CN108346795A - A kind of water system Zinc ion battery negative material Zn3(OH)2V2O7·2H2The preparation method of O - Google Patents
A kind of water system Zinc ion battery negative material Zn3(OH)2V2O7·2H2The preparation method of O Download PDFInfo
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- CN108346795A CN108346795A CN201810074816.7A CN201810074816A CN108346795A CN 108346795 A CN108346795 A CN 108346795A CN 201810074816 A CN201810074816 A CN 201810074816A CN 108346795 A CN108346795 A CN 108346795A
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- zinc
- ion battery
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- battery negative
- organic solvent
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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
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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 present invention provides a kind of water system zinc ion negative material Zn3(OH)2V2O7·2H2O and its synthetic method.By zinc source, vanadium source, C6H12N4, sodium sulphate mixing after add organic solvent, be stirred well to raw material and be mixed thoroughly.Uniformly mixed suspension is transferred in autoclave, adds deionized water and organic solvent mixed liquor to the 80% of liner volume.24 ~ 36h is heated in 80 DEG C ~ 100 DEG C constant temperature blast drying ovens, the precipitation in autoclave is transferred in centrifuge tube after being cooled to room temperature, and 5 ~ 20h of baking in 70 DEG C ~ 90 DEG C constant temperature blast drying ovens is placed on after centrifugation, washing, obtains Zn3(OH)2V2O7·2H2O powder.Battery is assembled as Zinc ion battery negative material, shows good chemical property.In addition, this negative material can also be used in the water systems battery system such as sodium ion, potassium ion.
Description
Technical field
The present invention relates to a kind of high performance Zinc ion battery negative material, more particularly to a kind of Zn3(OH)2V2O7·2H2O
Preparation method, belong to field of electrochemical power source.
Technical background
The features such as lithium ion battery is due to high-energy density, low self-discharge, memory-less effect, long circulation life is by widely
Power supply as portable electronic product, hybrid vehicle and pure power vehicle.Demand with market to lithium ion battery
Measure it is increasing, lithium resource shortage be increasingly becoming limiting lithium ion cell development lethal factor.In addition, conventional lithium ion battery
Organic electrolyte used has certain toxicity, and there is the security risk of burning, explosion.Therefore, novel, green, peace is found
Full energy-storage battery becomes current research hotspot.Aqueous electrolyte Zinc ion battery has and fills as a kind of new secondary battery
The electric time is short, capacity is high, good cycle, it is safe and environment-friendly, inexpensive the features such as, future be expected to consumer electronics, track hand over
It is used widely in the fields such as logical, power transport.Its key developed, which is to develop, reversible can store and release zinc ion
New electrode materials.
Zn3(OH)2V2O7·2H2O is concentrated mainly on magnetic performance and optics as a kind of multifunctional material, tradition research
Aspect of performance.Simultaneously the study found that Zn3(OH)2V2O7·2H2O has the layer structure similar to graphite, can be used as potential electricity
Pole material.However, under conventional organic solution liquid system, Zn3(OH)2V2O7·2H2The crystallization water in O will occur instead with electrolyte
It answers, leads to electrolyte decomposition, while destroying Zn3(OH)2V2O7·2H2The crystal structure of O itself, finally inhibits ion（As lithium from
Son）Reversible insertion and abjection, to limit its practical application.We pass through to the material the study found that crystallization therein
Water plays an important roll its crystal structural stability, and the crystallization water will keep stablizing under the conditions of water system.This make its
There is important application value in water system battery.
Based on background above, a kind of low-temperature solvent heat method of invention prepares Zn3(OH)2V2O7·2H2O, and for the first time
Have studied its chemical property as water system Zinc ion battery cathode.
Invention content
The present invention relates to a kind of preparation method of new zinc ion battery cathode material, the negative material is Zn3
(OH)2V2O7·2H2O is used as surfactant by sodium sulphate, while controlling reaction temperature, solvent composition obtain different-shape
Zn3(OH)2V2O7·2H2O.By introducing organic solvent, obtaining the reaction temperature of product can effectively reduce.Specific synthesis side
Method is as follows：Organic solvent is added after zinc source, vanadium source, hexamethylenetetramine and sodium sulphate are mixed, stirring to raw material is thoroughly mixed
Uniformly, uniformly mixed brown suspension is transferred in autoclave, the mixing for adding deionized water and organic solvent is molten
Liquid to high pressure reaction kettle body accumulate 80% after, in 70 DEG C ~ 90 DEG C constant temperature blast drying ovens heat 5 ~ 20 h；It will be generated after reaction
Precipitation be transferred in culture dish after being centrifuged 2 ~ 6 times in the decentralized medium of deionized water and absolute ethyl alcohol respectively, 70 DEG C ~
Dry 5 ~ 20h, obtains Zn in 90 DEG C of thermostatic drying chambers3(OH)2V2O7·2H2O powder.
