CN108511738A - A kind of preparation method of composite material, nickel iron cell electrode and nickel iron cell comprising the composite material - Google Patents
A kind of preparation method of composite material, nickel iron cell electrode and nickel iron cell comprising the composite material Download PDFInfo
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- CN108511738A CN108511738A CN201810605314.2A CN201810605314A CN108511738A CN 108511738 A CN108511738 A CN 108511738A CN 201810605314 A CN201810605314 A CN 201810605314A CN 108511738 A CN108511738 A CN 108511738A
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- composite material
- organic solvent
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- porous carbon
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
Nickel iron cell electrode and nickel iron cell the present invention relates to a kind of preparation method of composite material, comprising the composite material；Wherein, one embodiment of the preparation method of composite material, includes the following steps：Organoiron compound and organic indium compound are dissolved in organic solvent by step 1；Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, so that mixed solution is impregnated into the duct of porous carbon, while organic solvent being made to volatilize；Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is fitted into the vial of sealing, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/InSxThe composite material of/C.The preparation method of the present invention is simple for process, and the material of preparation is environmentally protective, and restrained effectively dissolving side reaction and the liberation of hydrogen side reaction of iron, plays higher specific discharge capacity and coulombic efficiency, can meet practical application request.
Description
Technical field
The present invention relates to the technologies of preparing of composite material, more particularly to prepare a kind of preparation method of composite material, include
The nickel iron cell electrode and nickel iron cell of the composite material.
Background technology
With the fast development of ev industry so that the lithium, cobalt element used in lithium ion battery material are all the more deficient,
And the toxicity of cobalt is big, used organic electrolyte poor chemical stability, is easy on fire from explosion.And used by nickel iron cell
Iron, nickel element reserves are high, at low cost, small toxicity, using aqueous electrolyte, environmental-friendly, safe.Therefore, nickel iron cell
The advantage of bigger is shown in extensive energy storage field.Certainly, traditional nickel iron cell at present there is also many problems, most critical
The problem of be that the dissolving of iron causes shuttle effect, cause electrode structure is unstable to cause battery capacity low, cyclical stability is poor.It passes
The solution of system is that active material and various carbon materials are carried out physics or chemically composited, improves battery to a certain extent
Capacity, but confinement cannot be played the role of to the dissolving of iron, to make side reaction product ferrous acid radical ion diffuse to anode, and
Positive electrode surface deposits to form one layer of passivating film, hinders OH-Fast transport is to positive electrode surface and reacts, therefore increases electrode
Polarization, reduces battery capacity.
Invention content
It is an object of the present invention to solve the above problem existing for traditional nickel iron cell.
To achieve the above object, on the one hand, the present invention provides a kind of preparation method of composite material, the preparation method packets
Include following steps：Organoiron compound and organic indium compound are dissolved in organic solvent by step 1；Step 2, by above-mentioned mixing
Solution is added dropwise on porous carbon materials, is constantly vacuumized after pressing stirring, so that mixed solution is impregnated into the duct of porous carbon, together
When so that organic solvent is volatilized；Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into sealing
Vial in, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/InSx/ C's is compound
Material.Wherein, FeSxFor iron sulfide, InSxFor indium sulfide, C is porous carbon, 0<x≤3.
In one embodiment of the invention, described that organoiron compound and organic indium compound are dissolved in organic solvent step
Suddenly, including：By organoiron compound and organic indium compound according to 95:5、90:10 or 85:15 molar ratio is dissolved in organic molten
Agent.
In another embodiment of the present invention, described be put into the tube furnace of logical argon gas is calcined, and obtains FeSx/
InSxIn the composite material step of/C, the temperature of calcining is 500-700 degree, and preferable temperature is 600 degree.
In another embodiment of the present invention, described be put into the tube furnace of logical argon gas is calcined, and obtains FeSx/
InSxIn the composite material step of/C, calcination time is 3-5 hours, preferably 4 hours.
