CN105322167B - A kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material - Google Patents
A kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material Download PDFInfo
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- CN105322167B CN105322167B CN201510732890.XA CN201510732890A CN105322167B CN 105322167 B CN105322167 B CN 105322167B CN 201510732890 A CN201510732890 A CN 201510732890A CN 105322167 B CN105322167 B CN 105322167B
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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
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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
It is adapted to that there is some strength it is an object of the invention to provide one kind, material surface has a clad, while the de-agglomerated synthetic method of the small lithium iron phosphate positive material of powder body material primary particle size.Process of the invention using the reaction of ultrasonic wave added microwave reaction kettle echelon progress material, mixing and cladding, finally realize homogeneous reaction, the process control of nearly nanoscale raw material.Prepared battery material has higher particle uniformity and uniformity, while powder granule is small, therefore LiFePO 4 material has higher electrical conductivity and ion diffusion rates, drastically increases the chemical property of material.
Description
Technical field
The present invention relates to a kind of preparation method of iron phosphate lithium positive pole lithium ion battery material, and in particular to a kind of ferric phosphate
The pressure control de-agglomerated synthetic method of lithium anode material.
Background technology
LiFePO4It is a kind of current most common anode material for lithium-ion batteries, there is stable olivine structural, energy
Reversible insertion and deintercalate lithium ions.And high-energy-density, stable performance, safe, environment-friendly, price are more just
Preferably.It is considered as most potential anode material for lithium-ion batteries.Pure phase LiFePO4Electrical conductivity is small by (about 10-9S/cm), from
Sub- diffusion coefficient is low, limits discharge capability under its high current density, the poor difference of cycle performance, limits LiFePO4Application.
In view of such shortcoming, each manufacturer and colleges and universities carry out successively improves LiFePO4The research of performance, including coat, adulterate, modified skill
Art etc., but crystal grain thinning technology is appreciated by more people here, but in view of the common preparation method of LiFePO4, such as high
Warm solid phase method, sol-gel process, liquid-phase coprecipitation, carbothermic method etc., it can not fundamentally prevent caused by high temperature sintering
Agglomeration, and conventional hydrothermal rule is difficult to industrialize, and meanwhile it is high to equipment requirement, costly；Complex manufacturing,
Long preparation period, repeatability is poor, can not meet the needs of volume production；Therefore solve LiFePO4 finished particle agglomeration techniques to become
Obtain particularly important.
Such as patent《The de-agglomerated and stage division of CN02139764.3 Nano diamonds》In refer to nanometer Buddha's warrior attendant first
Stone mechanical lapping is synchronous with chemical modification to be carried out, and is dispersed into the small agglomerates that particle mean size is 7 ~ 200nm, then will be suspended
Thick nano diamond particles and other compositions in liquid remove；Finally add wetting agent, surfactant, dispersion stabilizer and pH
It is worth conditioning agent, using the classification for being dispersed with stirring diamond and finally realizing Nano diamond, its particle diameter can be made at 7 ~ 200 nanometers
Between controllable adjustment；And for example University Of Tianjin's patent《CN201010224986.2 dispersing detonation method nano-diamonds in the liquid phase
Method》In mention using business detonation method nano-diamond powder as raw material, be mixed in liquid medium, formed suspension；Make
With the pulsed laser ablation suspension, action time 1-3h, obtained effect suspension stabilization, do not precipitate；Finally to laser bombardment
Product afterwards carries out strong acid oxidation processes, obtains monodispersed diamond nano-particles.All it is referred to and is coordinated using liquid phase above
The means of mechanical lapping can realize the micronization processes of powder body material, or even use laser bombardment means, and this certain methods is adapted to
Hardness is big, and hardness is big, the good diamond of stability, but is difficult to transit among the de-agglomerated technique of LiFePO 4 material.
The content of the invention
It is an object of the invention to provide one kind to be adapted to some strength, material surface with clad, powder body material
The pressure control de-agglomerated synthetic method of the small lithium iron phosphate positive material of particle diameter.Prepared battery material has higher particle equal
Even property and uniformity, powder granule is small, therefore LiFePO 4 material has higher electrical conductivity and ion diffusion rates, greatly
Improve the chemical property of material.
