CN105322167A - Pressure-controlling deaggregating synthetic method for lithium iron phosphate positive electrode material - Google Patents

Pressure-controlling deaggregating synthetic method for lithium iron phosphate positive electrode material Download PDF

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Publication number
CN105322167A
CN105322167A CN201510732890.XA CN201510732890A CN105322167A CN 105322167 A CN105322167 A CN 105322167A CN 201510732890 A CN201510732890 A CN 201510732890A CN 105322167 A CN105322167 A CN 105322167A
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ultrasonic wave
pressure
wave added
kettle
iron phosphate
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CN105322167B (en
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关成善
宗继月
孟博
杜显振
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Shandong Goldencell Electronics Technology Co Ltd
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Shandong Goldencell Electronics Technology Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/265—General methods for obtaining phosphates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • 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
    • 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

The invention aims to provide a pressure-controlling deaggregating synthetic method for a lithium iron phosphate positive electrode material. The method is suitable for the lithium iron phosphate positive electrode material with certain strength, with a coating layer on the surface of the material, and with small primary grain diameters. The pressure-controlling deaggregating synthetic method performs the reaction, uniform mixing and coating of the materials in gradient through an ultrasonic microwave reaction kettle; and a uniform reaction and a controllable process of the approximate nanoscale raw materials are finally realized. The prepared battery material is relatively high in particle uniformity and consistency; meanwhile, the powder is small in particles; and therefore, the lithium iron phosphate material is higher in the conductivity and the ion diffusion rate, and the electroelectroless performance of the material is greatly improved.

