CN107128892A - A kind of preparation method of lithium iron manganese phosphate anode material - Google Patents
A kind of preparation method of lithium iron manganese phosphate anode material Download PDFInfo
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- CN107128892A CN107128892A CN201710438371.1A CN201710438371A CN107128892A CN 107128892 A CN107128892 A CN 107128892A CN 201710438371 A CN201710438371 A CN 201710438371A CN 107128892 A CN107128892 A CN 107128892A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 anode material for lithium-ion batteries technical field, specifically disclose a kind of preparation method of lithium iron manganese phosphate anode material, this method is sintered using source of iron, phosphorus source, manganese source, lithium source, carbon source and iron manganese phosphate for lithium is made, by in phosphorus source and source of iron, manganese source, lithium source input reactor, by being mixed admittedly containing 5% 60% input pure water stirrings；Carbon source is added by mass ratio 50% 200% is contained admittedly；Mixture stirs hybrid reaction in reactor at a temperature of 120 150 DEG C；Material is spray-dried；Material is calcined in nitrogen atmosphere；Material is subjected to tunnel drying.Material is directly uniformly mixed by the inventive method in autoclave pressure, saves traditional ball milling process, saves equipment investment and power consumption, reduces production cost；The a small amount of carbon of doping can effectively improve the performance of product；Direct spraying is dried after material reaction under high pressure, is reduced EAT, is effectively reduced energy consumption.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, and in particular to a kind of lithium iron manganese phosphate anode material
Preparation method.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, with voltage is high, energy density is big, good cycle, from
The many merits such as small, memory-less effect, the operating temperature range of discharging be wide, are widely used in mobile phone, notebook computer, number
Camera, video camera, electronic instrument etc., also have in fields such as UPS, electric tool, electric bicycle, electric automobile, energy-storage batteries
There is the application prospect of light.In recent years, the yield of lithium ion battery is skyrocketed through, and application field constantly expands, it has also become two
The eleventh century new high-tech product significant to national economy and people's lives.
At present, lithium ion battery has reached its maturity in the compact battery field of portable type electronic product, and application is just
Progressively to middle Large Copacity, in high-power power type and accumulation energy type field of batteries expand.Positive electrode is the weight of lithium ion battery
Part is wanted, its performance largely determines the combination property of battery.Positive electrode is studied and performance improvement is lithium
One of core of ion battery development.
Mainly lithium ion is used as currently as lithium ion anode material including LiCoO2, LiNiO2, LiMn2O4, LiFePO4
Cell positive material is extensively studied.LiFePO4 wherein by goodenough seminars proposition in 1997 is low with price
Honest and clean, abundance, the reason such as good cycling stability is considered to have one of anode material for lithium-ion batteries of development prospect.By
In using voltage only 3.2V, high rate performance is not enough, and electrical conductivity is low, it is impossible to meets the requirement of high-energy electrokinetic cell, limits
It further develops.Improving the method for specific energy has two kinds：Find the higher positive electrode of specific capacity；Improve the work electricity of material
Pressure.LiMnPO4 cyclical stabilities for LiFePO4 are weaker, but with higher (being 3.8V), the self discharge using voltage
Rate is low, and material is ripe, the characteristics of cost is low.Require that both Fe and Mn can be combined by characteristic according to electrokinetic cell, have both concurrently
Advantage, the LiFePO4 adulterated using Mn is as lithium ion anode material-iron manganese phosphate for lithium (LiMnxFe1-xPO4), at this
Plant in material, Mn3+/Mn2+4.0V or so operating voltages are located between the two, Li insertions can be realized and deviate from, before having more
Scape is that the general electrolyte of in the market can keep stabilization not decompose in 4.0V voltage ranges, also will not be because of brownout
Reduce specific energy.Therefore LiMnxFe1-xPO4 positive electrodes become the new study hotspot of people.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of lithium ferric manganese phosphate positive pole material in view of the shortcomings of the prior art
The preparation method of material, be sintered using source of iron, phosphorus source, manganese source, lithium source, carbon source and iron manganese phosphate for lithium be made, it is to avoid phosphate
The processing of the salt of a large amount of by-products when producing ferric phosphate with molysite, while the effectively energy consumption of reduction production, reduces industrial water, reach
Energy-saving purpose.
