Voltage is 1.44V, and capacity is 285 mA h/g (Nature Energy 2016,1,16119)；The preparation such as Zhang β-
MnO2As positive electrode, capacity is 225 mA h/g, and is still kept after the long circulating of 2000 circles with 94% capacity
(Nature Communication 2017, 8, 405).But the electronic conductivity and charge/discharge capacity of manganese dioxide are relatively low, because
This needs to be modified manganese bioxide material, to prepare high performance Zinc ion battery positive electrode.
The content of the invention
The present invention seeks to improved using the good electric conductivity of conducting polymer two in secondary water system Zinc ion battery
Aoxidize the performance of manganese anode material.
This method preparation process is simple, low raw-material cost, specific capacity are higher, green non-pollution, can group in atmosphere
Packed battery and post-processed for old and useless battery simpler, can apply to large-scale energy storage device, and the composite wood being prepared
Expecting the manganese bioxide material than pure phase has higher electrical conductivity and reversible capacity.
To realize the purpose of the present invention, there is provided following technical scheme：
A kind of method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano, its
It is characterised by, comprises the following steps：
（1）By four hydrated manganese sulfates, 0.5mol/L sulfuric acid, deionized water according to mol ratio 3:2000:5000~10000 mixing
Uniformly, liquor potassic permanganate is then added dropwise, forms homogeneous solution, is then transferred into reactor, is placed in 120~150 DEG C of baking
In case, 12~24h of successive reaction, product is obtained.After ethanol and deionized water alternately washing several times, by product 50~
8~12h is dried in vacuo at 100 DEG C and obtains the manganese dioxide of nano bar-shape；
（2）By step（1）Products therefrom is with nitrogenous carbon or nitrogen sulphur carbon monomer according to mol ratio 1:1~20 is dissolved in appropriate solvent
In, appropriate emulsifying agent, 2~24h of stirring are added, forms homogeneous dispersion liquid；
（3）By step（2）In mixed solution be transferred in -10 DEG C~10 DEG C of cryostat device, the molten of initiator is added dropwise
Liquid, stir 24~36h, centrifugation obtain solid matter, wash several times with solvent displacement, at 50~100 DEG C vacuum drying 8~
24h；
（4）Solid matter obtained by step (3) is calcined into 2~6h in 200 DEG C~500 DEG C inert gas shielding atmosphere,
Obtain nitrogen or nitrogen sulfur doping carbon coating manganese dioxide；
（5）Take step（4）In powdery product, acetylene black and Kynoar according to mass ratio 7:2:1, add N- methyl pyrroles
Pyrrolidone, the slurry of stable uniform is formed, after grinding 3~6h, mixed slurry is coated on stainless steel foil, in 80~120 DEG C
10~14h of lower vacuum drying, obtains positive electrode.
Further, the step（2）Middle carbon source monomer is at least one of pyrroles, aniline, thiophene.
Further, the step（2）Middle solvent is at least one of deionized water, chloroform.
Further, the step（2）Middle emulsifying agent is neopelex, ethoxylated dodecyl alcohol carboxylic acid
At least one of sodium, ammonium lauryl sulfate.
Further, the step（3）Middle initiator is at least one of potassium peroxydisulfate, ammonium persulfate, iron chloride.
Further, the step（3）Middle solvent is at least one of deionized water, ethanol, 1mol/L hydrochloric acid.
It is characteristic of the invention that：Preparation process is simple, cost is cheap, yield is higher, electricity of the electrolyte compared with organic electrolyte
Conductance is higher by two orders of magnitude, nonflammable and green non-pollution；Prepare nitrogen or nitrogen sulfur doping carbon coating manganese dioxide composite material
With high electronic conductivity, and with higher electron transport ability and more preferable electrochemistry storage zinc performance.
Embodiment
Following examples are intended to illustrate invention rather than limitation of the invention further.
