CN101764203A - Method for preparing high-density lithium iron manganese phosphate for lithium ion battery positive electrode material - Google Patents
Method for preparing high-density lithium iron manganese phosphate for lithium ion battery positive electrode material Download PDFInfo
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- CN101764203A CN101764203A CN200910019099A CN200910019099A CN101764203A CN 101764203 A CN101764203 A CN 101764203A CN 200910019099 A CN200910019099 A CN 200910019099A CN 200910019099 A CN200910019099 A CN 200910019099A CN 101764203 A CN101764203 A CN 101764203A
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Abstract
The invention relates to a method for preparing high-density lithium iron manganese phosphate for a lithium ion battery positive electrode material, and belongs to the technical field of new energy materials. The preparation method mainly comprises the following steps of: using ferric iron as a raw material; mixing the ferric iron and a manganese source, a phosphorous source and a reducer; adding aqueous solution of ammonia into the mixture to perform reaction to synthesize a precursor of the lithium iron manganese phosphate; and sintering the precursor and the lithium source in protective atmosphere at a high temperature to obtain lithium iron manganese phosphate powder with high bulk density, good electrical conductivity and high specific capacity. The method has the advantages of simple process, convenient implementation, obvious effect and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material, it belongs to energy new material technology field.
Background technology
Lithium ion battery is a kind of green high-capacity battery, and development in the last few years is very rapid, is mainly used in various portable type electronic products and communication tool etc., is with a wide range of applications.Anode material for lithium-ion batteries is the important component part of lithium ion battery, and the development of novel anode material becomes the research focus.The maximum positive electrode of research has LiCoO2, LiNiO2, LiMn2O4 etc. at present.LiCoO2 toxicity is big, costs an arm and a leg, and has certain safety problem; The LiNiO2 cost is low, and capacity is higher, but the preparation difficulty, and also there is safety problem in the poor reproducibility of thermal stability and material; Spinelle LiMn2O4 cost is low, and security performance is good, but capacity is low, and cycle performance especially high temperature cyclic performance is poor.Therefore, novel good positive electrode research becomes the trend that present anode material for lithium-ion batteries is studied.
LiFePO4 LiFeO4 positive electrode has been concentrated LiCoO2, LiNiO2, LiMn2O4 three's advantage, and is cheap, Stability Analysis of Structures, and fail safe is good, and operating voltage is moderate, and theoretical capacitance is big, and the avirulence environmentally safe is a kind of real green material.LiFeO4 exists in the form of occurring in nature with triphylite, has orderly olivine structural.Its structures shape its have very strong thermodynamics and kinetics stability, but also exist the low and low shortcoming of bulk density of tangible conductivity.These two shortcomings have hindered the practical application of material.
At present, major measure has on the low problem of solution conductivity: mix electric conducting material or conductive metal particle in LiFePO4 inside, perhaps at LiFePO4 surface coated with conductive material with carbon element; In the lattice of LiFePO4, mix a spot of metal ion, replace the position of a part of Li+, make the LiFePO4 intrinsic semiconductor change n type or p N-type semiconductor N into, improve the material electronics conductance; Impurity element such as doped with Mn 2+ in LiFePO4 replaces the position of a part of Fe2+, and synthetic iron manganese phosphate for lithium improves the lithium ion conductivity of material.
The shortcoming that the LiFePO4 bulk density is low also is a difficult point problem of needing solution badly.The solid density of LiFePO4 is 3.6g/cm3, in order to improve conductivity, mix the bulk density that conductive carbon material can reduce material again, volume and capacity ratio reduces many, therefore, the bulk density and the volume and capacity ratio of raising LiFePO4 are significant to its application.At present, the lithium iron phosphate positive material of report is made up of random sheet or granular solid matter mostly both at home and abroad, and bulk density is lower.And the bulk density of powder is relevant with granule-morphology, particle size and the distribution thereof of powder.Therefore, the powder body material of the LiFePO4 that the spheric granules of preparation rule is formed will improve its bulk density greatly.