Description

A kind of pressure control solution reunion synthetic method of lithium iron phosphate positive material
Technical field
The present invention relates to a kind of preparation method of iron phosphate lithium positive pole lithium ion battery material, be specifically related to a kind of pressure control solution reunion synthetic method of lithium iron phosphate positive material.
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., but here crystal grain thinning technology appreciate by more people, but in view of the common preparation method of LiFePO4, as high temperature solid-state method, sol-gel process, liquid-phase coprecipitation, carbothermic method etc., fundamentally cannot stop the agglomeration that high temperature sintering produces, and conventional hydrothermal rule is difficult to realize industrialization, simultaneously high to equipment requirement, costly; Complex manufacturing, manufacturing cycle is long, repeatable poor, cannot meet the demand of volume production; Therefore solve LiFePO4 finished particle agglomeration techniques and become particularly important.
First Nano diamond mechanical lapping and chemical modification are synchronously carried out as mentioned in patent " solution of CN02139764.3 Nano diamond is reunited and stage division ", be dispersed into the small agglomerates that particle mean size is 7 ~ 200nm, then the thick nano diamond particles in suspension and other composition removed; Finally add wetting agent, surfactant, dispersion stabilizer and pH value regulator, adopt dispersed with stirring diamond finally to realize the classification of Nano diamond, its particle diameter controllable adjustment between 7 ~ 200 nanometers can be made; And for example mention in the University Of Tianjin's patent method of dispersing detonation method nano-diamond " CN201010224986.2 in the liquid phase " with business detonation method nano-diamond powder for raw material, be mixed in liquid medium, form suspension; Use pulsed laser ablation this suspension, action time is 1-3h, the effect suspension stabilization obtained, does not precipitate; Finally strong acid oxidation processes is carried out to the product after laser bombardment, obtain monodispersed diamond nano-particles.Below the micronization processes that the means utilizing liquid phase cooperative mechanical to grind can realize powder body material is all referred to, even use laser bombardment means, it is large that this certain methods is applicable to hardness, and hardness is large, the diamond of good stability, but in the middle of the solution agglomeration process being difficult to transit to LiFePO 4 material.
Summary of the invention
The object of the present invention is to provide and be a kind ofly applicable to having some strength, material surface with the pressure control solution reunion synthetic method of coating layer, lithium iron phosphate positive material that powder body material particle diameter is little.Prepared battery material has higher particle uniformity and consistency, and powder granule is little, and therefore LiFePO 4 material has higher conductivity and ion diffusion rates, drastically increases the chemical property of material.
For achieving the above object, the preparation method that the present invention adopts is as follows.
A pressure control solution reunion synthetic method for lithium iron phosphate positive material, it is characterized in that, preparation process is divided into following step:
1) by FePO 42H 2o, after high temperature dewaters, is added to ultrasonic wave added microwave reaction kettle, adds LiOHH according to the mol ratio of Li: Fe=1 ~ 1.02: 1 2o or Li 2cO 3add than the ratio for 1:0.5 ~ 1 the Vc aqueous solution that concentration is 10%-40% again according to cumulative volume, open ultrasonic wave added and microwave heating simultaneously, control material temperature at 20 DEG C-50 DEG C, duration 5-10min, forming predecessor A, by predecessor A through cooling fast after 200-300 DEG C of sintering 30min to 50min under revolving burner nitrogen protection, obtaining powder predecessor B;
2) predecessor B to be weighed and after loading ultrasonic wave added microwave reaction kettle, 1:0.2 ~ 0.5 takes the D/W that concentration is 50% in mass ratio, after unlatching ultrasonic wave added 5min, close ultrasonic wave added microwave reaction kettle kettle cover, adjustment pressure is 0.2-0.3MPa, open ultrasonic wave added, high-power unlatching microwave heating disappears to air pressure, obtains solid precursors C;
3) precursor C is sent back to revolving burner, cool fast after 400-500 DEG C of sintering 30min to 60min under nitrogen protection, then take out gained material and repeat 2) operation, product D is obtained after 500-700 under nitrogen protection DEG C of sintering 60min to 90min, finally, the dextrin in aqueous solution that concentration is 30% is taken according to the mass ratio of mass ratio 1:0.5 ~ 1, close ultrasonic wave added microwave reaction kettle kettle cover, independent unlatching microwave heating, adjustment pressure is 0.1-0.15MPa, duration is that about 10-20min disappears to air pressure, anode material for lithium-ion batteries is cooled to obtain fast after 150-250 under nitrogen protection DEG C of sintering 20min to 40min.
The pressure control solution reunion synthetic method of a kind of lithium iron phosphate positive material described above, is characterized in that, described ultrasonic wave added microwave reaction kettle be by 1, outside kettle; 2, kinetoplast; 3, spiral live body; 4, inner kettle; 5, pressure controller; 6, kettle cover; 7. pressure release passage; 8, microwave source; 9, supersonic source is formed.
Ultrasonic disperse is as the sound wave of a kind of frequency higher than 20000 hertz, its good directionality, penetration capacity is strong, produces cavitation effect simultaneously, forms the microjet of powerful impulsive force, can greatly improve heterogeneous reaction speed, realize the Homogeneous phase mixing between heterogeneous reaction thing, the diffusion of accelerated reaction thing and product, promote the formation of solid cenotype, energy refinement of particle size simultaneously, controls size and the distribution of particle.Microwave is then as a kind of electromagnetic wave, can to polar molecule optionally carry out repeatedly fast fetching to and frictional heat, do not affect the response characteristic of nonpolar material simultaneously, therefore can be discharged by the heat energy of microwave by polar molecule, heating reaction mass, the volatilization of polar solvent simultaneously makes dissolved matter be uniformly distributed thereupon, produces coated process again and again in volatilization and disappearance process.In addition, the polar solvent that microwave heat production causes volatilizees the pressure increased in closed container, make material produce further refinement in hyperbaric environment coupling ultrasonic wave ability and obtain narrow diameter distribution, good dispersion, reunite few perfect particle, in process of the present invention, making full use of the characteristics design such as the solubility of reaction raw materials, decomposition temperature ladder multilayer, to decompose refinement even coated, this is compared with conventional method, and its synthetic effect is more clear.The hyperbaric environment of microwave, ultrasonic and attached generation combines by the present invention, achieves the preparation of the LiFePO 4 powder of uniform particle sizes.
