CN104269522B - The preparation method and application of the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding - Google Patents
The preparation method and application of the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding Download PDFInfo
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- CN104269522B CN104269522B CN201410527991.9A CN201410527991A CN104269522B CN 104269522 B CN104269522 B CN 104269522B CN 201410527991 A CN201410527991 A CN 201410527991A CN 104269522 B CN104269522 B CN 104269522B
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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
- H01M4/136—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
- H01M4/13—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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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Abstract
The invention discloses the preparation method and application of the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding; the preparation method of the cerium Fluorin doped LiFePO 4 of described aluminum phosphate cladding is: first prepare cerium Fluorin doped LiFePO 4; then the suspension of the LiFePO 4 of cerium Fluorin doped will add aluminium salt and phosphate; the aluminum phosphate generated is evenly coated at the LiFePO 4 particle surface of cerium Fluorin doped; the LiFePO 4 granule of the cerium Fluorin doped being coated with by aluminum phosphate is calcined in vacuum or protective gas atmosphere, obtains the LiFePO 4 of the cerium Fluorin doped of aluminum phosphate cladding.The preparation method preparation process of the present invention is simple, reacts pollution-free, and product uniformity is good, and the LiFePO 4 of the cerium Fluorin doped of the aluminum phosphate cladding prepared has high gram volume, has good prospects for commercial application.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to the preparation of lithium ion secondary battery anode material
Method and application.
Background technology
Lithium iron phosphate cathode material is subject in new-energy automobile and energy storage with its safety and high cycle life
Be widely applied, but the conductivity lower limit of LiFePO 4 self its in heavy-current discharge should
With.It is the common method improving LiFePO 4 electric conductivity that carbon cladding and ion doping improve its crystal structure.
Although it is safe anode material of lithium battery that LiFePO 4 be it is believed that, but in actually used process
In, LiFePO 4 there is also potential safety hazard.
Using Phosphate coating lithium ion battery plus-negative plate material is the one side improving lithium ion battery security
Method.
Use Phosphate coating lithium ion secondary battery anode material can reduce hexafluorophosphate in electrolyte
(LiPF6) decompose Fluohydric acid. (HF) concentration produced, reduce the dissolved corrosion side reaction to positive electrode.
In phosphate radical polyanion, phosphorus oxygen double bond is the most stable at electrode and electrolyte interface, can keep the internal electricity of clad
Pond material Stability Analysis of Structures in electrochemical reaction process.
The preparation method and application using the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding at present yet there are no report
Road.
Summary of the invention
In order to improve electric conductivity and the safety of ferrousphosphate lithium material simultaneously, the present invention proposes a kind of phosphoric acid
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum cladding, and by the cerium Fluorin doped of the aluminum phosphate cladding of preparation
LiFePO 4 is applied in lithium rechargeable battery.
The present invention adopts the following technical scheme that
The preparation method of cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding, its be characterized in that include with
Lower step:
1) LiFePO 4, ammonium fluoride and cerous nitrate are mixed in ethanol, be placed in vacuum or protective gas atmosphere
Enclose middle ball milling, mix homogeneously；
2) material after mixing is dried, then at vacuum or protective gas in vacuum or protective gas atmosphere
Atmosphere is calcined, natural cooling, obtain the LiFePO 4 granule of cerium Fluorin doped, cerium Fluorin doped ferrous phosphate
The molecular formula of lithium is expressed as LiCexFePO4Fy, 0≤x≤0.3,0≤y≤0.3, wherein, x is that doped chemical cerium exists
The molar fraction of the Ce elements in cerium Fluorin doped LiFePO 4 molecular formula, y is that doped chemical fluorine is at cerium Fluorin doped
The molar fraction of the fluorine element in LiFePO 4 molecular formula；
3) the LiFePO 4 even particulate dispersion of cerium Fluorin doped to suspension solvent will form suspension,
Adding aluminium salt and phosphate in suspension, the aluminum phosphate of generation is uniformly coated on the ferrous phosphate of cerium Fluorin doped
Lithium particle surface, filters product and is placed in vacuum or protective gas atmosphere calcining, natural cooling, obtain
The cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding.