Summary of the invention
Purpose of the present invention just is to overcome and avoid the shortcoming and defect of prior art, and a kind of preparation method of novel with low cost, the simple high-density lithium iron manganese phosphate for lithium ion battery positive electrode material of technology is provided.
The present invention adopts following technical measures to realize its goal of the invention.
A kind of preparation method of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material, the process of its preparation method is as follows:
(1), preparation ferric iron, manganese source, phosphorus source, reducing agent mixed aqueous solution, wherein the total concentration of iron and manganese is the 0.2-2 mol, 0＜manganese/(iron+manganese)≤40% (molar percentage), the concentration of phosphorus is phosphorus: (iron+manganese)=(1.1-2.0): 1 (mol ratio), reductant concentration are reducing agent: (iron+manganese)=(0.01-0.3): 1 (mol ratio).
(2), compound concentration is the ammonia spirit of 3-10 mol.
(3), with above-mentioned ferric iron, manganese source, phosphorus source, reducing agent mixed aqueous solution, ammonia spirit is input to respectively in the reactor of belt stirrer continuously with pump, the temperature of control reactor internal reaction liquid is 50-90 ℃; 120 milliliters in constant ferrous sulfate, manganese source, phosphorus source, reducing agent mixed aqueous solution/time flow, regulate the flow of ammonia spirit simultaneously, make the pH value of reactor internal reaction liquid be 5.0-8.0.
(4), step 3) gained material changed over to carry out Separation of Solid and Liquid in the solid-liquid separator, with the solid product of deionized water wash Separation of Solid and Liquid gained; Product after the washing in 80-100 ℃ of dry 2-4 hour, obtains manganese phosphate ferrous ammonium precursor (NH in drier
4Fe
1-xMn
xPO
4H
2O, 0＜x≤0.4).
(5), the lithium source is mixed with deionized water, made slurry and in ball mill in ball milling 2-4 hour with mass ratio 1: 1.
(6), in " Li: (Fe+Mn): P=1: the ratio of 1: 1 (mol ratio) takes by weighing spherical manganese phosphate ferrous ammonium of step (4) gained and step (5) gained lithium source slurry and mixes.
(7), step (6) products therefrom is placed stove, under protective atmosphere, be warming up to 500-900 ℃, constant temperature 12-48 hour, natural cooling in stove obtained iron manganese phosphate for lithium (LiFe
1-xMn
xPO
4, 0＜x≤0.4).
In the phosphorus source described in above-mentioned preparation method's the process a kind of in phosphoric acid, ammonium dihydrogen phosphate and the diammonium hydrogen phosphate; Described reducing agent is a kind of in the dextrose plus saccharose; Described ferric iron source is a kind of in di-iron trioxide, the ferric phosphate; Described lithium source is a kind of in lithium carbonate, lithium hydroxide, lithium oxalate, lithium phosphate, lithium acetate, the lithium nitrate; Described manganese salt is a kind of in manganese sulfate, the manganese nitrate; Described protective atmosphere is the mist of nitrogen or nitrogen and hydrogen or nitrogen and argon gas.
Adopt ferric iron as source of iron in the present invention, cost of material is cheap, has avoided ferrous salt synthesis step loaded down with trivial details in the synthetic method, has solved the problem of the easy oxidation of ferrous salt.Reducing agent is reduced into divalence with ferric iron in the course of reaction, and the ferrous iron activity that generates in the process is good, and is fast with the reaction speed in phosphorus source and lithium source, in conjunction with stable, and the product purity height of generation.
The phosphoric acid LiMn2O4 average grain diameter that the present invention obtains is 8-14um, even particle distribution, tap density can reach 2.0-2.3g/cm3, first discharge specific capacity can reach 160-180mAh/g under 25 ℃ and the above temperature, it is a kind of high-bulk-density, the lithium ion positive electrode of high-volume and capacity ratio, the high conductivity positive electrode that be particularly suitable in the higher torrid zone of mean temperature, uses the subtropical zone.
