CN108493413A - A kind of anode material for lithium-ion batteries and preparation method thereof - Google Patents

A kind of anode material for lithium-ion batteries and preparation method thereof Download PDF

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Publication number
CN108493413A
CN108493413A CN201810231389.9A CN201810231389A CN108493413A CN 108493413 A CN108493413 A CN 108493413A CN 201810231389 A CN201810231389 A CN 201810231389A CN 108493413 A CN108493413 A CN 108493413A
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parts
lithium
ion batteries
anode material
preparation
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付强
徐丹军
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Shaanxi Hayne New Material Co Ltd
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Shaanxi Hayne New Material Co Ltd
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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
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of anode material for lithium-ion batteries and preparation method thereof, and according to mass fraction meter, constitutive material is：30 50 parts of LiMn2O4,20 40 parts of nickel protoxide, 35 55 parts of ferrous phosphate, 10 15 parts of chrome green, 15 20 parts of carbon nano-fiber, 8 10 parts of electrically conductive graphite, 45 parts of modified oxidized lanthanum, 24 parts of zirconium fluoride；Cell positive material processing performance of the present invention is excellent, energy density is high, the small significant advantage of self discharge, improve performance of the lithium ion battery in terms of accumulation energy type battery, by adding the modifying elements such as chromium, lanthanum, zirconium, improves electric conductivity, thermal conductivity, the chemical property stabilization of battery, greatly prolongs the service life of material.

