CN104269530A - Method for hydro-thermal synthesis of lithium iron phosphate-lithium vanadium phosphate composite material - Google Patents
Method for hydro-thermal synthesis of lithium iron phosphate-lithium vanadium phosphate composite material Download PDFInfo
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- CN104269530A CN104269530A CN201410517369.XA CN201410517369A CN104269530A CN 104269530 A CN104269530 A CN 104269530A CN 201410517369 A CN201410517369 A CN 201410517369A CN 104269530 A CN104269530 A CN 104269530A
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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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- 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
The invention discloses a method for hydro-thermal synthesis of a lithium iron phosphate-lithium vanadium phosphate composite material. The method comprises the following steps: (1) adding 0.5-2 mol/L of iron source solution and 0.5-2mol/L of vanadium source solution in a high-pressure stirrer reactor, adding a proper amount of urea to ensure that pH is equal to 1-7, stirring to obtain a turbid slurry; (2) adding a lithium source compound, a phosphorus source compound and a compound carbon source to ensure that a mol ratio of an iron element to a vanadium element to a lithium element to a phosphorus element to a carbon element is 1 to 1 to 2.5 to 2.5 to (2.5-7.5), reacting for 10-30h, washing and filtering obtained sediments, performing freeze drying, controlling the temperature to be -30 to -50 DEG C, and controlling the drying time to be 10-20h to obtain the lithium iron phosphate-lithium vanadium phosphate composite material. The method disclosed by the invention is simple in process, wide in raw material source, low in cost and low in energy consumption; meanwhile, a cathode material obtained by adopting the method is relatively uniform in particle size distribution, and relatively thin and uniform in distribution. The prepared lithium iron phosphate-lithium vanadium phosphate composite material is good in uniformity, high in reaction activity and excellent in electrochemical performance.
Description
Technical field
The present invention relates to a kind of synthetic method of anode material for lithium-ion batteries, especially relate to the method for a kind of Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material.
Background technology
There is the LiFePO4-phosphoric acid vanadium lithium composite positive pole of olivine structural and monocline two kinds of principal goods phases simultaneously, because it has theoretical specific capacity high (between 170mAh/g and 197mAh/g), good cycle, good rate capability, Heat stability is good, cheap, advantages of environment protection, become the important development direction of current anode material for lithium-ion batteries.But the conductivity of LiFePO4 is very poor, when heavy-current discharge, capacity attenuation is fast, cryogenic property and high rate performance poor; In phosphoric acid vanadium lithium crystal structure, metal ion relatively far apart, reduce the mobility of electronics in material, cause the electronic conductivity of material lower, discharge and recharge effect is carried out undesirable under big current, two kinds of traditional phosphate-based positive electrodes together compound are prepared, utilizing the advantages such as the high ion conductivity of phosphoric acid vanadium lithium, high theoretical specific capacity, high discharge voltage plateau, good low temperature performance to carry out modification to LiFePO4 sill, is a kind of effective method.But while the uniformity how ensureing material and the large high rate performance of material, improve the production efficiency of composite manufacturing process further and reduce the energy consumption of production process, reducing production cost further, is current problem demanding prompt solution.CN 102299303 B discloses a kind of method that LiFePO4-phosphoric acid vanadium lithium composite material is prepared in spraying dry-heat treatment, but synthesis step is complicated, production process is through Overheating Treatment, and energy consumption is high, the particle size range of the composite material prepared is 0.1-2 micron, and uniformity is poor.
Summary of the invention
The technical problem to be solved in the present invention is, overcome production cost in prior art high, the defects such as product is uneven, provide the method for a kind of Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material, to realize the object that raw material sources are wide, technological process simple, product uniformity is good, cost is low.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of method of Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material, comprises the following steps:
(1) the vanadium source solution of the source of iron solution of 0.5 ~ 2mol/L and 0.5 ~ 2mol/L is joined in high-pressure stirring reactor, the mol ratio controlling ferro element and v element is 1:1, add appropriate urea (addition of urea is determined with pH value), make pH in preferred pH3 ~ 4 of 1 ~ 7(), under temperature 100 DEG C ~ 150 DEG C conditions, control mixing speed is the preferred 120-180r/min of 100 ~ 300r/min(), controlled pressure is 2 ~ 4Mpa, and reaction 2 ~ 4h, obtains being suspended slurry;
(2) in step (1) gained slurry, Li source compound is added, P source compound and compounded carbons, make iron, vanadium, lithium, phosphorus and carbon mol ratio are 1 ︰ 1 ︰ 2.5 ︰ 2.5 ︰ (2.5-7.5), in high-pressure stirring reactor, controlled pressure is the preferred 5-6 Mpa of 4 ~ 8Mpa(), controlling rotating speed is 100 ~ 200 rpm(preferably 140 ~ 180 rpm), reaction temperature is 100 DEG C ~ 300 DEG C (preferably 150 DEG C ~ 250 DEG C), reaction 10 ~ 30h(preferably 15 ~ 25h), the precipitation obtained is through washing, filter, carry out freeze drying again, control temperature is-30 ~-50 DEG C, control drying time is 10 ~ 20h, obtain LiFePO4-phosphoric acid vanadium lithium composite powder.