The method of the doped derivatives high density iron manganese phosphate for lithium of preparation LiFePO4; the employing ferric iron is a raw material; mix with manganese source, phosphorus source, reducing agent; the precursor that adds the synthetic iron manganese phosphate for lithium of ammonia spirit reaction; and then with lithium source high temperature sintering under protective atmosphere; obtain the bulk density height, good conductivity, the iron manganese phosphate powder for lithium that specific capacity is high.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Preparation ferric phosphate, manganese sulfate, phosphoric acid, glucose mixed aqueous solution, wherein ferric phosphate concentration is that 0.9 mol, manganese sulfate concentration are that 0.6 mol, phosphoric acid concentration are that 2.25 mol, concentration of glucose are 0.15 mol.Compound concentration is the ammonia spirit of 6 mol.Respectively ferric phosphate, manganese sulfate, phosphoric acid, glucose mixed aqueous solution and ammonia spirit are input to measuring pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferric phosphate, manganese sulfate, phosphoric acid, glucose mixed aqueous solution is 120 milliliters/hour, regulate the flow of ammonia spirit, the pH value of control reactor internal reaction liquid is 8.0 ± 0.1.The control reactor temperature is 80 ℃.Mixed material nature overflow in the reactor enters in the pans.After the continuous feed 30 hours, stop charging, the material in the reactor is discharged, carry out Separation of Solid and Liquid with centrifuge.Solid product with deionized water wash Separation of Solid and Liquid gained.With the product after the washing in drying box in 80 ℃ dry 3 hours down, obtain manganese phosphate ferrous ammonium ((NH
4Fe
1-xMn
xPO
4H
2O).Take by weighing 18.5 gram lithium carbonates and measure 18.5 milliliters of deionized waters, place the ball mill ball milling to stop after 3 hours.Take by weighing the above-mentioned manganese phosphate ferrous ammonium that makes of 93.5 grams, place the lithium carbonate slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.
Mixed slurry is put into alumina crucible, in tube furnace by 200 ℃/time speed be warming up to 600 ℃, constant temperature 16 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen in this process, gas flow is 1 liter/minute, obtains spherical iron manganese phosphate for lithium (LiFe
1-xMn
xPO
4) product.Recording this product average grain diameter is 8um, and tap density is 2.10g/cm
2With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 160mAh/g.
Embodiment 2
Preparation ferric phosphate, manganese nitrate, ammonium dihydrogen phosphate, sucrose mixed aqueous solution, wherein ferric phosphate concentration is that 0.5 mol, manganese nitrate concentration are that 0.2 mol, biphosphate ammonium concentration are that 1.50 mol, sucrose concentration are 0.08 mol.Compound concentration is the ammonia spirit of 8 mol.Respectively ferric phosphate, manganese nitrate, ammonium dihydrogen phosphate, sucrose mixed aqueous solution and ammonia spirit are input to measuring pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferric phosphate, manganese nitrate, ammonium dihydrogen phosphate, sucrose mixed aqueous solution is 120 milliliters/hour, regulate the flow of ammonia spirit, the pH value of control reactor internal reaction liquid is 9.0 ± 0.1.The control reactor temperature is 90 ℃.Mixed material nature overflow in the reactor enters in the pans.After the continuous feed 30 hours, stop charging, the material in the reactor is discharged, carry out Separation of Solid and Liquid with centrifuge.Solid product with deionized water wash Separation of Solid and Liquid gained.With the product after the washing in drying box in 90 ℃ dry 2 hours down, obtain manganese phosphate ferrous ammonium ((NH
4Fe
1-xMn
xPO
4H
2O).Take by weighing 15.0 gram lithium carbonates and measure 15.0 milliliters of deionized waters, place the ball mill ball milling to stop after 4 hours.Take by weighing the above-mentioned manganese phosphate ferrous ammonium that makes of 93.5 grams, place the lithium hydroxide slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.
