CN105428617B - A method of preparing the modified LiFePO4 of inside and outside conductive carbon - Google Patents
A method of preparing the modified LiFePO4 of inside and outside conductive carbon Download PDFInfo
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- 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
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Abstract
The preparation method that a kind of ferric phosphate carbon ball synchronized compound is carbonized and prepares the modified LiFePO4 of inside and outside conductive carbon has just been opened in the invention, its step are as follows: 1) glucose and distilled water being put into reaction kettle, heating reaction, to after reaction, solution in autoclave body is filtered, solution A is obtained；2) above-mentioned solution A and distilled water being imported in reaction flask, ferrous sulfate is added for stirring, and hydrogen peroxide is added, pH value is adjusted using ammonium hydroxide, when integrally there is yellow-white precipitating in solution, ageing；Small particle and suspension fine particle are removed through centrifuge washing, obtains ferric phosphate predecessor B；3) predecessor B high temperature is removed water；After water removal, the ferric phosphate raw material of acquisition and Li source compound, organic carbon source are put into the atmosphere furnace of inert gas shielding, calcining at constant temperature；4) step 3) crushed, obtain a kind of lithium iron phosphate positive material for realizing inside and outside conductive carbon and being modified after classification.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, and in particular to a kind of to prepare what inside and outside conductive carbon was modified
The method of LiFePO4.
Background technique
LiFePO4It is current one of the most common type anode material for lithium-ion batteries, there is stable olivine structural, energy can
Inverse insertion and deintercalate lithium ions.And high-energy density, performance is stable, highly-safe, environmental-friendly, price is cheaper.
It is considered as most potential anode material for lithium-ion batteries.Pure phase LiFePO4Conductivity is small by (about 10-9S/cm), ion
Diffusion coefficient is low, limits discharge capability under its high current density, and the poor difference of cycle performance limits LiFePO4Application.Mirror
In such disadvantage, each manufacturer and colleges and universities carry out improvement LiFePO successively4The research of performance, including cladding, doping, modification technology
It is refinement crystal grain, ion doping and carbon coating Deng, the mode generallyd use herein, in view of the conventional preparation side of LiFePO4
Method, such as high temperature solid-state method, sol-gel method, liquid-phase coprecipitation, carbothermic method, ion excessively refine the group that can be generated
Poly- phenomenon, and ion doping is then difficult to realize industrialize, while being easy to produce new impurity, production technology complexity stability is poor,
It is unable to satisfy the demand of volume production；Generally speaking, carbon coating production is simple and convenient, can obtain good improvement, therefore solve
LiFePO4 electrical conductivity problems, carbon coating become existing market main flow direction.
At the same time, carbon coating still remains part short slab, and such as good carbon coating can obtain the Gao Rong under low range
Amount plays, but in big multiplying power, heavy-current discharge, it, can not inside LiFePO4 according to " the radial model " of charge and discharge electric theory
Avoid there are dead zone areas, lead to the irreversible capacitance loss of LiFePO4；Rarely have people to refer in the industry in this problem uplink
Solution, only in field of graphene in recent years, academia proposed the theory being doped using graphene, such as patent
" a kind of preparation method of graphene doping vario-property LiFePO4 " and a kind of " nanometer metal oxide/graphene doping phosphoric acid iron
The preparation method of lithium electrode material " refer to the reaction raw material mixture obtained in the way of high-energy ball milling etc. containing graphene,
Then the iron lithium material of graphene doping is realized by calcining together, this point is coated better than simple outer layer carbon source, but same
Sample be limited to graphene with the broken scale particle size of degree of mixedness and graphene that reacts raw material, there are larger unevenness for material
Even property, and not can avoid capacitance loss caused by core inner dead zone area, therefore the dead zone area in LiFePO4 circulation
Still have in terms of capacitance loss caused by increasing and has masses of work to do.
Summary of the invention
It is poor that the present invention is directed to conventional carbon-coated LiFePO 4 for lithium ion batteries material improvement, and it is low to change material electric conductivity, multiplying power
The problems such as electric discharge difference, propose the technical method and technique for carrying out the modified LiFePO4 of conductive carbon inside and outside a kind of realize respectively:
1) by the preparation of Nano carbon balls, screening, using its nanoscale sphere structure as the growth in ferric phosphate synthesis process
Epipole realizes the system of the internal ferric phosphate " having core structure " comprising carbon ball by the nanosphere method almost synchronous with ferric phosphate
It is standby；
2) it will be removed water under the ferric phosphate nitrogen atmosphere of aqueous " the having core structure " of acquisition, be on the one hand conducive to phosphoric acid iron material
Expect the reduction of lattice defect and the stabilization of cell configuration, is on the other hand also beneficial to the carbonisation of " heart " carbon ball；
3) ferric phosphate raw material and Li source compound, organic carbon source are by calcining at constant temperature acquisition phosphorus under inert gas shielding
Sour iron lithium finished-product material.