Embodiment 1：
（1）The hydrated manganese sulfates of 0.507g tetra-, 2ml 0.5mol/L sulfuric acid, 80ml deionized waters are mixed, ultrasonic 10min forms clear
Clear solution, stir 30min, 20ml liquor potassic permanganates be added dropwise, mixed solution is put into 150ml reactor 120 DEG C it is anti-
Answer 12h.Centrifugation obtains brown precipitate, is dried after ethanol and deionized water washing；
（2）Take above-mentioned steps（1）Middle product 0.1218g is dissolved in 50ml deionized waters with 2.5mg neopelexes, is surpassed
Sound 10min forms dispersion liquid, after stirring 2h, adds 40ul pyrroles, stirs 2h, 0.5g potassium peroxydisulfate is dissolved in into 50ml's
In deionized water, 24h is stirred at 0 DEG C in cryostat, solution gradually becomes black.Centrifugation is precipitated, and washing alcohol is washed, and 60 DEG C true
Sky dries 12h, obtains composite；
（3）Take above-mentioned steps（2）In composite using mortar grinder into powder, be placed in crucible, carried out using tube furnace
Roast, condition are：Ar atmosphere is enclosed, 300 DEG C, is incubated 3h, and heating rate is 2 DEG C/min, is taken out crucible, is obtained black solid, be
The manganese dioxide powder of nitrogen-doped carbon cladding；
（4）Take above-mentioned steps（3）In composite 0.14g, acetylene black 0.04g and Kynoar 0.02g, appropriate N- is added dropwise
Methyl pyrrolidone, after ball mill grinding 4h, mixed slurry is coated on stainless steel foil, 10h is dried in vacuo at 110 DEG C,
Obtain positive electrode.
Embodiment 2：
（1）The hydrated manganese sulfates of 0.510g tetra-, 2ml 0.5mol/L sulfuric acid, 80ml deionized waters are mixed, ultrasonic 10min forms clear
Clear solution, stir 30min, 20ml liquor potassic permanganates be added dropwise, mixed solution is put into 150ml reactor 120 DEG C it is anti-
Answer 12h.Centrifugation obtains brown precipitate, is dried after ethanol and deionized water washing；
（2）Take above-mentioned steps（1）Middle product 0.1210g is dissolved in 50ml deionizations with 1.29mg ethoxylated dodecyl alcohol carboxylic acid sodiums
In water, ultrasonic 10min forms dispersion liquid, after stirring 2h, adds 50ul aniline, 2h is stirred, afterwards by 0.52g ammonium persulfate
It is dissolved in 50ml deionized water, the mechanical agitation 24h at 0 DEG C in cryostat, solution gradually becomes black, and centrifugation is sunk
Form sediment, washing alcohol is washed, and 60 DEG C of vacuum drying 12h, obtains composite；
（3）Take above-mentioned steps（2）In composite using mortar grinder into powder, be placed in crucible, carried out using tube furnace
Roast, condition are：Ar atmosphere is enclosed, 300 DEG C, is incubated 3h, and heating rate is 2 DEG C/min, is taken out crucible, is obtained black solid, be
The manganese dioxide powder of nitrogen-doped carbon cladding；
（4）Take above-mentioned steps（3）In composite 0.07g, acetylene black 0.02g and Kynoar 0.01g, appropriate N- is added dropwise
Methyl pyrrolidone, after ball mill grinding 4h, mixed slurry is coated on stainless steel foil, 10h is dried in vacuo at 110 DEG C,
Obtain positive electrode.
