CN102104144B - Method for preparing lithium iron phosphate compound anode material - Google Patents
Method for preparing lithium iron phosphate compound anode material Download PDFInfo
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- CN102104144B CN102104144B CN2010106158665A CN201010615866A CN102104144B CN 102104144 B CN102104144 B CN 102104144B CN 2010106158665 A CN2010106158665 A CN 2010106158665A CN 201010615866 A CN201010615866 A CN 201010615866A CN 102104144 B CN102104144 B CN 102104144B
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Abstract
The invention discloses a method for preparing a lithium iron phosphate compound anode material. In the method, a lithium source compound, an iron source compound, a phosphorus source compound and a carbon source compound serve as raw materials according to the mol ratio of Li:Fe:P:C of 0.9-1.2:0.95-1:1:0-1; and polyoxyethylene serves as a surfactant. The method has less process steps, shortens a production period, saves cost, improves the electric conductivity of a lithium iron phosphate compound material to the maximum by utilizing least carbon, and simultaneously improves the content of active substances in the material.
Description
Technical field
The present invention relates to the secondary lithium battery field, relate in particular to a kind of method for preparing iron phosphate compound anode material of lithium.
Background technology
Lithium ion battery is a kind of commercial batteries that recent two decades just grows up, because it has the energy density height, have extended cycle life, in light weight, characteristics such as volume is little, fail safe is good, now progressively substitute traditional lead acid accumulator, Ni-MH battery etc., be widely used as the power supply of communication apparatus such as portable electronic electrical equipment, digital camera, notebook computer and mobile phone.In all business-like rechargeable battery, why lithium battery has outstanding energy advantage and high voltage, mainly has benefited from negative material (LiC
6/ C) the advantage of electronegative potential and high power capacity.Therefore, the key that is selected to raising lithium ion battery overall performance of positive electrode.
In existing anode material for lithium-ion batteries, consider from fail safe, environmental protection, cost performance, specific capacity, cycle life etc. are many-sided, the LiFePO4 of olivine structural is considered to have most the power type lithium-ion battery anode material of application potential, have great application prospect in fields such as electric automobile, hybrid vehicle, electric bicycles, existing many companies are that the electric automobile of core power supply has begun listing with the ferric phosphate lithium cell at present.The synthetic method of LiFePO4 is a lot, amplifies difficulty but produce, and main cause is that the electric conductivity of LiFePO4 is low, building-up process is difficult to guarantee that carbon coats and material thing whole uniformity mutually, granularity is wayward, and coating process instability etc. cause product batches poor.Substantially all there is such problem in present domestic LiFePO 4 material manufacturer, and product quality and technological level are not enough to satisfy the demand of electrokinetic cell.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of inner heating fast, reaction rate improves greatly, and it is low to consume energy, a kind of method for preparing iron phosphate compound anode material of lithium that processing step is few.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method for preparing iron phosphate compound anode material of lithium, be raw material with Li source compound, Fe source compound, P source compound, carbon-source cpd, count in molar ratio, above-mentioned proportion scale is: Li: Fe: P: C=0.9～1.2: 0.95～1: 1: 0～1; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1), under 30～90 ℃ and ultrasound condition, polyethylene glycol oxide and carbon-source cpd are added in the reactor, solubilizer stirred 1～5 hour, charged into inert gas then;
(2) solution of preparation P source compound and Li source compound joins these two kinds of solution in the described reactor of step (1) simultaneously, and is ultrasonic and stirred 1～5 hour;
(3) solution of preparation Fe source compound adds antioxidant, constantly stirs, and adds in the described reactor of step (2), and is ultrasonic and stirred 1～10 hour, described antioxidant, and by mass percentage, its consumption is 0～0.1% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, under 100～350 ℃ of conditions, be incubated 5～60 minutes, then cool to room temperature;
(5) solid product that step (4) is obtained filters, and repeatedly cleans with distilled water, and is dry then, is incubated 0.5-4 hour under 400～800 ℃ of conditions at last under inert atmosphere;
Detect the amount of substance of participating in reaction in the above-mentioned steps, when polyethylene glycol oxide concentration at 0～0.3mol/L, lithium atom concentration is at 0～3.6mol/L, iron atom and phosphate concentration are at 0～3mol/L, compactedness 50～80% stops reaction, namely gets required iron phosphate compound anode material of lithium.