Mixed slurry is put into alumina crucible, in tube furnace by 200 ℃/time speed be warming up to 800 ℃, constant temperature 24 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen and hydrogen mixed gas in this process, gas flow is 1 liter/minute, obtains spherical iron manganese phosphate for lithium (LiFe
1-xMn
xPO
4) product.Recording this product average grain diameter is 10um, and tap density is 2.20g/cm
2With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 170mAh/g.
Embodiment 3
Preparation di-iron trioxide, manganese sulfate, phosphoric acid, glucose mixed aqueous solution, wherein di-iron trioxide concentration is that 0.6 mol, manganese sulfate concentration are that 0.5 mol, phosphoric acid concentration are that 1.15 mol, concentration of glucose are 0.33 mol.Compound concentration is the ammonia spirit of 8 mol.Respectively di-iron trioxide, manganese sulfate, phosphoric acid, glucose mixed aqueous solution and ammonia spirit are input to measuring pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control di-iron trioxide, manganese sulfate, phosphoric acid, glucose mixed aqueous solution is 120 milliliters/hour, regulate the flow of ammonia spirit, the pH value of control reactor internal reaction liquid is 8.0 ± 0.1.The control reactor temperature is 80 ℃.Mixed material nature overflow in the reactor enters in the pans.After the continuous feed 30 hours, stop charging, the material in the reactor is discharged, carry out Separation of Solid and Liquid with centrifuge.Solid product with deionized water wash Separation of Solid and Liquid gained.With the product after the washing in drying box in 100 ℃ dry 2 hours down, obtain manganese phosphate ferrous ammonium ((NH
4Fe
1-xMn
xPO
4H
2O).Take by weighing 20.5 gram lithium acetates and measure 20.5 ml deionized water, place the ball mill ball milling to stop after 4 hours.Take by weighing the above-mentioned manganese phosphate ferrous ammonium that makes of 93.5 grams, place the lithium carbonate slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.
Mixed slurry is put into alumina crucible, in tube furnace by 200 ℃/time speed be warming up to 900 ℃, constant temperature 48 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen in this process, gas flow is 1 liter/minute, obtains spherical iron manganese phosphate for lithium (LiFe
1-xMn
xPO
4) product.Recording this product average grain diameter is 14um, and tap density is 2.30g/cm
2With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 180mAh/g.
In a word, technology of the present invention is simple, enforcement is convenient, effect is remarkable, with low cost.
Claims (7)
1. the preparation method of a high-density lithium iron manganese phosphate for lithium ion battery positive electrode material is characterized in that preparation method's process is as follows:
(1), preparation ferric iron, manganese source, phosphorus source, reducing agent mixed aqueous solution, wherein the total concentration of iron and manganese is the 0.2-2 mol, 0＜manganese/(iron+manganese)≤40% (molar percentage), the concentration of phosphorus is phosphorus: (iron+manganese)=(1.1-2.0): 1 (mol ratio), reductant concentration are reducing agent: (iron+manganese)=(0.01-0.3): 1 (mol ratio).
(2), compound concentration is the ammonia spirit of 3-10 mol.
(3), with above-mentioned ferric iron, manganese source, phosphorus source, reducing agent mixed aqueous solution, ammonia spirit is input to respectively in the reactor of belt stirrer continuously with pump, the temperature of control reactor internal reaction liquid is 50-90 ℃; 120 milliliters in constant ferrous sulfate, manganese source, phosphorus source, reducing agent mixed aqueous solution/time flow, regulate the flow of ammonia spirit simultaneously, make the pH value of reactor internal reaction liquid be 5.0-8.0.
(4), step 3) gained material changed over to carry out Separation of Solid and Liquid in the solid-liquid separator, with the solid product of deionized water wash Separation of Solid and Liquid gained; Product after the washing in 80-100 ℃ of dry 2-4 hour, obtains manganese phosphate ferrous ammonium precursor (NH in drier
4Fe
1-xMn
xPO
4H
2O, 0＜x≤0.4).