Embodiment 3：
（1）The hydrated manganese sulfates of 0.509g tetra-, 2ml 0.5mol/L sulfuric acid, 80ml deionized waters are mixed, ultrasonic 10min forms clear
Clear solution, stir 30min, 20ml liquor potassic permanganates be added dropwise, mixed solution is put into 150ml reactor 120 DEG C it is anti-
Answer 12h.Centrifugation obtains brown precipitate, is dried after ethanol and deionized water washing；
（2）Take above-mentioned steps（1）Middle product 0.1210g is dissolved in 25ml chloroforms with 2.0mg ammonium lauryl sulfates, 60ul thiophene
In, ultrasonic 30min forms dispersion liquid A, meanwhile, 0.3g anhydrous ferric chlorides are added in 25ml chloroforms, and ultrasonic 30min forms scattered
Liquid B, then A dispersion liquids are transferred in 0 DEG C of cryostat, dispersion liquid B is added dropwise, stirred 24h, at room temperature steam solvent after the completion of reaction
It is dry, 1mol/L hydrochloric acid solution washing 24h is poured into, is filtered, 1mol/L hydrochloric acid and deionized water filtering and washing, 80 DEG C of vacuum are done
Dry 24h, obtains composite；
（3）Take above-mentioned steps（2）In composite using mortar grinder into powder, be placed in crucible, carried out using tube furnace
Roast, condition are：Ar atmosphere is enclosed, 300 DEG C, is incubated 3h, and heating rate is 2 DEG C/min, is taken out crucible, is obtained black solid, be
The manganese dioxide powder of nitrogen sulfur doping carbon coating；
（4）Take above-mentioned steps（3）In composite 0.21g, acetylene black 0.06g and Kynoar 0.03g, appropriate N- is added dropwise
Methyl pyrrolidone, after ball mill grinding 4h, mixed slurry is coated on stainless steel foil, 10h is dried in vacuo at 110 DEG C,
Obtain positive electrode.
Claims (7)
1. a kind of method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano,
It is characterised in that it includes following steps：
（1）By four hydrated manganese sulfates, 0.5mol/L sulfuric acid, deionized water according to mol ratio 3:2000:5000~10000 mixing
Uniformly, liquor potassic permanganate is then added dropwise, forms homogeneous solution, is transferred to reactor, is placed in 120~150 DEG C of baking oven,
12~24h of successive reaction, obtains product, with ethanol and deionized water alternately washing several times, by product at 50~100 DEG C it is true
Sky dries 8~12h and obtains the manganese dioxide of nano bar-shape；
（2）By step（1）Products therefrom is with nitrogenous carbon or nitrogen sulphur carbon monomer according to mol ratio 1:1~20 is dissolved in appropriate solvent
In, appropriate emulsifying agent, 2~24h of stirring are added, forms homogeneous dispersion liquid；
（3）By step（2）In mixed solution be transferred in -10 DEG C~10 DEG C of cryostat device, the molten of initiator is added dropwise
Liquid, stirs 24~36h, and centrifugation obtains solid matter, it is washed several times with solvent displacement, 8 are dried in vacuo at 50~100 DEG C
~24h；
（4）Solid matter obtained by step (3) is calcined into 2~6h in 200 DEG C~500 DEG C inert gas shielding atmosphere,
Obtain nitrogen or nitrogen sulfur doping carbon coating manganese dioxide；
（5）Take step（4）In powdery product, acetylene black and Kynoar according to mass ratio 7:2:1, add N- methyl pyrroles
Pyrrolidone, the slurry of stable uniform is formed, after grinding 3~6h, mixed slurry is coated on stainless steel foil, at 80~120 DEG C
10~14h is dried in vacuo, obtains positive electrode.
2. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：The step（2）In nitrogenous carbon or nitrogen sulphur carbon monomer be pyrroles, aniline, thiophene
At least one of.
3. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：The step（2）Middle solvent is at least one of deionized water, chloroform.
4. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：The step（2）Middle emulsifying agent is neopelex, laruyl alcohol gathers
At least one of oxygen vinethene carboxylic acid sodium, ammonium lauryl sulfate.
5. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：Initiator is in potassium peroxydisulfate, ammonium persulfate, iron chloride in the step (3)
At least one.
6. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：Solvent is in deionized water, ethanol, 1mol/L hydrochloric acid in the step (3)
It is at least one.