Described solvent is selected for use: a kind of in nitrile compounds or the multicomponent alcoholics compound.
Described carbon-source cpd is selected for use: a kind of in carboxymethyl cellulose, β～cyclodextrin, polyvinyl alcohol, polyacrylamide or the carbon nano-tube.
Described P source compound is selected for use: a kind of in phosphoric acid, lithium dihydrogen phosphate, phosphoric acid hydrogen two lithiums, pyrophosphoric acid lithium or the lithium phosphate.
Described Fe source compound is selected for use: a kind of in ferrous citrate, frerrous chloride, ferrous carbonate, ferrous oxalate, ferrous nitrate or the ferrous phosphate.
Described Li source compound is selected for use: lithium hydroxide, pyrophosphoric acid lithium, lithium citrate or lithium oxalate a kind of.
Described antioxidant is selected for use: a kind of among antioxidant 1010, antioxidant 1076, antioxidant 2246, antioxidant 245 or the VC.
The drying mode that described step (5) adopts is a kind of in spray drying, film drying, freeze drying or the azeotropic distillation drying.
Beneficial effect of the present invention is:
(1) use of ultrasonic dispersion has guaranteed uniformity and the fineness of predecessor thing: keep ultrasonic state in the predecessor process for preparation always, be conducive to even dispersion and the refinement of reaction system, help the uniformity of follow-up solvent thermal reaction product.
(2) creation of inert reaction condition has guaranteed that ferrous iron can be not oxidized: with the oxygen of antioxidant except dissolving in anhydrating; with the air in the inert gas eliminating reactor; with microwave solvent thermal response crystallization LiFePO4, also blanketing with inert gas of final drying and heat treatment.
(3) by the microwave solvent thermal response, (with respect to conventional solid-state method) is synthetic at a lower temperature obtains LiFePO4 crystal grain, and the mode of heating of microwave has utilized energy to greatest extent, and the reaction time is short, less energy consumption.
(4) one steps synthesized and all disperse carbon-coated nano-grade lithium iron phosphate (containing doped iron lithium phosphate) composite positive pole, and processing step is few, has shortened the production cycle, is conducive to improve consistency of product.
(5) by the adjusting of microwave reaction temperature and time, nano-grade lithium iron phosphate crystal formation and particle diameter are controlled, are conducive to improve the diffusivity of lithium ion in material; Non-ionic surface active agent (with the part carbon source) can be controlled the pattern of product, carbon source under microwave the decomposition carbonization and the crystallization of LiFePO4 carry out simultaneously, realized that real " original position " coats, can be with minimum carbon, farthest improve the conductivity of composite ferric lithium phosphate material, also improved content of active substance in the material simultaneously, so the material that adopts this technology to obtain has high capacity (0.2C can reach 165mAh/g) and outstanding big high rate performance (5C can reach 130mAh/g), the minimizing of carbon content can also improve the tap density of product in addition.
Description of drawings
Fig. 1 makes the XRD spectrum of material for adopting embodiment 1;
Fig. 2 makes the SEM figure of material for adopting embodiment 1;
Fig. 3 makes the cyclic curve under different multiplying of material for adopting embodiment 1.
Embodiment
Specifically describe below by the present invention of embodiment.
