CN101693532A - Method for preparing lithium ferrous phosphate - Google Patents
Method for preparing lithium ferrous phosphate Download PDFInfo
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- CN101693532A CN101693532A CN200910093735A CN200910093735A CN101693532A CN 101693532 A CN101693532 A CN 101693532A CN 200910093735 A CN200910093735 A CN 200910093735A CN 200910093735 A CN200910093735 A CN 200910093735A CN 101693532 A CN101693532 A CN 101693532A
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- lithium
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- ferrous phosphate
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- lithium ferrous
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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 preparing a lithium ferrous phosphate material by a spray drying-carbothermic reduction method. The method comprises the following steps: (1) roasting and dewatering iron phosphate hydrate for 2-12 hours at 200-600 DEG C to obtain anhydrous iron phosphate powder; (2) weighing the anhydrous iron phosphate, lithium source compounds and carbon source compounds according to a stoichiometric proportion, adding pure water and ball milling at high speed to uniformly mix so as to obtain a slurry with the solid content of 20-50 percent, wherein the mean grain size D50 of suspended solid particles in the slurry is 0.1-1 micrometer; (3) spraying and drying the obtained slurry to obtain a mixed powder precursor, and carrying out heat treatment and carbothermic reduction on the precursor at 700-900 DEG C under the protection of inert gas to obtain a lithium ferrous phosphate powder material. The lithium ferrous phosphate material prepared by the method has uniform constituents and good batch stability. The 2C discharge specific capacity of the lithium ferrous phosphate material at room temperature is larger than 130mAh/g, thus the lithium ferrous phosphate material has great application value in the field of power type lithium ion batteries.
Description
Technical field
The present invention relates to the method that a kind of spraying drying-carbothermic method prepares ferrousphosphate lithium material, belong to materials science field.
Background technology
Fast development along with electronics and information industry, a large amount of portable type electronic products such as mobile communication equipment, notebook computer, digital product have obtained widespread use, make society go up the demands for higher performance to battery especially rechargeable secondary cell: higher capacity, littler size, lighter weight and longer work-ing life.Lithium ion battery becomes the focus of people's research with its energy density height, operating voltage height, advantages such as load characteristic is good, charge velocities is fast, safety non-pollution, memory-less effect.
Positive electrode material is the important component part of lithium ion battery, mainly contains lamellated LiCoO
2, LiNiO
2, LiNi
0.8Co
0.2O
2, LiNi
1/3Co
1/3Mn
1/3O
2, spinel type LiMn
2O
4LiFePO with olivine structural
4Deng.Olivine-type LiFePO
4With its abundant raw materials, cheap, the specific storage height, good cycle, environmental pollution is little and be considered to the power-type lithium ion battery ideal positive electrode material of tool application potential.
But LiFePO
4Also has inevitable shortcoming during as positive electrode material.LiFePO
4The room temperature electronic conductivity low, can be by being improved at LiFePO4 particle surface coated with conductive material or ion doping.Lithium ion is at LiFePO
4In the speed of diffusion slow, make that battery only is adapted at discharging and recharging under the little electric current, can improve by the control product cut size.Under the same terms, particle diameter is more little, and the lithium ion velocity of diffusion is fast more, LiFePO under the then big current condition
4Specific discharge capacity is high more.
At present, LiFePO
4The synthetic method of material is a lot, comprises high temperature solid-state method, hydrothermal method, coprecipitation method, sol-gel method and microwave process for synthesizing, and wherein high temperature solid-state method is suitable for suitability for industrialized production most.Ferrox that traditional high temperature solid-state method employing price is comparatively expensive or ferrous acetate divalent iron salt and phosphoric acid salt and lithium salt compound mix, and pyroreaction makes under inert atmosphere.Consider that the divalent iron salt cost is higher, and oxidation easily in the building-up process, research in recent years turns to low cost gradually and is difficult for the trivalent iron salt of oxidation, after promptly adopting ferric oxide or tertiary iron phosphate and phosphoric acid salt and lithium salt compound to mix evenly, add carbon-source cpd or iron powder again, pyrocarbon thermal reduction or high temperature iron thermal reduction reaction make under inert atmosphere.Though the high temperature solid-state method synthesis process is simple, reactant is difficult for mixing, long reaction time, and need repeatedly sintering, synthetic product particle diameter major part is a micron order, and skewness, often contain impurity, pattern is irregular, and chemical property is also relatively poor.
Summary of the invention
The purpose of this invention is to provide a kind of with low cost, synthesis technique simple, be fit to suitability for industrialized production, product lot quantity good stability, and under room temperature and big current condition, have the preparation method of the LiFePO 4 of height ratio capacity and good circulation performance.
