CN101826617B - Preparation method of lithium iron phosphate - Google Patents
Preparation method of lithium iron phosphate Download PDFInfo
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- CN101826617B CN101826617B CN2010101629953A CN201010162995A CN101826617B CN 101826617 B CN101826617 B CN 101826617B CN 2010101629953 A CN2010101629953 A CN 2010101629953A CN 201010162995 A CN201010162995 A CN 201010162995A CN 101826617 B CN101826617 B CN 101826617B
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Abstract
The invention provides a preparation method of lithium iron phosphate, which comprises the following steps: 1, dissolving an iron source in water to obtain ferric ion/ferrous ion; adding ascorbic acid, phosphorus source solution and aqueous alkali and adjusting the pH value; and filtering to obtain ferrous phosphate sediment and drying the ferrous phosphate sediment; 2, dispersing the ferrous phosphate into the deionized water, adding phosphoric acid solution, heating and mixing the solution and stirring; and adding a lithium source solution into the mixed solution for reaction to obtain suspension; 3 dissolving a sugar source into the water and adding into the suspension obtained in step 2, stirring and drying to obtain the precursor of lithium iron phosphate; and 4, under the protection of inert gas, increasing, keeping and then reducing the temperature of the lithium iron phosphate obtained in step 3, to obtain lithium iron phosphate; and crushing lithium iron phosphate until the particle size is less than 15 mu m, to obtain the finished product. The lithium iron phosphate product prepared by the method of the invention has perfect electrical conductivity, large specific capacity and uniform particle size.
Description
Technical field:
The present invention relates to the preparation method of energy functional material, specially refer to the method preparing phosphate iron lithium of anode material for lithium-ion batteries.
Background technology:
Advantages such as lithium ion battery has platform voltage height, good cycle, operating temperature range is wide, energy density is big, memory-less effect; Be widely used in fields such as mobile communication, portable type electronic product, electric tool, weapon assembling, in power vehicle, also have broad application prospects at present.Therefore develop novel, chemical property is good, safe lithium ion battery has important significance for theories and use value, and key wherein is to prepare stable, available anode material of lithium battery.
At present, the highest lithium battery of commercialization degree is a cobalt acid lithium battery on the market, but because the crystal structure of cobalt acid lithium, there is bigger potential safety hazard in its poor heat stability; And cobalt resource is limited, and cost of material is high, can only be used in compact battery at present.Recent years, in big capacity, high power battery field, LiMn2O4, nickel-cobalt-manganese ternary system are main positive electrodes, but LiMn2O4 because birth defect, cycle performance is not good.The cost of material of nickel-cobalt-manganese ternary system is too high, and the time is difficult to leading market.
LiFePO4 is as anode material of lithium battery, though tap density is low, voltage platform is low, and its excellent safety, environmental protection, high life are that other materials does not possess.The characteristics of LiFePO4 mainly comprise: safe in utilization, high-temperature stability can reach 400 ℃, and not can because of overcharge, short circuit, bump and produce blast; Overlong service life, after room temperature discharged and recharged 1800 times, capacity attenuation can not surpass 10%; Nontoxic, this material does not contain any heavy metal and rare metal, and is environmentally friendly.
Because the continuous development of material science, novel synthesis method continues to bring out.The selection research of process route becomes a kind of important channel of improving material microstructure and character.At present, the method for laboratory synthesizing iron lithium phosphate material is more, and it is main method that high temperature is drawn the phase sintering method, in addition, also has synthetic methods such as sol-gel process, hydro thermal method, chemical precipitation method, microwave method, and these methods respectively have pluses and minuses.
Publication number is that the technological process of 1762798 method preparing phosphate iron lithium is: (a) preparation LiFePO4 precursor.Phosphoric acid solution with 0.05～3mol/L under normal pressure and temperature adds reduced iron powder and doping element compound or conductive agent under nitrogen atmosphere; Under agitation mixed, control temperature and be 30～100 ℃, reaction 1～5 hour; The lithium hydroxide solution that dropwise adds 0.05～5mol/L then reacted 4～6 hours; The back dropping phosphoric acid that finishes is regulated pH to neutral; When treating that solution obviously changes thick suspension into temperature is risen to 100 ℃, use vacuum filtration, obtain precursor through absolute ethanol washing final vacuum drying; (b) this precursor being transferred in the tube furnace, in inert atmosphere or nonoxidizing atmosphere, is 500～800 ℃, roasting 5～24 hours with the heating of the heating rate of 1～30 ℃/min, control temperature, obtains end product.
