CN106784810A - A kind of LiFePO 4 material and preparation method thereof - Google Patents
A kind of LiFePO 4 material and preparation method thereof Download PDFInfo
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- CN106784810A CN106784810A CN201611021106.5A CN201611021106A CN106784810A CN 106784810 A CN106784810 A CN 106784810A CN 201611021106 A CN201611021106 A CN 201611021106A CN 106784810 A CN106784810 A CN 106784810A
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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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- 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
- 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
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Abstract
The invention discloses a kind of LiFePO 4 material and preparation method thereof, including lithium hydroxide and phosphoric acid solution are mixed, form mixed liquor A, it is standby；Green-vitriol, potassium dihydrogen phosphate and vitamin C acid reagent are mixed, mixed liquid B is formed, it is standby；Poured into autoclave after mixed liquor A and mixed liquid B are mixed, constant temperature pressurize is carried out after heating, suction filtration is carried out after decrease temperature and pressure, excluded filtrate and collect filter cake, obtain the LiFePO4.The positive electrode security performance that solves traditional lithium ion battery is poor, preparation cost is increased, and capacity is low, and specific energy is not met by the problem of demand.
Description
Technical field
The present invention relates to battery material, more particularly to a kind of LiFePO 4 material and preparation method thereof.
Background technology
At present, lithium ion battery turns into focus of concern as first-selected green energy resource storage device.For accounting for lithium
Ion battery cost about 30%, while determining that the positive electrode of its security has become the focus of research.
The patent of invention of Application No. 201210235625.7, the invention discloses a kind of side for preparing LiFePO 4 material
Method, the method is comprised the following steps：The raw material of LiFePO 4 material is mixed with, raw material includes lithium source, source of iron, phosphorus source and carbon
Source, wherein source of iron are ferrous iron and ferric mixture；Raw material after ball milling dry mixed, ball milling drying is will be mixed
Raw material is first put into ball milling in ball mill, and treatment is then dried again；The dried raw material of pre-burning ball milling, obtains LiFePO4 material
The presoma of material；The presoma of the LiFePO 4 material obtained after broken pre-burning；The forerunner of the LiFePO 4 material after will be broken
Body carries out double sintering, obtains LiFePO 4 material finished product.LiFePO 4 material specific capacity obtained by the method for the present invention is high,
Tap density is moderate, specific surface area is moderate, cycle performance is excellent, processing characteristics is excellent.
The patent of invention of Application No. 201510382325.5, the present invention provides a kind of lithium iron phosphate battery positive material.
The material includes LiFePO4/graphene composite material, and the LiFePO4/graphene composite material Surface coating has Graphene
Nanometer sheet.The present invention provide LiFePO4/graphene composite material in, graphene dispersion uniformly be coated on composite table
The Graphene in face can improve the electric conductivity of positive electrode, improve power density, charge/discharge rates and the capacitance of battery, reduce
The consumption of conductive material；Positive electrode good conductivity of the invention, tap density is high, can prepare high capacity cell, can meet rule
The need for modelling is produced.
Lithium ion is the secondary cell that chemical energy and electric energy phase co-conversion are realized by redox reaction, groundwork
Part is made up of three parts, positive pole, negative pole and dividing electrolyte solution.Positive pole negative pole is all to fix active material
On a current collector, plus plate current-collecting body is generally aluminium foil, and negative current collector is Copper Foil, and electrolyte is the lithium salt solution structure of nonaqueous solvents
Into, including one layer of barrier film, electrolyte, generally polypropylene film can be passed through.During charging process, lithium ion takes off from positive electrode
Go out, be diffused near negative pole by electrolyte solution, be then embedded into negative material, at this moment, electronics leads to from positive electrode
Cross plus plate current-collecting body and enter negative current collector along wire, then reacted with negative material.During exoelectrical reaction then in contrast, Li from
Son enters electrolyte from negative pole abjection, and in the Lithium-ion embeding around positive electrode to positive electrode, electronics is from negative pole along leading
Line enters positive pole and participates in reaction.The positive electrode security performance of traditional lithium ion battery is poor, preparation cost is increased, capacity
Low, specific energy is not met by demand.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of LiFePO 4 material and preparation method thereof, solve tradition
Lithium ion battery positive electrode security performance is poor, preparation cost is increased, capacity is low, and specific energy is not met by demand
Problem.
