CN103840159B - A kind of lithium ion anode material LiFePO4the synthetic method of/C - Google Patents
A kind of lithium ion anode material LiFePO4the synthetic method of/C Download PDFInfo
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- CN103840159B CN103840159B CN201410113390.3A CN201410113390A CN103840159B CN 103840159 B CN103840159 B CN 103840159B CN 201410113390 A CN201410113390 A CN 201410113390A CN 103840159 B CN103840159 B CN 103840159B
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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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- 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
Abstract
A kind of lithium ion anode material LiFePO4The synthetic method of/C, relates to anode material for lithium-ion batteries.1) add water mixing by iron sesquioxide, doped metal ion oxide and organic carbon source, mist projection granulating after ball-milling treatment, and the powder body obtained pretreatment in an inert atmosphere obtains carbon-encapsulated iron source powder body；2) phosphorus source is soluble in water, add the carbon-encapsulated iron source powder body that step 1) obtains, be subsequently adding Lithium hydrate, mist projection granulating after ball-milling treatment, obtain being dried powder body；3) by step 2) the dry powder body that obtains processes in an inert atmosphere, then carries out high-temperature heat treatment, i.e. obtains lithium ion anode material LiFePO through air current classifying4/C.By to LiFePO4Particle surface carbon coated, at LiFePO4Structure introduces dopant ion and changes its semiconductor property, improve its electron conduction；By reducing LiFePO4The particle diameter of crystal, improves lithium ion diffusion rate in title is crossed in discharge and recharge.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries, especially relate to use a kind of lithium ion anode material LiFePO of carbon cladding iron sesquioxide technique4The synthetic method of/C.
Background technology
The LiFePO of olivine-type structure is found from Googenough in 19974Since, owing to it has the feature such as abundant raw materials, cheap, environmental friendliness, when accordingly acting as positive electrode, have that Heat stability is good, cycle performance be excellent and safety advantages of higher.But due to self the Nomenclature Composition and Structure of Complexes, determining its native electronic electrical conductivity relatively low, lithium ion is relatively low in the diffusion rate of charge and discharge process, and these shortcomings limit its large current density power.It is thus desirable to improve LiFePO4Electron conduction, improve lithium ion in the diffusion rate of charging process.
At present, preparation LiFePO4Method mainly include solid phase method and liquid phase method.Solid phase method is applicable to produce on a large scale, and traditional high temperature solid-state method typically uses Fe2+Compound is source of iron, its price relatively Fe3+Compound is high.On the other hand, Fe2+Easily it is oxidized to Fe3+Impurity, to LiFePO4Electrical property have harmful effect.
U.S. Valence Technology Inc. company uses iron sesquioxide to be source of iron, uses pyrocarbon thermal reduction technology, adds excessive carbon black when raw material mix and prepare LiFePO4 [United States Patent (USP) US6528033B1, US6702961, US6716372B2]；It is source of iron that Chinese patent CN200410072070.4 proposes employing iron sesquioxide, white carbon black is reducing agent, it is simultaneously introduced Carbon fibe or the metallic fiber with certain length-width ratio, and it is combined in the elements such as lithium position doping metals magnesium, reduce the white carbon black usage amount in material, improve the processing characteristics of electrode；Chinese patent CN200510015888.7 introduces, uses a step spray technique to realize LiFePO4/MXP, wherein: M is Ni, Fe, W, Mo or Co, the low temperature controlled preparation process of x=1 or 2, by soluble ferric iron salt and LiH2PO4Stoichiometrically ratio mixing, or by adding soluble metallic salt, Na3C6H5O7·2H2O and NaH2PO2·H2The mixed solution of O, under nitrogen protection 300～500 DEG C of sprayings, finally by impurity deionized water and washing with alcohol, be dried and i.e. can get LiFePO4And LiFePO4/MxP。
Summary of the invention
It is an object of the invention to provide process route simple, it is adaptable to large-scale industrial production, use a kind of lithium ion anode material LiFePO of carbon cladding iron sesquioxide technique4The synthetic method of/C.