Publication number is to mention among the preparation method of a kind of lithium ion battery anode material lithium iron phosphate of 101645504: lithium source, P source compound and doping element compound are dissolved in the deionized water; Regulate pH=2～4 then; Fully after the reaction, add conductive organic matter precursor and Fe source compound, mix; Obtain containing the mixture of lithium, iron, phosphorus and doped metallic elements, obtain lithium ion battery anode material lithium iron phosphate through calcination processing again.
Publication number is that the preparation technology's of 101575093 LiFePO 4 material technological process is: first step configuration contains the lithium salt solution of dispersant polyethylene glycol; Second step was progressively put into ferric orthophosphate in the above-mentioned lithium salt solution, was continuously stirring to abundant reaction, mixing, formed colloidal solution, and lithium, iron mol ratio are 1.05: 1.0 in the colloid; The 3rd step is with adding carbon source in the colloidal solution that makes.Addition is 20～40G/MOL (LI+), mixes the back oven dry; Material after the 4th step dried for the 3rd step carries out sintering under nitrogen protection, process the LiFePO4 finished product.
Publication number is that a kind of technology for preparing the wet chemical method of LiFePO4 of l431147 is: the solution or the suspension that will contain Li source compound, Fe source compound, P source compound and doping element compound or conductive agent and precipitation reagent mix; In 5～120 ℃ airtight stirred reactor; Reacted 0.5～24 hour; Obtain the nanometer precursor after the filtration washing oven dry, wherein the concentration of Li source compound, Fe source compound, P source compound is 0.1～3mol/L; Said nanometer precursor is put into high temperature furnace; In non-air or nonoxidizing atmosphere, with the heating of the heating rate of 1～30 ℃/min, 500～800 ℃ of constant temperature calcinings 5～48 hours; And, obtain the lithium iron phosphate nano powder with the rate of temperature fall cooling of 1～20 ℃/min or with the stove cooling.
But the whole bag of tricks all can only mix material precursor through mechanical at present; And this mixing can only rest on macro-scale; Can not guarantee that iron, lithium, three kinds of elements of phosphorus can else evenly mix contact by molecular level; Thereby cause final LiFePO4 properties of product unstable, capacity is less, and resistance is bigger.
Summary of the invention:
The objective of the invention is to prepare the lithium ion battery anode material lithium iron phosphate poor electric conductivity in order to overcome existing method; The shortcoming that specific capacity is little and electric property is difficult stable; A kind of liquid phase preparation process of LiFePO4 is provided; The LiFePO4 product that this method is prepared has excellent electrical conductivity, big specific capacity, and uniform crystallite dimension.
The purpose of invention realizes like this:
Method preparing phosphate iron lithium of the present invention comprises the steps:
1) source of iron is dissolved in the water; Being configured to concentration is iron ion/ferrous ion aqueous solution of 0.1～5mol/L; Be incorporated as 1～100% ascorbic acid of iron ion/ferrous ion mole percent, adding concentration is that 0.1～5mol/L, mol ratio Fe: P is 1: 0.5～0.7 phosphorus source solution, adds aqueous slkali and regulates pH value to 4～11; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 80～160 ℃ of dryings 1～10 hour;
2) ferrous phosphate is distributed in the deionized water; Add mol ratio Fe: P is 1: 0.3～0.4 phosphoric acid solution; And heating mixed solution to 20～100 ℃, stirring 0.1～5 hour, adding mol ratio Fe in mixed solution: Li is 1: 0.9～1.1 lithium source solution; And stirring reaction 0.1～5 hour, obtain suspension-turbid liquid;
3) be that the carbon source of ferrous phosphate quality 5～60% is dissolved in the water with quality, and add 2) in the step gained suspension-turbid liquid, stir after 0.1～5 hour through dry, obtain the LiFePO4 precursor;
4) with 3) step gained LiFePO4 precursor under inert gas shielding, be warming up to 500～900 ℃, be incubated 3～40 hours, cooling obtains LiFePO4, through pulverizing, particle diameter obtains finished product less than 15um.
Above-mentioned source of iron is at least a in ferrous sulfate, frerrous chloride, iron chloride, ferric nitrate, the ferrous oxalate; The phosphorus source is at least a in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, the ammonium phosphate; The lithium source is at least a in lithium carbonate, lithium hydroxide, lithium phosphate, phosphoric acid hydrogen two lithiums, the lithium dihydrogen phosphate; Aqueous slkali is at least a in NaOH, potassium hydroxide, the ammoniacal liquor, and carbon source is at least a in glucose, sucrose, starch, the dextrin.
