CN105428617A - Iron phosphate carbon sphere synchronous synthesis and internal-external conductive carbon modified lithium iron phosphate preparation method - Google Patents
Iron phosphate carbon sphere synchronous synthesis and internal-external conductive carbon modified lithium iron phosphate preparation method Download PDFInfo
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- CN105428617A CN105428617A CN201510780949.2A CN201510780949A CN105428617A CN 105428617 A CN105428617 A CN 105428617A CN 201510780949 A CN201510780949 A CN 201510780949A CN 105428617 A CN105428617 A CN 105428617A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
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- 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
- H01M4/36—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
- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an iron phosphate carbon sphere synchronous synthesis carbonization and internal-external conductive carbon modified lithium iron phosphate preparation method. The method comprises the following steps of: 1) putting glucose and distilled water into a reaction kettle, performing a heating reaction, and after the reaction is ended, performing suction filtration on a solution in the kettle to obtain a solution A; 2) leading the solution A and the distilled water into a reaction flask, stirring, adding ferrous sulfate and hydrogen peroxide, regulating the pH value by utilizing ammonia water, and ageing when yellow white deposits occur in the whole solution; performing centrifugal washing to remove small-sized and suspended fine particles so as to obtain an iron phosphate precursor B; 3) performing high-temperature dehydration on the precursor B; after the dehydration, adding an obtained iron phosphate raw material, a lithium source compound and an organic carbon source into an atmosphere furnace protected by an inert gas, and performing constant-temperature calcination; and 4) grinding and grading a calcined material in the step 3) to obtain an internal-external conductive carbon modified lithium iron phosphate positive electrode material.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, be specifically related to the method for the LiFePO4 of a kind of lithium iron phosphate/carbon ball synchronized compound and the inside and outside conductive carbon modification of preparation.
Background technology
LiFePO
4be current modal a kind of anode material for lithium-ion batteries, there is stable olivine structural, can reversible embedding and deintercalate lithium ions.And high-energy-density, stable performance, fail safe is high, environmental friendliness, price are more cheap.Be considered to the potential anode material for lithium-ion batteries of most.Pure phase LiFePO
4conductivity is little (is about 10
-9s/cm), ionic diffusion coefficient is low, and limit discharge capability under its high current density, the poor difference of cycle performance, limits LiFePO
4application.In view of this type of shortcoming, each manufacturer and colleges and universities carry out successively and improve LiFePO
4the research of performance, comprise coated, doping, modification technology etc., the mode here usually adopted is that crystal grain thinning, ion doping and carbon are coated, in view of the customary preparation methods of LiFePO4, as high temperature solid-state method, sol-gel process, liquid-phase coprecipitation, carbothermic method etc., the agglomeration that the excessive refinement of ion can produce, ion doping is then difficult to realize industrialization, easily produce new impurity, complex manufacturing poor stability, cannot meet the demand of volume production simultaneously; Generally speaking, the coated production of carbon is simple and convenient, can obtain good improvement effect, and therefore solve LiFePO4 electrical conductivity problems, carbon is coated becomes existing market main flow direction.
Meanwhile, carbon is coated still exists part short slab, carbon as good is coated, and the high power capacity that can obtain under low range plays, but when large multiplying power, heavy-current discharge, according to " the radial model " of discharge and recharge theory, inevitably there is dead zone area in LiFePO4 inside, causes the irreversible capacitance loss of LiFePO4, people is rarely had in the industry to mention solution this problem is up, only in field of graphene in recent years, academia proposed to utilize Graphene to carry out the theory of adulterating, as patent " a kind of preparation method of Graphene doping vario-property LiFePO4 " and " a kind of preparation method of nanometer metallic oxide/graphene doped lithium iron phosphate electrode material " mention that modes such as utilizing high-energy ball milling obtains the reaction raw material mixture containing Graphene, then by calcining the iron lithium material realizing Graphene doping together, it is coated that this point is better than simple outer carbon source, but be limited to Graphene and the scale particle size reacted after raw-material degree of mixedness and Graphene fragmentation equally, there is larger inhomogeneities in material, and the capacitance loss that core inner dead zone area causes cannot be avoided, therefore in LiFePO4 circulation, dead zone area to increase in the capacitance loss that causes still tool and has masses of work to do.