The present invention is the method that a kind of spraying drying-carbothermic reduction prepares ferrousphosphate lithium material, and its feature comprises the steps:
(1) hypophosphite monohydrate iron was dewatered 2～12 hours 200～600 ℃ of following roastings, obtain the anhydrous phosphoric acid iron powder body;
(2) according to amount of substance than Li: C: Fe=(1～1.05): (1～1.2): 1 takes by weighing the anhydrous iron phosphate in Li source compound, carbon-source cpd and the step (1), add pure water, the high speed ball milling mixes, obtain solid content and be 20～50% slurry, the median size D50 of suspended solids is 0.1～1 micron in the slurry;
(3) the prepared slurry of step (2) is carried out spraying drying, the powder that obtains mixing;
(4) with 700～900 ℃ of thermal treatment 6～24 hours under protection of inert gas of the resulting powder of step (3), promptly obtain ferrousphosphate lithium material of the present invention.
Described Li source compound is a kind of in Quilonum Retard, lithium hydroxide, Lithium Acetate and the lithium oxalate.
Described carbon-source cpd is one or more in sucrose, glucose, citric acid, tetramethylolmethane, vitamins C, polyoxyethylene glycol and the polyethers.
Carbon content in the described ferrousphosphate lithium material is 2～10%.
Compared to existing technology, the present invention has following advantage:
(1) makes raw material with the tertiary iron phosphate of cheapness, do not use expensive ferrous iron, not only reduced production cost, and avoided the easy oxidation of ferrous iron to generate the impurity that is difficult to remove and cause product impure;
(2) with tertiary iron phosphate as source of iron and phosphorus source, the distributing very evenly and fixed ratio of iron, phosphorus atom;
(3) adopt the high speed ball milling that iron phosphate grains is milled to submicron order, shortened the evolving path of lithium ion in iron phosphate grains;
(4) adopt a step agglomerating high temperature solid-state method, production technique is simple, and the cycle is short, and power consumption is few, and is emission-free waits pollution, is fit to large batch of suitability for industrialized production;
(5) adopt spray-dired method, the wink-dry slurry is avoided segregation in the composition drying process, and the products obtained therefrom composition is even, in batches good stability;
(6) this method realizes the even carbon dope of metal ion mixing and granule interior with comparalive ease, further improves the electroconductibility of material;
(7) the synthetic ferrousphosphate lithium material has good electrochemical as anode material for lithium-ion batteries, and at room temperature 2C multiplying power discharging specific storage is suitable as the power anode material for lithium-ion batteries greater than 130mAh/g.
Description of drawings
Fig. 1 is the prepared discharge curve of LiFePO 4 under different multiplying of embodiment one.
Fig. 2 is the prepared cycle performance curve (0.1C three circulations, 0.5C ten circulations, 1C ten circulations, 2C two hundred circulations) of LiFePO 4 under different multiplying of embodiment one.
Fig. 3 is the stereoscan photograph of the prepared LiFePO 4 of embodiment one.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further, following examples do not produce restriction to the present invention.
Embodiment one:
Get 620g hypophosphite monohydrate iron FePO
4.2H
2O temperature rise rate with 4 ℃/min in air atmosphere is raised to 550 ℃ of roasting 10hr dehydrations, gets the anhydrous phosphoric acid iron powder.Take by weighing 110g sucrose, 500g anhydrous iron phosphate and 125g Quilonum Retard (Li: C: Fe=1.02: 1.16: 1), add 1000ml water, at basket ball mill high speed ball milling mixing 2hr, rotational speed of ball-mill 1200rpm forms uniform slurry (slurry solid content 38%).The median size D50 of suspended solids is 0.5 micron in the slurry.The slurry of gained adopts and the fluidized drying mode with pneumatic spray drying device drying, and atomisation unit adopts the double-current method nozzle.Use the peristaltic pump charging, input speed is 15ml/min.The orifice gas flow produces atomizing by compressed-air actuated pressure-controlling under about 0.4MPa, the control air inlet temperature is 300 ℃, and temperature out is 120 ℃, and outlet air separates emptying through the one-level whirlpool.The mixed powder of spraying drying gained promptly obtains ferrousphosphate lithium material behind 700 ℃ of thermal treatment 20hr under the high pure nitrogen protection, the weight content that records carbon in the ferrousphosphate lithium material is 4.2%.