To reach above-mentioned purpose, the preparation method that the present invention uses is as follows.
A kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material, it is characterized in that, preparation process is divided into following several
Individual step：
1) by FePO4·2H2O is added to ultrasonic wave added microwave reaction kettle after high temperature removes water, according to Li: Fe=1~
1.02: 1 mol ratio adds LiOHH2O or Li2CO3, it is 1 according still further to internal kettle volume and Vc aqueous solution volume ratios：0.5
~1 ratio adds concentration and is the 10%-40% Vc aqueous solution, while opens ultrasonic wave added and microwave heating, and control material temperature is 20
DEG C -50 DEG C, duration 5-10min, predecessor A is formed, the rotated stove nitrogen of predecessor A is protected into lower 200-300 DEG C of sintering 30min
Quickly cooled down after to 50min, obtain powder predecessor B；
2) after weighing by predecessor B and load ultrasonic wave added microwave reaction kettle, by predecessor B and D/W quality
Than 1:0.2~0.5 weighs the D/W that concentration is 50%, and after ultrasonic wave added 5min is opened, it is micro- to close ultrasonic wave added
Ripple reactor kettle cover, adjustment pressure are 0.2-0.3MPa, open ultrasonic wave added, and high-power unlatching microwave is heated to air pressure disappearance,
Obtain solid precursors C；
3) precursor C is sent back to revolving burner, under nitrogen protection fast quickly cooling after 400-500 DEG C of sintering 30min to 60min
But, then take out resulting material and repeat 2）Operation, product is obtained after the lower 500-700 DEG C of sintering 60min to 90min of nitrogen protection
D, finally, according to product D and dextrin in aqueous solution mass ratio 1：0.5~1 weighs the dextrin in aqueous solution that concentration is 30%, closes ultrasound
Assisted microwave synthesis reactor kettle cover, individually open microwave heating, adjustment pressure is 0.1-0.15MPa, when a length of 10-20min to gas
Pressure is disappeared, and anode material for lithium-ion batteries is quickly cooled down to obtain after the lower 150-250 DEG C of sintering 20min to 40min of nitrogen protection.
A kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material described above, it is characterized in that, described ultrasound
Assisted microwave synthesis reactor is by outside kettle, kinetoplast, spiral live body, internal kettle, pressure controller, kettle cover, pressure release passage, micro-
Wave source and supersonic source are formed.
Ultrasonic disperse is higher than 20000 hertz of sound wave as a kind of frequency, and its good directionality, penetration capacity is strong, simultaneously
Cavitation effect is produced, the microjet of strong impact power is formed, heterogeneous reaction speed can be greatly improved, realize heterogeneous reaction thing
Between uniform mixing, accelerate the diffusion of reactant and product, promote the formation of solid cenotype, at the same can refinement of particle size, control
The size of pelleting and distribution.Microwave is then used as a kind of electromagnetic wave, and the progress of polar molecule selectivity quickly can be orientated repeatedly
And frictional heat, while the response characteristic of nonpolar material is not influenceed, therefore can be released the heat energy of polar molecule by microwave
Release, heating response material, while the volatilization of polar solvent causes dissolved matter to be uniformly distributed therewith, in volatilization and disappearance process
The cladding process of middle generation again and again.In addition, polar solvent volatilization increases closed container caused by microwave heat production
Interior pressure, making material, further refinement acquisition particle diameter distribution is narrow in the generation of hyperbaric environment matching ultrasonic wave ability, good dispersion,
Reunite few perfect particle, in process of the present invention, make full use of the characteristics such as solubility, the decomposition temperature of reaction raw materials to devise rank
Terraced multilayer is decomposed refinement and even coated, and compared with conventional method, its synthetic effect is more clear for this.The present invention is by microwave, super
Sound and attached caused hyperbaric environment are combined, and realize the preparation of the LiFePO 4 powder of uniform particle sizes.
Brief description of the drawings
Fig. 1 are ultrasonic wave added microwave reaction kettle structural representation involved in the present invention；
The gained LiFePO4 finished product SEM of Fig. 2 embodiments 1 schemes；
The gained LiFePO4 finished product SEM of Fig. 3 comparative examples 1 schemes；
Fig. 4 embodiments 1 and comparative example 1 detain electro-detection discharge curve.