A kind of method for preparing iron phosphate compound anode material of lithium is raw material with lithium citrate, frerrous chloride, lithium dihydrogen phosphate, sodium carboxymethylcellulose, counts in molar ratio, and above-mentioned proportion scale is: Li: Fe: P: C=1.2: 1: 1: 1; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1) under 80 ℃ and ultrasound condition, polyethylene glycol oxide and sodium carboxymethylcellulose are added in the reactor, add the tetraethyl ethylene glycol solvent and stirred 3 hours, charge into argon gas then;
(2) the tetraethyl ethylene glycol solution of preparation lithium dihydrogen phosphate and lithium citrate joins these two kinds of solution in the described reactor of step (1) simultaneously, and is ultrasonic and stirred 4 hours;
(3) the tetraethyl ethylene glycol solution of preparation frerrous chloride adds antioxidant 1010, constantly stirs, add in the described reactor of step (2), ultrasonic and stirred described antioxidant 4 hours, by mass percentage, its consumption is 0.05% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, insulation is 10 minutes under 300 ℃ of conditions, then cool to room temperature;
(5) solid product that step (4) obtained filters, repeatedly cleans with distilled water, and spray drying then, at last in argon hydrogen gaseous mixture (containing 5% hydrogen), 700 ℃ of insulations 2 hours down;
Detect the amount of substance of participating in reaction in the above-mentioned steps, when polyethylene glycol oxide concentration at 0.1mol/L, lithium atom concentration is at 1.2mol/L, iron atom and phosphate concentration are at 1mol/L, compactedness 70% stops reaction, namely gets required iron phosphate compound anode material of lithium.
Example 1 gained material is carried out X diffraction crystal structure and morphology analysis, the results are shown in Figure 1 and Fig. 2, the gained material particle size evenly, good crystallinity, have the olivine-type structure of high-sequential; Wait the rate charge-discharge test with button cell in the 2.5-4.2V voltage range under the normal temperature, test result is seen Fig. 3, and the 0.2C capacity is 165mAh/g, 5C capacity 130mAh/g, and 100 circulations are undamped substantially.
Embodiment 2
A kind of method for preparing iron phosphate compound anode material of lithium is raw material with lithium hydroxide, ferrous nitrate, phosphoric acid, beta-schardinger dextrin-, counts in molar ratio, and above-mentioned proportion scale is: Li: Fe: P: C=0.9: 1: 1: 1; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1) under 90 ℃ and ultrasound condition, polyethylene glycol oxide and beta-schardinger dextrin-are added in the reactor, add acetonitrile solvent and stirred 3 hours, charge into argon gas then;
(2) acetonitrile solution of preparation phosphoric acid and lithium hydroxide joins these two kinds of solution in the described reactor of step (1) simultaneously, and is ultrasonic and stirred 5 hours;
(3) acetonitrile solution of preparation ferrous nitrate adds antioxidant 2246, constantly stirs, and adds in the described reactor of step (2), and is ultrasonic and stirred 3 hours, described antioxidant, and by mass percentage, its consumption is 0.03% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, insulation is 15 minutes under 280 ℃ of conditions, then cool to room temperature;
(5) solid product that step (4) is obtained filters, and repeatedly cleans with distilled water, and freeze drying then under 400 ℃ of nitrogen protections, is incubated 4 hours at last;
Detect the amount of substance of participating in reaction in the above-mentioned steps, when polyethylene glycol oxide concentration at 0.2mol/L, lithium atom concentration is at 2.7mol/L, iron atom and phosphate concentration are at 3mol/L, compactedness 65% stops reaction, namely gets required iron phosphate compound anode material of lithium.
Under the normal temperature, make button cell with example 2 gained materials, wait the rate charge-discharge test in the 2.5-4.2V voltage range, the 0.2C capacity is 131mAh/g, 5C capacity 80mAh/g.