(5), the lithium source is mixed with deionized water, made slurry and in ball mill in ball milling 2-4 hour with mass ratio 1: 1.
(6), in " Li: (Fe+Mn): P=1: the ratio of 1: 1 (mol ratio) takes by weighing spherical manganese phosphate ferrous ammonium of step (4) gained and step (5) gained lithium source slurry and mixes.
(7), step (6) products therefrom is placed stove, under protective atmosphere, be warming up to 500-900 ℃, constant temperature 12-48 hour, natural cooling in stove obtained iron manganese phosphate for lithium (LiFe
1-xMn
xPO
4, 0＜x≤0.4).
2. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 1 is characterized in that described phosphorus source is a kind of in phosphoric acid, ammonium dihydrogen phosphate and the diammonium hydrogen phosphate.
3. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 2 is characterized in that described reducing agent is a kind of in the dextrose plus saccharose.
4. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 3 is characterized in that described ferric iron source is a kind of in di-iron trioxide, the ferric phosphate.
5. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 4 is characterized in that described lithium source is a kind of in lithium carbonate, lithium hydroxide, lithium oxalate, lithium phosphate, lithium acetate, the lithium nitrate.
6. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 5 is characterized in that described manganese salt is a kind of in manganese sulfate, the manganese nitrate.
7. the preparation method of a kind of high-density lithium iron manganese phosphate for lithium ion battery positive electrode material according to claim 6 is characterized in that described protective atmosphere is the mist of nitrogen or nitrogen and hydrogen or nitrogen and argon gas.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874789A (en) * | 2012-10-22 | 2013-01-16 | 苏州大学 | Lithium ion battery anode material lithium iron manganese phosphate and preparation method thereof |
| CN103887491A (en) * | 2012-12-24 | 2014-06-25 | 上海比亚迪有限公司 | Preparation method of lithium ion battery positive electrode active material LiMnxFe1-xPO4/C |
| CN106252657A (en) * | 2015-06-04 | 2016-12-21 | 深圳市比克电池有限公司 | A kind of anode material of lithium battery preparation method |
| CN108336352A (en) * | 2017-12-29 | 2018-07-27 | 贵州唯特高新能源科技有限公司 | A kind of preparation method of high conductivity high vibration high density lithium iron phosphate |
| CN115849330A (en) * | 2022-12-29 | 2023-03-28 | 广东邦普循环科技有限公司 | Lithium manganese iron phosphate cathode material and preparation method thereof |
-
2009
- 2009-10-14 CN CN200910019099A patent/CN101764203A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874789A (en) * | 2012-10-22 | 2013-01-16 | 苏州大学 | Lithium ion battery anode material lithium iron manganese phosphate and preparation method thereof |
| CN103887491A (en) * | 2012-12-24 | 2014-06-25 | 上海比亚迪有限公司 | Preparation method of lithium ion battery positive electrode active material LiMnxFe1-xPO4/C |
| CN103887491B (en) * | 2012-12-24 | 2016-08-10 | 上海比亚迪有限公司 | A kind of anode active material of lithium ion battery LiMnxfe1-xpO4the preparation method of/C |
| CN106252657A (en) * | 2015-06-04 | 2016-12-21 | 深圳市比克电池有限公司 | A kind of anode material of lithium battery preparation method |
| CN108336352A (en) * | 2017-12-29 | 2018-07-27 | 贵州唯特高新能源科技有限公司 | A kind of preparation method of high conductivity high vibration high density lithium iron phosphate |
| CN115849330A (en) * | 2022-12-29 | 2023-03-28 | 广东邦普循环科技有限公司 | Lithium manganese iron phosphate cathode material and preparation method thereof |
| CN115849330B (en) * | 2022-12-29 | 2024-05-10 | 广东邦普循环科技有限公司 | Lithium iron manganese phosphate positive electrode material and preparation method thereof |
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Application publication date: 20100630 |