Technical scheme is as follows:
A method of preparing the modified LiFePO4 of inside and outside conductive carbon, characterized in that preparation method is:
1) glucose and distilled water are put into reaction kettle according to 1:10 ratio, liquor capacity accounts for the 2/ of entire autoclave body volume
3, reaction kettle is tightened after glucose all dissolution, heating is reacted, and 150 DEG C -160 DEG C of heating temperature, reaction time 2-3 h, to
Reaction terminates and is cooled to room temperature, and solution in autoclave body was filtered the organic filter membrane of 200-300nm, obtains solution A；
2) after by above-mentioned solution A and distilled water according to 1:3-5 dilution proportion, rotating speed of agitator 200-300r/min is opened,
Then ferrous sulfate is added and is dissolved, excessive hydrogen peroxide is added, adjusted pH value between 3-4 using ammonium hydroxide, integrally go out to solution
When existing yellow-white precipitating, adjusting revolving speed is 500-700r/min, starts to be aged, and digestion time is 5-10 hours；After ageing,
Small particle and suspension fine particle are removed through centrifuge washing, obtains ferric phosphate predecessor B；
3) above-mentioned predecessor B is placed in progress high temperature water removal under nitrogen protection, temperature for removing water is 500-600 DEG C；After water removal,
By the ferric phosphate raw material of acquisition and Li source compound, organic carbon source according to Li:Fe: organic carbon source=1.00-1.05:1:0.05-
Then the ratio ingredient of 0.5 molar ratio is put into the atmosphere furnace of inert gas shielding, in 650-750 DEG C of calcining at constant temperature 4-6h；
4) one kind is obtained after the LiFePO 4 material that step 3) obtains being crushed, is classified realizes inside and outside conductive carbon modification
Lithium iron phosphate positive material.
The Li source compound is one of lithium carbonate, lithium hydroxide, lithium oxalate and lithium nitrate or several mixing
Object.
The organic carbon source is one of glucose, sucrose and polyvinyl alcohol or several mixtures.
The present invention has the following advantages:
1, the preparation of carbon ball and the screening of the organic filter membrane of predetermined size obtain growth cores for ferric phosphate precursor preparation
Point, excessive specific surface area are conducive to the attachment that crystallization is precipitated, and stirring makes whole ferric phosphate persursor material particle almost spherical,
Material is set to be provided with better consistency and uniformity；
2, on the one hand the filling of carbon ball improves material internal electric conductivity, improves the conductivity of integral material, reduces simultaneously
The specific gravity of active material, reduces caused by the electric discharge dead zone area that " radial diffusion " model refers to inside single material granule
Capacity loss.The capacity for improving LiFePO 4 material plays specific gravity.
3, the dehydration of the ferric phosphate of aqueous " having core structure " on the one hand enhances the crystalline state of material itself, realizes crystalline substance
Type conversion, reduction of the another aspect cell parameter in removal process also further reduce monomer particle volume and " intentionally " knot
The stabilization of structure.
Detailed description of the invention
Fig. 1 is 1 synthesizing iron lithium phosphate positive electrode electron microscope of embodiment；
Fig. 2 is 1 graphene of comparative example doping synthesis iron lithium material electron microscope；
Fig. 3 is the complete electric rate discharge curves of LiFePO4 prepared by embodiment 1.
Specific embodiment
The preparation of the modified LiFePO4 of conductive carbon is carried out inside and outside realizing below with reference to embodiment is a kind of to the present invention respectively
Method makees explanation in detail.
Embodiment 1:
1) glucose and distilled water are put into 50mL reaction kettle according to 1:10 ratio, liquor capacity accounts for entire autoclave body volume
2/3, after glucose all dissolution after tighten reaction kettle, be put into baking oven.Set reaction condition are as follows: 150 DEG C of temperature, when reaction
Between 3 h.It to the end of reacting and is cooled to room temperature, solution in autoclave body was filtered into the organic filter membrane of 200nm, obtains solution A；
2) it after diluting above-mentioned solution A and distilled water according to 1:3, imports in reaction flask, opens rotating speed of agitator 300r/
Then ferrous sulfate is added and dissolves by min, excessive hydrogen peroxide is added, and adjusting pH value using ammonium hydroxide is 3, integrally occurs to solution
When yellow-white precipitates, adjusting revolving speed is 500r/min, starts timing ageing, and digestion time is 5 hours；After ageing, through from
Heart washing removes, and small particle and suspension fine particle obtain ferric phosphate predecessor B；
3) above-mentioned predecessor B is placed in progress high temperature water removal in the Muffle furnace under nitrogen protection, temperature for removing water is 600 DEG C；
After water removal, by the ferric phosphate raw material of acquisition and Li source compound, organic carbon source according to Li:Fe: organic carbon source=1.05:1:
Then the ratio ingredient of 0.055 molar ratio is put into the atmosphere furnace of the inert gas shieldings such as nitrogen or argon gas, in 750 DEG C of perseverances
Temperature calcining 4h；
4) one kind is obtained after the LiFePO 4 material that step 3) obtains being crushed, is classified realizes inside and outside conductive carbon modification
Lithium iron phosphate positive material.
