CN103700856B - The preparation method of high-performance lithium manganese phosphate material for lithium-ion-power cell - Google Patents
The preparation method of high-performance lithium manganese phosphate material for lithium-ion-power cell Download PDFInfo
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- CN103700856B CN103700856B CN201310689352.8A CN201310689352A CN103700856B CN 103700856 B CN103700856 B CN 103700856B CN 201310689352 A CN201310689352 A CN 201310689352A CN 103700856 B CN103700856 B CN 103700856B
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- 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 the preparation method of a kind of lithium-ion-power cell high-performance lithium manganese phosphate material. The method adopts crystallization control legal system for lithium phosphate presoma, then adopts solvent-thermal method to prepare lithium manganese phosphate. Mix iron, magnesium and nickel in solvent heat process, substitute the position of manganese. Finally adopt organic precursor pyrolysis carry out carbon coated obtain final products LiMn (1-x-y-z)FexMgyNizPO4/ C. Doping phosphoric acid manganese lithium material composition prepared by the method is stablized controlled, without dephasign, and excellent performance, large multiplying power discharging ability is strong. Material can reach 155mAhg at 0.1C specific discharge capacity-1, 2C specific discharge capacity can reach 120mAhg-1。
Description
Technical field
The present invention relates to a kind of anode material for lithium ion battery, particularly relate to a kind of lithium ion power electricityThe preparation method of high-performance lithium manganese phosphate material for pond.
Background technology
Lithium ion battery is the secondary cell that a kind of energy density is high, merit metric density is high, the life-span is long, existingFor playing an important role in society. In the mini-plant such as mobile phone, notebook computer, lithium ion battery shouldWith very extensive. Meanwhile, along with the fast development of the industry such as electric automobile, intelligent grid, lithium ion is movingThe demand of power battery sharply rises, and its performance requirement is improved day by day. Be applied in lithium ion batteryPositive electrode is the deciding factor of its performance and cost. As anode material for lithium-ion batteries, manganese phosphateLithium has that operating voltage is high, electric discharge steadily, the advantage such as cost is low, security is good, be highly suitable for lithium fromSub-dynamical system. Lithium manganese phosphate material is applied to lithium-ion-power cell, and by making, the energy of battery system is closeDegree obtains larger raising, and the amount of monomer of connecting under output voltage on the same group mutually reduces, and contributes to improve battery packReliability.
The key issue that the poorly conductive of lithium manganese phosphate need solve while being its application. Meanwhile, due to manganese elementCommon oxidation state is more, and in lithium manganese phosphate building-up process, the oxidation state of manganese element easily changes and makesMaterial is impure, degradation. Though lithium manganese phosphate material is closely similar with LiFePO4 structure, its preparationMethod and LiFePO4 have relatively big difference, and the some factors that affects this material property is also that it is peculiar. Conductive agent is coated, element doping and to reduce primary particle particle diameter be the main method that improves electric conductivity.Preparation method aspect, high temperature solid-state method and solvent-thermal method are conventional methods.
Summary of the invention
Technical problem to be solved by this invention is, a kind of excellent performance is provided, and large multiplying power discharging ability is strongThe preparation method of high-performance lithium manganese phosphate material for lithium-ion-power cell.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of lithium ion power electricityThe preparation method of high-performance lithium manganese phosphate material for pond, comprises the following steps successively:
1) will be mixed with respectively the aqueous solution containing the raw material of lithium ion and phosphorus-containing acid ion;
2) with measuring pump, material solution being injected to normal-pressure reaction kettle in proportion reacts;
3) reacted rear isolated by filtration and obtained solid content, solid content is washed, is dried;
4), by the solid content obtaining, exist with the raw material that contains manganese ion, iron ion, magnesium ion and nickel ionIn solvent thermal reaction medium, mix, carry out solvent thermal reaction;
5) after having reacted, filter and obtain solid content, and it is washed, is dried;
6) solid content taking organic matter as presoma, step 5) being obtained is coated, then in protectionUnder atmosphere, heat-treat;
7) the solid content product obtaining is pulverized, sieves, is packed, and obtains target product lithium ion movingPower positive electrode for battery material LiMn (1-x-y-z)FexMgyNizPO4/C。
The described raw material containing lithium ion is soluble lithium salts or hydroxide, the raw material of phosphorus-containing acid ionPhosphoric acid or soluble phosphate.
Described raw material injects molar ratio: n (Li+):n(PO4 3-)=3～3.3:1。
The described raw material containing manganese ion is the soluble salt of bivalent manganese, is ferrous containing the raw material of iron ionSoluble salt, is solvable magnesium salts containing the raw material of magnesium ion, is the soluble salt of nickelous containing the raw material of nickel ion.