In accompanying drawing 1：1st, outside kettle；2nd, kinetoplast；3rd, spiral live body；4th, internal kettle；5th, pressure controller； 6、
Kettle cover；7th, 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.
FePO4·2H2O、Li2CO3、Vc and glucose are that analysis is pure；Dextrin is white dextrin.
Embodiment 1
1) by analytically pure FePO4·2H2O is added to kettle inside ultrasonic wave added microwave reaction kettle after high temperature removes water
（4）In, add Li according to Li: Fe=1.02: 1 mol ratio2CO3, it is 1 according still further to cumulative volume ratio：0.5 ratio adds concentration
For the 20% Vc aqueous solution, while open ultrasonic wave added（9）And microwave（8）Heating, control material temperature is at 50 DEG C, duration 10min, shape
Into predecessor A, it will quickly be cooled down after the lower 300 DEG C of sintering 30min of the rotated stove nitrogen protections of predecessor A, obtain powder predecessor
B；
2) predecessor B is weighed and loads kettle inside ultrasonic wave added microwave reaction kettle（4）Afterwards, in mass ratio 1:0.2 claims
The D/W that concentration is 50% is taken, after ultrasonic wave added 5min is opened, ultrasonic wave added microwave reaction kettle kettle cover is closed, adjusts
Seamless force controller（5）Pressure is 0.2MPa, and high-power unlatching microwave is heated to air pressure disappearance, obtains solid precursors C；
3) send precursor C back to revolving burner, quickly cooled down after 450 DEG C of sintering 30min under nitrogen protection, then take out institute
Obtain material and repeat 2）Operation, product D is obtained after the lower 700 DEG C of sintering 90min of nitrogen protection, finally, according to mass ratio 1：0.5
Mass ratio weighs the dextrin in aqueous solution that concentration is 30%, closes ultrasonic wave added microwave reaction kettle kettle cover（6）, individually open microwave and add
Heat, adjust pressure controller（5）Pressure is 0.1MPa, when a length of 20min or so disappear to air pressure, through lower 200 DEG C of nitrogen protection
Anode material for lithium-ion batteries is quickly cooled down to obtain after sintering 30min.
Ultrasonic wave added microwave reaction kettle echelon is utilized to carry out material by can be seen that on the pattern of Fig. 2 and Fig. 3 materials
LiFePO4 finished-product material obtained by reaction, the process for mixing and coating has higher decentralization and uniformity；And roll into a ball
Poly- situation is curbed, hence it is evident that LiFePO4 finished product prepared by well usual manner（Fig. 3）；
The intrinsic conductivity of lithium ion anode material LiFePO4 is relatively low, and the voltage level and attenuation degree of battery discharge are straight
The electric conductivity for reflecting material and lithium ion diffusivity are connect, as seen in Figure 4, embodiment 1 is protected with more preferable voltage
Holdup and capability retention, the ferric phosphate reason material of institute's output have the electric conductivity of more preferable ion-diffusibility and Geng Gao.
Embodiment 1 and the physical index of comparative example 1 are as follows.
| Carbon content % | Electrical 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 FePO4·2H2O is added to kettle inside ultrasonic wave added microwave reaction kettle after high temperature removes water
（4）In, add Li according to Li: Fe=1.02: 1 mol ratio2CO3, it is 1 according still further to cumulative volume ratio：0.6 ratio adds concentration
For the 30% Vc aqueous solution, while open ultrasonic wave added（9）And microwave（8）Heating, control material temperature is at 40 DEG C, duration 10min, shape
Into predecessor A, it will quickly be cooled down after the lower 300 DEG C of sintering 30min of the rotated stove nitrogen protections of predecessor A, obtain powder predecessor
B；
2) predecessor B is weighed and loads kettle inside ultrasonic wave added microwave reaction kettle（4）Afterwards, in mass ratio 1:0.2 claims
The D/W that concentration is 40% is taken, after ultrasonic wave added 5min is opened, ultrasonic wave added microwave reaction kettle kettle cover is closed, adjusts
Seamless force controller（5）Pressure is 0.25MPa, and high-power unlatching microwave is heated to air pressure disappearance, obtains solid precursors C；
3) send precursor C back to revolving burner, quickly cooled down after 450 DEG C of sintering 60min under nitrogen protection, then take out institute
Obtain material and repeat 2）Operation, product D is obtained after the lower 700 DEG C of sintering 90min of nitrogen protection, finally, according to mass ratio 1：0.8
Mass ratio weighs the dextrin in aqueous solution that concentration is 30%, closes ultrasonic wave added microwave reaction kettle kettle cover（6）, individually open microwave and add
Heat, adjust pressure controller（5）Pressure is 0.1MPa, when a length of 20min or so disappear to air pressure, through lower 300 DEG C of nitrogen protection
Anode material for lithium-ion batteries is quickly cooled down to obtain after sintering 30min.