Above-mentioned aluminium salt is one or more in aluminum sulfate, aluminum nitrate and aluminum acetate；
Described phosphate is one or more in ammonium dihydrogen phosphate, diammonium phosphate and triammonium phosphate.
The mass percent of above-mentioned phosphate and cerium Fluorin doped LiFePO 4 is 0.1～20:100.
Above-mentioned suspension solvent is the mixed solution of water and alcohol, described alcohol include ethanol, propanol, isopropanol,
One or more in butanol, isobutanol and ethylene glycol；
The volume ratio of described water and alcohol is 100～40:1～60.
Above-mentioned protective gas is one or more of nitrogen, helium and argon.
Above-mentioned steps 1) ball milling condition is: in vacuum or protective gas atmosphere, with the speed of 200～500rpm
Degree ball milling 1-5 days；
Step 2) calcination condition is: in vacuum or protective gas atmosphere, heats up with the speed of 2～5 DEG C/min
To 300～800 DEG C, and keep 0.5～6 hour at this temperature, react after terminating at vacuum or protective gas atmosphere
Room temperature is naturally cooled in enclosing；
Step 3) calcination condition is: in vacuum or protective gas atmosphere, heats up with the speed of 2～5 DEG C/min
To 300～800 DEG C, and keep 0.5～2 hour at this temperature, react after terminating at vacuum or protective gas atmosphere
Room temperature is naturally cooled in enclosing.
The cerium Fluorin doped LiFePO 4 of the aluminum phosphate cladding prepared by said method is at lithium rechargeable battery just
Application in the material of pole.
The invention has the beneficial effects as follows:
1, the present invention is that lithium ion secondary battery anode material adds a kind of new material, provides this simultaneously
The preparation method of material, and prepare material there is high gram volume and security performance.
2, preparation process of the present invention is simple, and equipment requirements is low, and course of reaction is pollution-free, and product uniformity is good,
There is good prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is embodiment step 3) the cerium Fluorin doped LiFePO 4 XRD spectra for preparing；
Fig. 2 is embodiment step 4) XRD of the cerium Fluorin doped LiFePO 4 of the aluminum phosphate for preparing cladding
Spectrogram；
Fig. 3 is the cerium Fluorin doped lithium iron phosphate electrochemical circulation volt of the aluminum phosphate cladding that embodiment prepares
Antu.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, but the invention is not limited in this.
Embodiment raw materials, is analytical pure, content >=99.9%.
Embodiment
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding, comprises the following steps:
Step 1)
By molecular formula LiCe0.1FePO4F0.1Weigh LiFePO 4 10g, ammonium fluoride 0.235g, six nitric hydrates
Cerium 2.75g, adds 20mL ethanol, is mixed by mixture, puts in agate jar, be subsequently placed in Nanjing University
Ball milling 2 days in argon gas atmosphere in instrument plant QM-2SP12 type ball mill, rotating speed 300rpm, by equal for material ball milling
Even；
Step 2)
After ball milling completes, take out under argon gas atmosphere is protected, 50 DEG C of dry 10h in vacuum drying oven；
Step 3)
Dried sample is placed in Shanghai Jiu Gong Electrical Appliances Co., Ltd JQF1400-30 high-temperature atmosphere electric furnace, takes out
Vacuum, logical 99.9% nitrogen protection gas, then it is warmed up to 500 DEG C with the speed of 5 DEG C/min, protect at nitrogen
Lower 500 DEG C of calcining 3h, obtain brown color LiCe after being then cooled to room temperature in nitrogen atmosphere0.1FePO4F0.1；
Step 4)
Weigh 0.456g ANN aluminium nitrate nonahydrate, be dissolved in 50mL water, add 7.407g positive electrode, ultrasonic disperse
30min, forms suspension；
Claim 1.61g diammonium phosphate, be dissolved in 30mL water, be stirred vigorously down and be added dropwise over suspension, continue super
Sound 20min, then sucking filtration, solid is at 100 DEG C of dry 3h；
Dried solid is put into crucible, is placed in Shanghai Jiu Gong Electrical Appliances Co., Ltd JQF1400-30 High Temperature Gas
Atmosphere electric furnace, evacuation, logical 99.9% nitrogen protection gas, then it is warmed up to 300 DEG C with the speed of 5 DEG C/min,
And keep 1 hour at this temperature, after natural cooling, stop being passed through nitrogen, i.e. obtain brown color AlPO4Bag
The LiCe covered0.1FePO4F0.1Positive electrode, wherein, AlPO4The quality of clad is LiCe0.1FePO4F0.1Just
The 2% of pole quality of materials.