Description

A kind of anode material for lithium-ion batteries and preparation method thereof
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries and preparation method thereof, belong to battery material preparation field.
Background technology
With the development of technology, lithium ion battery has extraordinary application prospect in electric vehicle and energy storage field, must Deep effect will be generated to the following people’s lives.
Lithium ion battery has that operating voltage is high, energy density is big, have extended cycle life, self-discharge rate is small, environmentally protective etc. Advantage becomes the trend of secondary cell development；It is portable to be widely used to wireless telecommunications, digital camera, laptop etc. Electric appliance；With the development of technology, lithium battery is given great expectations, has become the preferred electrical source of power of electric vehicle at present；Mangaic acid For lithium battery because it has many advantages, such as cheap, safety is good, and by it is believed that being the first choice electricity of electric vehicle；But it is electric Electrical automobile is more demanding to the energy density and storge quality of battery, and current lithium manganate battery, since there are Mn3+It is molten , there is larger irreversible capacity loss in solution after storage, and negative material is by the lower influence of graphite charge specific capacity, still Requirement of the electric vehicle to power battery energy density and storge quality cannot be met, it is therefore necessary to develop new LiMn2O4 electricity Pond.
Invention content
In order to effectively improve the performance of lithium ion battery, mesh easy to use convenient for better using lithium battery, of the invention Be a kind of anode material for lithium-ion batteries and preparation method thereof is provided.
To achieve the goals above, the present invention adopts the following technical scheme that：
Anode material for lithium-ion batteries, according to mass fraction meter, constitutive material is：30-50 parts of LiMn2O4, nickel protoxide 20- 40 parts, it is 35-55 parts of ferrous phosphate, 10-15 parts of chrome green, 15-20 parts of carbon nano-fiber, 8-10 parts of electrically conductive graphite, modified 4-5 parts of lanthana, 2-4 parts of zirconium fluoride.
The preparation method of anode material for lithium-ion batteries, specifically includes the following contents：
（1）Each raw material is weighed by the parts by weight of constitutive material, chrome green, electrically conductive graphite, zirconium fluoride are first sent into rotary furnace Pre-burning is passed through 1-2 hours at room temperature, is warming up to 650-800 DEG C, heat preservation batch mixing 2-3 hours；Cooling is taken out, then uses and grinds Grinding media is acetone soln, wherein added with acetone soln weight 6.0%-8.0% silicon carbide, 10%-12% aluminium powders, 2%- is equivalent to 3% magnesium stearate, 5%-8% sodium lignin sulfonates；Grinding 8-10 hours, control the stone size are 50-100 μm；
（2）LiMn2O4, nickel protoxide, ferrous phosphate are weighed, is placed in dissolution vessel, appropriate weak acid is first added and is dissolved, then Appropriate amount of deionized water is added, ultrasonic disperse processing is allowed to uniformly mixed and obtains solution；
（3）Lanthana is weighed, is ground, the lanthanum oxide powder that grain size is 50-80nm is obtained, the 3-4 times of first measured then is added Base silicone oil, is warming up to 70-80 DEG C, is dispersed with stirring, and is then added and is equivalent to lanthanum oxide powder quality 3%-5% silane coupling agents KH550,5.5%-6.0% dodecyl sodium sulfate, are mixed and heated to 100-120 DEG C, through filtering, wash, dry, obtain modified oxygen Change lanthanum powder；
（4）By above-mentioned steps（1）, step（2）All materials are uniformly mixed, and modified oxidized lanthanum and nano-sized carbon are then added thereto Fiber is sintered after being uniformly mixed, during the sintering carries out under inert gas protection, first with 120-140 DEG C/h rate is warming up to 450-500 DEG C, when keeping the temperature 1-2 hours, then 650-750 DEG C be warming up to 80-90 DEG C/h of rate, Heat preservation 2.5-3.0 hours；After being cooled down with 50-70 DEG C/h after sintering to obtain the final product.
The step（2）Middle ultrasonic disperse processing power is 450-550W, and temperature is 40-50 DEG C, sonication treatment time For 20-30min.
The inert gas is preferably argon gas.
The step（2）Middle weak acid is carbonic acid, acetic acid, sulfurous acid or formic acid.
The molten replacement of absolute ethyl alcohol can be used in the abrasive media acetone soln.
The step（3）Dry to use infrared drying, the wavelength of infrared ray is 0.6nm to 0.75nm, dry temperature Degree is 45-55 DEG C, drying time 25-30min.
Beneficial effects of the present invention：
Compared with prior art, cell positive material processing performance of the present invention is excellent, and energy density is high, small notable excellent of self discharge Gesture improves performance of the lithium ion battery in terms of accumulation energy type battery, by adding the modifying elements such as chromium, lanthanum, zirconium, improves battery Electric conductivity, thermal conductivity, chemical property is stable, greatly prolongs the service life of material.
The anode material for lithium-ion batteries of the present invention is by being pre-sintered, acetone soln is ground and re-sinters technique, improves The particle size of lithium ion anode material improves the tap density and energy density of material.
The anode material for lithium-ion batteries of the present invention can be fabricated to green high-capacity battery, have the characteristics that：High voltage, height Capacity, low consumption, self discharge is few, cycle-index is more, may be used on mobile phone, laptop, video camera, digital camera etc. Numerous civilian and military field.
Addition carbon nano-fiber, modified oxidized lanthanum, zirconium fluoride are as filler, nanometer in the cell positive material of the present invention Carbon fiber has the advantages such as high intensity, high tenacity, good thermal stability and electric conductivity, extends making for the material of anode With the service life, modified oxidized lanthanum, zirconium fluoride have corrosion-resistant, high temperature resistant, antioxygenic property, effectively prevent cell positive material because High temperature, tidewater alleviate the damage for leading to battery material, reduce the leakage of harmful metal elements, while extending the use longevity of battery Life.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, is not used to Limit the present invention.