The raw material of described manganese ion, iron ion, magnesium ion and nickel ion add mole proportioning by materialFormula LiMn (1-x-y-z)FexMgyNizPO4X in/C, y, z value is calculated, and span is0.01 < x≤0.05,0.01 < y≤0.05,0.01 < z≤0.05, total addition and step 3) obtainThe phosphorus element content of solid content etc. mole.
Described solvent thermal reaction medium is in the polyethylene glycol of ethylene glycol, glycerine and the degree of polymerization >=2A kind of mixture of and water.
Described solvent thermal reaction temperature is 100～200 DEG C, and the reaction time is 2～24h.
Described is glucose, sucrose, starch and cellulose for the coated organic matter precursor of carbonOne, by mass fraction, addition is 10%～50% of the solid content that obtains of step 5).
Described heat treatment protective atmosphere is argon gas atmosphere or nitrogen atmosphere.
Described heat treatment temperature is 400～600 DEG C, and heat treatment time is 0.5～3h.
The invention has the beneficial effects as follows: adopt crystallization control legal system for lithium phosphate presoma, then adopt moltenThe hot legal system of agent is for lithium manganese phosphate. Mix iron, magnesium and nickel in solvent heat process, substitute the position of manganese. FinallyAdopt organic precursor pyrolysis to carry out the coated final products that obtain of carbon. The doping phosphoric acid manganese lithium material of preparationCan be excellent, large multiplying power discharging ability is strong.
Brief description of the drawings
Fig. 1 is preparation method's of the present invention technological process;
Fig. 2 is the XRD pattern of the product prepared of embodiment 1;
Fig. 3 is the capacity of the different discharge-rates of the product prepared of embodiment 1.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
As shown in Figure 1, the system of high-performance lithium manganese phosphate material for the lithium-ion-power cell that the present invention adoptsPreparation Method, comprises the following steps successively:
1) will be mixed with respectively the aqueous solution containing the raw material of lithium ion and phosphorus-containing acid ion;
2) with measuring pump, material solution being injected to normal-pressure reaction kettle in proportion reacts;
3) reacted rear isolated by filtration and obtained solid content, solid content is washed, is dried;
4), by the solid content obtaining, exist with the raw material that contains manganese ion, iron ion, magnesium ion and nickel ionIn solvent thermal reaction medium, mix, carry out solvent thermal reaction;
5) after having reacted, filter and obtain solid content, and it is washed, is dried;
6) solid content taking organic matter as presoma, step 5) being obtained is coated, then in protectionUnder atmosphere, heat-treat;
7) the solid content product obtaining is pulverized, sieves, is packed, and obtains target product lithium ion movingPower positive electrode for battery material LiMn (1-x-y-z)FexMgyNizPO4/C。
The described raw material containing lithium ion is soluble lithium salts or hydroxide, the raw material of phosphorus-containing acid ionPhosphoric acid or soluble phosphate.
Described raw material injects molar ratio: n (Li+):n(PO4 3-)=3～3.3:1。
The raw material of described manganese ion, iron ion, magnesium ion and nickel ion add mole proportioning by materialFormula LiMn (1-x-y-z)FexMgyNizPO4X in/C, y, z value is calculated, and span is0.01 < x≤0.05,0.01 < y≤0.05,0.01 < z≤0.05, total addition and step 3) obtainThe phosphorus element content of solid content etc. mole.
The addition of the raw material of described manganese ion, iron ion, magnesium ion and nickel ion is pressed in materials chemistry formulaX, y, z value is calculated, span is 0.01 < x≤0.05,0.01 < y≤0.05,0.01<z≤0.05。
Described solvent thermal reaction medium is in the polyethylene glycol of ethylene glycol, glycerine and the degree of polymerization >=2A kind of mixture of and water.
Described solvent thermal reaction temperature is 100～200 DEG C, and the reaction time is 2～24h.
Described is glucose, sucrose, starch and cellulose for the coated organic matter precursor of carbonOne, by mass fraction, addition is 10%～50% of the solid content that obtains of step 5).
Described heat treatment protective atmosphere is argon gas atmosphere or nitrogen atmosphere.
Described heat treatment temperature is 400～600 DEG C, and heat treatment time is 0.5～3h.
Described normal-pressure reaction kettle is with constant temperature and agitating device.
Adopt crystallization control legal system for lithium phosphate presoma, then adopt solvent-thermal method to prepare lithium manganese phosphate.Mix iron, magnesium and nickel in solvent heat process, substitute the position of manganese. Finally adopt organic precursor pyrolysis to enterThe coated final products that obtain of row carbon. Doping phosphoric acid manganese lithium material composition prepared by the method is stablized controlled, nothingDephasign, excellent performance, large multiplying power discharging ability is strong. Material can reach 155 at 0.1C specific discharge capacitymAh·g-1, 2C specific discharge capacity can reach 120mAhg-1。
Below in conjunction with specific embodiment, material preparation method of the present invention is described.