In order to solve the above technical problems, a kind of preparation method of lithium iron manganese phosphate anode material of the invention, preparation method is such as
Under：
S1, phosphorus source and source of iron, manganese source, lithium source put into reactor, mixed by 5%-60% input pure water stirrings are contained admittedly；
S2, by 50%-200% containing mass ratio admittedly add carbon source into mixed solution obtained by S1；
S3, mixture obtained by S2 stirred into hybrid reaction 1-3h in reactor at a temperature of 120-150 DEG C；
S4, S3 resulting materials are spray-dried, 120-150 DEG C of EAT, 100-120 DEG C of outlet temperature；
S5, spray-dried material calcined in nitrogen atmosphere；
S6, by obtained by S5 material carry out tunnel drying, dry after the completion of obtain lithium iron manganese phosphate anode material.
Further, phosphorus source, manganese source, source of iron and lithium source mol ratio are 0.95-1.05：x：1-x：1, wherein 0.2≤x
≤0.6。
Specifically, phosphorus source is the one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate or phosphoric acid.
Specifically, the lithium source is the one or more in lithium hydroxide, lithium carbonate, lithium acetate or lithium oxalate.
Specifically, the manganese source is one kind in manganese carbonate, manganese dioxide, mangano-manganic oxide, manganous hydroxide or manganese nitrate
Or it is a variety of；
Specifically, the source of iron is the one or more of ferric phosphate, ferrous phosphate, ironic citrate or ferric acetate.
Specifically, the carbon source is trimethylolpropane, pentaerythrite, bipentaerythrite polyalcohol or electrically conductive graphite, carbon
One or more in nanotube, graphene, sucrose, glucose, fructose, citric acid, polyvinyl alcohol, polyethylene glycol and polyethers.
Further, calcining heat described in S5 is 700-950 DEG C, and calcination time is 5-12h.
Further, drying temperature described in S6 is 120-150 DEG C.
The beneficial effects of the invention are as follows：
1) material is directly uniformly mixed in autoclave pressure, saves traditional ball milling process, save equipment investment with
Power consumption, reduces production cost；
2) a small amount of carbon that adulterates can effectively improve the performance of product；
3) Direct spraying is dried after material reaction under high pressure, is reduced EAT, is effectively reduced energy consumption.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained on the premise of creative work is not made, belongs to what the present invention was protected
Scope.
In the specific embodiment of the present invention, a kind of preparation method of lithium iron manganese phosphate anode material is disclosed, is prepared
Method is as follows：
S1,0.2mol ammonium dihydrogen phosphates and 0.08mol ferric acetates, 0.12mol manganese carbonates, 0.2mol lithium carbonates put into it is anti-
Answer in kettle, mixed by 30% input pure water stirring is contained admittedly；
S2, add polyethylene glycol by containing mass ratio 5% admittedly into mixed solution obtained by S1；
S3, mixture obtained by S2 stirred into hybrid reaction 1h in reactor at a temperature of 150 DEG C；
S4, S3 resulting materials are fed directly to spray dryer be spray-dried, 120 DEG C of EAT, outlet temperature
100 DEG C of degree；
S5, spray-dried material calcined in nitrogen atmosphere, 950 DEG C of calcining heat, calcination time 8h；
S6, the material obtained by S5 carries out to a tunnel drying again, drying temperature is 120 DEG C, can be obtained after the completion of drying
To lithium iron phosphate positive material.
A certain proportion of iron manganese phosphate lithium material, polyvinyl chloride, nmp solvent, conductive black etc. are mixed, through ultrasound
The scattered laggard step of mixing is stirred 3-5h and fully mixes to obtain slurry, slurry is applied on aluminium foil front, drying is obtained just
Pole pole piece.Suitable diameter is cut into, using lithium paper tinsel as to electrode, button cell is assembled into the glove box full of argon gas, with
Constant current carries out charge-discharge test, and charging/discharging voltage is 2.5-4.2V, the specific capacity of test material difference discharge-rate and circulation
Performance.