Accompanying drawing explanation
Fig. 1. be ultrasonic wave added microwave reaction kettle structural representation involved in the present invention;
Fig. 2. embodiment 1 gained LiFePO4 finished product SEM schemes;
Fig. 3. comparative example 1 gained LiFePO4 finished product SEM schemes;
Fig. 4. embodiment 1 and comparative example 1 detain electro-detection discharge curve.
In accompanying drawing 1: 1, outside kettle; 2, kinetoplast; 3, spiral live body; 4, inner kettle; 5, pressure controller; 6, kettle cover; 7, pressure release passage, 8, microwave source, 9, supersonic source.
specific implementation method:
Below by way of specific embodiment, the present invention is further described, not limitation of the present invention.
FePO 42H 2o, Li 2cO 3,it is pure that Vc and glucose are analysis; Dextrin is white dextrin.
embodiment 1
1) by analytically pure FePO 42H 2o, after high temperature dewaters, is added in the inner kettle (4) of ultrasonic wave added microwave reaction kettle, adds Li according to the mol ratio of Li: Fe=1.02: 1 2cO 3add than the ratio for 1:0.5 the Vc aqueous solution that concentration is 20% again according to cumulative volume, open ultrasonic wave added (9) and microwave (8) heating simultaneously, control material temperature at 50 DEG C, duration 10min, form predecessor A, predecessor A is cooled fast after the lower 300 DEG C of sintering 30min of revolving burner nitrogen protection, obtains powder predecessor B;
2) predecessor B to be weighed and after loading the inner kettle (4) of ultrasonic wave added microwave reaction kettle, 1:0.2 takes the D/W that concentration is 50% in mass ratio, after unlatching ultrasonic wave added 5min, close ultrasonic wave added microwave reaction kettle kettle cover, adjustment pressure controller (5) pressure is 0.2MPa, high-power unlatching microwave heating disappears to air pressure, obtains solid precursors C;
3) precursor C is sent back to revolving burner, cool fast after 450 DEG C of sintering 30min under nitrogen protection, then take out gained material and repeat 2) operation, product D is obtained after the lower 700 DEG C of sintering 90min of nitrogen protection, finally, the dextrin in aqueous solution that concentration is 30% is taken according to the mass ratio of mass ratio 1:0.5, close ultrasonic wave added microwave reaction kettle kettle cover (6), independent unlatching microwave heating, adjustment pressure controller (5) pressure is 0.1MPa, duration is that about 20min disappears to air pressure, anode material for lithium-ion batteries is cooled to obtain fast after the lower 200 DEG C of sintering 30min of nitrogen protection.
By the pattern of Fig. 2 and Fig. 3 material can be found out, LiFePO4 finished-product material that the reaction of material, mixing and coated process obtain has higher decentralization and consistency to utilize ultrasonic wave added microwave reaction kettle echelon to carry out; And the situation of reunion is curbed, LiFePO4 finished product (Fig. 3) prepared by usual manner of being obviously better than;
The intrinsic conductivity of lithium ion anode material LiFePO4 is lower, the voltage levvl of battery discharge and attenuation degree directly reflect conductivity and the lithium ion diffusivity of material, as seen in Figure 4, embodiment 1 has better voltage retention and capability retention, and the ferric phosphate reason material of institute's output has the conductivity of better ion-diffusibility and Geng Gao.
The physical index of embodiment 1 and comparative example 1 is as follows.
Carbon content % Conductivity/s cm -1
Embodiment 1 3.10 5.63×10 -2
Comparative example 1 3.08 1.21×10 -2
embodiment 2
1) by analytically pure FePO 42H 2o, after high temperature dewaters, is added in the inner kettle (4) of ultrasonic wave added microwave reaction kettle, adds Li according to the mol ratio of Li: Fe=1.02: 1 2cO 3add than the ratio for 1:0.6 the Vc aqueous solution that concentration is 30% again according to cumulative volume, open ultrasonic wave added (9) and microwave (8) heating simultaneously, control material temperature at 40 DEG C, duration 10min, form predecessor A, predecessor A is cooled fast after the lower 300 DEG C of sintering 30min of revolving burner nitrogen protection, obtains powder predecessor B;
2) predecessor B to be weighed and after loading the inner kettle (4) of ultrasonic wave added microwave reaction kettle, 1:0.2 takes the D/W that concentration is 40% in mass ratio, after unlatching ultrasonic wave added 5min, close ultrasonic wave added microwave reaction kettle kettle cover, adjustment pressure controller (5) pressure is 0.25MPa, high-power unlatching microwave heating disappears to air pressure, obtains solid precursors C;
3) precursor C is sent back to revolving burner, cool fast after 450 DEG C of sintering 60min under nitrogen protection, then take out gained material and repeat 2) operation, product D is obtained after the lower 700 DEG C of sintering 90min of nitrogen protection, finally, the dextrin in aqueous solution that concentration is 30% is taken according to the mass ratio of mass ratio 1:0.8, close ultrasonic wave added microwave reaction kettle kettle cover (6), independent unlatching microwave heating, adjustment pressure controller (5) pressure is 0.1MPa, duration is that about 20min disappears to air pressure, anode material for lithium-ion batteries is cooled to obtain fast after the lower 300 DEG C of sintering 30min of nitrogen protection.
comparative example 1
Be Li: Fe according to reaction ratio: carbon source=1.02: the ratio of 1: 0.3 takes analyzes pure FePO 4and Li 2cO 3and glucose; add in sand mill; adding a certain proportion of distilled water makes reaction raw materials solid content 35%; continue grinding 10 hours; then spray-dried acquisition precursor; by presoma under nitrogen atmosphere protection in sintering furnace the continuous high temperature sintering of 5 hours under 2 hours and 750 DEG C of conditions under 350 DEG C of conditions, finally cool, acquisition LiFePO4 finished-product material.
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 (2)

