CN110316712A - A method of LiFePO4 is prepared with nanoscale iron phosphate - Google Patents
A method of LiFePO4 is prepared with nanoscale iron phosphate Download PDFInfo
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- CN110316712A CN110316712A CN201910709044.4A CN201910709044A CN110316712A CN 110316712 A CN110316712 A CN 110316712A CN 201910709044 A CN201910709044 A CN 201910709044A CN 110316712 A CN110316712 A CN 110316712A
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- 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
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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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- 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
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Abstract
The invention discloses a kind of method for preparing LiFePO4 with nanoscale iron phosphate, include the following steps: that synthesis has the ferric phosphate of the crystallization water；Phosphoric acid iron material containing the crystallization water is warming up to 500-850 degrees Celsius；The present invention provides by anhydrous iron phosphate obtained by the above method；The present invention provides a kind of LiFePO4s, the LiFePO4 is prepared by the phosphoric acid iron material containing the crystallization water, the anhydrous iron phosphate is the above-mentioned anhydrous iron phosphate of the present invention, ferric phosphate obtained by this method, the LiFePO4 of the Material synthesis containing the anhydrous iron phosphate, containing lithium ion cell positive made of the LiFePO4 and including the lithium ion battery of the lithium ion cell positive.The features such as ferric phosphate that the present invention obtains has product uniformity preferable, with high purity.
Description
Technical field
The present invention relates to prepare LiFePO4 technical field more particularly to a kind of prepare LiFePO4 with nanoscale iron phosphate
Method.
Background technique
Lithium ion battery have specific energy is big, operating voltage is high, have extended cycle life, self-discharge rate is low, memory-less effect with
And advantages of environment protection, and it is widely used in field of portable electronic apparatus.And the substance as positive electrode is not yet
Disconnected extension restricts always the large-scale promotion application of lithium ion battery as the important component in lithium ion battery,
It is mainly manifested in that specific discharge capacity under big multiplying power is low and poor circulation, is all the time a kind of by surface coating modification
Improve the method for positive electrode chemical property well.However, being big by adding although its discharge performance significantly improves
The conductive agent of amount makes up the defect of electron conduction, due to improving the dosage of conductive agent, so that activity substance content reduces,
To make the specific capacity of integral material be substantially reduced.
Summary of the invention
The invention proposes a kind of methods for preparing LiFePO4 with nanoscale iron phosphate, to solve in above-mentioned background technique
The problem of proposition.
The invention proposes a kind of methods for preparing LiFePO4 with nanoscale iron phosphate, comprising the following steps:
S1: Fe source compound is added in the solution containing phosphate radical, is heated under the revolving speed of 1500-2800r/min
It is completely dissolved iron to 90-100 DEG C of stirring, excess H is added in the solution2O2Solution, make Fe as much as possible2+It is oxidized to Fe3+,
The material of the ferric phosphate containing the crystallization water is obtained after reacting and carrying out 5-15h drying；
S2: the liquor ferri phosphatis in S1 is dried, and 120 degrees Celsius of temperature, is put into Muffle after drying time 12-24h
It is pre-sintered in furnace, temperature setting is 700 degrees Celsius, and time 10h finally obtains the iron phosphate material without the crystallization water；
S3: iron phosphate material obtained in S1 is subjected to weighing and calculates mole in case using；
S4: ferric phosphate, lithium source solution, the reproducibility acid solution in S3, reproducibility are weighed according to certain stoichiometric ratio
The dosage of acid solution and the molal quantity of metal ion are directly proportional, and the amount of ascorbic acid is the 1% of Citric Acid Dosage；
S5: being added drop-wise in reproducibility acid solution by liquor ferri phosphatis, lithium source solution, and be stirred continuously, and adjusts PH with ammonium hydroxide
To between 8-9, temperature setting is 90-100 DEG C, is stirred to react on heating stirrer to solution in gel；
S6: gained colloid substance in S5 is put into vacuum oven and is dried, drying time 12h obtains phosphoric acid
Iron lithium presoma；
S7: sintered material is clayed into power shape by S6 after 500 DEG C of pre-sintering 5h, then carries out tabletting, pressure is big
Small is 10MPa；
S8: resulting materials in S7 are placed in Muffle furnace and carry out being warming up to 750 DEG C with 5 DEG C of speed per minute, are sintered material
The material time is 12h, in N2Atmosphere under be sintered.Natural cooling is then carried out in furnace is cooled to room temperature；
S9: the material being sintered in S8 is ground in the agate mortar, obtains required phosphorus after crossing 200 meshes
Sour iron lithium anode material.