Zinc source, vanadium source, hexamethylenetetramine and sodium sulphate are weighed in small beaker, addition organic solution is stirred well to original
Material uniformly mixing.Uniformly mixed suspension is transferred in autoclave, addition have a certain proportion of organic solvent and
The mixed solution of deionized water is to the 80% of liner volume.24 ~ 36h is heated in 70 DEG C ~ 90 DEG C constant temperature blast drying ovens, it is cooling
The precipitation in autoclave is transferred in centrifuge tube after to room temperature, centrifugation is placed on 70 DEG C ~ 90 DEG C perseverances after washing 2 ~ 6 times
5 ~ 20h is toasted in warm air dry oven, obtains Zn3(OH)2V2O7·2H2O powder.
The zinc source is zinc sulfate, zinc carbonate, zinc nitrate or zinc acetate.
The vanadium source is vanadic anhydride or ammonium metavanadate.
The organic solvent is the alcohols solvents such as methanol, ethyl alcohol, polyethylene glycol.
The zinc source, vanadium source, hexamethylenetetramine and sodium sulphate molar ratio be 3:2:2~5:5~10.
Zn according to the present invention3(OH)2V2O7·2H2Preparation method, material and the performance of O negative materials have following several
A outstanding feature：
（1）Synthesis temperature is low, simple for process, easily operated, reproducible；
（2）Zn obtained by the present invention3(OH)2V2O7·2H2O is used as Zinc ion battery negative material for the first time, shows preferable
Chemical property.
Description of the drawings
Fig. 1：The XRD spectrum of prepared sample in embodiment 1；
Fig. 2：Prepared sample assembly encloses charge and discharge curve at first three of battery in embodiment 1;
Fig. 3：First three circle charge and discharge curve of 2 assembled batteries of embodiment；
Fig. 4：First three circle charge and discharge curve of 3 assembled batteries of embodiment；
Fig. 5：First three circle charge and discharge curve of 4 assembled batteries of embodiment；
Fig. 6：First three circle charge and discharge curve of 5 assembled batteries of embodiment.
Specific implementation mode
Embodiment 1：Weigh 3 mmol zinc carbonates, 1mmol vanadic anhydrides, 5mmol hexamethylenetetramines and 0.5g sulfuric acid
Sodium is dissolved in the small beaker equipped with 20mL absolute ethyl alcohols, stirs 4h；Obtained mixing suspension is transferred to 50mL reaction under high pressures
In kettle, deionized water and absolute ethyl alcohol volume ratio 1 are added:1 mixed solution is to the 80% of liner volume, later in 95 DEG C of perseverance
30 h of hydro-thermal, cooled to room temperature in warm convection oven obtain pyrovanadic acid zinc precipitation.Using water as decentralized medium and with anhydrous second
Alcohol is that decentralized medium centrifuges 4 times respectively, and precipitation is put into 70 DEG C ~ 90 DEG C constant temperature blast drying ovens dry 12h, obtains pyrovanadic acid
Zinc powder.Prepared sample is through XRD diagram spectrum analysis, and as shown in figure, all diffraction maximums and XRD cards 50-0570 are corresponded to,
Show successfully to be prepared for Zn3(OH)2V2O7·2H2O.By pyrovanadic acid zinc powder made from above-mentioned steps（70wt%）With acetylene black
（20 wt%）And PVDF（10 wt%）It is added in small beaker, stirring 1h is coated in titanium sheet to after mixing, is cut into diameter
The disk of 14mm is dried in vacuo 12h at 120 DEG C.Finally, with 0.1mol L-1Zn (NO3)2Solution is as electrolyte, glass
Glass tunica fibrosa is diaphragm, and zinc metal sheet is directly to be assembled into CR2025 type button cells in air to electrode.Battery pack installs rear quiet
2 ~ 12h is set, then constant current charge and discharge test is carried out with CT2001A battery test systems, test voltage is 0.1 ~ 1.3V.Two table of figure
It is bright, the Zn prepared by embodiment 13(OH)2V2O7·2H2Charge and discharge capacity is respectively 51 mAh/g and 59mAh/ to O electrodes for the first time
G, highest charge/discharge capacity are 90mAh/g and 81mAh/g, it is shown that preferable chemical property.