Further, in step (1), described Fe source compound is the one in ferric nitrate, nine water ferric nitrates, iron chloride, ferric sulfate, nine water ferric sulfate, ferrous sulfate or ferrous acetate.
Further, in step (1), described vanadium source compound is ammonium metavanadate or sodium vanadate.
Further, in step (2), described Li source compound is the one in lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or lithium nitrate.
Further, in step (2), described P source compound is the one in diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, lithium dihydrogen phosphate, tertiary sodium phosphate, triethyl phosphate, tributyl phosphate or phosphate.
Further, in step (2), described compounded carbons is at least two kinds in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenolic resins, acrylic resin, epoxy resin, oxalic acid or citric acid.
Present invention process flow process is simple, and raw material sources are wide, and cost is low, and energy consumption is low, and meanwhile, comparatively evenly (thickness is about 0.08-0.15 μm), distribute the positive electrode domain size distribution that the present invention obtains more fine uniform.Obtained LiFePO4-phosphoric acid vanadium lithium product homogeneity is good, and reactivity is high, electrochemical performance.
Accompanying drawing explanation
The SEM collection of illustrative plates of Fig. 1 LiFePO4 obtained by embodiment 1-phosphoric acid vanadium lithium composite material;
The XRD collection of illustrative plates of Fig. 2 LiFePO4 obtained by embodiment 1-phosphoric acid vanadium lithium composite material;
First charge-discharge curve chart under 0.1C, 1C, 10C condition of the battery that Fig. 3 LiFePO4 obtained by embodiment 1-phosphoric acid vanadium lithium composite material is assembled into;
Cyclic curve figure under 1C, 10C condition of the battery that Fig. 4 LiFePO4 obtained by embodiment 1-phosphoric acid vanadium lithium composite material is assembled into.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) take 0.5mol nine water ferric nitrate, 0.5mol ammonium metavanadate, be dissolved in 500ml deionized water respectively, stir and make it to dissolve; Iron nitrate solution and ammonium metavanadate solution are joined in high-pressure stirring reactor, add 5g urea, make pH be 4, under temperature 120 DEG C of conditions, control mixing speed is 200r/min, and controlled pressure is 3Mpa, and reaction 3h, obtains being suspended slurry;
(2) 1.25mol lithium dihydrogen phosphate, 1mol oxalic acid and 0.2mol glucose is added in the slurry, in high-pressure stirring reactor, controlled pressure is 6Mpa, controlling rotating speed is 150 rpm, reaction temperature is 200 DEG C, reaction 20h, the precipitation obtained is through washing, filtration and freeze drying, and control temperature is-40 DEG C, control drying time is 15h, obtains LiFePO4-phosphoric acid vanadium lithium composite powder.
The assembling of battery: the LiFePO4-phosphoric acid vanadium lithium taking 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025,0.1C first discharge specific capacity is 149.5 mAh/g, 1C first discharge specific capacity be 142.9 mAh/g, 10C first discharge specific capacity is 126.8mAh/g; The 1C capability retention after 40 times that circulates be 91.45%, the 10C capability retention after 40 times that circulates is 84.97%.
One-step synthesis of the present invention, processing step is short, and flow process is simple, and without heat treatment, greatly reduces energy consumption.Meanwhile, the material granule obtained is tiny, even particle size distribution, and thickness is about 0.08-0.15 μm.
Embodiment 2
The present embodiment comprises the following steps:
(1) take 0.5mol iron chloride, 0.5mol sodium vanadate, be dissolved in 500ml deionized water respectively, stir and make it to dissolve; Ferric chloride solution and sodium vanadate solution are joined in high-pressure stirring reactor, add 2g urea, make pH be 1, under temperature 100 DEG C of conditions, control mixing speed is 100r/min, and controlled pressure is 2Mpa, and reaction 2h, obtains being suspended slurry;
(2) 1.25mol ammonium dihydrogen phosphate, 0.625mol lithium carbonate, 0.1mol citric acid, 0.1mol malic acid and 0.01mol shitosan is added in the slurry, in high-pressure stirring reactor, controlled pressure is 4Mpa, controlling rotating speed is 100 rpm, reaction temperature is 100 DEG C, reaction 10h, the precipitation obtained is through washing, filtration and freeze drying, and control temperature is-30 DEG C, control drying time is 10h, obtains LiFePO4-phosphoric acid vanadium lithium composite powder.
The assembling of battery: the LiFePO4-phosphoric acid vanadium lithium taking 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025,0.1C first discharge specific capacity is 140.8 mAh/g, 1C first discharge specific capacity be 127.5 mAh/g, 10C first discharge specific capacity is 115.7mAh/g; The 1C capability retention after 40 times that circulates be 89.38%, the 10C capability retention after 40 times that circulates is 80.97%.
One-step synthesis of the present invention, processing step is short, and flow process is simple, and without heat treatment, greatly reduces energy consumption.Meanwhile, the material granule obtained is less, and domain size distribution is comparatively even, and thickness is about 0.15-0.35 μm.