Measure the lithium iron manganese phosphate anode material room temperature and measure discharge performance of the iron manganese phosphate for lithium under different multiplying, 0.1C
Averaged discharge specific capacity is 188mAh/g under multiplying power, and averaged discharge specific capacity is average under 178mAh/g, 10C multiplying powers under 1C multiplying powers
Specific discharge capacity 120mAh/g.
In another specific embodiment of the present invention, a kind of preparation method of lithium iron manganese phosphate anode material is disclosed, is made
Preparation Method is as follows：
S1,0.21mol phosphoric acid and 0.14mol ferric nitrates, 0.06mol manganous hydroxides, 0.2mol lithium hydroxides put into it is anti-
Answer in kettle, mixed by 10% input pure water stirring is contained admittedly；
S2, by adding citric acid into above-mentioned mixed solution containing mass ratio 80% admittedly；
S3, mixture obtained by S2 stirred into hybrid reaction 2h in reactor at a temperature of 120 DEG C；
S4, S3 resulting materials are fed directly to spray dryer be spray-dried, 150 DEG C of EAT, outlet temperature
120 DEG C of degree；
S5, spray-dried material calcined in nitrogen atmosphere, 800 DEG C of calcining heat, calcination time 10h；
S6, the material obtained by S5 carries out to a tunnel drying again, drying temperature is 120 DEG C, can be obtained after the completion of drying
To lithium iron phosphate positive material.
A certain proportion of iron manganese phosphate lithium material, polyvinyl chloride, nmp solvent, conductive black etc. are mixed, through ultrasound
The scattered laggard step of mixing is stirred 3-5h and fully mixes to obtain slurry, slurry is applied on aluminium foil front, drying is obtained just
Pole pole piece.Suitable diameter is cut into, using lithium paper tinsel as to electrode, button cell is assembled into the glove box full of argon gas, with
Constant current carries out charge-discharge test, and charging/discharging voltage is 2.5-4.2V, the specific capacity of test material difference discharge-rate and circulation
Performance.
Measure the lithium iron manganese phosphate anode material room temperature and measure discharge performance of the iron manganese phosphate for lithium under different multiplying, 0.1C
Averaged discharge specific capacity is 182mAh/g under multiplying power, and averaged discharge specific capacity is average under 180mAh/g, 10C multiplying powers under 1C multiplying powers
Specific discharge capacity 118mAh/g.
In another specific embodiment of the present invention, a kind of preparation method of lithium iron manganese phosphate anode material is disclosed, is made
Preparation Method is as follows：
S1,0.19mol phosphoric acid and 0.16mol ferric nitrates, 0.04mol manganese dioxide, 0.2mol lithium carbonates input reacted
In kettle, mixed by 30% input pure water stirring is contained admittedly；
S2, add pentaerythrite by containing mass ratio 100% admittedly into mixed solution obtained by S1；
S3, mixture obtained by S2 stirred into hybrid reaction 2h in reactor at a temperature of 140 DEG C；
S4, S3 resulting materials are fed directly to spray dryer be spray-dried, 150 DEG C of EAT, outlet temperature
120 DEG C of degree；
S5, spray-dried material calcined in nitrogen atmosphere, 700 DEG C of calcining heat, calcination time 12h；
S6, the material obtained by S5 carries out to a tunnel drying again, drying temperature is 120 DEG C, can be obtained after the completion of drying
To lithium iron phosphate positive material.
A certain proportion of iron manganese phosphate lithium material, polyvinyl chloride, nmp solvent, conductive black etc. are mixed, through ultrasound
The scattered laggard step of mixing is stirred 3-5h and fully mixes to obtain slurry, slurry is applied on aluminium foil front, drying is obtained just
Pole pole piece.Suitable diameter is cut into, using lithium paper tinsel as to electrode, button cell is assembled into the glove box full of argon gas, with
Constant current carries out charge-discharge test, and charging/discharging voltage is 2.5-4.2V, the specific capacity of test material difference discharge-rate and circulation
Performance.