In another embodiment of the present invention, described to be uniformly mixed obtained material in step with sulphur simple substance, material
It is 3 with sulphur simple substance:1、2:1 or 3:2 molar ratios mix.
In another embodiment of the present invention, the organic solvent includes methanol, ethyl alcohol, acetone, chloroform or ether.
On the other hand, the present invention provides a kind of preparation method of composite material, include the following steps：
Organoiron compound and bismuth organic compound are dissolved in organic solvent by step 1；Step 2, by above-mentioned mixed solution
It is added dropwise on porous carbon materials, is constantly vacuumized after pressing stirring, so that mixed solution is impregnated into the duct of porous carbon, make simultaneously
Organic solvent volatilizees；Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into the glass of sealing
In glass bottle, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/BiSxThe composite wood of/C
Material.Wherein, FeSxFor iron sulfide, BiSxFor bismuth sulfide, C is porous carbon, 0<x≤3.
On the other hand, the present invention provides a kind of preparation method of composite material, include the following steps：
Organoiron compound and organotungsten compounds are dissolved in organic solvent by step 1；Step 2, by above-mentioned mixed solution
It is added dropwise on porous carbon materials, is constantly vacuumized after pressing stirring, so that mixed solution is impregnated into the duct of porous carbon, make simultaneously
Organic solvent volatilizees；Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into the glass of sealing
In glass bottle, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/WSxThe composite material of/C.
Wherein, FeSxFor iron sulfide, WSxFor tungsten sulfide, C is porous carbon, 0<x≤3.
On the other hand, the present invention provides alkaline nickel iron cell cathode, including obtaining composite material by upper made Preparation Method.
Another aspect, the present invention provide alkaline nickel iron cell, including above-mentioned alkaline nickel iron cell cathode.
The beneficial effects of the present invention are：
First, FeS can be made by vacuum-assisted infusionxAnd InSx(or BiSx、WSx) be equably fixed on it is porous
In the duct of carbon, realizes that the confinement to lysate ferrous acid radical ion acts on, avoid ferrous acid root from shuttling between positive and negative electrode, press down
The passivation rate of positive and negative electrode material surface processed, improves the high rate performance of battery.
Second, the duct of porous carbon controls FeSxAnd InSx(or BiSx、WSx) particle size that nanoscale, to increase
The specific surface area for having added active material improves the reaction site and reactivity of electrode material, improves the specific capacity of battery.
Third, FeSxWith InSx(or BiSx、WSx) uniform mixing, InSx(or BiSx、WSx) to FeSxFurther carry out
Confinement acts on, and inhibits FeSxVolume change in reaction process improves the stability of electrode structure.
4th, InSx、BiSxOr WSxIt can inhibit FeS in situxThe evolving hydrogen reaction rate on surface improves the coulomb effect of battery
Rate.
Description of the drawings
Fig. 1 is a kind of preparation method flow diagram of composite material provided in an embodiment of the present invention.
Specific implementation mode
After embodiments of the present invention are described in detail by way of example below in conjunction with attached drawing, of the invention its
His features, characteristics, and advantages will be more obvious.
Embodiment 1
Fig. 1 is a kind of preparation method flow diagram of composite material provided in an embodiment of the present invention.It, should as shown in Fig. 1
Preparation method includes the following steps：
Organoiron compound and organic indium compound are dissolved in organic solvent by step 1；
In one embodiment, by organoiron compound and organic indium compound according to 95:5、90:10 or 85:15 rub
You are dissolved in organic solvent by ratio, and organic solvent includes methanol, ethyl alcohol, acetone, chloroform or ether.
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, keeps mixing molten
Liquid is impregnated into the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into the vial of sealing
In, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/InSxThe composite material of/C.Its
In, FeSxFor iron sulfide, InSxFor indium sulfide, C is porous carbon, 0<x≤3.
In another embodiment, it is 500-700 degree to be put into the temperature setting calcined in the tube furnace of logical argon gas,
Preferred calcination temperature is 600 degree.Calcination time is set as 3-5 hours, preferably 4 hours.