Embodiment 2：Weigh 3 mmol zinc sulfate, 1 mmol vanadic anhydrides, 5 mmol hexamethylenetetramines and 0.5 g sulphur
Sour sodium is dissolved in the small beaker equipped with 20 mL absolute methanol solutions, stirs 4h；Obtained mixing suspension is transferred to 50 mL
In autoclave, deionized water and absolute methanol volume ratio 1 are added:1 mixed solution to liner volume 80%, Zhi Hou
36 h of hydro-thermal, cooled to room temperature in 90 DEG C of constant temperature convection oven obtain pyrovanadic acid zinc precipitation.Described in embodiment 1
Method centrifuges and is assembled into battery and tested.Fig. 3 shows the Zn prepared by embodiment 23(OH)2V2O7·2H2O electrodes
Charge and discharge capacity is respectively 28.1 mAh g for the first time-1With 5.1 mAh g-1。
Embodiment 3：Weigh 3 mmol zinc acetates, 1 mmol vanadic anhydrides, 5 mmol hexamethylenetetramines and 0.5 g sulphur
Sour sodium is dissolved in the small beaker equipped with 20 mL polyglycol solutions, stirs 4h；Obtained mixing suspension is transferred to 50 mL
In autoclave, deionized water and polyethylene glycol volume ratio 2 are added:1 mixed solution to liner volume 80%, Zhi Hou
36 h of hydro-thermal, cooled to room temperature in 90 DEG C of constant temperature convection oven obtain pyrovanadic acid zinc precipitation.Described in embodiment 1
Method centrifuges and is assembled into battery and tested.Fig. 3 shows the Zn prepared by embodiment 23(OH)2V2O7·2H2O electrodes
Charge and discharge capacity is respectively 55.2 mAh g for the first time-1With 23.1 mAh g-1。
Embodiment 4：Weigh 3 mmol zinc nitrates, 1 mmol vanadic anhydrides, 5 mmol hexamethylenetetramines and 0.5 g sulphur
Sour sodium is dissolved in the small beaker equipped with 20 mL ethanol solutions, stirs 4h；Obtained mixing suspension is transferred to 50 mL
In autoclave, deionized water and absolute ethyl alcohol volume ratio 1 are added:1 mixed solution to liner volume 80%, Zhi Hou
24 h of hydro-thermal, cooled to room temperature in 95 DEG C of constant temperature convection oven obtain pyrovanadic acid zinc precipitation.Described in embodiment 1
Method centrifuges and prepares electrode.Finally with 1 mol L-1K2SO4For solution as electrolyte, glass fibre membrane is diaphragm,
Zinc metal sheet is directly to be assembled into CR2025 type button cells in air to electrode.Battery pack stands 2 ~ 12h after installing, and uses
CT2001A battery test systems carry out constant current charge and discharge test, and test voltage section is 0.1 ~ 1.3V.Fig. 5 shows embodiment 4
Prepared Zn3(OH)2V2O7·2H2Charge and discharge capacity is respectively 4.4 mAh g to O electrodes for the first time-1With 1.7 mAh g-1。
Embodiment 5：Weigh 3 mmol zinc carbonates, 1 mmol vanadic anhydrides, 5 mmol hexamethylenetetramines and 0.5 g sulphur
Sour sodium is dissolved in the small beaker equipped with 20 mL ethanol solutions, stirs 4h；Obtained mixing suspension is transferred to 50 mL
In autoclave, deionized water and absolute ethyl alcohol volume ratio 1 are added:1 mixed solution to liner volume 80%, Zhi Hou
36 h of hydro-thermal, cooled to room temperature in 90 DEG C of constant temperature convection oven obtain pyrovanadic acid zinc precipitation.Described in embodiment 1
Method centrifuges and prepares electrode.Finally with 1 mol L-1Na2SO4For solution as electrolyte, glass fibre membrane is diaphragm,
Zinc metal sheet is directly to be assembled into CR2025 type button cells in air to electrode.Battery pack stands 2 ~ 12h after installing, and uses
CT2001A battery test systems carry out constant current charge and discharge test, and test voltage section is 0.1 ~ 1.3V.Fig. 5 shows embodiment 4
Prepared Zn3(OH)2V2O7·2H2Charge and discharge capacity is respectively 4.8 mAh g to O electrodes for the first time-1With 1.7 mAh g-1。
Claims (6)
1. a kind of Zn3(OH)2V2O7·2H2The preparation method of O water system Zinc ion battery negative materials, which is characterized in that main system
Standby technique is as follows：
（1）Organic solvent is added after zinc source, vanadium source, hexamethylenetetramine and sodium sulphate are mixed, stirring to raw material is thoroughly mixed
Uniformly, uniformly mixed brown suspension is transferred in autoclave, the mixing for adding deionized water and organic solvent is molten
Liquid to high pressure reaction kettle body accumulate 80% after, in 70 DEG C ~ 90 DEG C constant temperature blast drying ovens heat 24 ~ 36h；
（2）The precipitation that will be generated after reaction after being centrifuged 2 ~ 6 times in the decentralized medium of deionized water and absolute ethyl alcohol respectively, turns
It moves in culture dish, dry 5 ~ 20h, obtains Zn in 70 DEG C ~ 90 DEG C thermostatic drying chambers3(OH)2V2O7·2H2O powder.
