CN1255887C - Method of preparing positive electrode composite material of lithium ion cell contg, ferrous phosphate lithium salt-carbon - Google Patents
Method of preparing positive electrode composite material of lithium ion cell contg, ferrous phosphate lithium salt-carbon Download PDFInfo
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- CN1255887C CN1255887C CNB2004100173825A CN200410017382A CN1255887C CN 1255887 C CN1255887 C CN 1255887C CN B2004100173825 A CNB2004100173825 A CN B2004100173825A CN 200410017382 A CN200410017382 A CN 200410017382A CN 1255887 C CN1255887 C CN 1255887C
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a method for preparing composite materials of the positive electrode of a lithium ion battery of carbon containing ferrous phosphate lithium salt. The method comprises: lithium salt with certain proportion, a Fe<3+> compound and phosphate are uniformly mixed by a one-step solid phase method, and then the mixture is pyrolyzed at inert atmosphere; before the pyrolysis, a certain quantity of high molecular polymers are added, and the composite materials of the positive electrode of carbon containing ferrous phosphate lithium salt are obtained. The method has the advantages of no need for expensive raw materials of Fe<2+>, simple production technology, safety and low cost. The obtained composite materials of the positive electrode have high purity, improved conducting performance, greatly improved electrochemical performance, high specific capacity and excellent cycle performance, and have a stable discharge voltage platform of 3.4V or so. The lithium ion battery material prepared by the method can be widely applied to mobile telephones, notebook computers, minitype cameras and video recorders, electric automobiles, etc.
Description
Technical field
The present invention relates to a kind of preparation method of anode composite material of lithium ion battery, particularly a kind of preparation method of ferrous phosphate base lithium salts-carbon composite.
Background technology
Lithium ion battery is the novel green high-power rechargeable battery that occurs early 1990s, has become the emphasis that competitively research and develop countries in the world at present.Positive electrode is an important component part of lithium ion battery, in the lithium ion battery charge and discharge process, not only to be provided in the both positive and negative polarity lithium intercalation compound the needed lithium of back and forth embedding/take off, form the needed lithium of SEI film but also will bear the negative material surface, therefore, research and develop the key point that high performance positive electrode has become the lithium ion battery development.Present research mainly concentrates on the lithium-containing transition metal oxide aspect, and transition metal is mainly cobalt, nickel, manganese.In recent years, based on Fe
3+/ Fe
2+The material of oxidation-reduction pair causes people's very big interest, the LiFePO that particularly has olivine crystal structure
4Become the most promising alternative positive electrode of recent research, compare with other positive electrodes, it has multiple advantages such as safer, more environmental protection, more cheap and suitable height ratio capacity.
Goodenough[A.K.Padhi, K.S.Nanjundaswarmy, J.B.Goodenough, J.Electrochem.Soc., 144 (1997) 1188] research group synthesized a kind of iron content lithium salts LiFePO
4, this material has high theoretical specific capacity (170mAh/g) as anode material for lithium-ion batteries, greater than commercial LiCoO
2Actual discharge specific capacity 140mAh/g, so cause researcher's very big concern.But the conductivity of this material is very poor, can only discharge and recharge under minimum multiplying power under the room temperature, and its preparation needs Fe
2+Do source of iron, price is than Fe
3+Salt is high and need repeatedly heat treatment and grinding, and complicated process of preparation, product purity are not easy control, thereby cost is increased, and these have all limited its application in practical lithium-ion greatly.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid,, reduce preparation cost, improve product purity, improve the material electric conductivity to simplify preparation technology;
The preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid of the present invention may further comprise the steps:
1) with lithium salts, Fe
3+Compound and phosphate mix in proportion, wherein Li: Fe: the P mol ratio is (0.95-1.1): 1: 1;
2) milled mixtures fully mixes it;
3) in mixture, mix polyethylene or polypropylene; polyethylene or polyacrylic consumption make that the carbon weight percent content is 1-20% in the product; put into tube furnace then; flow velocity be the 5-40 liter/minute inert gas protection under; under 450-900 ℃ of temperature heat treatment 8-50 hour, be cooled to room temperature and get final product.
Said lithium salts can be selected from Li among the present invention
2CO
3, LiOH, lithium oxalate, lithium acetate or lithium phosphate etc., Fe
3+Compound can adopt di-iron trioxide, tri-iron tetroxide or ferric phosphate etc. to contain Fe
3+Compound, phosphate can be selected from ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ferric phosphate etc.Said inert gas can be nitrogen or argon gas.High molecular polymer is a hydrocarbon polymer, is advisable with polypropylene.
Usually, reach well-mixed effect, can when grinding, add an amount of alcohol for making mixture.
The present invention adopt one the step solid phase method prepared iron content lithium salts-carbon composite anode active material, the raw material wide material sources that adopted, be easy to get, cheap, the preparation method is simple; The composite material that makes does not contain Co, Ni etc. has the element of bigger pollution to environment, thereby environmentally friendly; This anode composite material purity height is just having the charging/discharging voltage platform about 3.4V stably, and electric conductivity and high rate during charging-discharging are good; This anode composite material Stability Analysis of Structures, thermal stability is good, and cycle performance is good.
