CN106129366A - A kind of anode material of lithium battery and preparation method thereof - Google Patents
A kind of anode material of lithium battery and preparation method thereof Download PDFInfo
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- CN106129366A CN106129366A CN201610709205.6A CN201610709205A CN106129366A CN 106129366 A CN106129366 A CN 106129366A CN 201610709205 A CN201610709205 A CN 201610709205A CN 106129366 A CN106129366 A CN 106129366A
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- lithium
- lithium battery
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- anode material
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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
- H01M4/366—Composites as layered products
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
- H01M4/623—Binders being polymers fluorinated polymers
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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Abstract
The present invention relates to battery material technical field, especially a kind of anode material of lithium battery and preparation method thereof, it is raw material by using LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent, it is fabricated to anode material of lithium battery, its preparation technology is simple, and energy consumption is low, low cost, and can effectively improve the chemical property of battery, extend the service life of battery.
Description
Technical field
The present invention relates to battery material technical field, especially a kind of anode material of lithium battery and preparation method thereof.
Background technology
Currently, lithium battery, due to advantages such as its energy density height, operating temperature width, life-span length, is widely used.And for
For lithium battery, its of paramount importance ingredient is positive electrode, and positive electrode decides the characteristic of lithium battery, its electrode material
The quality of material performance, it will affect the quality of lithium battery.
In prior art, the positive electrode of lithium battery is mostly cobalt acid lithium, LiMn2O4 or ternary material etc., and its component is main
It is to use active material to add conductive agent, then adds bonding agent so that the lithium battery of acquisition has the spy that capacity is high, have extended cycle life
Point, but the resource such as manganese, cobalt is the deficientest, expensive, and there is toxicity, easily cause the pollution of environment；In addition,
The most of positive electrodes used in prior art, the phase after discharge, its voltage decrease speed is the fastest so that lithium battery is rear
Continue and be difficult to meet the demand of production application, greatly hinder lithium battery and advance；In consideration of it, prior art occurs in that phosphoric acid
Lithium iron battery positive electrode, its security performance is the most excellent with service life, but, LiFePO4 bulk density is relatively low, electric conductivity
Can be poor so that when LiFePO4 is applied in lithium battery, researchers mix the material with carbon elements such as electrically conductive graphite wherein, in this,
The bulk density that result in LiFePO4 greatly declines so that its bulk density only only has 1-1.2g/cm3, compare
Bulk density 2-2.4g/cm of cobalt acid lithium3For, it is nothing like cobalt acid lithium so that the volume of the lithium battery of making is relatively big, difficult
To apply in actual production；And by doping electrically conductive graphite so that with LiFePO4 formed point cantact, and in order to
Make electric conductivity more excellent so that doping is relatively big, so that the volume of positive electrode that LiFePO4 is prepared as raw material
Also increase.
To this end, have researcher to use include lithium iron phosphate/carbon nanotube complex, and cover Graphene in this composite surface
Nanometer sheet so that tap density and the electric conductivity of LiFePO4 are all improved, but its relatively costly in manufacturing process,
Especially cover the operation easier of graphene nanometer sheet relatively greatly in composite surface, relatively costly.
Summary of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provide a kind of anode material of lithium battery and
Preparation method.
It is achieved particular by techniques below scheme:
A kind of anode material of lithium battery, is former with LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent
Material, is LiFePO4 5-10 part, ferric nitrate lithium 2-3 part, Iron sulfuret. 1-3 part, rare earth metal 0.00001-in parts by weight
0.00005 part, bonding agent 4-8 part.
Described raw material, is LiFePO4 8 parts, ferric nitrate lithium 2.5 parts, Iron sulfuret. 2 parts, rare earth gold in parts by weight
Belong to 0.00003 part, bonding agent 6 parts.
Above-mentioned anode material of lithium battery preparation method, after being mixed with LiFePO4 by Iron sulfuret., in noble gas
Using temperature is 200-270 DEG C of heat treated 2-4h, then is placed in ferric nitrate lithium, after stirring, adds rare earth metal
And bonding agent, mix and blend 3-7h, it is thus achieved that.
Described noble gas is the one in nitrogen, helium, argon.