The invention provides a kind of preparation method of LiFePO 4 material, wherein, the preparation method includes：
(1) lithium hydroxide and phosphoric acid solution are mixed, forms mixed liquor A, it is standby；
(2) green-vitriol, potassium dihydrogen phosphate and vitamin C acid reagent are mixed, forms mixed liquid B, it is standby；
(3) poured into autoclave after mixing mixed liquor A and mixed liquid B, constant temperature pressurize is carried out after heating, after decrease temperature and pressure
Suction filtration is carried out, filtrate is excluded and is collected filter cake, obtain the LiFePO4, wherein,
Relative to the lithium hydroxide of 100 weight portions, the consumption of the phosphoric acid solution is 200-250 weight portions, seven water
The consumption of ferric sulfate is 30-55 weight portions, and the consumption of the potassium dihydrogen phosphate is 70-95 weight portions, the vitamin C acid reagent
Consumption be 5-15 weight portions.
Preferably, relative to the lithium hydroxide of 100 weight portions, the consumption of the phosphoric acid solution is 220-230 weight portions, institute
The consumption of green-vitriol is stated for 40-45 weight portions, the consumption of the potassium dihydrogen phosphate is 80-85 weight portions, the vitamin C
The consumption of acid reagent is 8-12 weight portions.
Preferably, the temperature of constant temperature pressurize is 100-150 DEG C in the step (3).
Preferably, the pressure of constant temperature pressurize is 10-15KPa in the step (3).
Preferably, filter paper aperture used by the suction filtration is 80-120 μm.
Preferably, the time of the suction filtration is 5-8min.
Present invention also offers a kind of LiFePO 4 material, the LiFePO 4 material is obtained by above-mentioned preparation method.
Beneficial effect：The invention provides a kind of LiFePO 4 material and preparation method thereof, obtained LiFePO 4 material
Security is higher, traditional lithium battery, and its electrolyte is overcharged using inflammable organic solvent and with corrosive electrolytic salt
Electrolyte is easily reacted generation imflammable gas on the positive electrode surface of high oxidation state when electric, and internal pressure is raised, and battery occurs
The phenomenons such as flatulence, leakage, cause the corrosion and damage of electrical appliance；Negative terminal surface easily forms Li dendrite puncture barrier film and causes during electric discharge
Internal short-circuit of battery, makes internal temperature of battery drastically raise and explode, and anode prepared by phosphoric acid lithium material, resistance to height
Warm ability is strong, and not perishable and Sun Hua, safety issue is effectively solved.LiFePO 4 material preparation cost is relatively low simultaneously,
The preparation method step for providing of the invention is simple, energy consumption is low, can effectively reduce production cost.
Specific embodiment
The following detailed description of the preferred embodiment of the present invention.
Embodiment 1
100g lithium hydroxides and 220g phosphoric acid solutions are mixed, mixed liquor A is formed, it is standby；By 40g green-vitriols, 80g
Potassium dihydrogen phosphate and 8g vitamin Cs acid reagent mix, and form mixed liquid B, standby；Poured into after mixed liquor A and mixed liquid B are mixed
Constant temperature pressurize (temperature is 100 DEG C, and pressure is 10KPa) is carried out in autoclave, after heating, suction filtration (filter paper is carried out after decrease temperature and pressure
Aperture is 80 μm, and the suction filtration time is 5min), exclude filtrate and collect filter cake, obtain the LiFePO 4 material A1.