7. according to claim 1, one kind prepares nitrogen or the bar-shaped zinc ion of nitrogen sulfur doping carbon coating manganese dioxide composite Nano
The method of cell positive material, it is characterised in that：The content of nitrogen or nitrogen sulfur doping is 2~4wt% in the composite.
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Cited By (18)
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|---|---|---|---|---|
| CN108417811A (en) * | 2018-03-26 | 2018-08-17 | 电子科技大学 | A kind of carbon coating club shaped structure ternary ferrimanganic sulfide graphene composite material and its synthetic method |
| CN108539163A (en) * | 2018-04-08 | 2018-09-14 | 齐鲁工业大学 | A kind of preparation method of mesoporous hollow nitrogen-doped carbon nanosphere/manganese dioxide Zinc ion battery positive electrode |
| CN109244479A (en) * | 2018-08-06 | 2019-01-18 | 江苏大学 | Netted nitrogen-doped carbon cladding manganese dioxide carbon cloth electrode and preparation method and application |
| CN109759144A (en) * | 2019-02-21 | 2019-05-17 | 江汉大学 | A kind of preparation method of the polyaniline photochemical catalyst of doped ferric oxide |
| CN109768262A (en) * | 2019-01-25 | 2019-05-17 | 天津理工大学 | A kind of cadmium modified manganese dioxide positive electrode and its preparation method and application |
| CN110148716A (en) * | 2019-04-24 | 2019-08-20 | 浙江浙能技术研究院有限公司 | Structure and preparation method of multi-sphere stacked carbon-coated manganese dioxide composite material |
| CN110190272A (en) * | 2019-07-09 | 2019-08-30 | 齐鲁工业大学 | A kind of preparation method of the nanocomposite for water system Zinc ion battery anode |
| CN110364710A (en) * | 2019-07-02 | 2019-10-22 | 华南理工大学 | High-performance manganese-based zinc ion battery positive electrode material and preparation method and application thereof |
| CN110571417A (en) * | 2019-08-22 | 2019-12-13 | 齐鲁工业大学 | Solvothermal preparation of VS4Polyaniline sodium ion battery cathode material |
| CN111825119A (en) * | 2019-04-23 | 2020-10-27 | 赵彦霖 | Preparation method of zinc ion battery positive electrode material |
| CN112397711A (en) * | 2020-11-20 | 2021-02-23 | 内蒙古大学 | Water-based zinc ion battery positive electrode material and preparation method and application thereof |
| CN112421028A (en) * | 2020-12-02 | 2021-02-26 | 齐鲁工业大学 | Preparation method of novel water-based zinc ion battery positive electrode material |
| CN112670495A (en) * | 2019-10-16 | 2021-04-16 | 中国科学院大连化学物理研究所 | Iron-doped manganese dioxide composite carbon nanotube material and preparation and application thereof |
| CN113130893A (en) * | 2021-04-22 | 2021-07-16 | 齐鲁工业大学 | N-doped VSe2Composite anode material of/MXene sodium battery and preparation method thereof |
| CN113823777A (en) * | 2021-08-11 | 2021-12-21 | 中国地质大学（武汉） | Porous nitrogen-doped carbon coaxial coating manganese dioxide nanotube and preparation method and application thereof |
| CN113937266A (en) * | 2021-09-30 | 2022-01-14 | 江苏理工学院 | Water-based zinc ion battery positive electrode material and preparation method thereof |
| CN114792606A (en) * | 2022-04-20 | 2022-07-26 | 北京航空航天大学 | Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate |
| CN115000395A (en) * | 2022-05-11 | 2022-09-02 | 中南大学 | K-doped alpha-manganese dioxide nanorod, direct-writing forming ink, zinc ion battery anode and preparation methods thereof |
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| CN113937266A (en) * | 2021-09-30 | 2022-01-14 | 江苏理工学院 | Water-based zinc ion battery positive electrode material and preparation method thereof |
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| CN114792606A (en) * | 2022-04-20 | 2022-07-26 | 北京航空航天大学 | Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate |
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