Embodiment 1：Anode material for lithium-ion batteries weighs the following raw material：LiMn2O4 40g, nickel protoxide 30g, phosphoric acid are sub- Iron 45g, chrome green 12g, carbon nano-fiber 18g, electrically conductive graphite 9g, modified oxidized lanthanum 5g, zirconium fluoride 3g.
The preparation method of anode material for lithium-ion batteries is as follows：
（1）Chrome green, electrically conductive graphite, zirconium fluoride are first sent into rotary furnace pre-burning, passed through 1.5 hours at room temperature, heating To 700 DEG C, heat preservation batch mixing 2.5 hours；Cooling is taken out, then uses abrasive media for acetone soln, wherein added with being equivalent to 7.0% silicon carbide of acetone soln weight, 11% aluminium powder, 2.5% magnesium stearate, 6.5% sodium lignin sulfonate；Grinding 10 hours, control The stone size is 50 μm；
（2）LiMn2O4, nickel protoxide, ferrous phosphate are weighed, is placed in dissolution vessel, proper amount of acetic acid is first added and is dissolved, then Appropriate amount of deionized water, ultrasonic disperse processing is added, ultrasonic disperse processing power is 500W, and temperature is 45 DEG C, sonication treatment time For 25min, it is allowed to uniformly mixed and obtains solution；
（3）Lanthana is weighed, is ground, the lanthanum oxide powder that grain size is 50nm is obtained, the methyl silicon of 3 times of amounts is then added Oil is warming up to 75 DEG C, is dispersed with stirring, and is then added and is equivalent to 4% Silane coupling agent KH550 of lanthanum oxide powder quality, 5.5% 12 Sodium alkyl sulfonate is mixed and heated to 110 DEG C, and through filtering, washing, infrared drying obtains modified oxidized lanthanum powder, infrared ray Wavelength is 0.6nm, and drying temperature is 50 DEG C, drying time 25min；
（4）By above-mentioned steps（1）, step（2）All materials are uniformly mixed, and modified oxidized lanthanum and nano-sized carbon are then added thereto Fiber is sintered after being uniformly mixed, during the sintering carries out under inert gas protection, first with 130 DEG C/it is small When rate be warming up to 480 DEG C, when keeping the temperature 1.5 hours, then 700 DEG C are warming up to 85 DEG C/h of rates, keep the temperature 2.5 hours；Sintering After being cooled down afterwards with 60 DEG C/h to obtain the final product.
Embodiment 2：Anode material for lithium-ion batteries weighs the following raw material：LiMn2O4 32g, nickel protoxide 38g, phosphoric acid are sub- Iron 46g, chrome green 12g, carbon nano-fiber 16g, electrically conductive graphite 8g, modified oxidized lanthanum 4.5g, zirconium fluoride 2g.
The preparation method of anode material for lithium-ion batteries is as follows：
（1）Chrome green, lanthana, zirconium fluoride are first sent into rotary furnace pre-burning, passes through 1.5 hours at room temperature, is warming up to 700 DEG C, heat preservation batch mixing 2 hours；Cooling is taken out, then uses abrasive media for absolute ethyl alcohol, wherein anhydrous added with being equivalent to 7.0% silicon carbide of ethyl alcohol weight, 11% aluminium powder, 2.5% magnesium stearate, 6% sodium lignin sulfonate；Grinding 8 hours controls mixture grain Diameter is 100 μm；
（2）LiMn2O4, nickel protoxide, ferrous phosphate are weighed, is placed in dissolution vessel, appropriate sulfurous acid is first added and is dissolved, Appropriate amount of deionized water, ultrasonic disperse processing are added, the ultrasonic disperse processing power is 500W, and temperature is 45 DEG C, ultrasound Processing time is 25min, is allowed to uniformly mixed and obtains solution；
（3）Lanthana is weighed, is ground, the lanthanum oxide powder that grain size is 50nm is obtained, the methyl silicon of 3 times of amounts is then added Oil is warming up to 75 DEG C, is dispersed with stirring, and is then added and is equivalent to 4% Silane coupling agent KH550 of lanthanum oxide powder quality, 5.5% 12 Sodium alkyl sulfonate is mixed and heated to 110 DEG C, and through filtering, washing, infrared drying obtains modified oxidized lanthanum powder, infrared ray Wavelength is 0.65nm, and drying temperature is 50 DEG C, drying time 25min；
（4）By above-mentioned steps（1）, step（2）All materials are uniformly mixed, and modified oxidized lanthanum and nano-sized carbon are then added thereto Fiber is sintered after being uniformly mixed, during the sintering carries out under protection of argon gas, first with 130 DEG C/h of speed Rate is warming up to 450 DEG C, when keeping the temperature 2 hours, then being warming up to 700 DEG C with 85 DEG C/h of rates, keeps the temperature 2.5 hours；With 60 after sintering DEG C/h cooling after to obtain the final product.
Embodiment 3：Anode material for lithium-ion batteries weighs the following raw material：LiMn2O4 42g, nickel protoxide 28g, phosphoric acid are sub- It is prepared by iron 48g, chrome green 11g, carbon nano-fiber 16g, electrically conductive graphite 8g, modified oxidized lanthanum 4.2g, zirconium fluoride 3.2g Method is such as embodiment 1 and embodiment 2.
Embodiment 4：Anode material for lithium-ion batteries weighs the following raw material：LiMn2O4 45g, nickel protoxide 33g, phosphoric acid are sub- It is prepared by iron 46g, chrome green 12g, carbon nano-fiber 17g, electrically conductive graphite 8.5g, modified oxidized lanthanum 4.8g, zirconium fluoride 4g Method is such as embodiment 1 and embodiment 2.
The anode material for lithium-ion batteries of the present invention has that high voltage, high power capacity, low consumption, self discharge be few, cycle-index The features such as more, it may be used on that mobile phone, laptop, video camera, digital camera etc. be numerous civilian and military field.
It is described above；It is merely preferred embodiments of the present invention；But scope of protection of the present invention is not limited thereto； Any one skilled in the art is in the technical scope disclosed by the present invention；According to the technique and scheme of the present invention and its It improves design and is subject to equivalent substitution or change；Should all it cover within the scope of the present invention.