Described bonding agent be Kynoar be that 1:0.15-0.31 mixes with N methyl pyrrolidone according to mass ratio
Mixture.
A kind of anode material of lithium battery preparation method, is to be 5-10:2-3 with Iron sulfuret. according to mass ratio by LiFePO4
After mixing, being placed in during temperature is 180-250 DEG C, after heat treated 1-3h, then the sulphuric acid being used mass concentration to be 3-7% is molten
Immersion bubble 0.5-1.3h, then by after its filtration drying, add ferric nitrate lithium, ferric nitrate lithium is 2-3 with the mass ratio of Iron sulfuret.:
1-3, stirs 10-20min, and addition accounts for the rare earth metal of Iron sulfuret. quality 0.2-0.5% and is 4-with Iron sulfuret. mass ratio
The bonding agent of 8:1-3, stirring mixing 2-3h, it is thus achieved that.
Compared with prior art, the technique effect of the present invention is embodied in:
It is raw material by using LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent, is fabricated to lithium battery
Positive electrode, its preparation technology is simple, and energy consumption is low, low cost, and can effectively improve the chemical property of battery, extends
The service life of battery.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is further limited, but claimed
Scope is not only limited to description.
The addition of the bonding agent in following example is can be fully by material mix homogeneously, and the amount of being preferably added to is
Account for 0.3-0.6 times of ferrous disulfide quality.
Embodiment 1
A kind of anode material of lithium battery, is former with LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent
Material, is calculated as LiFePO4 5kg, ferric nitrate lithium 2kg, Iron sulfuret. 1kg, rare earth metal 0.00001kg, bonding agent according to weight
4kg。
Above-mentioned anode material of lithium battery preparation method, after being mixed with LiFePO4 by Iron sulfuret., in noble gas
Using temperature is 200 DEG C of heat treated 2h, then is placed in ferric nitrate lithium, after stirring, adds rare earth metal and bonding
Agent, mix and blend 3h, it is thus achieved that.Described noble gas is the one in nitrogen, helium, argon.The present embodiment uses nitrogen.Institute
The bonding agent stated be Kynoar be the mixture that 1:0.15 mixes with N methyl pyrrolidone according to mass ratio.
This positive electrode is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, draw electric discharge specific volume
Amount is 213mAh g-1, and carry out 100 times circulation discharge process after, its specific discharge capacity is 198mAh g-1。
Embodiment 2
A kind of anode material of lithium battery, is former with LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent
Material, is calculated as LiFePO4 10kg, ferric nitrate lithium 3kg, Iron sulfuret. 3kg, rare earth metal 0.00005kg, bonding agent according to weight
8kg。
Above-mentioned anode material of lithium battery preparation method, after being mixed with LiFePO4 by Iron sulfuret., in noble gas
Using temperature is 270 DEG C of heat treated 4h, then is placed in ferric nitrate lithium, after stirring, adds rare earth metal and bonding
Agent, mix and blend 7h, it is thus achieved that.Described noble gas is the one in nitrogen, helium, argon.The helium that the present embodiment uses.
Described bonding agent be Kynoar be that 1:0.31 mixes with N methyl pyrrolidone according to mass ratio
Mixture.
This positive electrode is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, draw electric discharge specific volume
Amount is for 208mAh g-1, and after carrying out 100 circulation discharge process, its specific discharge capacity is 199mAh g-1.
Embodiment 3
A kind of anode material of lithium battery, is former with LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, bonding agent
Material, is calculated as LiFePO4 8kg, ferric nitrate lithium 2.5kg, Iron sulfuret. 2kg, rare earth metal 0.00003kg, bonding agent according to weight
6kg。
Above-mentioned anode material of lithium battery preparation method, after being mixed with LiFePO4 by Iron sulfuret., in noble gas
Using temperature is 250 DEG C of heat treated 3h, then is placed in ferric nitrate lithium, after stirring, adds rare earth metal and bonding
Agent, mix and blend 5h, it is thus achieved that.Described noble gas is the one in nitrogen, helium, argon.The present embodiment uses argon
Gas.
Described bonding agent be Kynoar be that 1:0.23 mixes with N methyl pyrrolidone according to mass ratio
Mixture.