Embodiment 3
The present embodiment comprises the following steps:
(1) take 0.5mol nine water ferric sulfate, 0.5mol ammonium metavanadate, be dissolved in 500ml deionized water respectively, stir and make it to dissolve; Ferrum sulfuricum oxydatum solutum and ammonium metavanadate solution are joined in high-pressure stirring reactor, add 10g urea, make pH be 7, under temperature 150 DEG C of conditions, control mixing speed is 300r/min, and controlled pressure is 4Mpa, and reaction 4h, obtains being suspended slurry;
(2) 1.25mol diammonium hydrogen phosphate, 1.25mol lithium hydroxide, 0.625mol acetic acid and 0.625mol lactic acid is added in the slurry, in high-pressure stirring reactor, controlled pressure is 8Mpa, controlling rotating speed is 200 rpm, reaction temperature is 300 DEG C, reaction 30h, the precipitation obtained is through washing, filtration and freeze drying, and control temperature is-50 DEG C, control drying time is 20h, obtains LiFePO4-phosphoric acid vanadium lithium composite powder.
The assembling of battery: the LiFePO4-phosphoric acid vanadium lithium taking 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025,0.1C first discharge specific capacity is 135.3 mAh/g, 1C first discharge specific capacity be 126.9mAh/g, 10C first discharge specific capacity is 110.8mAh/g; The 1C capability retention after 40 times that circulates be 90.36%, the 10C capability retention after 40 times that circulates is 86.35%.
One-step synthesis of the present invention, processing step is short, and flow process is simple, and without heat treatment, greatly reduces energy consumption.Meanwhile, the material granule obtained is less, and domain size distribution is comparatively even, and thickness is about 0.10-0.50 μm.
Claims (9)
1. a method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material, is characterized in that, comprise the following steps:
(1) the vanadium source solution of the source of iron solution of 0.5 ~ 2mol/L and 0.5 ~ 2mol/L is joined in high-pressure stirring reactor, the mol ratio controlling ferro element and v element is 1:1, add appropriate urea, make pH 1 ~ 7, under temperature 100 DEG C ~ 150 DEG C conditions, control mixing speed is 100 ~ 300r/min, controlled pressure is 2 ~ 4Mpa, and reaction 2 ~ 4h, obtains being suspended slurry;
(2) in step (1) gained slurry, Li source compound, P source compound and compounded carbons is added, iron, vanadium, lithium, phosphorus and carbon mol ratio is made to be 1 ︰ 1 ︰ 2.5 ︰ 2.5 ︰ (2.5-7.5), in high-pressure stirring reactor, controlled pressure is 4 ~ 8Mpa, controlling rotating speed is 100 ~ 200 rpm, reaction temperature is 100 DEG C ~ 300 DEG C, reaction 10 ~ 30h, the precipitation obtained is through washing, filtration, carry out freeze drying again, control temperature is-30 ~-50 DEG C, control drying time is 10 ~ 20h, obtains LiFePO4-phosphoric acid vanadium lithium composite powder.
2. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1, is characterized in that, in step (1), and control pH3 ~ 4.
3. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, is characterized in that, in step (1), control mixing speed is 120-180r/min.
4. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, is characterized in that, in step (2), in high-pressure stirring reactor, controlled pressure is 5-6 Mpa, controlling rotating speed is 140 ~ 180 rpm, and reaction temperature is 150 DEG C ~ 250 DEG C, reaction 15 ~ 25h.
5. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, it is characterized in that, in step (1), described Fe source compound is the one in ferric nitrate, nine water ferric nitrates, iron chloride, ferric sulfate, nine water ferric sulfate, ferrous sulfate or ferrous acetate.
6. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, is characterized in that, in step (1), described vanadium source compound is ammonium metavanadate or sodium vanadate.
7. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, it is characterized in that, in step (2), described Li source compound is the one in lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or lithium nitrate.
8. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, it is characterized in that, in step (2), described P source compound is the one in diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, lithium dihydrogen phosphate, tertiary sodium phosphate, triethyl phosphate, tributyl phosphate or phosphate.
9. the method for Hydrothermal Synthesis LiFePO4-phosphoric acid vanadium lithium composite material according to claim 1 and 2, it is characterized in that, in step (2), described compounded carbons is at least two kinds in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenolic resins, acrylic resin, epoxy resin, oxalic acid or citric acid.
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Cited By (4)
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| CN105129758A (en) * | 2015-06-30 | 2015-12-09 | 中南大学 | Porous manganese vanadium lithium lithium phosphate composite cathode material and preparation method thereof |
| CN105870428A (en) * | 2016-06-16 | 2016-08-17 | 中南大学 | Preparing method for lithium iron phosphate and lithium vanadium phosphate composite anode material precursor |
| CN110783546A (en) * | 2019-11-04 | 2020-02-11 | 桑顿新能源科技有限公司 | Lithium ion battery positive electrode material and preparation method thereof, lithium ion battery positive electrode slurry and positive electrode, lithium ion battery and equipment |
| CN111422852A (en) * | 2020-04-18 | 2020-07-17 | 蒋央芳 | Preparation method of iron vanadium phosphate |
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Application publication date: 20150107 |