CN111009653A - Preparation method of zinc cathode material of zinc-nickel secondary battery - Google Patents
Preparation method of zinc cathode material of zinc-nickel secondary battery Download PDFInfo
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- CN111009653A CN111009653A CN201911259501.0A CN201911259501A CN111009653A CN 111009653 A CN111009653 A CN 111009653A CN 201911259501 A CN201911259501 A CN 201911259501A CN 111009653 A CN111009653 A CN 111009653A
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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
- H01M10/24—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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- H01M4/62—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
- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a zinc cathode material of a zinc-nickel secondary battery, which comprises the following specific steps: dissolving soluble zinc salt, soluble tin salt and soluble copper salt in deionized water, adding a precipitator for precipitation, then filtering, washing, drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere, preserving heat for 1-10 h, and cooling to room temperature along with the furnace to obtain Zn of the zinc-nickel secondary battery negative electrode material containing Zn, Sn and CuxCuySnO4Crystal, the zinc-nickel secondary battery zinc cathode material ZnxCuySnO4The crystal is used as the cathode active substance or additive of the zinc-nickel secondary battery, can improve the power and specific energy performance of the zinc-nickel secondary battery, prevent the zinc cathode of the zinc-nickel secondary battery from expanding, falling off and dendritic crystal growth, and further prolong the zinc-nickel secondary batteryThe service life of (2).
Description
Technical Field
The invention belongs to the technical field of preparation of zinc cathode materials of zinc-nickel secondary batteries, and particularly relates to a preparation method of a zinc cathode material of a zinc-nickel secondary battery.
Background
The current available square secondary battery mainly comprises a lead-acid storage battery, a hydrogen-nickel battery and a lithium ion battery, wherein the specific energy of the lead-acid storage battery is low and generally can only reach 30-35 Wh/Kg, the cycle life is about 300-350 times, a longer charging time is needed, lead is toxic heavy metal, and the production process and the recovery process have been restricted by countries in the world to produce and use if the lead is improperly treated, so that the environment is seriously polluted. The nickel-hydrogen battery has low working voltage, large self-discharge at high temperature, needs a large amount of rare earth raw materials, has high cost price, and is only suitable for being used as a power supply of small-sized electrical appliances at present. 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 traditional zinc-nickel battery cathode adopts zinc oxide powder with fine granularity as an active substance, zinc ions are easy to dissolve out in the discharge process of alkaline electrolyte, the zinc ions are deposited on the uneven convex part of the electrode surface to form dendrites in the charging process, and the dendrites penetrate through a diaphragm to cause short circuit of a positive electrode and a negative electrode, so that the battery fails. Although researchers have done a great deal of work in recent years trying to extend the cycle life of zinc-nickel batteries, current research work is primarily limited to zinc-nickel battery electrolytes and separators, and a small portion of the research work is seeking strategies for electrode additives. The problems of expansion, falling off, dendritic crystal growth and the like of the zinc cathode material of the zinc-nickel battery cannot be well solved by the conventional method.
Disclosure of Invention
The technical problem solved by the invention is to provide a preparation method of a zinc cathode material of a zinc-nickel secondary battery, the zinc cathode material of the zinc-nickel secondary battery prepared by the method effectively solves the problems of expansion, falling off, dendrite growth and the like of the zinc cathode of the zinc-nickel secondary battery, and simultaneously effectively prolongs the service life of the zinc-nickel secondary battery.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the zinc cathode material of the zinc-nickel secondary battery is characterized by comprising the following specific processes: dissolving soluble zinc salt, soluble tin salt and soluble copper salt in deionized water, adding a precipitator for precipitation, then filtering, washing, drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere, preserving heat for 1-10 h, and cooling to room temperature along with the furnace to obtain a target product Zn-Ni secondary battery zinc cathode material containing Zn, Sn and CuxCuySnO4Crystal, wherein x + y =2, x > 0, y > 0, the zinc-nickel secondary battery zinc cathode material ZnxCuySnO4The crystal is used as a cathode active substance or an additive of the zinc-nickel secondary battery, can improve the power and specific energy performance of the zinc-nickel secondary battery, and prevent the zinc cathode of the zinc-nickel secondary battery from expanding, falling off and dendritic crystal growth, thereby prolonging the service life of the zinc-nickel secondary battery;
the soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate or zinc acetate; the soluble tin salt is one or more of stannous chloride, stannous sulfate, stannic chloride or stannous nitrate; the soluble copper salt is one or more of copper chloride, copper sulfate, copper nitrate or copper acetate; the precipitator is one or more of sodium hydroxide solution, ammonia water or oxalic acid solution.