In another embodiment, by obtained material and sulphur simple substance by 3:1、2:1 or 3:2 molar ratios are mixed, excellent
It is 2 to select ratio:1.
The preparation method of the present invention is simple for process, and the material of preparation is environmentally protective, and effectively inhibits the dissolving pair of iron
Reaction and liberation of hydrogen side reaction, play higher specific discharge capacity and coulombic efficiency, can meet practical application request.
Embodiment 2
The preparation method of another kind composite material provided in an embodiment of the present invention, the preparation method include the following steps：
Organoiron compound and bismuth organic compound are dissolved in organic solvent by step 1；
In one embodiment, by organoiron compound and bismuth organic compound according to 95:5、90:10 or 85:15 rub
You are dissolved in organic solvent by ratio, and organic solvent includes methanol, ethyl alcohol, acetone, chloroform or ether.
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, keeps mixing molten
Liquid is impregnated into the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into the vial of sealing
In, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/BiSxThe composite material of/C.Its
In, FeSxFor iron sulfide, BiSxFor bismuth sulfide, C is porous carbon, 0<x≤3.
In another embodiment, it is 500-700 degree to be put into the temperature setting calcined in the tube furnace of logical argon gas,
Preferred calcination temperature is 600 degree.Calcination time is set as 3-5 hours, preferably 4 hours.
In another embodiment, by obtained material and sulphur simple substance by 3:1、2:1 or 3:2 molar ratios are mixed, excellent
It is 2 to select ratio:1.
The preparation method of the present invention is simple for process, and the material of preparation is environmentally protective, and effectively inhibits the dissolving pair of iron
Reaction and liberation of hydrogen side reaction, play higher specific discharge capacity and coulombic efficiency, can meet practical application request.
Embodiment 3
The preparation method of another kind composite material provided in an embodiment of the present invention, the preparation method include the following steps：
Organoiron compound and organotungsten compounds are dissolved in organic solvent by step 1；
In one embodiment, by organoiron compound and organotungsten compounds according to 95:5、90:10 or 85:15 rub
You are dissolved in organic solvent by ratio, and organic solvent includes methanol, ethyl alcohol, acetone, chloroform or ether.
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, keeps mixing molten
Liquid is impregnated into the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is packed into the vial of sealing
In, jacketed stainless steel protection set is put into the tube furnace of logical argon gas and is calcined, obtains FeSx/WSxThe composite material of/C.Its
In, FeSxFor iron sulfide, WSxFor tungsten sulfide, C is porous carbon, 0<x≤3.
In another embodiment, it is 500-700 degree to be put into the temperature setting calcined in the tube furnace of logical argon gas, excellent
It is 600 degree to select calcination temperature.Calcination time is set as 3-5 hours, preferably 4 hours.
In another embodiment, by obtained material and sulphur simple substance by 3:1、2:1 or 3:2 molar ratios are mixed, excellent
It is 2 to select ratio:1.
The preparation method of the present invention is simple for process, and the material of preparation is environmentally protective, and effectively inhibits the dissolving pair of iron
Reaction and liberation of hydrogen side reaction, play higher specific discharge capacity and coulombic efficiency, can meet practical application request.
Correspondingly, the embodiment of the present invention additionally provides alkaline nickel iron cell cathode, which includes logical
Cross the FeS that made Preparation Method obtainsx/InSx/C、FeSx/BiSx/ C or FeSx/WSxThe composite material of/C.
Correspondingly, the embodiment of the present invention additionally provides alkaline nickel iron cell, including above-mentioned alkaline nickel iron cell cathode.
It should be noted that above-described embodiment only is used for illustrating the structure and its working effect of the present invention, and it is not used as
It limits the scope of the invention.One of ordinary skilled in the art is right without prejudice to thinking of the present invention and structure
The adjustment or optimization that above-described embodiment carries out, should regard as the claims in the present invention and be covered.