The present invention comprises the following steps:
1) add water mixing by iron sesquioxide, doped metal ion oxide and organic carbon source, mist projection granulating after ball-milling treatment, and the powder body obtained pretreatment in an inert atmosphere obtains carbon-encapsulated iron source powder body；
2) phosphorus source is soluble in water, add the carbon-encapsulated iron source powder body that step 1) obtains, be subsequently adding Lithium hydrate, mist projection granulating after ball-milling treatment, obtain being dried powder body；
3) by step 2) the dry powder body that obtains processes in an inert atmosphere, then carries out high-temperature heat treatment, i.e. obtains lithium ion anode material LiFePO through air current classifying4/C。
In step 1), described doped metal ion oxide is selected from MnO2、TiO2, at least one in MgO etc.；Described organic carbon source can use the one in water-soluble Organic substance, described water-soluble Organic substance to be selected from the one in glucose, sucrose, fructose, Polyethylene Glycol, polyacrylic acid, chitosan etc.；The time of described ball-milling treatment can be 5～10h；The temperature of described pretreatment can be 400～500 DEG C, and the time of pretreatment can be 5～8h；
In step 2) in, phosphorus source can use microcosmic salt compound, described microcosmic salt compound to be selected from (NH4)3PO4、(NH4)2HPO4、NH4H2PO4、H3PO4One in Deng；The time of described ball-milling treatment can be 2～3h.
In step 1) and 2) in, it can be Li: Fe: P that described Lithium hydrate, iron sesquioxide, P source compound, metal ion oxide press element molal quantity: doping metals M=1.01: 1: 1: (0.01～0.05)；In step 1), the quality of described organic carbon source can be the 10%～15% of iron sesquioxide quality；In step 1) and 2) in, described water can use salt-free water, and wherein in step 1), the addition of water can be 3～4 times of iron sesquioxide in mass ratio, step 2) in the addition of water can be 3～4 times of carbon-encapsulated iron source powder quality in mass ratio；
In step 1) and 3) in, described inert atmosphere can use nitrogen or argon etc..
In step 3), the temperature of described process can be 500～600 DEG C, and the time of process can be 10～20h；The temperature of described high-temperature heat treatment can be 750～850 DEG C, and the time of high-temperature heat treatment can be 10～20h.
With existing lithium ion anode material LiFePO4The synthetic method of/C is compared, and it is an advantage of the current invention that: first synthesis material iron sesquioxide carries out carbon cladding, and by presintering by Fe3+It is reduced into Fe2+After, it is to avoid the later stage causes LiFePO4 to be reunited because of high-temperature process, and adds the carbon source of excess, it is ensured that by Fe3+Restore All becomes Fe2+.Have employed water-soluble organic carbon source, make carbon source evenly be coated on particle surface, the electrical conductivity height nano-carbon coated layer that Organic substance is formed after oversintering is pyrolyzed, greatly improve the electrical property of material.
Research shows, by LiFePO4Particle surface carbon coated, at LiFePO4Structure introduces dopant ion and changes its semiconductor property, can preferably improve its electron conduction；By reducing LiFePO4The particle diameter of crystal, can be effectively improved lithium ion diffusion rate in title is crossed in discharge and recharge.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the LiFePO 4 material prepared by embodiment 1.In FIG, abscissa is angle of diffraction 2 θ (°), and vertical coordinate is diffracted intensity (a.u).
Fig. 2 is the scanning electron microscope (SEM) photograph (2000 times) of the LiFePO 4 material prepared by embodiment 1.
Fig. 3 is that the LiFePO 4 material prepared by embodiment 1 is fabricated to 18650 cylindrical batteries charging and discharging curve under 1C multiplying power.In figure 3, abscissa is capacity (mAh/g), and vertical coordinate is voltage (V).
Fig. 4 is the cycle performance curve that the LiFePO 4 material prepared by embodiment 1 is fabricated to 18650 cylindrical batteries.In the diagram, abscissa is cycle-index, and vertical coordinate is capacity (mAh/g).
Detailed description of the invention
Embodiment 1
By 5.0mol Fe2O3、0.05mol MnO2、0.05mol TiO2With 100g glucose, adding 2.5L salt-free water mix homogeneously, ball-milling treatment 8h, mist projection granulating, the powder body obtained, in an inert atmosphere in 500 DEG C of pretreatment 7h, obtains carbon-encapsulated iron source powder body.10.0mol ammonium dihydrogen phosphate is dissolved in 2.5L salt-free water, adds carbon-encapsulated iron source powder body, be then slowly added into 10.0molLiOH H2O, stirs, ball-milling treatment 3h, and mist projection granulating obtains being dried powder body.This powder body is joined in rotary furnace, at N2650 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 20h, cooling, sieve, air current classifying and obtain product.
Products obtained therefrom carbon content is 2.1%.