Preferably, the inert atmosphere is one or more of a nitrogen atmosphere, an argon atmosphere or a hydrogen atmosphere.
Preferably, the preparation method of the zinc cathode material of the zinc-nickel secondary batteryThe method is characterized in that a zinc cathode material ZnCuSnO4The specific preparation steps of the crystal are as follows: zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1:1:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, putting the product into a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere, keeping the temperature for 1h, cooling to room temperature along with the furnace, and finally preparing a target product of the zinc cathode material ZnCuSnO of the zinc-nickel secondary battery4Crystal, the zinc cathode material ZnCuSnO4The crystal can be used as a negative electrode active substance or an additive of a zinc-nickel secondary battery, and can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material ZnCuSnO45wt% of conductive graphite is added into the crystal, and paste with 10000cP viscosity is prepared by HPMC and SBR binding agent and coated on the crystal with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode on the foamed nickel substrate, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive electrode and the negative electrode are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 230 mAh/g.
Preferably, the preparation method of the zinc negative electrode material of the zinc-nickel secondary battery is characterized in that the zinc negative electrode material Zn1.5Cu0.5SnO4The specific preparation steps of the crystal are as follows: zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1.5:0.5:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, placing the product in a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min under a nitrogen atmosphere, preserving heat for 1h, cooling to room temperature along with the furnace, and finally preparing a target product Zn cathode material Zn of the zinc-nickel secondary battery1.5Cu0.5SnO4Crystal of the zinc negative electrode material Zn1.5Cu0.5SnO4The crystal can be used as a negative electrode active substance or an additive of a zinc-nickel secondary battery, and can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material Zn1.5Cu0.5SnO4The crystal is added with 5wt% of conductive graphite and bonded by HPMC and SBRPreparing slurry with 10000cP viscosity by using a binding agent and coating the slurry on a coating with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive and negative electrodes are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 300 mAh/g.
Compared with the prior art, the invention has the following beneficial effects: the zinc cathode material Zn prepared by the invention2SnO4The crystal can be used as a cathode active substance or an additive of the zinc-nickel secondary battery, can effectively improve the power and specific energy performance of the zinc-nickel secondary battery, prevent the zinc cathode of the zinc-nickel secondary battery from expanding, falling off and dendritic crystal growth, prolong the service life of the zinc-nickel secondary battery, and meet the requirements of commercial application and environmental protection.
Drawings
FIG. 1 shows ZnCuSnO prepared in example 14The charge-discharge contrast curve of the negative electrode material and the conventional zinc negative electrode material is obtained;
FIG. 2 shows ZnCuSnO prepared in example 24The charge-discharge contrast curve of the negative electrode material and the conventional zinc negative electrode material is obtained;
FIG. 3 is a ZnCuSnO doped4The charge-discharge curve of the zinc 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
Zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1:1:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, putting the product into a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere, keeping the temperature for 1h, cooling to room temperature along with the furnace, and finally preparing a target product of the zinc cathode material ZnCuSnO of the zinc-nickel secondary battery4Crystal, the zinc cathode material ZnCuSnO4The crystal can be used for zincThe cathode active material or additive of the nickel secondary battery can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material ZnCuSnO45wt% of conductive graphite is added into the crystal, and paste with 10000cP viscosity is prepared by HPMC and SBR binding agent and coated on the crystal with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode on the foamed nickel substrate, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive electrode and the negative electrode are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 230 mAh/g.
Example 2
Zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1.5:0.5:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, placing the product in a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min under a nitrogen atmosphere, preserving heat for 1h, cooling to room temperature along with the furnace, and finally preparing a target product Zn cathode material Zn of the zinc-nickel secondary battery1.5Cu0.5SnO4Crystal of the zinc negative electrode material Zn1.5Cu0.5SnO4The crystal can be used as a negative electrode active substance or an additive of a zinc-nickel secondary battery, and can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material Zn1.5Cu0.5SnO45wt% of conductive graphite is added into the crystal, and paste with 10000cP viscosity is prepared by HPMC and SBR binding agent and coated on the crystal with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive and negative electrodes are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 300 mAh/g.