Above-mentioned 3) adopt spray drying or vacuumize in the step.
The assembling of battery and detection
After the grinding of sample powder, prepare battery according to the button cell program.Use three layers of micro-pore composite diaphragm of barrier film PP/PE/PP; Adopt the LiPF6/EC of electrolyte 1mol/L: DMC (weight ratio is 1: 1); The lithium sheet of positive pole and Φ=14mm that adopts stamping forming Φ=12mm is as negative pole, and adopts above-mentioned barrier film and electrolyte, in Ar atmosphere glove box, is assembled into the button cell of CR2025 model and seals; And battery carried out charge-discharge test, test its chemical property.
The present invention prepares LiFePO4 through liquid phase method, with all or part of phosphoric acid solution that is dissolved in of ferrous phosphate, adds the lithium source again; Make iron, lithium, phosphate radical can the element uniform distribution, parcel, mixed precipitation mutually; Add spray drying behind the sugared source subsequently, let sugared source evenly be coated on the precursor surface, obtain the conductivity height after the high-temperature process; Specific capacity is big, the LiFePO4 product of stable electrochemical property.
Description of drawings
Fig. 1 is LiFePO4 X-ray diffraction analysis and contrast spectrogram.
Fig. 2 is a LiFePO4 sem photograph image pattern.
Fig. 3 is a ferric phosphate lithium cell 0.5C first charge-discharge figure spectrogram.
Embodiment
Embodiment 1:
The 1mol ferric nitrate is dissolved in the water; Be configured to the ferric ion solutions that concentration is 1mol/L; Be incorporated as 100% ascorbic acid of iron ion mole percent, adding concentration subsequently is that 1.5mol/L, mol ratio Fe: P is 1: 0.6 a phosphoric acid solution, adds sodium hydroxide solution and regulates pH value to 11; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 150 ℃ of dryings 9 hours.Ferrous phosphate is dispersed in the water, and add mol ratio Fe: P is 1: 0.35 a phosphoric acid solution, and heating mixed solution to 60 ℃, stirs 2 hours; In mixed solution, slowly add mol ratio Fe: Li is 1: 0.95 a lithium hydroxide solution, and stirring reaction 3 hours, obtains suspension-turbid liquid.Be that the glucose of ferrous phosphate quality 5% is dissolved in the water with quality subsequently, and slowly add in the suspension-turbid liquid, stir after 2 hours, obtain the LiFePO4 precursor through spray drying.The LiFePO4 precursor is warming up to 500 ℃ under argon shield, is incubated 12 hours, with the stove cooling, obtain LiFePO4, through pulverizing, particle diameter obtains finished product less than 15 μ m.
Embodiment 2:
1mol iron chloride is dissolved in the water; Be configured to the ferric ion solutions that concentration is 2mol/L; Be incorporated as 100% ascorbic acid of iron ion mole percent, adding concentration subsequently is that 1mol/L, mol ratio Fe: P is 1: 0.62 a ammonium dihydrogen phosphate, adds potassium hydroxide and regulates pH value to 10; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 150 ℃ of dryings 9 hours.Ferrous phosphate is dispersed in the water, and add mol ratio Fe: P is 1: 0.38 a phosphoric acid solution, and heating mixed solution to 70 ℃, stirs 3 hours; In mixed solution, slowly add mol ratio Fe: Li is 1: 1 a lithium hydroxide solution, and stirring reaction 2 hours, obtains suspension-turbid liquid.Subsequently with quality be the sucrose dissolved of ferrous phosphate quality 10% in water, and slowly add in the suspension-turbid liquid, stir after 3 hours through spray drying, obtain the LiFePO4 precursor.The LiFePO4 precursor is warming up to 520 ℃ under argon shield, is incubated 10 hours, with the stove cooling, obtain LiFePO4, through pulverizing, particle diameter obtains finished product less than 15 μ m.