Preferably, Fe source compound in S1 are as follows: Fe (CH3COO)2、FeC2O4·2H2O、FeSO4·7H2O、Fe(NO3)3·
9H2O、Fe2O3With iron powder one of which.
Preferably, the solution of phosphate radical is NH in S14H2PO4Or H3PO4Solution.
Preferably, lithium source solution in S5 are as follows: Li (CH3COO)·2H2O、LiOH·H2O、LiNO3It is one of.
Preferably, reproducibility acid solution in S5 are as follows: glycolic, ascorbic acid, citric acid, ethylene glycol, sucrose, acetone are wherein
Two kinds of mixed liquor.
Preferably, in S2 drying and processing condition are as follows: heating rate not less than 5 DEG C per minute, pressure be not less than 10kPa,
And water-bearing phosphate iron material is warming up to 500-800 DEG C.
A kind of method preparing LiFePO4 with nanoscale iron phosphate proposed by the present invention, beneficial effect are: the present invention
Purpose be a kind of preparation method for being not bound with water ferric phosphate to be provided, by the party to overcome the shortcomings of existing synthetic technology
Ferric phosphate made from method, the Material synthesis containing the anhydrous iron phosphate LiFePO4, contain lithium made of the LiFePO4
Ion battery anode and the lithium ion battery including the lithium ion cell positive.The ferric phosphate that the present invention obtains has product uniform
The features such as property is preferable, with high purity.
Specific embodiment
It is next combined with specific embodiments below that the present invention will be further described.
The invention proposes a kind of methods for preparing LiFePO4 with nanoscale iron phosphate, comprising the following steps:
S1: Fe source compound is added in the solution containing phosphate radical, is heated under the revolving speed of 1500-2800r/min
It is completely dissolved iron to 90-100 DEG C of stirring, excess H is added in the solution2O2Solution, make Fe as much as possible2+It is oxidized to Fe3+,
The material of the ferric phosphate containing the crystallization water is obtained after reacting and carrying out 5-15h drying；Fe source compound are as follows: Fe (CH3COO)2、
FeC2O4·2H2O、FeSO4·7H2O、Fe(NO3)3·9H2O、Fe2O3With iron powder one of which, the solution of phosphate radical is
NH4H2PO4Or H3PO4Solution.
S2: the liquor ferri phosphatis in S1 is dried, and 120 degrees Celsius of temperature, is put into Muffle after drying time 12-24h
It is pre-sintered in furnace, temperature setting is 700 degrees Celsius, and time 10h finally obtains the iron phosphate material without the crystallization water；
The condition of drying and processing in S2 are as follows: per minute not less than 5 DEG C, pressure is not less than 10kPa to heating rate, and will be aqueous
Phosphoric acid iron material is warming up to 500-800 DEG C.
S3: iron phosphate material obtained in S1 is subjected to weighing and calculates mole in case using；
S4: ferric phosphate, lithium source solution, the reproducibility acid solution in S3, reproducibility are weighed according to certain stoichiometric ratio
The dosage of acid solution and the molal quantity of metal ion are directly proportional, and the amount of ascorbic acid is the 1% of Citric Acid Dosage；
S5: being added drop-wise in reproducibility acid solution by liquor ferri phosphatis, lithium source solution, and be stirred continuously, and adjusts PH with ammonium hydroxide
To between 8-9, temperature setting is 90-100 DEG C, is stirred to react on heating stirrer to solution in gel；Lithium source is molten
Liquid are as follows: Li (CH3COO)·2H2O、LiOH·H2O、LiNO3One of which, reproducibility acid solution are as follows: glycolic, ascorbic acid,
Citric acid, ethylene glycol, sucrose, acetone two of them mixed liquor.
S6: gained colloid substance in S5 is put into vacuum oven and is dried, drying time 12h obtains phosphoric acid
Iron lithium presoma；
S7: sintered material is clayed into power shape by S6 after 500 DEG C of pre-sintering 5h, then carries out tabletting, pressure is big
Small is 10MPa；
S8: resulting materials in S7 are placed in Muffle furnace and carry out being warming up to 750 DEG C with 5 DEG C of speed per minute, are sintered material
The material time is 12h, in N2Atmosphere under be sintered.Natural cooling is then carried out in furnace is cooled to room temperature；
S9: the material being sintered in S8 is ground in the agate mortar, obtains required phosphorus after crossing 200 meshes
Sour iron lithium anode material.