Claims (7)

1. a kind of anode material for lithium-ion batteries, which is characterized in that according to mass fraction meter, constitutive material is：LiMn2O4 30- 50 parts, it is 20-40 parts of nickel protoxide, 35-55 parts of ferrous phosphate, 10-15 parts of chrome green, 15-20 parts of carbon nano-fiber, conductive 8-10 parts of graphite, lanthanum 4-5 parts modified oxidized, 2-4 parts of zirconium fluoride.
2. a kind of preparation method of anode material for lithium-ion batteries as described in claim 1, which is characterized in that specifically include with Lower content：
（1）Each raw material is weighed by the parts by weight of constitutive material, chrome green, electrically conductive graphite, zirconium fluoride are first sent into rotary furnace Pre-burning is passed through 1-2 hours at room temperature, is warming up to 650-800 DEG C, heat preservation batch mixing 2-3 hours；Cooling is taken out, then uses and grinds Grinding media is acetone soln, wherein added with acetone soln weight 6.0%-8.0% silicon carbide, 10%-12% aluminium powders, 2%- is equivalent to 3% magnesium stearate, 5%-8% sodium lignin sulfonates；Grinding 8-10 hours, control the stone size are 50-100 μm；
（2）LiMn2O4, nickel protoxide, ferrous phosphate are weighed, is placed in dissolution vessel, appropriate weak acid is first added and is dissolved, then Appropriate amount of deionized water is added, ultrasonic disperse processing is allowed to uniformly mixed and obtains solution；
（3）Lanthana is weighed, is ground, the lanthanum oxide powder that grain size is 50-80nm is obtained, the 3-4 times of first measured then is added Base silicone oil, is warming up to 70-80 DEG C, is dispersed with stirring, and is then added and is equivalent to lanthanum oxide powder quality 3%-5% silane coupling agents KH550,5.5%-6.0% dodecyl sodium sulfate, are mixed and heated to 100-120 DEG C, through filtering, wash, dry, obtain modified oxygen Change lanthanum powder；
（4）By above-mentioned steps（1）, step（2）All materials are uniformly mixed, and modified oxidized lanthanum and nano-sized carbon are then added thereto Fiber is sintered after being uniformly mixed, during the sintering carries out under inert gas protection, first with 120-140 DEG C/h rate is warming up to 450-500 DEG C, when keeping the temperature 1-2 hours, then 650-750 DEG C be warming up to 80-90 DEG C/h of rate, Heat preservation 2.5-3.0 hours；After being cooled down with 50-70 DEG C/h after sintering to obtain the final product.
3. the preparation method of anode material for lithium-ion batteries according to claim 2, which is characterized in that the step （2）Middle ultrasonic disperse processing power is 450-550W, and temperature is 40-50 DEG C, sonication treatment time 20-30min.
4. the preparation method of anode material for lithium-ion batteries according to claim 2, which is characterized in that the indifferent gas Body is preferably argon gas.
5. the preparation method of anode material for lithium-ion batteries according to claim 2, which is characterized in that the step （2）Middle weak acid is carbonic acid, acetic acid, sulfurous acid or formic acid.
6. the preparation method of anode material for lithium-ion batteries according to claim 2, which is characterized in that the grinding medium Matter acetone soln is substituted using ethanol solution.
7. the preparation method of anode material for lithium-ion batteries according to claim 2, which is characterized in that the step （3）Dry to use infrared drying, the wavelength of infrared ray is 0.6nm to 0.75nm, and drying temperature is 45-55 DEG C, when dry Between be 25-30min.
CN201810231389.9A 2018-03-20 2018-03-20 A kind of anode material for lithium-ion batteries and preparation method thereof Pending CN108493413A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109494361A (en) * 2018-10-29 2019-03-19 安徽五行动力新能源有限公司 A kind of anode material of lithium battery and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109494361A (en) * 2018-10-29 2019-03-19 安徽五行动力新能源有限公司 A kind of anode material of lithium battery and preparation method thereof

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