The lithium ion battery material of being prepared by this method can be widely used in fields such as mobile phone, notebook computer, small-sized Video Camera, electric automobile.
Description of drawings
Fig. 1 is the crystallogram by the prepared ferrous phosphate base lithium salts-carbon composite of embodiment 1, adopts Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer (Cu target K
αRay, wavelength X=0.154056nm).
Fig. 2 is that voltage range 2.5-4.2V, electrolyte are 1mol/L LiPF by the prepared simulation lithium ion battery charging and discharging curve figure of embodiment 1
6/ EC-DMC (1: 1), charge-discharge magnification are 0.1C, and measuring temperature is 30 ℃ ± 0.5 ℃.
Fig. 3 is that voltage range 2.5-4.2V, electrolyte are 1mol/L LiPF by the prepared discharge curve of simulation lithium ion battery under different charge-discharge magnifications of embodiment 1
6/ EC-DMC (1: 1), charge-discharge magnification is respectively 0.1C, 0.2C, 0.5C, and measuring temperature is 30 ℃ ± 0.5 ℃.
Fig. 4 is that voltage range 2.5-4.2V, electrolyte are 1mol/L LiPF by the cycle performance figure of the prepared simulation lithium ion battery of embodiment 1
6/ EC-DMC (1: 1), charge-discharge magnification are 0.2C, and measuring temperature is 30 ℃ ± 0.5 ℃.
Embodiment
0.5 moles of hydrogen lithia and 0.5 mole of phosphoric acid iron are mixed, put into the nylon jar, and adding 80ml alcohol, after mixing 2 hours on the ball mill, this mixture is mixed 14 gram polypropylene put into tube furnace, under 5 liters/minute blanket of nitrogen, rise to 700 ℃ with 5 ℃/minute speed, and under this temperature constant 10 hours, be cooled to room temperature then.
Record that the carbon weight percent content is 2.5% in the gained composite material, its XRD spectra is seen Fig. 1, and the reference standard card is the intact olivine-type LiFePO of crystal formation
4, and do not observe the diffraction maximum of carbon.
Composite material with embodiment 1 gained is made electrode as follows.
Take by weighing the composite material of embodiment 1 gained respectively with 80: 10: 10 mass ratioes: carbon black: polytetrafluoroethylene, make electrode after grinding evenly, being equipped with pour lithium slice is negative pole, to be dissolved in the 1.0mol/L LiPF in ethyl carbonate+dimethyl carbonate (volume ratio 1: 1) mixed solvent
6Be electrolyte, the polypropylene microporous membrane is a barrier film, is assembled into the simulation lithium ion battery.Fig. 2 presses the 0.1C multiplying power at the first charge-discharge curve of 4.2V-2.5V during by voltage for respective battery, shows that the battery of surveying has the platform of charging/discharging voltage stably about 3.4V, and the reversible specific capacity that can calculate embodiment 1 composite material is 164mAh/g.Fig. 3 is the discharge curve of respective battery under different charge-discharge magnifications.In the discharge-rate scope of 0.1C-0.5C, the reversible capacity of positive electrode active materials is between between+the 145-164mAh/g.Fig. 4 is the cycle performance of respective battery under the 0.2C multiplying power.Wherein, specific capacity is with LiFePO
4Mass Calculation, but not LiFePO
4The quality of-carbon complex is identical therewith in following examples.
Embodiment 2:
The ammonium dihydrogen phosphate of 0.5 moles of hydrogen lithia, 0.25 mole di-iron trioxide and 0.5 mole mixed and put into the nylon jar, add 80ml alcohol, after fully mixing 2 hours on the ball mill, this mixture is mixed 20 gram polypropylene put into tube furnace, under 5 liters/minute blanket of nitrogen, rise to 700 ℃ with 5 ℃/minute speed, and under this temperature constant 20 hours, be cooled to room temperature then.The carbon weight percent content that records the gained composite material is 4.6%, and equally the method by embodiment 1 prepares electrode slice, is assembled into behind the battery with the 0.2C rate charge-discharge, and the mensuration reversible capacity is 157mAh/g.
Embodiment 3:
0.5 moles of hydrogen lithia and 0.5 mole of phosphoric acid iron are mixed, put into the nylon jar, and adding 80ml alcohol, after mixing 1 hour on the ball mill, this mixture is mixed 25 gram polyethylene put into tube furnace, under 5 liters/minute blanket of nitrogen, rise to 500 ℃ with 5 ℃/minute speed, and under this temperature constant 24 hours, be cooled to room temperature then.The carbon weight percent content that records the gained composite material is 3.1%, and prepares electrode slice by the method for embodiment 1, is assembled into behind the battery with the 0.5C rate charge-discharge, and the mensuration reversible capacity is 148mAh/g.