When material containing certain crystallization water is dried under specific drying temperature, the condition packet of drying and processing
It including, per minute not less than 5 DEG C, pressure is not less than 10kPa to heating rate, and water-bearing phosphate iron material is warming up to 500-800 DEG C,
A kind of anhydrous iron phosphate crystal can be obtained, compared to other treatment process, anhydrous iron phosphate that preceding method of the present invention obtains
It is good with uniformity, it is with high purity the features such as.Lithium ion battery made of LiFePO4 using anhydrous iron phosphate preparation, has
Internal resistance is small, while its performance is substantially unaffected.
Therefore, in order to realize above-mentioned experiment purpose, firstly, the present invention provides the preparation method of anhydrous iron phosphate, the party
Method includes:
First, synthesize the ferric phosphate with the crystallization water.
Second, the phosphoric acid iron material containing the crystallization water is warming up to 500-850 degrees Celsius.
Third, the present invention provides by anhydrous iron phosphate obtained by the above method.
4th, the present invention provides a kind of LiFePO4, the LiFePO4 is by the phosphoric acid iron material system containing the crystallization water
Standby to form, the anhydrous iron phosphate is the above-mentioned anhydrous iron phosphate of the present invention.
Sol-gal process be will prepare Fe source compound, Li source compound, P source compound that LiFePO 4 uses and
Other addO-on therapy compounds, by forming three solution, colloidal sol, gel processes, formation lithium iron phosphate precursor consolidates gel,
In the inert gas atmospheres such as nitrogen or argon gas, 500 DEG C -850 DEG C at a temperature of, Gu gel occur high temperature solid state reaction generate
The LiFePO 4 of olivine structural.Sol-gal process is a kind of method emerging in wet chemical method.With other conventional methods
It compares, sol-gal process more can be in low temperature synthetic material, and guarantees the purity and uniformity of material, and the initial procedure of reaction can
To control material nano level structures.Colloidal sol be colloidal dispersions in the solution.Colloid is the solid that diameter is 100nm or so
Grain.Gel is a kind of rigid network connected each other, its hole is submicron-scale, and the average length of polymer chain is greater than
1 micron.Term " gel " includes the diversity of substance combination, is divided into four classes: (1) well-regulated layer structure；(2) entirely without
The covalent polymer network of sequence；(3) assemble the principal polymeric network to be formed by physics；(4) especially unordered
Structure
With Fe (NO3)3、LiH2PO4, Nano carbon balls and polyvinyl alcohol are raw material, prepare olive by sol-gal process
Stone structure lithium iron phosphate cathode material.
Polyvinyl alcohol and Nano carbon balls are dispersed in water in the case where being stirred continuously, with ultrasonication half an hour,
Later by FePO4And LiH2PO4Mixture is added in the mixture previously prepared, and 12h or more is stirred at 50 DEG C, is made wet solidifying
Glue, by wet gel, dry 12h, water evaporation obtain solid gel later at 120 DEG C, then by solid gel in the inertia such as nitrogen or argon gas
In gas atmosphere, at 700 DEG C, the LiFePO 4 of olivine structural is obtained through high temperature solid state reaction 10h.
In conjunction with example specific implementation step are as follows:
Step 1: weighing 168g iron powder (or iron oxide 232g) in beaker, the phosphoric acid of 3mol is measured, is added dropwise to
In the beaker, excessive H is added2O2Make the Fe in solution2+It is converted into the Fe of needs as far as possible3+。
It is placed in a vacuum drying oven step 2: the iron phosphate material obtained containing the crystallization water will be reacted, in 120 DEG C do
Dry 12-24h is placed in Muffle furnace at dry temperature is sintered with 700 DEG C of temperature, finally obtains the phosphorus without the crystallization water
Sour iron material, weighing.
Step 3: weighing the second step reaction iron phosphate material obtained without the crystallization water of 151g, 24g hydroxide respectively
Lithium, 210g citric acid, the ascorbic acid of 2.1g and suitable deionized water.
Step 4: respectively by without the crystallization water iron phosphate material and lithium hydroxide be put into beaker 1 be dissolved in 250ml go from
Sub- water, citric acid and ascorbic acid put three-necked flask into and are dissolved in deionization, and ammonium hydroxide is put into beaker 2, and three kinds of mixtures are spare.
Step 5: the mixed liquor in beaker 1 and beaker 2 is pumped into three-necked flask respectively with peristaltic pump, reaction temperature 90-
100 DEG C, heating stirring is carried out with the revolving speed of 1500-2800r/min, PH is adjusted in the process and stablizes between 8-9.