Embodiment 2
100g lithium hydroxides and 230g phosphoric acid solutions are mixed, mixed liquor A is formed, it is standby；By 45g green-vitriols, 85g
Potassium dihydrogen phosphate and 12g vitamin Cs acid reagent mix, and form mixed liquid B, standby；Fallen after mixed liquor A and mixed liquid B are mixed
Enter in autoclave, constant temperature pressurize (temperature is 150 DEG C, and pressure is 15KPa) is carried out after heating, suction filtration (filter is carried out after decrease temperature and pressure
Sheet hole footpath is 120 μm, and the suction filtration time is 8min), exclude filtrate and collect filter cake, obtain the LiFePO 4 material A2.
Embodiment 3
100g lithium hydroxides and 225g phosphoric acid solutions are mixed, mixed liquor A is formed, it is standby；By 42g green-vitriols, 82g
Potassium dihydrogen phosphate and 10g vitamin Cs acid reagent mix, and form mixed liquid B, standby；Fallen after mixed liquor A and mixed liquid B are mixed
Enter in autoclave, constant temperature pressurize (temperature is 120 DEG C, and pressure is 12KPa) is carried out after heating, suction filtration (filter is carried out after decrease temperature and pressure
Sheet hole footpath is 100 μm, and the suction filtration time is 7min), exclude filtrate and collect filter cake, obtain the LiFePO 4 material A3.
Embodiment 4
Method according to embodiment 1 is prepared, unlike, the consumption of lithium hydroxide is 100g, the phosphoric acid solution
Consumption be 200g, the consumption of the green-vitriol is 30g, and the consumption of the potassium dihydrogen phosphate is 70g, the vitamin C
The consumption of acid reagent is 5g, obtains the LiFePO 4 material A4.
Embodiment 5
It is prepared by the method according to embodiment 1, unlike, the consumption of lithium hydroxide is 100g, the use of the phosphoric acid solution
It is 250g to measure, and the consumption of the green-vitriol is 55g, and the consumption of the potassium dihydrogen phosphate is 95g, the vitamin C acid examination
The consumption of agent is 15g, obtains the LiFePO 4 material A5.
Comparative example 1
Method according to embodiment 1 is prepared, unlike, the consumption of lithium hydroxide is 100g, the phosphoric acid solution
Consumption be 150g, the consumption of the green-vitriol is 20g, and the consumption of the potassium dihydrogen phosphate is 60g, the vitamin C
The consumption of acid reagent is 2g, obtains the LiFePO 4 material D1.
Comparative example 2
It is prepared by the method according to embodiment 1, unlike, the consumption of lithium hydroxide is 100g, the use of the phosphoric acid solution
It is 300g to measure, and the consumption of the green-vitriol is 65g, and the consumption of the potassium dihydrogen phosphate is 105g, the vitamin C acid examination
The consumption of agent is 25g, obtains the LiFePO 4 material D2.
Meanwhile, in order to verify the performance of present invention gained LiFePO4, carrying out performance has carried out volume test, high rate performance
Test, high temperature resistant test, moon self-discharge rate test and the test of 0.5C cycle lives, concrete outcome are as shown in table 1：、
The performance test results of table 1
It can be seen from Table 1 that, LiFePO4 A1-A5 obtained within the scope of the present invention is its capacity, high rate performance, resistance to
High-temperature behavior, moon self-discharge rate, 0.5C cycle lives are higher than in the scope of the invention outer obtained LiFePO4 D1 and D2, and
The highest tolerable temperature of A1-A5 is higher than D1 and D2, the obtained LiFePO4 A1-A3 each side in currently preferred scope
Performance will be higher than D1 and D2.