Using the lithium iron phosphate positive material being prepared as active material, (gather inclined fluorine with conductive agent (acetylene black), binder
Ethylene, PVDF) electrode slice is made, metal lithium sheet is that electrode and reference electrode are assembled half-cell, filled in 25 DEG C of environment
Discharge test.
1 lithium iron phosphate positive material multiplying power of embodiment and low temperature discharge data are as follows.
| Test serial number | 0.2C discharges (mAh/g) | 3C discharges (mAh/g) | Low temperature (- 20 DEG C) 0.5C discharges (mAh/g) |
| Embodiment 1 | 159.4 | 142.5 | 100.6 |
Embodiment 2:
1) glucose and distilled water are put into 100mL reaction kettle according to 1:10 ratio, liquor capacity accounts for entire autoclave body body
Long-pending 2/3 is tightened reaction kettle after glucose all dissolution, is put into baking oven.Set reaction condition are as follows: 160 DEG C of temperature, reaction
2 h of time.It to the end of reacting and is cooled to room temperature, solution in autoclave body was filtered into the organic filter membrane of 200nm, obtains solution A；
2) it after diluting above-mentioned solution A and distilled water according to 1:5, imports in reaction flask, opens rotating speed of agitator 300r/
Then ferrous sulfate is added and dissolves by min, excessive hydrogen peroxide is added, and adjusting pH value using ammonium hydroxide is 3, integrally occurs to solution
When yellow-white precipitates, adjusting revolving speed is 500r/min, starts timing ageing, and digestion time is 5 hours；After ageing, through from
Heart washing removes, and small particle and suspension fine particle obtain ferric phosphate predecessor B；
3) above-mentioned predecessor B is placed in progress high temperature water removal in the Muffle furnace under nitrogen protection, temperature for removing water is 560 DEG C；
After water removal, by the ferric phosphate raw material of acquisition and Li source compound, organic carbon source according to Li:Fe: organic carbon source=1.05:1:
Then the ratio ingredient of 0.05 molar ratio is put into the atmosphere furnace of the inert gas shieldings such as nitrogen or argon gas, in 750 DEG C of constant temperature
Calcine 4h；
4) one kind is obtained after the LiFePO 4 material that step 3) obtains being crushed, is classified realizes inside and outside conductive carbon modification
Lithium iron phosphate positive material.
2 lithium iron phosphate positive material multiplying power of embodiment and low temperature discharge data are as follows.
| Test serial number | 0.2C discharges (mAh/g) | 3C discharges (mAh/g) | Low temperature (- 20 DEG C) 0.5C discharges (mAh/g) |
| Embodiment 2 | 155.7 | 140.5 | 94.5 |
Comparative example 1:
By lithium carbonate, ferrous oxalate, ammonium dihydrogen phosphate, graphene according to Li:Fe:P: graphene or doped metallic elements=
The ratio of 0.95-1.05:1:1:0.05 (molar ratio), weigh respectively corrresponding quality investment ball mill in, by Φ=10mm, Φ=
Three kinds of zirconia balls of 250mm, Φ=50mm respectively claim 250g to put into ball mill, and ball milling 6h, material mixing are thrown afterwards in ball mill
Enter in the atmosphere furnace of nitrogen protection, in 670 DEG C of calcining at constant temperature 12h.One kind is obtained after sintered material is crushed, is classified
The LiFePO4 of doped graphene.
Managing material comparison with ferric phosphate obtained by the doping of ordinary graphite alkene as 1 resulting materials electron microscope of embodiment can see
Out, the obtained LiFePO4 of comparative example 1 is realized with the modification mode of graphene approximation mixing and doping, graphite for entirety
Alkene is not coated on inside lithium iron phosphate particles completely, and as shown in the elliptic region of Fig. 2, part graphene is still with larger
The state of pattern exists, and is doped between finished product lithium iron phosphate；And 1 gained iron lithium finished figure 1 of embodiment is orderly always, size is big
It is small uniform, it is different from the similar state of graphene doping " hybrid ".