Material property characterizes
1) crystal structure test is carried out on Japan Shimadzu X-ray diffractometer XRD-7000, uses copper target,
Scanning speed 2 °/minute, measuring accuracy ± 0.04 °, sweep limits 5～90 °.
Embodiment step 3) the cerium Fluorin doped LiFePO 4 LiCe for preparing0.1FePO4F0.1XRD spectra
See Fig. 1；Can analyze from this figure and draw cerium Fluorin doped LiFePO 4 LiCe0.1FePO4F0.1Crystal structure
For LiFePO 4 crystal structure；
Embodiment step 4) XRD spectra of cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding for preparing
See Fig. 2；The Fluorin doped LiFePO 4 LiCe showing that aluminum phosphate is coated with can be analyzed from this figure0.1FePO4F0.1
Crystal structure be LiFePO 4 crystal structure.
Electrochemical property test
90:2:8 in mass ratio takes the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding, super P and PVDF
(HSV900), add appropriate N-Methyl pyrrolidone as solvent, in glove box under argon shield, use
Magnetic stirrer 15 hours, prepares the required slurry of button electricity.Coating machine is that Shenzhen section crystalline substance intelligence reaches science and technology
Company limited MSK-AFA-III automatic spray dehydrator, coating clearance 25 microns, speed 5 cm per minute, slurry
Material is coated uniformly on 9 microns of thickness that Jinxiang Copper Foil Co., Ltd., Mei County produces, on purity 99.8% shiny copper foil,
It is vacuum dried 12 hours at 120 DEG C, then strikes out diameter at Shenzhen section crystalline substance MSK-T06 button cell sheet-punching machine
It is about the electrode foil of 16 millimeter.CR2032 button batteries is mounted at homemade full 99.9% high-purity argon
Gas glove box is carried out, uses Shenzhen section crystalline substance MSK-110 small-sized hydraulic button cell packaging machine.Negative pole is pure
Spending the high purity lithium sheet of 99.99% diameter 15.8 millimeters, barrier film is 16 microns of U.S.'s ENTEK LP16 types PE of thickness
Barrier film, electrolyte is DMC:EMC (50:50, volume ratio), adds 1%VC (volume ratio), 1.3M LiPF6。
Button cell circulation and multiplying power test are carried out on the CT2001A tester of Wuhan Lan electricity Electronics Co., Ltd..
Electrochemistry cyclic voltammetry experiment is carried out in Huachen CHI604E of Shanghai, and working electrode is the phosphorus prepared
The cerium Fluorin doped LiFePO 4 of acid aluminum cladding, is lithium sheet to electrode and reference electrode, and sweep speed is
200μV/s。
Fig. 3 is the electrochemistry circulation of the cerium Fluorin doped LiFePO 4 of the aluminum phosphate cladding that embodiment prepares
Volt-ampere curve.
The cerium Fluorin doped LiFePO 4 that the aluminum phosphate prepared by the present invention is coated with has high gram volume, at lithium
Ion secondary battery has good application prospect.