The invention has the characteristics of easy purchase and acquisition, low price and the like of the materials, prepares the zinc cathode material of the zinc-nickel secondary battery, solves or partially solves the problems of expansion, falling and dendritic crystal growth of the zinc cathode material of the current zinc-nickel secondary battery, improves the cycle stability of the zinc-nickel secondary battery, and prolongs the service life of the zinc-nickel secondary battery.
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 (4)
1. A preparation method of a zinc cathode material of a zinc-nickel secondary battery is characterized by comprising the following specific steps: dissolving soluble zinc salt, soluble tin salt and soluble copper salt in deionized water according to a certain proportion, adding a precipitator for precipitation, then filtering, washing, drying, placing in a tubular furnace, heating to 700-1050 ℃ in an inert atmosphere, preserving heat for 1-10 h, and cooling to room temperature along with the furnace to obtain a target product Zn-Ni secondary battery zinc cathode material containing Zn, Sn and CuxCuySnO4Crystal, wherein x + y =2, x > 0, y > 0, the zinc-nickel secondary battery zinc cathode material ZnxCuySnO4The crystal is used as a cathode active substance or an additive of the zinc-nickel secondary battery, can improve the power and specific energy performance of the zinc-nickel secondary battery, and prevent the zinc cathode of the zinc-nickel secondary battery from expanding, falling off and dendritic crystal growth, thereby prolonging the service life of the zinc-nickel secondary battery;
the soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate or zinc acetate; the soluble tin salt is one or more of stannous chloride, stannous sulfate, stannic chloride or stannous nitrate; the soluble copper salt is one or more of copper chloride, copper sulfate, copper nitrate or copper acetate; the precipitator is one or more of sodium hydroxide solution, ammonia water or oxalic acid solution.
2. The method for preparing the zinc negative electrode material of the zinc-nickel secondary battery according to claim 1, which is characterized in that: the inert atmosphere is one or more of nitrogen or argon.
3. The method for preparing the zinc cathode material of the zinc-nickel secondary battery according to claim 1, wherein the zinc cathode material is ZnCuSnO4Of crystalsThe preparation method comprises the following specific steps: zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1:1:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, putting the product into a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere, keeping the temperature for 1h, cooling to room temperature along with the furnace, and finally preparing a target product of the zinc cathode material ZnCuSnO of the zinc-nickel secondary battery4Crystal, the zinc cathode material ZnCuSnO4The crystal can be used as a negative electrode active substance or an additive of a zinc-nickel secondary battery, and can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material ZnCuSnO45wt% of conductive graphite is added into the crystal, and paste with 10000cP viscosity is prepared by HPMC and SBR binding agent and coated on the crystal with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode on the foamed nickel substrate, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive electrode and the negative electrode are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 230 mAh/g.
4. The method for preparing the zinc negative electrode material of the zinc-nickel secondary battery according to claim 1, wherein the zinc negative electrode material Zn1.5Cu0.5SnO4The specific preparation steps of the crystal are as follows: zinc chloride, tin tetrachloride and copper chloride are mixed according to the element molar ratio Zn: sn: dissolving Cu =1.5:0.5:1 in deionized water, carrying out precipitation reaction by using a sodium hydroxide solution, filtering, washing and drying a product, placing the product in a tubular furnace, heating to 850 ℃ at a heating rate of 20 ℃/min under a nitrogen atmosphere, preserving heat for 1h, cooling to room temperature along with the furnace, and finally preparing a target product Zn cathode material Zn of the zinc-nickel secondary battery1.5Cu0.5SnO4Crystal of the zinc negative electrode material Zn1.5Cu0.5SnO4The crystal can be used as a negative electrode active substance or an additive of a zinc-nickel secondary battery, and can effectively improve the cycling stability of the zinc-nickel secondary battery;
the zinc cathode material Zn1.5Cu0.5SnO45wt% of conductive graphite is added into the crystal, and HPMC and SBR bonding agents are usedThe paste with 10000cP viscosity is prepared and coated on the substrate with the density of 320g/m2After drying and rolling, the electrode lugs are spot-welded to form a negative electrode, a negative electrode is sandwiched between two positive plates of nickel hydroxide, the positive and negative electrodes are isolated by a diaphragm, and after 3 times of charging and discharging activation, the capacity is measured to be 300 mAh/g.
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