Embodiment 3:
The 1mol frerrous chloride is dissolved in the water; Be configured to the ferrous ions soln that concentration is 1.5mol/L; Be incorporated as 3% ascorbic acid of ferrous ion mole percent, adding concentration subsequently is that 1mol/L, mol ratio Fe:P are 1: 0.7 ammonium dibasic phosphate solution, adds NaOH and regulates pH value to 11; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 170 ℃ of dryings 6 hours.Ferrous phosphate is dispersed in the water, and add mol ratio Fe: P is 1: 0.3 a phosphoric acid solution, and heating mixed solution to 70 ℃, stirs 3 hours; In mixed solution, slowly add mol ratio Fe: Li is 1: 1.05 a lithium hydroxide solution, and stirring reaction 2 hours, obtains suspension-turbid liquid.With quality is that the dextrin of ferrous phosphate quality 5% is dissolved in the water, and slowly adds in the suspension-turbid liquid.Stir and pass through spray drying after 3 hours, obtain the LiFePO4 precursor.LiFePO4 is warming up to 560 ℃ with precursor under argon shield, be incubated 7 hours, with the stove cooling, obtains LiFePO4, and through pulverizing, the meta particle diameter obtains finished product less than 15 μ m.
Embodiment 4:
The 1mol frerrous chloride is dissolved in the water, is configured to the ferrous ions soln that concentration is 1.5mol/L, be incorporated as 5% ascorbic acid of ferrous ion mole percent, adding concentration subsequently is 2
Mol/L, mol ratio Fe: P is 1: 0.65 a ammonium dibasic phosphate solution, adds ammoniacal liquor and regulates pH value to 9, filters and obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 150 ℃ of dryings 8 hours.Ferrous phosphate is dispersed in the water, and add mol ratio Fe: P is 1: 0.35 a phosphoric acid solution, and heating mixed solution to 60 ℃, stirs 3 hours; In mixed solution, slowly add mol ratio Fe: Li is 1: 1.05 a lithium hydroxide solution, and stirring reaction 2 hours, obtains suspension-turbid liquid.With quality be the sucrose dissolved of ferrous phosphate quality 5% in water, and slowly add in the suspension-turbid liquid, stir after 3 hours through spray drying, obtain the LiFePO4 precursor.The LiFePO4 precursor is warming up to 750 ℃ under argon shield, is incubated 3 hours, with the stove cooling, obtain LiFePO4, through pulverizing, particle diameter obtains finished product less than 15 μ m.
Embodiment 5:
The 1mol ferric nitrate is dissolved in the water; Be configured to the ferric ion solutions that concentration is 1mol/L; Be incorporated as 100% ascorbic acid of iron ion mole percent, adding concentration subsequently is that 1.5mol/L, mol ratio Fe: P is 1: 0.58 a phosphoric acid solution, adds NaOH and regulates pH value to 11; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 140 ℃ of dryings 10 hours.Ferrous phosphate is dispersed in the water, and add mol ratio Fe: P is 1: 0.4 a phosphoric acid solution, and heating mixed solution to 70 ℃, stirs 2 hours; In mixed solution, slowly add mol ratio Fe: Li is 1: 1 a lithium hydroxide solution, and stirring reaction 3 hours, obtains suspension-turbid liquid.With quality is that the dextrin of ferrous phosphate quality 5% is dissolved in the water, and slowly adds in the suspension-turbid liquid, stirs after 2 hours through spray drying, obtains the LiFePO4 precursor.The LiFePO4 precursor is warming up to 700 ℃ under argon shield, is incubated 4 hours, with the stove cooling, obtain LiFePO4, through pulverizing, particle diameter obtains finished product less than 15 μ m.
The LiFePO4 that the inventive method makes has three aspect characteristics:
1) LiFePO4 has high-purity olivine crystalline phase, and in addition lattice length and lattice dimensions do not see other dephasign, referring to Fig. 1 all very near theoretical parameter;
2) the LiFePO4 particle appears spherical or type sphere, and distribution of sizes is concentrated, greatly about about 60nm, referring to Fig. 2;
3) after LiFePO4 was prepared into half-cell, under 0.5C first charge-discharge condition, specific capacity reached more than the 150mAh/g, and put a platform and reach more than the 3.32V, referring to Fig. 3.