Embodiment 1
Prepare the following aqueous solution: 3.3moldm-3LiOH solution, 1.0moldm-3H3PO4Solution.In reactor, add liquid (not having the minimum paddle of reactor) at the bottom of appropriate amount of deionized water, Temperature Setting 40DEG C. LiOH solution and H3PO4Solution charge velocity is set as 1.0dm3·min-1, inject, altogether simultaneouslyInject 30min. After reactant has added, precipitation 30min. Filter, heavy with deionized water washingForm sediment 5 times, dry and obtain presoma. Measure the phosphorus element content of presoma. Every mole (taking phosphorus as standard)Presoma and 0.93mol manganese sulfate, 0.05mol ferrous sulfate, 0.01mol nickelous sulfate and 0.01molMagnesium sulfate mixes, and adds 1:1 (volume ratio) the PEG400 aqueous solution of 3 times of this mixture qualities,After fully mixing, carry out 4h solvent thermal reaction at 190 DEG C. Filter, use deionized water washing precipitation4 times, with ethanol washing 1 time, be dried to obtain intermediate products. With the sucrose of 1/3 intermediate products quality with inBetween Product mix ball milling, the homogeneous mixture obtaining is heat treatment 2h under 550 DEG C of nitrogen protections. ?After pulverize, sieve, obtain target product.
The product of the present embodiment can not detect dephasign (Fig. 2), and 0.1C specific discharge capacity reaches 157mAh·g-1, 2C specific discharge capacity reaches 123mAhg-1(Fig. 3).
Embodiment 2
Prepare the following aqueous solution: 3.0moldm-3LiOH solution, 0.95moldm-3H3PO4Solution.In reactor, add liquid (not having the minimum paddle of reactor) at the bottom of appropriate amount of deionized water, Temperature Setting 35DEG C. LiOH solution and H3PO4Solution charge velocity is set as 1.5dm3·min-1, inject, altogether simultaneouslyInject 20min. After reactant has added, precipitation 40min. Filter, heavy with deionized water washingForm sediment 5 times, dry and obtain presoma. Measure the phosphorus element content of presoma. Every mole of presoma is (with phosphorusFor standard) with 0.94mol manganese acetate, 0.02mol ferrous acetate, 0.02mol nickel acetate and 0.02Mol magnesium acetate mixes, and adds 3:1 (volume ratio) diethylene glycol (3) water (1) of 4 times of this mixture qualitiesSolution, after fully mixing, carries out 20h solvent thermal reaction at 120 DEG C. Filter, use deionized waterWashing precipitation 4 times, with ethanol washing 1 time, is dried to obtain intermediate products. By 1/4 intermediate products qualityGlucose and intermediate products mixing and ball milling, the homogeneous mixture obtaining is heat place under 450 DEG C of nitrogen protectionsReason 3h. Finally pulverize, sieve, obtain target product.
The product of the present embodiment can not detect dephasign, and 0.1C specific discharge capacity reaches 150mAhg-1，2C specific discharge capacity reaches 120mAhg-1。
Embodiment 3
Prepare the following aqueous solution: 2.4moldm-3LiOH solution, 0.75moldm-3H3PO4Solution.In reactor, add liquid (not having the minimum paddle of reactor) at the bottom of appropriate amount of deionized water, Temperature Setting 45DEG C. LiOH solution and H3PO4Solution charge velocity is set as 1.5dm3·min-1, inject, altogether simultaneouslyInject 20min. After reactant has added, precipitation 20min. Filter, heavy with deionized water washingForm sediment 5 times, dry and obtain presoma. Measure the phosphorus element content of presoma. Every mole (taking phosphorus as standard)Presoma and 0.95mol manganese chloride, 0.01mol frerrous chloride, 0.03mol nickel chloride and 0.01molMagnesium chloride mixes, and adds 1:1 (volume ratio) glycerin solution of 4 times of this mixture qualities, fully mixedAfter closing, carry out 10h solvent thermal reaction at 160 DEG C. Filter, with deionized water washing precipitation 4 times,With ethanol washing 1 time, be dried to obtain intermediate products. With starch and the intermediate products of 1/4 intermediate products qualityMixing and ball milling, the homogeneous mixture obtaining is heat treatment 1h under 600 DEG C of nitrogen protections. Finally carry outPulverize, sieve, obtain target product.