Comparative example 1
It is Li: Fe according to reaction ratio:Carbon source=1.02: 1: 0.3 ratio weighs the pure FePO of analysis4And Li2CO3And Portugal
Grape sugar, is added in sand mill, and adding a certain proportion of distilled water makes reaction raw materials solid content 35%, persistently grinds 10 hours, so
By spray drying obtain precursor, by presoma nitrogen atmosphere protection under in sintering furnace under the conditions of 350 DEG C 2 hours and
The continuous high temperature sintering of 5 hours, finally cools, obtains LiFePO4 finished-product material under the conditions of 750 DEG C.
Technical scheme is described in detail embodiment described above, it should be understood that it is described above only
For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention
With improve etc., should be included in the scope of the protection.
Claims (2)
1. a kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material, it is characterized in that, preparation process is divided into following
Step：1) by FePO4·2H2O is added to ultrasonic wave added microwave reaction kettle, according to Li: Fe=1~1.02 after high temperature removes water:
1 mol ratio adds LiOHH2O or Li2CO3, it is 1 according still further to cumulative volume ratio：It is 10%-40% that 0.5~1 ratio, which adds concentration,
The Vc aqueous solution, while open ultrasonic wave added and microwave heating, control material temperature is at 20 DEG C -50 DEG C, duration 5-10min, before formation
Thing A is driven, is quickly cooled down after the rotated stove nitrogen of predecessor A is protected into lower 200-300 DEG C of sintering 30min to 50min, obtains powder
Predecessor B；2) after weighing by predecessor B and load ultrasonic wave added microwave reaction kettle, in mass ratio 1:0.2~0.5 weighs concentration
For 50% D/W, after ultrasonic wave added 5min is opened, ultrasonic wave added microwave reaction kettle kettle cover is closed, adjusts pressure
For 0.2-0.3MPa, high-power unlatching microwave is heated to air pressure disappearance, obtains solid precursors C；3) precursor C is sent back to rotation
Converter, quickly cooled down after 400-500 DEG C of sintering 30min to 60min under nitrogen protection, then take out resulting material and repeat 2）Behaviour
Make, product D is obtained after the lower 500-700 DEG C of sintering 60min to 90min of nitrogen protection, finally, according to mass ratio 1：0.5~1
Mass ratio weighs the dextrin in aqueous solution that concentration is 30%, closes ultrasonic wave added microwave reaction kettle kettle cover, individually opens microwave heating,
Adjustment pressure is 0.1-0.15MPa, when a length of 10-20min disappeared to air pressure, protect lower 150-250 DEG C of sintering 20min through nitrogen
Anode material for lithium-ion batteries is quickly cooled down to obtain after to 40min.
2. a kind of pressure control de-agglomerated synthetic method of lithium iron phosphate positive material as claimed in claim 1, it is characterized in that, it is described
Ultrasonic wave added microwave reaction kettle led to by outside kettle, kinetoplast, spiral live body, internal kettle, pressure controller, kettle cover, pressure release
Road, microwave source and supersonic source are formed.
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| CN106848289B (en) * | 2017-02-26 | 2020-04-14 | 桂林理工大学 | Lotus root-like flaky spinel type ZnMn2O4Method for preparing powder |
| 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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