The foregoing description is that foregoing of the present invention is further described, but should this scope that is interpreted as the above-mentioned theme of the present invention only not limited to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (3)
1. method preparing phosphate iron lithium comprises the steps:
1) source of iron is dissolved in the water; Being configured to concentration is iron ion/ferrous ion aqueous solution of 0.1～5mol/L; Be incorporated as 1～100% ascorbic acid of iron ion/ferrous ion mole percent, adding concentration is that 0.1～5mol/L, mol ratio Fe: P is 1: 0.5～0.7 phosphorus source solution, adds aqueous slkali and regulates pH value to 4～11; Filtration obtains the ferrous phosphate deposition, and ferrous phosphate is deposited in 80～160 ℃ of dryings 1～10 hour;
2) ferrous phosphate is distributed in the deionized water; Add mol ratio Fe: P is 1: 0.3～0.4 phosphoric acid solution; And heating mixed solution to 20～100 ℃, stirring 0.1～5 hour, adding mol ratio Fe in mixed solution: Li is 1: 0.9～1.1 lithium source solution; And stirring reaction 0.1～5 hour, obtain suspension-turbid liquid;
3) be that the carbon source of ferrous phosphate quality 5～60% is dissolved in the water with quality, and add 2) in the step gained suspension-turbid liquid, stir after 0.1～5 hour through dry, obtain the LiFePO4 precursor;
4) with 3) step gained LiFePO4 precursor under inert gas shielding, be warming up to 500～900 ℃, be incubated 3～40 hours, cooling obtains LiFePO4, through pulverizing, particle diameter obtains finished product less than 15 μ m.
2. method preparing phosphate iron lithium as claimed in claim 1; It is characterized in that source of iron is at least a in ferrous sulfate, frerrous chloride, iron chloride, ferric nitrate, the ferrous oxalate; The phosphorus source is at least a in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, the ammonium phosphate; The lithium source is at least a in lithium carbonate, lithium hydroxide, lithium phosphate, phosphoric acid hydrogen two lithiums, the lithium dihydrogen phosphate; Aqueous slkali is at least a in NaOH, potassium hydroxide, the ammoniacal liquor, and carbon source is at least a in glucose, sucrose, starch, the dextrin.
3. method preparing phosphate iron lithium as claimed in claim 1 is characterized in that 3) adopt spray drying or vacuumize in the step.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102479944B (en) * | 2010-11-22 | 2014-12-10 | 海洋王照明科技股份有限公司 | Preparation method and application of lithium iron phosphate composite material |
| CN102800863B (en) * | 2012-08-03 | 2014-12-03 | 江苏力天新能源科技有限公司 | Lithium iron phosphate/carbon composite material and purpose thereof |
| CN102779999B (en) * | 2012-08-10 | 2014-06-11 | 北京科锐志投资管理中心（有限合伙） | Preparation method of lithium iron phosphate material with high compacted density |
| CN103204486B (en) * | 2013-04-16 | 2015-02-25 | 成都牧甫科技有限公司 | Grapheme lithium iron phosphate in composite polycrystalline structure and preparation method thereof |
| CN104282904B (en) * | 2013-07-03 | 2016-12-28 | 河南科隆新能源有限公司 | A kind of method improving lithium iron phosphate positive material processing characteristics and cycle performance |
| EP3140254B1 (en) | 2014-05-07 | 2018-07-04 | Johnson Matthey Public Limited Company | Process for the preparation of carbon-coated lithium transition metal phosphate and its use |
| CN111847417B (en) * | 2020-07-24 | 2021-12-14 | 中南大学 | Preparation method of battery-grade hydrated iron phosphate |
| CN113582152A (en) * | 2021-08-17 | 2021-11-02 | 江西省金锂科技股份有限公司 | Preparation method of low-cost lithium ion battery cathode material lithium iron phosphate |
| CN114933291A (en) * | 2022-04-08 | 2022-08-23 | 四川顺应动力电池材料有限公司 | Method for preparing high-purity lithium iron phosphate by using nickel-iron alloy |
| CN115818610A (en) * | 2022-12-07 | 2023-03-21 | 合肥国轩科宏新能源科技有限公司 | Liquid-phase synthesis method of lithium iron phosphate |
| CN115744854A (en) * | 2022-12-16 | 2023-03-07 | 宜宾天原科创设计有限公司 | Method for preparing ferrous phosphate from ferrous chloride as byproduct of titanium white chloride |
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| CN101179124A (en) * | 2007-08-24 | 2008-05-14 | 郑州德朗能电池有限公司 | Method for producing high performance lithium ion battery anode material LiFePO4/C |
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| CN101179124A (en) * | 2007-08-24 | 2008-05-14 | 郑州德朗能电池有限公司 | Method for producing high performance lithium ion battery anode material LiFePO4/C |
Non-Patent Citations (1)
| Title |
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| 严红.锂离子电池正极材料球形LiFePO4的合成及改性研究.《江苏大学硕士学位论文》.2009,第25-42页. * |
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