By material by proportioning LiFePO4: the proportions of SP: KS6: HSV900: NMP=92.5: 2: 1: 4.5: 100, make 18650 cylindrical batteries.Battery testing 1C discharge capacity is 135.5mAh/g, and after circulating 500 weeks, capacity is 126.9mAh/g, for the 93.6% of initial capacity.
The XRD figure of LiFePO 4 material prepared by embodiment 1 is shown in that Fig. 1, scanning electron microscope (SEM) photograph (2000 times) are shown in that Fig. 2, prepared LiFePO 4 material are fabricated to 18650 cylindrical batteries charging and discharging curve under 1C multiplying power and see that Fig. 3, cycle performance curve are shown in Fig. 4.
Embodiment 2
By 5.0mol Fe2O3、0.05mol MnO2, 0.05mol MgO and 100g sucrose, add 3.0L salt-free water mix homogeneously, ball-milling treatment 8h, mist projection granulating, the powder body obtained, in an inert atmosphere in 500 DEG C of pretreatment 8h, obtains carbon-encapsulated iron source powder body.10.0mol ammonium dihydrogen phosphate is dissolved in 2.5L salt-free water, adds carbon-encapsulated iron source powder body, be then slowly added into 10.0molLiOH H2O, stirs, ball-milling treatment 3h, and mist projection granulating obtains being dried powder body.This powder body is joined in rotary furnace, at N2600 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 20h, cooling, sieve, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.9%.
By material by proportioning LiFePO4: the proportions of SP: KS6: HSV900: NMP=92.5: 2: 1: 4.5: 100, make 18650 cylindrical batteries.Battery testing 1C discharge capacity is 132.3mAh/g.
Embodiment 3
By 5.0mol Fe2O3、0.1mol MnO2With 100g Polyethylene Glycol, adding 2.5L salt-free water mix homogeneously, ball-milling treatment 8h, mist projection granulating, the powder body obtained, in an inert atmosphere in 500 DEG C of pretreatment 8h, obtains carbon-encapsulated iron source powder body.10.0mol ammonium dihydrogen phosphate is dissolved in 2.5L salt-free water, adds carbon-encapsulated iron source powder body, be then slowly added into 10.0mol LiOH H2O, stirs, ball-milling treatment 3h, and mist projection granulating obtains being dried powder body.This powder body is joined in rotary furnace, at N2650 DEG C of sintering 8h in atmosphere, then after being warming up to 820 DEG C of sintering 15h, cooling, sieve, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.8%.
By material by proportioning LiFePO4: the proportions of SP: KS6: HSV900: NMP=92.5: 2: 1: 4.5: 100, make 18650 cylindrical batteries.Battery testing 1C discharge capacity is 130.9mAh/g.
Embodiment 4
By 5.0mol Fe2O3, 0.1mol MgO and 100g chitosan, add 2.7L salt-free water mix homogeneously, ball-milling treatment 8h, mist projection granulating, the powder body obtained, in an inert atmosphere in 500 DEG C of pretreatment 8h, obtains carbon-encapsulated iron source powder body.By 10.0mol (NH4)3PO4It is dissolved in 2.5L salt-free water, adds carbon-encapsulated iron source powder body, be then slowly added into 10.0mol LiOH H2O, stirs, ball-milling treatment 3h, and mist projection granulating obtains being dried powder body.This powder body is joined in rotary furnace, at N2650 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 20h, cooling, sieve, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.8%.
By material by proportioning LiFePO4: the proportions of SP: KS6: HSV900: NMP=92.5: 2: 1: 4.5: 100, make 18650 cylindrical batteries.Battery testing 1C discharge capacity is 129.6mAh/g,.
Embodiment 5
By 5.0mol Fe2O3、0.03mol MgO、0.03mol MnO2、0.04mol TiO2With 100g fructose, adding 2.7L salt-free water mix homogeneously, ball-milling treatment 8h, mist projection granulating, the powder body obtained, in an inert atmosphere in 500 DEG C of pretreatment 8h, obtains carbon-encapsulated iron source powder body.By 10.0molH3PO4It is dissolved in 2.5L salt-free water, adds carbon-encapsulated iron source powder body, be then slowly added into 10.0mol LiOH H2O, stirs, ball-milling treatment 3h, and mist projection granulating obtains being dried powder body.This powder body is joined in rotary furnace, at N2650 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 20h, cooling, sieve, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.7%.
By material by proportioning LiFePO4: the proportions of SP: KS6: HSV900: NMP=92.5: 2: 1: 4.5: 100, make 18650 cylindrical batteries.Battery testing 1C discharge capacity is 133.4mAh/g.