Claims (10)
1. a kind of preparation method of composite material, which is characterized in that include the following steps：
Organoiron compound and organic indium compound are dissolved in organic solvent by step 1；
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, mixed solution is made to soak
In stain to the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is fitted into the vial of sealing, is added
Stainless steel protection set is covered, is put into the tube furnace of logical argon gas and is calcined, obtain FeSx/InSxThe composite material of/C, wherein 0<x
≤3。
2. according to the method described in claim 1, it is characterized in that, described be dissolved in organoiron compound and organic indium compound
Organic solvent step, including：
By organoiron compound and organic indium compound according to 95:5、90:10 or 85:15 molar ratio is dissolved in organic solvent.
3. according to the method described in claim 1, it is characterized in that, described be put into the tube furnace of logical argon gas is calcined, obtain
To FeSx/InSxIn the composite material step of/C, the temperature of calcining is 500-700 degree, and preferable temperature is 600 degree.
4. according to the method described in claim 1, it is characterized in that, described be put into the tube furnace of logical argon gas is calcined, obtain
To FeSx/InSxIn the composite material step of/C, calcination time is 3-5 hours, preferably 4 hours.
5. according to the method described in claim 1, it is characterized in that, described be uniformly mixed step by obtained material with sulphur simple substance
In, material is 3 with sulphur simple substance:1、2:1 or 3:2 molar ratios mix.
6. according to the method described in claim 1, it is characterized in that, the organic solvent includes methanol, ethyl alcohol, acetone, chloroform
Or ether.
7. a kind of preparation method of composite material, which is characterized in that include the following steps：
Organoiron compound and bismuth organic compound are dissolved in organic solvent by step 1；
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, mixed solution is made to soak
In stain to the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is fitted into the vial of sealing, is added
Stainless steel protection set is covered, is put into the tube furnace of logical argon gas and is calcined, obtain FeSx/BiSxThe composite material of/C, wherein 0<x
≤3。
8. a kind of preparation method of composite material, which is characterized in that include the following steps：
Organoiron compound and organotungsten compounds are dissolved in organic solvent by step 1；
Above-mentioned mixed solution is added dropwise on porous carbon materials step 2, is constantly vacuumized after pressing stirring, mixed solution is made to soak
In stain to the duct of porous carbon, while organic solvent being made to volatilize；
Step 3, constantly repeatedly step 2, obtained material is uniformly mixed with sulphur simple substance, is fitted into the vial of sealing, is added
Stainless steel protection set is covered, is put into the tube furnace of logical argon gas and is calcined, obtain FeSx/WSxThe composite material of/C, wherein 0<x
≤3。
9. alkaline nickel iron cell cathode, which is characterized in that comprising such as claim 7, claim 8 or as in claim 1-6
The composite material that preparation method described in any claim obtains.
10. alkaline nickel iron cell, which is characterized in that including alkaline nickel iron cell cathode as claimed in claim 9.
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| CN201810605314.2A CN108511738B (en) | 2018-06-13 | 2018-06-13 | Preparation method of composite material, nickel-iron battery electrode containing composite material and nickel-iron battery |
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| CN201810605314.2A CN108511738B (en) | 2018-06-13 | 2018-06-13 | Preparation method of composite material, nickel-iron battery electrode containing composite material and nickel-iron battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111477847A (en) * | 2020-04-08 | 2020-07-31 | 扬州大学 | Box-shaped necklace multilevel structure Fe7S8/WS2@ C-CNFs lithium ion battery negative electrode material and preparation method thereof |
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Effective date of registration: 20230831 Address after: 518000, Building 2601, Excellence Yulong Haoxuan, Xinyang Community, Shajing Street, Shenzhen City, Guangdong Province Patentee after: Guangdong Daqilian Technology Co.,Ltd. Address before: 518000 No.32, Fuzhong Road, Fuyong street, Bao'an District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN QIHANGYUAN TECHNOLOGY Co.,Ltd. |