The product of the present embodiment can not detect dephasign, and 0.1C specific discharge capacity reaches 155mAhg-1，2C specific discharge capacity reaches 120mAhg-1。
In sum, content of the present invention is not limited in the above-described embodiment, having in same areaThe scholar of knowledge can propose easily other embodiment within technological guidance's thought of the present invention, but thisPlanting embodiment all comprises within the scope of the present invention.
Claims (6)
1. a preparation method for high-performance lithium manganese phosphate material for lithium-ion-power cell, its feature existsIn, comprise the following steps successively:
1) adopt crystallization control legal system for lithium phosphate presoma, by containing lithium ion and phosphorus-containing acid ionRaw material is mixed with respectively the aqueous solution, adds liquid at the bottom of appropriate amount of deionized water, Temperature Setting in reactor35 DEG C, 40 DEG C or 45 DEG C;
2) with measuring pump, material solution being injected to normal-pressure reaction kettle in proportion reacts;
3) reacted rear isolated by filtration and obtained solid content, solid content is washed, is dried;
4), by the solid content obtaining, exist with the raw material that contains manganese ion, iron ion, magnesium ion and nickel ionIn solvent thermal reaction medium, mix, carry out solvent thermal reaction;
5) after having reacted, filter and obtain solid content, and it is washed, is dried;
6) taking organic matter as presoma is to step 5) solid content that obtains is coated, then in protectionUnder atmosphere, heat-treat;
7) the solid content product obtaining is pulverized, sieves, is packed, and obtains target product lithium ion movingPower positive electrode for battery material LiMn(1-x-y-z)FexMgyNizPO4/C；
Described step 2) Raw inject molar ratio be: n (Li+):n(PO4 3-)＝3～3.3:1；
The raw material of described manganese ion, iron ion, magnesium ion and nickel ion add mole proportioning by materialFormula LiMn(1-x-y-z)FexMgyNizPO4X in/C, y, z value is calculated, and span is0.01 < x≤0.05,0.01 < y≤0.05,0.01 < z≤0.05, total addition and step 3) obtainThe phosphorus element content of solid content etc. mole;
Described solvent thermal reaction temperature is 100～200 DEG C, and the reaction time is 2～24h;
Described heat treatment temperature is 400～600 DEG C, and heat treatment time is 0.5～3h.
2. the system of high-performance lithium manganese phosphate material for lithium-ion-power cell according to claim 1Preparation Method, is characterized in that, the described raw material containing lithium ion is soluble lithium salts or hydroxide, containsThe raw material of phosphate anion is phosphoric acid or soluble phosphate.
3. the system of high-performance lithium manganese phosphate material for lithium-ion-power cell according to claim 1Preparation Method, is characterized in that, the described raw material containing manganese ion is the soluble salt of bivalent manganese, containing iron ionRaw material be ferrous soluble salt, be solvable magnesium salts containing the raw material of magnesium ion, containing the raw material of nickel ion beThe soluble salt of nickelous.
4. the system of high-performance lithium manganese phosphate material for lithium-ion-power cell according to claim 1Preparation Method, is characterized in that, described solvent thermal reaction medium is ethylene glycol, glycerine and the degree of polymerization >=2Polyethylene glycol in a kind of mixture of and water.
5. the system of high-performance lithium manganese phosphate material for lithium-ion-power cell according to claim 1Preparation Method, is characterized in that, described for the coated organic matter precursor of carbon be glucose, sucrose,One in starch and cellulose, by mass fraction, addition is step 5) solid content that obtains 10％～50％。
6. the system of high-performance lithium manganese phosphate material for lithium-ion-power cell according to claim 1Preparation Method, is characterized in that, described heat treatment protective atmosphere is argon gas atmosphere or nitrogen atmosphere.
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| CN104124454A (en) * | 2014-07-31 | 2014-10-29 | 天津巴莫科技股份有限公司 | Preparation method of lithium manganese phosphate for lithium ion power battery |
| CN104900877A (en) * | 2015-06-09 | 2015-09-09 | 天津巴莫科技股份有限公司 | Preparing method for LiFexMn(1-x)PO4/C for lithium-ion batteries |
| CN108878782A (en) * | 2017-05-16 | 2018-11-23 | 创奕能源科技股份有限公司 | The preparation method of the positive electrode of lithium battery |
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Address after: 300384 in Tianjin Binhai Huayuan Industrial Park (outer ring) 8 Haitai Avenue Patentee after: Tianjin Bamo Technology Co., Ltd. Address before: 300384 in Tianjin Binhai Huayuan Industrial Park (outer ring) 8 Haitai Avenue Patentee before: Tianjin B & M Science and Technology Joint-Stock Co., Ltd. |