Step 6: pour into form colloidal sol in the 5th step and put vacuum oven in beaker into, drying temperature under vacuum condition
It is 120 DEG C, time 12h, material is put into quartz boat in Muffle furnace with 450 DEG C of temperature pre-burning 5h after taking out grinding.
It is put into Muffle furnace after tabletting with 900 DEG C of temperature after the material grinding in the 6th step Muffle furnace step 7: taking out
200 meshes, which are crossed, after taking-up grinding after calcining 12h obtains LiFePO 4 material.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a method of LiFePO4 is prepared with nanoscale iron phosphate, which comprises the following steps:
S1: Fe source compound is added in the solution containing phosphate radical, is heated to 90- under the revolving speed of 1500-2800r/min
100 DEG C of stirrings are completely dissolved iron, and excess H is added in the solution2O2Solution, make Fe as much as possible2+It is oxidized to Fe3+, to anti-
It should carry out the material that the ferric phosphate containing the crystallization water is obtained after 5-15h drying；
S2: the liquor ferri phosphatis in S1 is dried, and 120 degrees Celsius of temperature, is put into Muffle furnace after drying time 12-24h
It is pre-sintered, temperature setting is 700 degrees Celsius, and time 10h finally obtains the iron phosphate material without the crystallization water；
S3: iron phosphate material obtained in S1 is subjected to weighing and calculates mole in case using；
S4: weighing ferric phosphate, lithium source solution, the reproducibility acid solution in S3 according to certain stoichiometric ratio, and reproducibility acid is molten
The dosage of liquid and the molal quantity of metal ion are directly proportional, and the amount of ascorbic acid is the 1% of Citric Acid Dosage；
S5: being added drop-wise in reproducibility acid solution by liquor ferri phosphatis, lithium source solution, and be stirred continuously, and adjusts PH to 8-9 with ammonium hydroxide
Between, temperature setting is 90-100 DEG C, is stirred to react on heating stirrer to solution in gel；
S6: gained colloid substance in S5 is put into vacuum oven and is dried, drying time 12h obtains LiFePO4
Presoma；
S7: sintered material is clayed into power shape by S6 after 500 DEG C of pre-sintering 5h, then carries out tabletting, pressure size is
10MPa；
S8: resulting materials in S7 being placed in Muffle furnace and be warming up to 750 DEG C with 5 DEG C of speed per minute, when agglomerated material
Between be 12h, in N2Atmosphere under be sintered.Natural cooling is then carried out in furnace is cooled to room temperature；
S9: the material being sintered in S8 is ground in the agate mortar, obtains required ferric phosphate after crossing 200 meshes
Lithium anode material.
2. a kind of method for preparing LiFePO4 with nanoscale iron phosphate according to claim 1, it is characterised in that: in S1
Fe source compound are as follows: Fe (CH3COO)2、FeC2O4·2H2O、FeSO4·7H2O、Fe(NO3)3·9H2O、Fe2O3Wherein with iron powder
It is a kind of.
3. a kind of method for preparing LiFePO4 with nanoscale iron phosphate according to claim 1, it is characterised in that: in S1
The solution of phosphate radical is NH4H2PO4Or H3PO4Solution.
4. a kind of method for preparing LiFePO4 with nanoscale iron phosphate according to claim 1, it is characterised in that: in S5
Lithium source solution are as follows: Li (CH3COO)·2H2O、LiOH·H2O、LiNO3It is one of.
5. a kind of method for preparing LiFePO4 with nanoscale iron phosphate according to claim 1, it is characterised in that: in S5
Reproducibility acid solution are as follows: glycolic, ascorbic acid, citric acid, ethylene glycol, sucrose, acetone two of them mixed liquor.
6. a kind of method for preparing LiFePO4 with nanoscale iron phosphate according to claim 1, it is characterised in that: in S2
The condition of drying and processing are as follows: per minute not less than 5 DEG C, pressure is not less than 10kPa to heating rate, and by water-bearing phosphate iron material liter
Temperature is to 500-800 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022179291A1 (en) * | 2021-02-26 | 2022-09-01 | 广东邦普循环科技有限公司 | Method for separating ferronickel from lateritic nickel ore leach solution and preparing iron phosphate, and application |
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| CN108975297A (en) * | 2018-07-17 | 2018-12-11 | 桂林理工大学 | The method that the crystallization water by removing nanoscale iron phosphate prepares high performance lithium iron phosphate positive material |
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