Measure the lithium iron manganese phosphate anode material room temperature and measure discharge performance of the iron manganese phosphate for lithium under different multiplying, 0.1C
Averaged discharge specific capacity is 186mAh/g under multiplying power, and averaged discharge specific capacity is average under 181mAh/g, 10C multiplying powers under 1C multiplying powers
Specific discharge capacity 126mAh/g.
The beneficial effects of the invention are as follows：
1) material is directly uniformly mixed in autoclave pressure, saves traditional ball milling process, save equipment investment with
Power consumption, reduces production cost；
2) a small amount of carbon that adulterates can effectively improve the performance of product；
3) Direct spraying is dried after material reaction under high pressure, is reduced EAT, is effectively reduced energy consumption.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (9)
1. a kind of preparation method of lithium iron manganese phosphate anode material, it is characterised in that preparation method is as follows：
S1, phosphorus source and source of iron, manganese source, lithium source put into reactor, mixed by 5%-60% input pure water stirrings are contained admittedly；
S2, by 50%-200% containing mass ratio admittedly add carbon source into mixed solution obtained by S1；
S3, mixture obtained by S2 stirred into hybrid reaction 1-3h in reactor at a temperature of 120-150 DEG C；
S4, S3 resulting materials are spray-dried, 120-150 DEG C of EAT, 100-120 DEG C of outlet temperature；
S5, spray-dried material calcined in nitrogen atmosphere；
S6, by obtained by S5 material carry out tunnel drying, dry after the completion of obtain lithium iron manganese phosphate anode material.
2. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 1, it is characterised in that the phosphorus
Source, manganese source, source of iron and lithium source mol ratio are 0.95-1.05：x：1-x：1, wherein 0.2≤x≤0.6.
3. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 2, it is characterised in that phosphorus source
For the one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate or phosphoric acid.
4. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 2, it is characterised in that the lithium source
For the one or more in lithium hydroxide, lithium carbonate, lithium acetate or lithium oxalate.
5. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 2, it is characterised in that the manganese source
For the one or more in manganese carbonate, manganese dioxide, mangano-manganic oxide, manganous hydroxide or manganese nitrate.
6. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 2, it is characterised in that the source of iron
For the one or more of ferric phosphate, ferrous phosphate, ironic citrate or ferric acetate.
7. a kind of preparation method of lithium iron manganese phosphate anode material according to claim 1, it is characterised in that the carbon source
For trimethylolpropane, pentaerythrite, bipentaerythrite polyalcohol or electrically conductive graphite, CNT, graphene, sucrose, grape
One or more in sugar, fructose, citric acid, polyvinyl alcohol, polyethylene glycol and polyethers.
8. the preparation method of a kind of lithium iron manganese phosphate anode material according to claim 1, it is characterised in that described in S5
Calcining heat is 700-950 DEG C, and calcination time is 5-12h.
9. the preparation method of a kind of lithium iron manganese phosphate anode material according to claim 1, it is characterised in that described in S6
Drying temperature is 120-150 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108832119A (en) * | 2018-06-14 | 2018-11-16 | 方嘉城 | A kind of preparation method of carbon doping phosphoric acid ferrimanganic lithium |
| CN109264691A (en) * | 2018-10-19 | 2019-01-25 | 广东光华科技股份有限公司 | A method of iron manganese phosphate for lithium is prepared by LiFePO4 |
| CN109888205A (en) * | 2019-01-18 | 2019-06-14 | 北方奥钛纳米技术有限公司 | Receive microspheroidal carbon coating iron manganese phosphate for lithium composite material and preparation method, anode material of lithium battery, lithium battery |
| CN115676792A (en) * | 2022-07-06 | 2023-02-03 | 宜宾天原锂电新材有限公司 | Method for preparing iron-based phosphate lithium battery material by using phosphorus iron slag as raw material |
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| CN109888205A (en) * | 2019-01-18 | 2019-06-14 | 北方奥钛纳米技术有限公司 | Receive microspheroidal carbon coating iron manganese phosphate for lithium composite material and preparation method, anode material of lithium battery, lithium battery |
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