The invention provides a kind of LiFePO 4 material and preparation method thereof, obtained LiFePO 4 material security compared with
Height, traditional lithium battery, its electrolyte is electrolysed using inflammable organic solvent and with corrosive electrolytic salt during overcharge
Liquid is easily reacted generation imflammable gas on the LiFePO4 surface of high oxidation state, and internal pressure is raised, and battery occurs flatulence, leakage
Etc. phenomenon, the corrosion and damage of electrical appliance are caused；During electric discharge negative terminal surface easily formed Li dendrite pierce through barrier film cause inside battery
Short circuit, makes internal temperature of battery drastically raise and explode, and anode prepared by phosphoric acid lithium material, heat-resisting ability
By force, not perishable and Sun Hua, safety issue is effectively solved.LiFePO 4 material preparation cost is relatively low simultaneously, the present invention
The preparation method step of offer is simple, energy consumption is low, can effectively reduce production cost.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (7)
1. a kind of preparation method of LiFePO 4 material, it is characterised in that the preparation method includes：
(1) lithium hydroxide and phosphoric acid solution are mixed, forms mixed liquor A, it is standby；
(2) green-vitriol, potassium dihydrogen phosphate and vitamin C acid reagent are mixed, forms mixed liquid B, it is standby；
(3) poured into autoclave after mixing mixed liquor A and mixed liquid B, constant temperature pressurize is carried out after heating, carried out after decrease temperature and pressure
Suction filtration, excludes filtrate and collects filter cake, obtains the LiFePO4, wherein,
Relative to the lithium hydroxide of 100 weight portions, the consumption of the phosphoric acid solution is 200-250 weight portions, the seven water sulfuric acid
The consumption of iron is 30-55 weight portions, and the consumption of the potassium dihydrogen phosphate is 70-95 weight portions, the use of the vitamin C acid reagent
It is 5-15 weight portions to measure.
2. preparation method according to claim 1, it is characterised in that relative to the lithium hydroxide of 100 weight portions, the phosphorus
The consumption of acid solution is 220-230 weight portions, and the consumption of the green-vitriol is 40-45 weight portions, the potassium dihydrogen phosphate
Consumption be 80-85 weight portions, the consumption of the vitamin C acid reagent is 8-12 weight portions.
3. preparation method according to claim 1, it is characterised in that the temperature of constant temperature pressurize is in the step (3)
100-150℃。
4. preparation method according to claim 3, it is characterised in that the pressure of constant temperature pressurize is 10- in the step (3)
15KPa。
5. preparation method according to claim 1, it is characterised in that filter paper aperture used by the suction filtration is 80-120 μm.
6. preparation method according to claim 1, it is characterised in that the time of the suction filtration is 5-8min.
7. a kind of LiFePO 4 material, it is characterised in that the LiFePO 4 material is as described in any one in claim 1-6
Preparation method be obtained.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948133A (en) * | 2005-12-21 | 2007-04-18 | 湖南瑞翔新材料有限公司 | Preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate |
| CN102496715A (en) * | 2011-12-22 | 2012-06-13 | 中国计量学院 | Solvothermal method used for preparing LiFePO4 |
| CN103258993A (en) * | 2013-04-24 | 2013-08-21 | 北京化工大学 | Preparation method of lithium iron phosphate powder for anode material of lithium ion battery |
| CN105098145A (en) * | 2015-09-15 | 2015-11-25 | 常州市鼎日环保科技有限公司 | Preparation method of regular diamond lithium iron phosphate powder cathode material |
-
2016
- 2016-11-15 CN CN201611021106.5A patent/CN106784810A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948133A (en) * | 2005-12-21 | 2007-04-18 | 湖南瑞翔新材料有限公司 | Preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate |
| CN102496715A (en) * | 2011-12-22 | 2012-06-13 | 中国计量学院 | Solvothermal method used for preparing LiFePO4 |
| CN103258993A (en) * | 2013-04-24 | 2013-08-21 | 北京化工大学 | Preparation method of lithium iron phosphate powder for anode material of lithium ion battery |
| CN105098145A (en) * | 2015-09-15 | 2015-11-25 | 常州市鼎日环保科技有限公司 | Preparation method of regular diamond lithium iron phosphate powder cathode material |
Non-Patent Citations (1)
| Title |
|---|
| 邓龙征: "磷酸铁锂正极材料制备及其应用的研究", 《工程科技Ⅱ辑》 * |
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Application publication date: 20170531 |