CN111029564A - Preparation method of iron negative electrode material of iron-nickel secondary battery - Google Patents
Preparation method of iron negative electrode material of iron-nickel secondary battery Download PDFInfo
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- CN111029564A CN111029564A CN201911259620.6A CN201911259620A CN111029564A CN 111029564 A CN111029564 A CN 111029564A CN 201911259620 A CN201911259620 A CN 201911259620A CN 111029564 A CN111029564 A CN 111029564A
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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Abstract
The invention discloses a liquid phase preparation method of an iron cathode material of an iron-nickel secondary battery, which comprises the following specific steps: dissolving soluble ferric salt, soluble tin salt and soluble copper salt in deionized water according to a certain proportion, adding a precipitator for precipitation, then filtering, washing and drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere, preserving heat for 1-8 h, and cooling to room temperature along with the furnace to obtain Sn containing iron, tin and copperxCuyFe2O4Spinel crystal, wherein x + y =1, x > 0, y > 0. The iron negative electrode material prepared by the invention can be used as a negative electrode active substance or an additive of an iron-nickel secondary battery, can effectively eliminate a second platform of the iron-nickel battery, reduce the charging voltage of the iron-nickel battery, improve the specific capacity of the iron-nickel secondary battery, reduce the electrode expansion, reduce the gassing amount and prolong the service life of the iron-nickel secondary batteryThe service life of the battery.
Description
Technical Field
The invention belongs to the technical field of preparation of iron cathode materials of iron-nickel secondary batteries, and particularly relates to a preparation method of an iron cathode material of an iron-nickel secondary battery.
Background
The current available square secondary battery mainly comprises a lead-acid storage battery and a lithium ion battery, wherein the specific energy of the lead-acid storage battery is low and generally only reaches 30-35 Wh/Kg, the cycle life is about 300-350 times, a longer charging time is needed, meanwhile, lead is toxic heavy metal, and if the lead is not properly treated during the production process and recovery, the lead can cause serious pollution to the environment, and the production and the use are limited by countries in the world. The specific energy of the lithium ion battery is relatively high, and the lithium ion battery can be charged and discharged by heavy current; however, the environment is easily polluted in the production and recovery processes, so-called environmental protection is only compared with that of a lead-acid battery, and because the lithium ion battery has a safety problem, especially has poorer safety performance in a high-capacity and high-voltage use environment, and meanwhile, a series of problems that the waste lithium iron phosphate, lithium manganate and other lithium ion batteries are difficult to recover, have pollution and have no recovery value and the like, the lithium ion battery has a great influence on the future human environment to a certain extent.
The iron-nickel battery is firm and durable, has long cycle life, can be abused, has easily-bought and easily-obtained raw materials which are not controlled, and has the characteristics of environmental protection and safety in production, use and recovery. However, the hydrogen evolution potential of the iron cathode in the iron-nickel battery is low, a large amount of hydrogen can be evolved particularly in the later period, the current efficiency of the iron cathode is reduced due to the generation of the hydrogen, and meanwhile, the defects of poor low-temperature performance, long second discharge platform, no practical application value, low charging efficiency, poor large-current discharge performance and the like exist.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the iron negative electrode material of the iron-nickel secondary battery, and the iron negative electrode material of the iron-nickel secondary battery prepared by the method can effectively improve the hydrogen evolution overpotential of an iron electrode, reduce the charging voltage, improve the gram capacity and improve the low-temperature performance of the battery.
The invention is thatThe technical scheme is that the preparation method of the iron cathode material of the iron-nickel secondary battery is characterized by comprising the following steps: dissolving soluble ferric salt, soluble tin salt and soluble copper salt in deionized water, adding a precipitator for precipitation, then filtering, washing and drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere or a reducing atmosphere, preserving heat for 1-8 h, and cooling to room temperature along with the furnace to obtain SnFe2O4Or Sn containing Fe, Sn, CuxCuyFe2O4The spinel crystal, wherein x + y =1, x > 0, y > 0, the material is used for a cathode active substance or an additive of an iron-nickel secondary battery, and can effectively improve the specific capacity of the iron-nickel secondary battery, reduce the electrode expansion, reduce the gas evolution and prolong the service life of the battery.
Preferably, the soluble ferric salt is one or more of ferric chloride, ferric sulfate or ferric nitrate; the soluble tin salt is one or more of stannous chloride, stannous sulfate or stannous nitrate; the soluble copper salt is one or more of copper chloride, copper sulfate or copper nitrate; the precipitant is one or more of sodium hydroxide solution, potassium hydroxide solution and ammonia water solution.