Embodiment 4:
With 0.25 mole of lithium carbonate, 0.25 the di-iron trioxide of mole and 0.5 mole ammonium hydrogen phosphate mix, put into the nylon jar, and add 80ml alcohol, after mixing 1 hour on the ball mill, this mixture is mixed 25 gram polypropylene put into tube furnace, under 5 liters/minute blanket of nitrogen, rise to 600 ℃ with 5 ℃/minute speed, and under this temperature constant 48 hours, be cooled to room temperature then.The carbon weight percent content that records the gained composite material is 7.6%, and prepares electrode slice by the method for embodiment 1, is assembled into behind the battery with the 1C rate charge-discharge, and the mensuration reversible capacity is 125mAh/g.
Claims (5)
1. the preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid may further comprise the steps:
1) with lithium salts, Fe
3+Compound and phosphate mix in proportion, wherein Li: Fe: the P mol ratio is (0.95-1.1): 1: 1;
2) milled mixtures fully mixes it;
3) in mixture, mix polyethylene or polypropylene; polyethylene or polyacrylic consumption make that the carbon weight percent content is 1-20% in the product; put into tube furnace then; flow velocity be the 5-40 liter/minute inert gas protection under; under 450-900 ℃ of temperature heat treatment 8-50 hour, be cooled to room temperature and get final product.
2. the preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid according to claim 1 is characterized in that described lithium salts is selected from Li
2CO
3, LiOH, lithium oxalate, lithium acetate or lithium phosphate.
3. the preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid according to claim 1 is characterized in that described Fe
3+Compound is selected from di-iron trioxide, tri-iron tetroxide or ferric phosphate.
4. the preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid according to claim 1 is characterized in that described phosphate is selected from ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ferric phosphate.
5. the preparation method of the anode composite material of lithium ion battery of the ferrous lithium salts-carbon of phosphoric acid according to claim 1 is characterized in that described inert gas is selected from nitrogen or argon gas.
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| CNB2004100173825A CN1255887C (en) | 2004-03-25 | 2004-03-25 | Method of preparing positive electrode composite material of lithium ion cell contg, ferrous phosphate lithium salt-carbon |
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| CN1255887C true CN1255887C (en) | 2006-05-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI463727B (en) * | 2009-03-24 | 2014-12-01 | Battery Energy Technology Inc | A synthetic method of lithium-ion battery composite cathode material with olivine structure prepared by polymer carbon source |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100461506C (en) * | 2005-04-12 | 2009-02-11 | 广州融达电源材料有限公司 | Method for producing lithium battery positive pole material by carbon-covering method |
| CN1332462C (en) * | 2005-11-15 | 2007-08-15 | 厦门大学 | Lithium iron phosphate anode material and its preparing method |
| CN100347081C (en) * | 2005-12-29 | 2007-11-07 | 上海交通大学 | Process for preparing lithium ferrous phosphate coated with carbon |
| CN100404413C (en) * | 2006-03-22 | 2008-07-23 | 浙江大学 | Preparation method of carbon clocd ferrolithium phosphate of lithium ion battery anode material |
| CN100413781C (en) * | 2006-03-24 | 2008-08-27 | 山东科技大学 | Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell |
| FR2898885B1 (en) * | 2006-03-27 | 2008-05-30 | Commissariat Energie Atomique | COMPOUND BASED ON TITANIUM AND CARBON DISPHOSPHATE, PROCESS FOR THE PREPARATION AND USE AS ACTIVE MATERIAL OF ELECTRODE FOR LITHIUM ACCUMULATOR |
| CN101209821B (en) * | 2006-12-31 | 2010-05-19 | 比亚迪股份有限公司 | Preparation method for lithium ion secondary battery positive pole active substance lithium iron phosphate |
| CN101314463B (en) * | 2007-05-28 | 2011-04-06 | 上海比亚迪有限公司 | Method of producing active compound lithium iron phosphate of lithium ion secondary battery anode |
| CN101572305B (en) * | 2009-05-31 | 2011-08-17 | 浙江大学 | Preparation method of LiFePO*/C cathode material with high rate performance |
| CN101969118A (en) * | 2010-10-13 | 2011-02-09 | 武汉大学 | Method for synthesizing carbon-coated lithium iron phosphate of lithium ion battery cathode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI463727B (en) * | 2009-03-24 | 2014-12-01 | Battery Energy Technology Inc | A synthetic method of lithium-ion battery composite cathode material with olivine structure prepared by polymer carbon source |
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Address after: 336000 No. 10, No. 1, spring road, Yichun Economic Development Zone, Jiangxi, Yichun Patentee after: Yichun Tianzhi High-tech New Material Co., Ltd. Address before: 336000 No. 10, No. 1, spring road, Yichun Economic Development Zone, Jiangxi, Yichun Patentee before: Jiangxi aide Nano Technology Co., Ltd. |
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