This positive electrode is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, draw electric discharge specific volume
Amount is for 215mAh g-1, and after carrying out 100 circulation discharge process, its specific discharge capacity is 201mAh g-1.
Comparative example 1
It is raw material only with LiFePO4, and according to the proportioning of embodiment 1, by LiFePO4 and rare earth metal, bonding
Agent is processed being fabricated to positive electrode according to the preparation method of embodiment 1, then is made into 2025 button cells, and by it
Cycle charge discharge electrical property detect, show that specific discharge capacity is 165mAh g-1, and carry out 100 times circulation discharge process after, it is put
Electricity specific capacity is 148mAh g-1.
Comparative example 2
Only with ferrous disulfide as raw material, according to the proportioning in embodiment 2, by ferrous disulfide and rare earth gold
Belong to, bonding agent is processed being fabricated to positive electrode according to the preparation method of embodiment 2, then is made into 2025 button electricity
Pond, and it is recycled charge-discharge performance detection, show that specific discharge capacity is 200mAh g-1, and carry out at 100 circulation electric discharges
After reason, its specific discharge capacity is 150mAh g-1.
Comparative example 3
It is raw material only with LiFePO4, Iron sulfuret., according to the proportioning of embodiment 3, by Iron sulfuret., iron phosphate
Lithium, rare earth metal, bonding agent mix, and are processed being fabricated to positive electrode according to the preparation method of embodiment 3, then are made
Become 2025 button cells, and be recycled charge-discharge performance detection, show that specific discharge capacity is 209mAh g-1, and carry out 100
After secondary circulation discharge process, its specific discharge capacity is 167mAh g-1.
To sum up, comparative example 1-3 and embodiment 1-3 after positive electrode being fabricated to button cell, then carried out
Cycle charge discharge electrical property detects, and its result shows, the invention can significantly improve initial discharge specific capacity, and is following
After ring 100 times, the rate of change of its charging and discharging capacity is significantly lower than comparative example 1-3, it is seen then that it can significantly extend making of battery
With the life-span, improve the performance of anode material of lithium battery.
In addition, this researcher also to the material composition used in the invention, is carried out according to following preparation method
After process, it is thus achieved that anode material of lithium battery.
Embodiment 4
A kind of anode material of lithium battery preparation method, is to be that 5:2 mix with Iron sulfuret. according to mass ratio by LiFePO4
After, being placed in temperature is in 180 DEG C, and after heat treated 1h, then the sulfuric acid solution being used mass concentration to be 3% soaks 0.5h,
Again by after its filtration drying, adding ferric nitrate lithium, ferric nitrate lithium is 2:1 with the mass ratio of Iron sulfuret., stirs 10min, adds
Account for the rare earth metal of Iron sulfuret. quality 0.2% and be the bonding agent of 4:1 with Iron sulfuret. mass ratio, stirring mixing 2h, it is thus achieved that.
The bonding agent that bonding agent is embodiment 1 used.
It is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, show that specific discharge capacity is 203mAh
G-1, and carry out 100 times circulation discharge process after, its specific discharge capacity is 189mAh g-1.
Embodiment 5
A kind of anode material of lithium battery preparation method, is to be that 10:3 mix with Iron sulfuret. according to mass ratio by LiFePO4
After, being placed in temperature is in 250 DEG C, and after heat treated 3h, then the sulfuric acid solution being used mass concentration to be 7% soaks 1.3h,
Again by after its filtration drying, adding ferric nitrate lithium, ferric nitrate lithium is 1:1 with the mass ratio of Iron sulfuret., stirs 20min, adds
Account for the rare earth metal of Iron sulfuret. quality 0.5% and be the bonding agent of 8:3 with Iron sulfuret. mass ratio, stirring mixing 3h, it is thus achieved that.
The bonding agent using bonding agent to be embodiment 2.
It is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, show that specific discharge capacity is 211mAh
G-1, and carry out 100 times circulation discharge process after, its specific discharge capacity is 188mAh g-1.