Summary of the invention
The present invention is directed to conventional carbon-coated LiFePO 4 for lithium ion batteries material and improve weak effect, cannot change material electric conductivity low, the problems such as multiplying power discharging difference, propose technical method and the technique of the LiFePO4 carrying out conductive carbon modification inside and outside a kind of realization respectively:
1) by preparation, the screening of Nano carbon balls, with its nanoscale sphere structure for the growth epipole in ferric phosphate building-up process, be close to synchronous method by nanosphere and ferric phosphate and realize the preparation that the inner ferric phosphate comprising carbon ball " has core structure ";
2) dewater under the ferric phosphate nitrogen atmosphere of moisture " having core structure " of obtaining, be conducive to the minimizing of iron phosphate material lattice defect and the stable of cell configuration on the one hand, be also conducive to the carbonisation of " heart " carbon ball on the other hand;
3) ferric phosphate raw material and Li source compound, organic carbon source calcining at constant temperature under inert gas shielding obtain LiFePO4 finished-product material.
Technical scheme of the present invention is as follows:
A method for the LiFePO4 of lithium iron phosphate/carbon ball synchronized compound and the inside and outside conductive carbon modification of preparation, it is characterized in that, preparation method is:
1) glucose and distilled water are put into reactor according to 1:10 ratio, liquor capacity accounts for 2/3 of whole kettle volume, reactor is tightened after glucose all dissolves, add thermal response, heating-up temperature 150 DEG C-160 DEG C, reaction time 2-3h, question response terminates and after being down to room temperature, solution suction filtration in kettle is crossed the organic filter membrane of 200-300nm, obtains solution A;
2) by above-mentioned solution A and distilled water according to after 1:3-5 dilution proportion, open rotating speed of agitator 200-300r/min, then ferrous sulfate is added dissolving, add excessive hydrogen peroxide, utilize ammoniacal liquor to regulate pH value between 3-4, when solution entirety occurs that yellow-white precipitates, adjusting rotary speed is 500-700r/min, start ageing, digestion time is 5-10 hour; After ageing terminates, through centrifuge washing removing small particle diameter and suspension fine particle, obtain ferric phosphate predecessor B;
3) carry out high temperature under above-mentioned predecessor B being placed in nitrogen protection to dewater, temperature for removing water is 500-600 DEG C; After dewatering, by obtain ferric phosphate raw material and Li source compound, organic carbon source is according to Li:Fe:P: the ratio of the mol ratio of organic carbon source=1.00-1.05:1:0.05-0.5 is prepared burden, then drop in the atmosphere furnace of inert gas shielding, in 650-750 DEG C of calcining at constant temperature 4-6h;
4) a kind of lithium iron phosphate positive material achieving inside and outside conductive carbon modification is namely obtained after LiFePO 4 material pulverizing step 3) obtained, classification.
Described lithium salt compound is the mixture of one or several in lithium carbonate, lithium hydroxide, lithium oxalate and lithium nitrate.
Described organic carbon source is the mixture of one or several in glucose, sucrose and polyvinyl alcohol.
The present invention has following advantage:
1, the preparation of carbon ball and the screening of the organic filter membrane of given size, for ferric phosphate precursor power obtains growth epipole, excessive specific area is conducive to the attachment of crystallization, stirs and makes overall ferric phosphate persursor material particle almost spherical, make material be provided with better consistency and uniformity;
2, the filling of carbon ball on the one hand improves material internal conductivity, improves the conductivity of integral material, reduces the proportion of the inner active material of single material granule simultaneously, decreases the capacity loss that electric discharge dead zone area that " radial diffusion " model mentions causes.The capacity that improve LiFePO 4 material plays proportion.
3, the dehydration of the ferric phosphate of moisture " having core structure " enhances the crystalline state of material itself on the one hand, achieve crystal formation conversion, on the other hand the reduction of cell parameter in removal process also further reduces the stable of monomer particle volume and " intentionally " structure.