Preferably, the inert atmosphere is one or more of nitrogen and argon; the reducing atmosphere is hydrogen or a mixed gas of hydrogen and nitrogen.
Preferably, the liquid phase preparation method of the iron negative electrode material of the iron-nickel secondary battery is characterized in that the iron negative electrode material SnFe2O4The preparation method comprises the following specific steps: stannous sulfate and ferric sulfate are mixed according to the element molar ratio Sn: dissolving Fe =1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 800 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, preserving the heat for 1h, and then cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material SnFe2O4The iron negative electrode material can be used as a negative electrode active material of an iron-nickel secondary battery orThe additive effectively reduces the charging voltage, improves the gram capacity, and improves the formation speed and the discharge platform.
Preferably, the liquid phase preparation method of the iron negative electrode material of the iron-nickel secondary battery is characterized in that the iron negative electrode material Sn0.9Cu0.1Fe2O4The preparation method comprises the following specific steps: stannous sulfate, copper sulfate and ferric sulfate are mixed according to the element molar ratio Sn: cu: dissolving Fe =0.9:0.1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 850 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, preserving the heat for 1h, and then cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material Sn0.9Cu0.1Fe2O4The iron negative electrode material is a spinel crystal containing iron, tin and copper, can be used as a negative electrode active substance or an additive of the iron-nickel secondary battery, and tin is beneficial to improving the hydrogen evolution overpotential of the iron negative electrode material during charging so as to improve the charging efficiency of the iron-nickel secondary battery; during discharging, the action of tin ions and the discharge product iron hydroxide is utilized, the passivation phenomenon is weakened, and the increase of internal resistance is prevented, so that the discharge efficiency and the discharge platform of the iron-nickel secondary battery are improved.
Compared with the prior art, the invention has the following beneficial effects: the iron negative electrode material prepared by the invention can be used as a negative electrode active substance or an additive of an iron-nickel secondary battery, and compared with a conventional iron-nickel secondary battery which singly uses ferroferric oxide as a negative electrode material, the iron negative electrode material can effectively improve the specific capacity of the iron-nickel secondary battery, reduce the electrode expansion, reduce the gassing amount and prolong the service life of the battery.
Drawings
FIG. 1 shows SnFe obtained in example 12O4Cathode material and conventional Fe3O4A charge-discharge comparison curve of the negative electrode material;
FIG. 2 shows Sn obtained in example 20.9Cu0.1Fe2O4Cathode material and conventional Fe3O4Negative electrodeA charge-discharge comparison curve of the material;
FIG. 3 is SnFe doping2O4Fe (b) of3O4Charge and discharge curves of the negative electrode material.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Stannous sulfate and ferric sulfate are mixed according to the element molar ratio Sn: dissolving Fe =1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 800 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, preserving the heat for 2 hours, and cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material SnFe2O4The iron negative electrode material can be used as a negative electrode active material or an additive of an iron-nickel secondary battery.
Example 2
Stannous sulfate, copper sulfate and ferric sulfate are mixed according to the element molar ratio Sn: cu: dissolving Fe =0.9:0.1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 850 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, preserving the heat for 1h, and then cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material Sn0.9Cu0.1Fe2O4The iron negative electrode material can be used as a negative electrode active material or an additive of an iron-nickel secondary battery.
Example 3
Stannous chloride, copper chloride and ferric chloride are mixed according to the element molar ratio Sn: cu: dissolving Fe =0.9:0.1:2 in deionized water, and dissolving sodium hydroxide containing 2-4 mol/L at 40-90 deg.CPouring the solution into the solution, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing, drying, placing in a tubular furnace, heating to 850 ℃ at a heating rate of 10 ℃/min in a mixed atmosphere of nitrogen and hydrogen, preserving heat for 1h, cooling to room temperature along with the furnace, and finally obtaining the target product of the iron cathode material Sn0.9Cu0.1Fe2O4The iron negative electrode material can be used as a negative electrode active material or an additive of an iron-nickel secondary battery.
Through comparison of charging curves, the iron cathode material prepared by the invention is Fe with the conventional iron cathode material3O4Compared with the prior art, the charging voltage is effectively reduced, the gram capacity is improved, the formation speed is increased, and the discharging platform is improved.