2. Zn according to claim 13(OH)2V2O7·2H2The preparation method of O water system Zinc ion battery negative materials,
It is characterized in that, step（1）Described in organic solvent include methanol, ethyl alcohol, polyethylene glycol alcohol organic solvent, deionized water
It is 1 with organic solvent volume ratio：1-2.
3. Zn according to claim 13(OH)2V2O7·2H2The preparation method of O water system Zinc ion battery negative materials,
Be characterized in that, the zinc source, vanadium source, hexamethylenetetramine and sodium sulphate molar ratio be 3：2：2~5：5~10.
4. Zn according to claim 13(OH)2V2O7·2H2The preparation method of O water system Zinc ion battery negative materials,
It is characterized in that, the zinc source includes zinc sulfate, zinc carbonate, zinc nitrate or zinc acetate.
5. Zn according to claim 13(OH)2V2O7·2H2The preparation method of O water system Zinc ion battery negative materials,
It is characterized in that, the vanadium source is vanadic anhydride or ammonium metavanadate.
6. the Zn being prepared described in claim any one of 1-53(OH)2V2O7·2H2O water system Zinc ion battery negative materials exist
Application in sodium ion, potassium ion water system battery system.
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Cited By (4)
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| CN110479243A (en) * | 2019-09-03 | 2019-11-22 | 陕西科技大学 | A kind of flower-shaped Zn3(OH)2V2O7·2H2O photochemical catalyst and preparation method thereof |
| CN110745866A (en) * | 2019-11-15 | 2020-02-04 | 福建师范大学 | One-step synthesis method of stibium-based metal bromide and application of stibium-based metal bromide in reversible storage and release of bromine gas |
| CN114156451A (en) * | 2021-11-30 | 2022-03-08 | 安徽师范大学 | Carbon cloth composite material with surface growing three-dimensional structure zinc pyrovanadate nanosheets, preparation method of carbon cloth composite material and rechargeable battery |
| CN115536067A (en) * | 2022-11-03 | 2022-12-30 | 南昌大学 | Novel self-assembled vanadium strong hydrophobic material and preparation method thereof, and coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110479243A (en) * | 2019-09-03 | 2019-11-22 | 陕西科技大学 | A kind of flower-shaped Zn3(OH)2V2O7·2H2O photochemical catalyst and preparation method thereof |
| CN110745866A (en) * | 2019-11-15 | 2020-02-04 | 福建师范大学 | One-step synthesis method of stibium-based metal bromide and application of stibium-based metal bromide in reversible storage and release of bromine gas |
| CN110745866B (en) * | 2019-11-15 | 2021-11-19 | 福建师范大学 | One-step synthesis method of stibium-based metal bromide and application of stibium-based metal bromide in reversible storage and release of bromine gas |
| CN114156451A (en) * | 2021-11-30 | 2022-03-08 | 安徽师范大学 | Carbon cloth composite material with surface growing three-dimensional structure zinc pyrovanadate nanosheets, preparation method of carbon cloth composite material and rechargeable battery |
| CN114156451B (en) * | 2021-11-30 | 2023-11-03 | 安徽师范大学 | Carbon cloth composite material with three-dimensional structure zinc pyrovanadate nanosheets grown on surface, preparation method of carbon cloth composite material and rechargeable battery |
| CN115536067A (en) * | 2022-11-03 | 2022-12-30 | 南昌大学 | Novel self-assembled vanadium strong hydrophobic material and preparation method thereof, and coating and preparation method thereof |
| CN115536067B (en) * | 2022-11-03 | 2023-10-03 | 南昌大学 | Self-assembled vanadium-based strong hydrophobic material, preparation method thereof, coating and preparation method thereof |
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Application publication date: 20180731 |