Claims (4)
1. a lithium ion anode material LiFePO4The synthetic method of/C, it is characterised in that comprise the following steps:
1) add water mixing by iron sesquioxide, doped metal ion oxide and organic carbon source, mist projection granulating after ball-milling treatment,
The powder body arrived pretreatment in an inert atmosphere, obtains carbon-encapsulated iron source powder body；The quality of described organic carbon source is iron sesquioxide matter
The 10%～15% of amount；Described doped metal ion oxide is selected from MnO2、TiO2, at least one in MgO；Described organic
Carbon source uses the one in water-soluble Organic substance, and described water-soluble Organic substance is selected from glucose, sucrose, fructose, gathers
One in ethylene glycol, polyacrylic acid, chitosan；
2) phosphorus source is soluble in water, add step 1) the carbon-encapsulated iron source powder body that obtains, it is subsequently adding Lithium hydrate, at ball milling
Mist projection granulating after reason, obtains being dried powder body；Phosphorus source uses microcosmic salt compound, and described microcosmic salt compound is selected from (NH4)3PO4、
(NH4)2HPO4、NH4H2PO4、H3PO4In one；The time of described ball-milling treatment is 2～3h；
3) by step 2) the dry powder body that obtains processes in an inert atmosphere, then carries out high-temperature heat treatment, through air current classifying be
Obtain lithium ion anode material LiFePO4/C；
Described Lithium hydrate, iron sesquioxide, P source compound, metal ion oxide are Li: Fe: P by element molal quantity:
Doping metals M=1.01: 1: 1: (0.01～0.05)；Described hydromining salt-free water, wherein step 1) in the addition of water by matter
Amount than being 3～4 times of iron sesquioxide, step 2) in the addition of water be the 3～4 of carbon-encapsulated iron source powder quality in mass ratio
Times.
2. a kind of lithium ion anode material LiFePO4The synthetic method of/C, it is characterised in that in step 1)
In, the time of described ball-milling treatment is 5～10h；The temperature of described pretreatment is 400～500 DEG C, and the time of pretreatment is 5～8h.
3. a kind of lithium ion anode material LiFePO4The synthetic method of/C, it is characterised in that in step 1)
With 3) in, described inert atmosphere is argon.
4. a kind of lithium ion anode material LiFePO4The synthetic method of/C, it is characterised in that in step 3)
In, the temperature of described process is 500～600 DEG C, and the time of process is 10～20h；The temperature of described high-temperature heat treatment is
750～850 DEG C, the time of high-temperature heat treatment is 10～20h.
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| CN105047869A (en) * | 2015-06-16 | 2015-11-11 | 田东 | Synthetic method for lithium ion cathode material LiNiO2/C |
| CN104993118A (en) * | 2015-06-16 | 2015-10-21 | 田东 | Synthesizing method for lithium-ion negative electrode material of Li4Ti5O12/C |
| CN107093722B (en) * | 2017-04-26 | 2019-11-29 | 新乡市升华新能源有限公司 | The method that coating-doping technique prepares LiFePO4 is mixed based on ionic liquid phase grade |
| CN109607506A (en) * | 2018-12-29 | 2019-04-12 | 合肥融捷能源材料有限公司 | A method of promoting ferric lithium phosphate precursor tap density |
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| CN102651474A (en) * | 2012-05-24 | 2012-08-29 | 四川科能锂电有限公司 | Preparation method of anode active material lithium iron phosphate of lithium battery |
| CN103280579B (en) * | 2013-04-02 | 2016-08-03 | 合肥国轩高科动力能源有限公司 | A kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and preparation method thereof |
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Effective date of registration: 20170227 Address after: 361000 Xiamen, Fujian, China (Fujian) free trade test area, Xiamen area, one of the wells society, No. 300 Patentee after: Xiamen Xiamen tungsten new energy material Co., Ltd. Address before: 361026 Fujian Province, Xiamen City Haicang investment zone in Xiamen tungsten industry Limited by Share Ltd Patentee before: Xiamen Tungsten Co., Ltd. |
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Address after: 361000 Xiamen, Fujian, China (Fujian) free trade test area, Xiamen area, one of the wells society, No. 300 Patentee after: Xiamen xiaw new energy materials Co., Ltd Address before: 361000 Xiamen, Fujian, China (Fujian) free trade test area, Xiamen area, one of the wells society, No. 300 Patentee before: XTC NEW ENERGY MATERIALS(XIAMEN) Ltd. |