Accompanying drawing explanation
Fig. 1 is embodiment 1 synthesizing iron lithium phosphate positive electrode Electronic Speculum figure;
Fig. 2 is comparative example 1 Graphene doping synthesis iron lithium material Electronic Speculum figure;
Fig. 3 is the complete electric rate discharge curves of LiFePO4 prepared by embodiment 1.
Embodiment
Below in conjunction with embodiment to the present invention is a kind of realize inside and outside carry out the LiFePO4 of conductive carbon modification respectively preparation method do detailed explanation.
Embodiment 1:
1) glucose and distilled water are put into 50mL reactor according to 1:10 ratio, liquor capacity accounts for 2/3 of whole kettle volume, tightens reactor, put into baking oven after glucose all dissolves.Setting reaction condition is: temperature 150 DEG C, reaction time 3h.Question response terminates and after being down to room temperature, solution suction filtration in kettle is crossed the organic filter membrane of 200nm, obtains solution A;
2) after above-mentioned solution A and distilled water being diluted according to 1:3, import in reaction flask, open rotating speed of agitator 300r/min, then ferrous sulfate is added dissolving, add excessive hydrogen peroxide, utilize ammoniacal liquor to regulate pH value to be 3, when solution entirety occurs that yellow-white precipitates, adjusting rotary speed is 500r/min, and start timing ageing, digestion time is 5 hours; After ageing terminates, through centrifuge washing removing, small particle diameter and suspension fine particle, obtain ferric phosphate predecessor B;
3) be placed in by above-mentioned predecessor B and carry out high temperature in the Muffle furnace under nitrogen protection and dewater, temperature for removing water is 600 DEG C; After dewatering, by obtain ferric phosphate raw material and Li source compound, organic carbon source is according to Li:Fe:P: the ratio of the mol ratio of organic carbon source=1.05:1:0.055 is prepared burden, then drop in the atmosphere furnace of the inert gas shielding such as nitrogen or argon gas, in 750 DEG C of calcining at constant temperature 4h;
4) a kind of lithium iron phosphate positive material achieving inside and outside conductive carbon modification is namely obtained after LiFePO 4 material pulverizing step 3) obtained, classification.
With the lithium iron phosphate positive material prepared for active material, make electrode slice with conductive agent (acetylene black), binding agent (Kynoar, PVDF), metal lithium sheet is to electrode and reference electrode, assembling half-cell, carries out charge-discharge test in 25 DEG C of environment.
Embodiment 1 lithium iron phosphate positive material multiplying power and low temperature discharge data as follows.
| Experiment sequence 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 reactor according to 1:10 ratio, liquor capacity accounts for 2/3 of whole kettle volume, tightens reactor, put into baking oven after glucose all dissolves.Setting reaction condition is: temperature 160 DEG C, reaction time 2h.Question response terminates and after being down to room temperature, solution suction filtration in kettle is crossed the organic filter membrane of 200nm, obtains solution A;
2) after above-mentioned solution A and distilled water being diluted according to 1:5, import in reaction flask, open rotating speed of agitator 300r/min, then ferrous sulfate is added dissolving, add excessive hydrogen peroxide, utilize ammoniacal liquor to regulate pH value to be 3, when solution entirety occurs that yellow-white precipitates, adjusting rotary speed is 500r/min, and start timing ageing, digestion time is 5 hours; After ageing terminates, through centrifuge washing removing, small particle diameter and suspension fine particle, obtain ferric phosphate predecessor B;
3) be placed in by above-mentioned predecessor B and carry out high temperature in the Muffle furnace under nitrogen protection and dewater, temperature for removing water is 560 DEG C; After dewatering, by obtain ferric phosphate raw material and Li source compound, organic carbon source is according to Li:Fe:P: the ratio of the mol ratio of organic carbon source=1.05:1:0.05 is prepared burden, then drop in the atmosphere furnace of the inert gas shielding such as nitrogen or argon gas, in 750 DEG C of calcining at constant temperature 4h;
4) a kind of lithium iron phosphate positive material achieving inside and outside conductive carbon modification is namely obtained after LiFePO 4 material pulverizing step 3) obtained, classification.