The iron negative electrode active material is Sn containing iron, tin and copperxCuyFe2O4(x + y =1) spinel crystal. Tin is beneficial to improving the hydrogen evolution overpotential of the iron cathode material during charging, so that the charging efficiency of the iron-nickel secondary battery can be improved; during discharging, the action of tin ions and the discharge product iron hydroxide is utilized, the passivation phenomenon is weakened, and the increase of internal resistance is prevented, so that the discharge efficiency and the discharge platform of the iron-nickel secondary battery are improved.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, the invention further resides in various changes and modifications which fall within the scope of the invention as claimed.
Claims (5)
1. A preparation method of an iron cathode material of an iron-nickel secondary battery is characterized by comprising the following specific steps: dissolving soluble ferric salt, soluble tin salt and soluble copper salt in deionized water according to a ratio, adding a precipitator for precipitation, then filtering, washing and drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere or a reducing atmosphere, preserving heat for 1-8 h, and cooling to room temperature along with the furnace to obtain a target product, namely the iron cathode material Sn of the iron-nickel secondary batteryxCuyFe2O4Spinel crystal, wherein x + y =1, x > 0, y > 0, the iron-nickel secondaryThe battery iron negative electrode material is used for an iron-nickel secondary battery negative electrode active substance or an additive, can effectively eliminate a second platform of the iron-nickel battery, reduce the charging voltage of the iron-nickel battery, improve the specific capacity of the iron-nickel secondary battery, reduce electrode expansion, reduce gas evolution and prolong the service life of the battery.
2. The soluble ferric salt is one or more of ferric chloride, ferric sulfate or ferric nitrate; the soluble tin salt is one or more of stannous chloride, stannous sulfate or stannous nitrate; the soluble copper salt is one or more of copper chloride, copper sulfate or copper nitrate; the precipitator is one or more of sodium hydroxide solution, potassium hydroxide solution or ammonia water solution.
3. The method for preparing the iron negative electrode material of the iron-nickel secondary battery according to claim 1, characterized in that: the inert atmosphere is one or more of nitrogen or argon, and the reducing atmosphere is hydrogen or mixed gas of hydrogen and nitrogen.
4. The method for preparing the iron negative electrode material of the iron-nickel secondary battery according to claim 1, wherein the iron negative electrode material SnFe2O4The preparation method comprises the following specific steps: stannous sulfate and ferric sulfate are mixed according to the element molar ratio Sn: dissolving Fe =1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 800 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, preserving the heat for 1h, and then cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material SnFe2O4The iron negative electrode material can be used for negative electrode active substances or additives of iron-nickel secondary batteries, effectively reduces charging voltage, improves gram capacity, and improves formation speed and discharge platform.
5. The method for preparing the iron negative electrode material of the iron-nickel secondary battery according to claim 1Characterized in that the iron cathode material Sn0.9Cu0.1Fe2O4The preparation method comprises the following specific steps: stannous sulfate, copper sulfate and ferric sulfate are mixed according to the element molar ratio Sn: cu: dissolving Fe =0.9:0.1:2 in deionized water, pouring a sodium hydroxide solution containing 2-4 mol/L into the solution at the temperature of 40-90 ℃, stirring and mixing uniformly, and aging for 4-8 h; then filtering, washing and drying the mixture, putting the mixture into a tubular furnace, heating the mixture to 850 ℃ at the heating rate of 10 ℃/min in reducing atmosphere, preserving the heat for 1h, and then cooling the mixture to room temperature along with the furnace to finally obtain the target product, namely the iron negative electrode material Sn0.9Cu0.1Fe2O4The iron negative electrode material is a spinel crystal containing iron, tin and copper, can be used as a negative electrode active substance or an additive of the iron-nickel secondary battery, and tin is beneficial to improving the hydrogen evolution overpotential of the iron negative electrode material during charging so as to improve the charging efficiency of the iron-nickel secondary battery; during discharging, the action of tin ions and the discharge product iron hydroxide is utilized, the passivation phenomenon is weakened, and the increase of internal resistance is prevented, so that the discharge efficiency and the discharge platform of the iron-nickel secondary battery are improved.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113540431A (en) * | 2021-07-09 | 2021-10-22 | 沈阳理工大学 | Alkaline iron-nickel secondary battery negative electrode active material and preparation method thereof |
| CN114243006A (en) * | 2021-12-20 | 2022-03-25 | 上海华谊新材料有限公司 | Lithium iron manganese phosphate positive electrode material, preparation method thereof and soft package lithium battery |
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