1. a pressure control solution reunion synthetic method for lithium iron phosphate positive material, it is characterized in that, preparation process is divided into following step:
1) by FePO 42H 2o, after high temperature dewaters, is added to ultrasonic wave added microwave reaction kettle, adds LiOHH according to the mol ratio of Li: Fe=1 ~ 1.02: 1 2o or Li 2cO 3add than the ratio for 1:0.5 ~ 1 the Vc aqueous solution that concentration is 10%-40% again according to cumulative volume, open ultrasonic wave added and microwave heating simultaneously, control material temperature at 20 DEG C-50 DEG C, duration 5-10min, forming predecessor A, by predecessor A through cooling fast after 200-300 DEG C of sintering 30min to 50min under revolving burner nitrogen protection, obtaining powder predecessor B;
2) predecessor B to be weighed and after loading ultrasonic wave added microwave reaction kettle, 1:0.2 ~ 0.5 takes the D/W that concentration is 50% in mass ratio, after unlatching ultrasonic wave added 5min, close ultrasonic wave added microwave reaction kettle kettle cover, adjustment pressure is 0.2-0.3MPa, open ultrasonic wave added, high-power unlatching microwave heating disappears to air pressure, obtains solid precursors C;
3) precursor C is sent back to revolving burner, cool fast after 400-500 DEG C of sintering 30min to 60min under nitrogen protection, then take out gained material and repeat 2) operation, product D is obtained after 500-700 under nitrogen protection DEG C of sintering 60min to 90min, finally, the dextrin in aqueous solution that concentration is 30% is taken according to the mass ratio of mass ratio 1:0.5 ~ 1, close ultrasonic wave added microwave reaction kettle kettle cover, independent unlatching microwave heating, adjustment pressure is 0.1-0.15MPa, duration is that about 10-20min disappears to air pressure, anode material for lithium-ion batteries is cooled to obtain fast after 150-250 under nitrogen protection DEG C of sintering 20min to 40min.
2. the pressure control solution reunion synthetic method of a kind of lithium iron phosphate positive material as claimed in claim 1, is characterized in that, described ultrasonic wave added microwave reaction kettle be by 1, outside kettle; 2, kinetoplast; 3, spiral live body; 4, inner kettle; 5, pressure controller; 6, kettle cover; 7. pressure release passage; 8, microwave source; 9, supersonic source is formed.
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Cited By (2)

* Cited by examiner, † Cited by third party
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CN106848289A (en) * 2017-02-26 2017-06-13 桂林理工大学 One species lotus root sheet spinel-type ZnMn2O4Raw powder's production technology
CN108408710A (en) * 2018-04-25 2018-08-17 深圳市寒暑科技新能源有限公司 A kind of energy conservation and environmental protection prepares the device and preparation method of LiFePO4

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CN108408710A (en) * 2018-04-25 2018-08-17 深圳市寒暑科技新能源有限公司 A kind of energy conservation and environmental protection prepares the device and preparation method of LiFePO4

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