Embodiment 3
A kind of method for preparing iron phosphate compound anode material of lithium is raw material with ferrous citrate, lithium dihydrogen phosphate, polyvinyl alcohol, counts in molar ratio, and above-mentioned proportion scale is: Li: Fe: P: C=1: 1: 1: 0.3; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1) under 90 ℃ and ultrasound condition, polyethylene glycol oxide and polyvinyl alcohol are added in the reactor, added the glycerol stirring solvent 2 hours, charge into argon gas then;
(2) the glycerol solution of preparation lithium dihydrogen phosphate joins this solution in the described reactor of step (1) then, and is ultrasonic and stirred 5 hours;
(3) the glycerol solution of preparation ferrous citrate adds antioxidant 1076, constantly stirs, and adds in the described reactor of step (2), and is ultrasonic and stirred 3 hours, described antioxidant, and by mass percentage, its consumption is 0.1% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, insulation is 30 minutes under 250 ℃ of conditions, then cool to room temperature;
(5) solid product that step (4) is obtained filters, and repeatedly cleans with distilled water, adopts film drying then, and under nitrogen and hydrogen mixture (containing 5% hydrogen) protection, 750 ℃ are incubated 1 hour at last;
Detect the amount of substance of participating in reaction in the above-mentioned steps, when polyethylene glycol oxide concentration at 0.3mol/L, lithium atom concentration is at 1mol/L, iron atom and phosphate concentration are at 1mol/L, compactedness 80% stops reaction, namely gets required iron phosphate compound anode material of lithium.
Under the normal temperature, make button cell with example 3 gained materials, wait the rate charge-discharge test in the 2.5-4.2V voltage range, the 0.2C capacity is 145mAh/g, 5C capacity 103mAh/g.
Embodiment 4
A kind of method for preparing iron phosphate compound anode material of lithium is raw material with ferrous oxalate, phosphoric acid, lithium acetate, polyacrylamide, counts in molar ratio, and above-mentioned proportion scale is: Li: Fe: P: C=1.1: 1: 1: 0.1; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1) under 50 ℃ and ultrasound condition, polyethylene glycol oxide and polyacrylamide are added in the reactor, added the propionitrile stirring solvent 2 hours, charge into argon gas then;
(2) the propionitrile solution of preparation phosphoric acid and lithium acetate joins this solution in the described reactor of step (1) then, and is ultrasonic and stirred 4 hours;
(3) the propionitrile solution of preparation ferrous oxalate adds antioxidant 245, constantly stirs, and adds in the described reactor of step (2), and is ultrasonic and stirred 5 hours, described antioxidant, and by mass percentage, its consumption is 0.01% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, insulation is 10 minutes under 300 ℃ of conditions, then cool to room temperature;
(5) solid product that step (4) obtained filters, repeatedly cleans with distilled water, and azeotropic distillation drying then, at last under argon shield, 700 ℃ of insulations 1 hour;
Detect the amount of substance of participating in reaction in the above-mentioned steps, when polyethylene glycol oxide concentration at 0.2mol/L, lithium atom concentration is at 1.1mol/L, iron atom and phosphate concentration are at 1mol/L, compactedness 75% stops reaction, namely gets required iron phosphate compound anode material of lithium.
Under the normal temperature, make button cell with example 4 gained materials, wait the rate charge-discharge test in the 2.5-4.2V voltage range, the 0.2C capacity is 126mAh/g, 5C capacity 70mAh/g.
Claims (8)
1. method for preparing iron phosphate compound anode material of lithium, it is characterized in that, be raw material with Li source compound, Fe source compound, P source compound, carbon-source cpd, meter in molar ratio, above-mentioned proportion scale is: Li ︰ Fe ︰ P ︰ C=0.9～1.2 ︰, 0.95～1 ︰, 1 ︰ 0～1; Described method is surfactant with the polyethylene glycol oxide;
Described method comprises the steps:
(1), under 30～90 ℃ and ultrasound condition, polyethylene glycol oxide and carbon-source cpd are added in the reactor, solubilizer stirred 1～5 hour, charged into inert gas then;
(2) solution of preparation P source compound and Li source compound joins these two kinds of solution in the described reactor of step (1) simultaneously, and is ultrasonic and stirred 1～5 hour;
(3) solution of preparation Fe source compound adds antioxidant, constantly stirs, and adds in the described reactor of step (2), and is ultrasonic and stirred 1～10 hour, described antioxidant, and by mass percentage, its consumption is 0～0.1% of Fe source compound solution usage;
(4) the described reactor of step (3) is carried out microwave heating, under 100～350 ℃ of conditions, be incubated 5～60 minutes, then cool to room temperature;
Detect the amount of substance of participating in reaction in the above-mentioned steps (4), when polyethylene glycol oxide concentration at 0～0.3mol/L, lithium atom concentration is at 0～3.6mol/L, iron atom and phosphate concentration are at 0～3mol/L, compactedness 50～80% stops reaction;
(5) solid product that step (4) is obtained filters, and repeatedly cleans with distilled water, and is dry then, is incubated 0.5-4 hour under 400～800 ℃ of conditions at last under inert atmosphere, namely gets required iron phosphate compound anode material of lithium.
2. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described solvent is selected for use: a kind of in nitrile compounds or the multicomponent alcoholics compound.
3. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described carbon-source cpd is selected for use: a kind of in carboxymethyl cellulose, β～cyclodextrin, polyvinyl alcohol, polyacrylamide or the carbon nano-tube.
4. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described P source compound is selected for use: a kind of in phosphoric acid, lithium dihydrogen phosphate, phosphoric acid hydrogen two lithiums, pyrophosphoric acid lithium or the lithium phosphate.
5. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described Fe source compound is selected for use: a kind of in ferrous citrate, frerrous chloride, ferrous carbonate, ferrous oxalate, ferrous nitrate or the ferrous phosphate.
6. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described Li source compound is selected for use: lithium hydroxide, pyrophosphoric acid lithium, lithium citrate or lithium oxalate a kind of.
7. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that described antioxidant is selected for use: a kind of among antioxidant 1010, antioxidant 1076, antioxidant 2246, antioxidant 245 or the VC.
8. a kind of method for preparing iron phosphate compound anode material of lithium according to claim 1 is characterized in that, the drying mode that described step (5) adopts is a kind of in spray drying, film drying, freeze drying or the azeotropic distillation drying.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103367750A (en) * | 2012-03-30 | 2013-10-23 | 北京当升材料科技股份有限公司 | Preparation method of carbon-coated lithium iron phosphate material |
| CN102765708B (en) * | 2012-07-09 | 2014-06-04 | 陕西科技大学 | Microwave hydrothermal method for synthesizing lithium iron phosphate serving as cathode material of lithium ion battery |
| CA2794290A1 (en) | 2012-10-22 | 2014-04-22 | Hydro-Quebec | Method of producing electrode material for lithium-ion secondary battery and lithium-ion secondary battery using such electrode material |
| CN103035899B (en) * | 2013-01-14 | 2015-05-27 | 山东天润丰新能源科技有限公司 | Method for performing carbon coating modification on nano-powder by adopting water-soluble polymer |
| CN103311544B (en) * | 2013-05-14 | 2016-04-13 | 厦门大学 | A kind of preparation method of nanometer olivine-type anode material for lithium-ion batteries |
| 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 |
| CN103811754B (en) * | 2014-01-22 | 2016-01-20 | 东风商用车有限公司 | A kind of preparation method of lithium iron phosphate/carbon nano tube compound material |
| CN103996829B (en) * | 2014-05-29 | 2016-06-08 | 西安交通大学 | A kind of nano and micron composite structure lithium iron phosphate positive material and co-precipitation preparation method thereof |
| CN106169567B (en) * | 2016-08-08 | 2018-10-02 | 郑州百成新能源科技有限公司 | A kind of carbon-coated lithium iron phosphate positive material and preparation method thereof |
| CN109148836B (en) * | 2017-06-19 | 2022-01-04 | 中天新兴材料有限公司 | Carbon-coated lithium iron phosphate cathode material and preparation method thereof |
| CN109273695A (en) * | 2018-10-29 | 2019-01-25 | 安徽五行动力新能源有限公司 | A kind of iron phosphate compound anode material of lithium and preparation method thereof |
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