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
It for specific embodiments of the present invention, is not intended to restrict the invention, all any modifications made in spirit of the invention
With improve etc., should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of method for preparing the modified LiFePO4 of inside and outside conductive carbon, characterized in that preparation method is:
1) glucose and distilled water being put into reaction kettle according to 1:10 ratio, liquor capacity accounts for the 2/3 of entire autoclave body volume, to
Glucose tightens reaction kettle after all dissolving, heating is reacted, and 150 DEG C -160 DEG C of heating temperature, reaction time 2-3 h, wait react
Terminate and be cooled to room temperature, solution in autoclave body was filtered into the organic filter membrane of 200-300nm, obtains solution A；
2) after by above-mentioned solution A and distilled water according to 1:3-5 dilution proportion, rotating speed of agitator 200-300r/min is opened, then
Ferrous sulfate is added and is dissolved, excessive hydrogen peroxide is added, pH value is adjusted between 3-4 using ammonium hydroxide, Huang integrally occurs to solution
When white precipitate, adjusting revolving speed is 500-700r/min, starts to be aged, and digestion time is 5-10 hours；After ageing, through from
Heart washing removes small particle and suspension fine particle, obtains ferric phosphate predecessor B；
3) above-mentioned predecessor B is placed in progress high temperature water removal under nitrogen protection, temperature for removing water is 500-600 DEG C；After water removal, it will obtain
The ferric phosphate raw material and Li source compound, organic carbon source obtained are according to Li:Fe: organic carbon source=1.00-1.05:1:0.05-0.5
Molar ratio ratio ingredient, then put into inert gas shielding atmosphere furnace in, in 650-750 DEG C of calcining at constant temperature 4-6h；
4) LiFePO 4 material that step 3) obtains crushed, obtain a kind of phosphorus for realizing inside and outside conductive carbon and being modified after classification
Sour iron lithium anode material.
2. a kind of method for preparing the modified LiFePO4 of inside and outside conductive carbon as described in claim 1, characterized in that described
Li source compound is one of lithium carbonate, lithium hydroxide, lithium oxalate and lithium nitrate or several mixtures.
3. a kind of method for preparing the modified LiFePO4 of inside and outside conductive carbon as described in claim 1, characterized in that described
Organic carbon source is one of glucose, sucrose and polyvinyl alcohol or several mixtures.
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| CN101337666A (en) * | 2008-08-04 | 2009-01-07 | 清华大学 | Method for preparing spherical ferric lithium phosphate by oxidation control crystal-carbon thermal reduction method |
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| CN102810670A (en) * | 2012-08-01 | 2012-12-05 | 因迪能源（苏州）有限公司 | Composite anode material of lithium ion battery and preparation method |
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| JP5004413B2 (en) * | 2004-08-20 | 2012-08-22 | 日本コークス工業株式会社 | Method for producing positive electrode material for ammonium iron phosphate and lithium ion secondary battery, and lithium ion secondary battery |
| JP5776573B2 (en) * | 2012-02-06 | 2015-09-09 | 住友金属鉱山株式会社 | Positive electrode active material for lithium secondary battery and method for producing the same, precursor of the positive electrode active material and method for producing the same, and lithium secondary battery using the positive electrode active material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337666A (en) * | 2008-08-04 | 2009-01-07 | 清华大学 | Method for preparing spherical ferric lithium phosphate by oxidation control crystal-carbon thermal reduction method |
| CN102509643A (en) * | 2011-11-29 | 2012-06-20 | 西北师范大学 | Graphene/carbon ball composite material, and preparation and application thereof |
| CN102810670A (en) * | 2012-08-01 | 2012-12-05 | 因迪能源（苏州）有限公司 | Composite anode material of lithium ion battery and preparation method |
| CN103367724A (en) * | 2013-07-26 | 2013-10-23 | 烟台卓能电池材料有限公司 | Lithium iron phosphate cell material with core-shell structure, and preparation method thereof |
| CN103436269A (en) * | 2013-08-19 | 2013-12-11 | 太原理工大学 | Method for preparing flame retardant through coating carbon microsphere with magnesium hydroxide |
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Address after: 277800 No. x6699, Guangming Road, high tech Zone, Zaozhuang City, Shandong Province (north of the junction of Guangming Road and Huaxin Road) Patentee after: Shandong Jinggong Electronic Technology Co.,Ltd. Address before: Shandong Jinggong Electronic Technology Co., Ltd., No. 319, Fuyuan 5th Road, Thailand Industrial Park, Zaozhuang Hi tech Zone, Shandong 277000 Patentee before: Shandong Seiko Electronic Technology Co.,Ltd. |
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| CP03 | Change of name, title or address |