Embodiment 2 lithium iron phosphate positive material multiplying power and low temperature discharge data as follows.
| Experiment sequence 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: the ratio of Graphene or doped metallic elements=0.95-1.05:1:1:0.05 (mol ratio); taking respective quality respectively drops in ball mill; 250g is respectively claimed by three kinds of zirconia balls of Φ=10mm, Φ=250mm, Φ=50mm to drop in ball mill ball milling 6h in ball mill; mixing of materials drops in the atmosphere furnace of nitrogen protection all afterwards, in 670 DEG C of calcining at constant temperature 12h.Namely material after sintering is obtained after pulverizing, classification a kind of LiFePO4 of doped graphene.
Manage material contrast can find out by embodiment 1 resulting materials Electronic Speculum figure and the ordinary graphite alkene gained ferric phosphate that adulterates, the LiFePO4 that comparative example 1 obtains is similar to the modification mode realization of mixing and doping with Graphene, entirety Graphene is not coated on lithium iron phosphate particles inside completely, as shown in the elliptic region of Fig. 2, part Graphene is still exist with the state of larger pattern, is doped between finished product lithium iron phosphate; And embodiment 1 gained iron lithium finished figure 1 is always orderly, size is even, is different from the state that Graphene doping " hybrid " is similar.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any amendments and improvement etc. made in spirit of the present invention, all should be included within protection scope of the present invention.
Claims (3)
1. a method for the LiFePO4 of lithium iron phosphate/carbon ball synchronized compound and the inside and outside conductive carbon modification of preparation, it is characterized in that, preparation method is:
1) glucose and distilled water are put into reactor according to 1:10 ratio, liquor capacity accounts for 2/3 of whole kettle volume, reactor is tightened after glucose all dissolves, add thermal response, heating-up temperature 150 DEG C-160 DEG C, reaction time 2-3h, question response terminates and after being down to room temperature, solution suction filtration in kettle is crossed the organic filter membrane of 200-300nm, obtains solution A;
2) by above-mentioned solution A and distilled water according to after 1:3-5 dilution proportion, open rotating speed of agitator 200-300r/min, then ferrous sulfate is added dissolving, add excessive hydrogen peroxide, utilize ammoniacal liquor to regulate pH value between 3-4, when solution entirety occurs that yellow-white precipitates, adjusting rotary speed is 500-700r/min, start ageing, digestion time is 5-10 hour; After ageing terminates, through centrifuge washing removing small particle diameter and suspension fine particle, obtain ferric phosphate predecessor B;
3) carry out high temperature under above-mentioned predecessor B being placed in nitrogen protection to dewater, temperature for removing water is 500-600 DEG C; After dewatering, by obtain ferric phosphate raw material and Li source compound, organic carbon source is according to Li:Fe:P: the ratio of the mol ratio of organic carbon source=1.00-1.05:1:0.05-0.5 is prepared burden, then drop in the atmosphere furnace of inert gas shielding, in 650-750 DEG C of calcining at constant temperature 4-6h;
4) a kind of lithium iron phosphate positive material achieving inside and outside conductive carbon modification is namely obtained after LiFePO 4 material pulverizing step 3) obtained, classification.
2. the method for the LiFePO4 of a kind of lithium iron phosphate/carbon ball synchronized compound as claimed in claim 1 and the inside and outside conductive carbon modification of preparation, it is characterized in that, described lithium salt compound is the mixture of one or several in lithium carbonate, lithium hydroxide, lithium oxalate and lithium nitrate.
3. the method for the LiFePO4 of a kind of lithium iron phosphate/carbon ball synchronized compound as claimed in claim 1 and the inside and outside conductive carbon modification of preparation, it is characterized in that, described organic carbon source is the mixture of one or several in glucose, sucrose and polyvinyl alcohol.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114678526A (en) * | 2022-02-28 | 2022-06-28 | 合肥国轩高科动力能源有限公司 | Preparation method of high-performance carbon-coated lithium iron phosphate composite material |
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