Claims (7)
1. the preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding, it is characterised in that: include following
Step:
1) LiFePO 4, ammonium fluoride and cerous nitrate are mixed in ethanol, be placed in vacuum or protective gas atmosphere
Enclose middle ball milling, mix homogeneously；
2) material after mixing is dried, then at vacuum or protective gas in vacuum or protective gas atmosphere
Atmosphere is calcined, natural cooling, obtain the LiFePO 4 granule of cerium Fluorin doped, cerium Fluorin doped ferrous phosphate
The molecular formula of lithium is expressed as LiCexFePO4Fy, 0≤x≤0.3,0≤y≤0.3, wherein, x is that doped chemical cerium exists
The molar fraction of the Ce elements in cerium Fluorin doped LiFePO 4 molecular formula, y is that doped chemical fluorine is at cerium Fluorin doped
The molar fraction of the fluorine element in LiFePO 4 molecular formula；
3) the LiFePO 4 even particulate dispersion of cerium Fluorin doped to suspension solvent will form suspension,
Adding aluminium salt and phosphate in suspension, the aluminum phosphate of generation is uniformly coated on the ferrous phosphate of cerium Fluorin doped
Lithium particle surface, filters product and is placed in vacuum or protective gas atmosphere calcining, natural cooling, obtain
The cerium Fluorin doped LiFePO 4 of aluminum phosphate cladding.
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate the most according to claim 1 cladding,
It is characterized in that:
Described aluminium salt is one or more in aluminum sulfate, aluminum nitrate and aluminum acetate；
Described phosphate is one or more in ammonium dihydrogen phosphate, diammonium phosphate and triammonium phosphate.
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate the most according to claim 1 cladding,
It is characterized in that:
The mass percent of described phosphate and cerium Fluorin doped LiFePO 4 is 0.1～20:100.
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate the most according to claim 1 cladding,
It is characterized in that:
Described suspension solvent is the mixed solution of water and alcohol, described alcohol include ethanol, propanol, isopropanol,
One or more in butanol, isobutanol and ethylene glycol；
The volume ratio of described water and alcohol is 100～40:1～60.
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate the most according to claim 1 cladding,
It is characterized in that:
Described protective gas is one or more of nitrogen, helium and argon.
The preparation method of the cerium Fluorin doped LiFePO 4 of aluminum phosphate the most according to claim 1 cladding,
It is characterized in that:
Step 1) ball milling condition is: in vacuum or protective gas atmosphere, with the speed ball of 200～500rpm
Grind 1-5 days；
Step 2) calcination condition is: in vacuum or protective gas atmosphere, heats up with the speed of 2～5 DEG C/min
To 300～800 DEG C, and keep 0.5～6 hour at this temperature, react after terminating at vacuum or protective gas atmosphere
Room temperature is naturally cooled in enclosing；
Step 3) calcination condition is: in vacuum or protective gas atmosphere, heats up with the speed of 2～5 DEG C/min
To 300～800 DEG C, and keep 0.5～2 hour at this temperature, react after terminating at vacuum or protective gas atmosphere
Room temperature is naturally cooled in enclosing.
7. prepared by any one of claim 1～6 aluminum phosphate cladding cerium Fluorin doped LiFePO 4 lithium from
Application in sub-secondary battery positive electrode material.
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| CN109904449A (en) * | 2017-12-08 | 2019-06-18 | 平高集团有限公司 | A kind of cerous phosphate cladding tertiary cathode material and preparation method thereof, lithium ion battery |
| CN114515585B (en) * | 2020-11-20 | 2023-12-19 | 浙江省化工研究院有限公司 | Preparation method and application of fluorine-doped aluminum phosphate catalyst |
| CN115432690A (en) * | 2022-10-10 | 2022-12-06 | 湖州南木纳米科技有限公司 | Aluminum phosphate coated titanium aluminum lithium phosphate material and preparation method and application thereof |
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