Embodiment 6
A kind of anode material of lithium battery preparation method, is to be that 7:3 mix with Iron sulfuret. according to mass ratio by LiFePO4
After, being placed in temperature is in 190 DEG C, and after heat treated 2h, then the sulfuric acid solution being used mass concentration to be 5% soaks 0.9h,
Again by after its filtration drying, adding ferric nitrate lithium, ferric nitrate lithium is 2:3 with the mass ratio of Iron sulfuret., stirs 15min, adds
Account for the rare earth metal of Iron sulfuret. quality 0.4% and be the bonding agent of 7:2 with Iron sulfuret. mass ratio, stirring mixing 2.5h, obtains
?.The bonding agent using bonding agent to be embodiment 3.
It is fabricated to 2025 button cells, and is recycled charge-discharge performance detection, show that specific discharge capacity is 213mAh
G-1, and carry out 100 times circulation discharge process after, its specific discharge capacity is 197mAh g-1.
In above-described embodiment 4-6, in particular during a heating process, lower inert gas environment is carried out, employing lazy
The nitrogen of property gas.
Above example is only limitted to the concrete technical scheme of the present invention is made further explanation, in order to this area skill
This scheme is understood by art personnel, and essential characteristics and the non-significant of the non-protruding that those skilled in the art make on this basis are entered
The improvement of step, belongs to the protection category of the present invention.
Claims (6)
1. an anode material of lithium battery, it is characterised in that with LiFePO4, ferric nitrate lithium, Iron sulfuret., rare earth metal, glue
Connecing agent is raw material, is LiFePO4 5-10 part, ferric nitrate lithium 2-3 part, Iron sulfuret. 1-3 part, rare earth metal in parts by weight
0.00001-0.00005 part, bonding agent 4-8 part.
2. anode material of lithium battery as claimed in claim 1, it is characterised in that described raw material, is phosphorus in parts by weight
Acid ferrum lithium 8 parts, ferric nitrate lithium 2.5 parts, Iron sulfuret. 2 parts, 0.00003 part of rare earth metal, bonding agent 6 parts.
3. anode material of lithium battery preparation method as claimed in claim 1 or 2, it is characterised in that by Iron sulfuret. and phosphoric acid
After the mixing of ferrum lithium, using temperature in noble gas is 200-270 DEG C of heat treated 2-4h, then is placed in ferric nitrate lithium,
After stirring, add rare earth metal and bonding agent, mix and blend 3-7h, it is thus achieved that.
4. anode material of lithium battery preparation method as claimed in claim 3, it is characterised in that described noble gas is nitrogen
One in gas, helium, argon.
5. anode material of lithium battery preparation method as claimed in claim 3, it is characterised in that described bonding agent is poly-inclined fluorine
Ethylene and N methyl pyrrolidone are the mixture that 1:0.15-0.31 mixes according to mass ratio.
6. an anode material of lithium battery preparation method, it is characterised in that be according to mass ratio by LiFePO4 and Iron sulfuret.
After mixing for 5-10:2-3, being placed in during temperature is 180-250 DEG C, after heat treated 1-3h, then to be used mass concentration be 3-
The sulfuric acid solution of 7% soaks 0.5-1.3h, then by after its filtration drying, adds ferric nitrate lithium, ferric nitrate lithium and Iron sulfuret.
Mass ratio is 2-3:1-3, stir 10-20min, add account for Iron sulfuret. quality 0.2-0.5% rare earth metal and with sulfuration Asia
Weight of iron is than the bonding agent for 4-8:1-3, stirring mixing 2-3h, it is thus achieved that.
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Cited By (1)
| 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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| CN105591104A (en) * | 2016-01-21 | 2016-05-18 | 河南师范大学 | Lithium iron phosphate electrode for alkaline secondary cell cathode and preparation method of lithium iron phosphate electrode |
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| US20040191617A1 (en) * | 2002-10-15 | 2004-09-30 | Polyplus Battery Company | Ionically conductive membranes for protection of active metal anodes and battery cells |
| CN102427134A (en) * | 2011-12-02 | 2012-04-25 | 湘潭大学 | Mixed conductor composite material LiFePO4-MXy and preparation method thereof |
| CN103972502A (en) * | 2014-04-02 | 2014-08-06 | 芜湖浙鑫新能源有限公司 | Modified cathode material for lithium battery |
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| 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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Application publication date: 20161116 |