Ferrousphosphate lithium material, Super-P conductive carbon black, PVDF binding agent are pressed mass ratio to be mixed at 8: 1: 1, with NMP is that solvent is made uniform slurry, then with its blade coating on the aluminium foil of 20 micron thickness, after 120 ℃ of vacuum-drying, obtain anode pole piece, with the lithium paper tinsel is counter electrode, in being full of the glove box of argon gas, adorn Experimental cell, carry out charge-discharge test with continuous current, charging/discharging voltage is 2.5-4.2V, room temperature records under the 0.1C multiplying power first that reversible specific capacity is 162mAh/g, reversible specific capacity 140mAh/g under the 2C multiplying power.
Embodiment two:
Get 620g hypophosphite monohydrate iron FePO
4.2H
2O is 300 ℃ of roasting 12hr dehydrations in air atmosphere, get the anhydrous phosphoric acid iron powder.Take by weighing 120g glucose, 500g anhydrous iron phosphate and 145g lithium hydroxide (LiOH.H
2O) (Li: C: Fe=1.04: 1.2: 1), add 1500ml water, at basket ball mill high speed ball milling mixing 2hr, rotational speed of ball-mill 2000rpm, form uniform slurry (slurry solid content 34%), the median size D50 of suspended solids is 0.3 micron in the slurry.The gained slurry adopts and the fluidized drying mode with pneumatic spray drying device drying, and atomisation unit adopts the double-current method nozzle.Use the peristaltic pump charging, input speed is 10ml/min.The orifice gas flow produces atomizing by compressed-air actuated pressure-controlling under about 0.4MPa, the control air inlet temperature is 260 ℃, and temperature out is 110 ℃, and outlet air separates emptying through the one-level whirlpool.The mixed powder of spraying drying gained promptly obtains ferrousphosphate lithium material behind 750 ℃ of thermal treatment 10hr under the high pure nitrogen protection, the weight content that records carbon in the ferrousphosphate lithium material is 4.8%.
Carry out charge-discharge performance test with embodiment one: carry out charge-discharge test with continuous current, charging/discharging voltage is 2.5-4.2V, and room temperature records under the 0.1C multiplying power first that reversible specific capacity is 155mAh/g, reversible specific capacity 135mAh/g under the 2C multiplying power.
Embodiment three:
Get 620g hypophosphite monohydrate iron FePO
4.2H
2O is 450 ℃ of roasting 6hr dehydrations in air atmosphere, get the anhydrous phosphoric acid iron powder.Take by weighing 100g tetramethylolmethane, 500g anhydrous iron phosphate and 350g Lithium Acetate (CH
3COOLi.2H
2O) (Li: C: Fe=1.03: 1.11: 1), add 1000ml water, at basket ball mill high speed ball milling mixing 2hr, rotational speed of ball-mill 1500rpm, form uniform slurry (slurry solid content 49%), the median size D50 of suspended solids is 0.6 micron in the slurry.The gained slurry adopts and the fluidized drying mode with pneumatic spray drying device drying, and atomisation unit adopts the double-current method nozzle.Use the peristaltic pump charging, input speed is 10ml/min.The orifice gas flow produces atomizing by compressed-air actuated pressure-controlling under about 0.4MPa, the control air inlet temperature is 300 ℃, and temperature out is 110 ℃, and outlet air separates emptying through the one-level whirlpool.The mixed powder of spraying drying gained promptly obtains ferrousphosphate lithium material behind 800 ℃ of thermal treatment 10hr under the high pure nitrogen protection, the weight content that records carbon in the ferrousphosphate lithium material is 3.7%.
Carry out charge-discharge performance test with embodiment one: carry out charge-discharge test with continuous current, charging/discharging voltage is 2.5-4.2V, and room temperature records under the 0.1C multiplying power first that reversible specific capacity is 160mAh/g, reversible specific capacity 138mAh/g under the 2C multiplying power.
Embodiment four:
Get 620g hypophosphite monohydrate iron FePO
4.2H
2O is 600 ℃ of roasting 2hr dehydrations in air atmosphere, get the anhydrous phosphoric acid iron powder.Take by weighing 100g vitamins C, 500g anhydrous iron phosphate and 170g lithium oxalate (Li
2C
2O
4) (Li: C: Fe=1.01: 1.03: 1), add 1000ml water, at basket ball mill high speed ball milling mixing 2hr, rotational speed of ball-mill 1000rpm, form uniform slurry (slurry solid content 44%), the median size D50 of suspended solids is 1 micron in the slurry.The gained slurry adopts and the fluidized drying mode with pneumatic spray drying device drying, and atomisation unit adopts the double-current method nozzle.Use the peristaltic pump charging, input speed is 10ml/min.The orifice gas flow produces atomizing by compressed-air actuated pressure-controlling under about 0.4MPa, the control air inlet temperature is 300 ℃, and temperature out is 100 ℃, and outlet air separates emptying through the one-level whirlpool.The mixed powder of spraying drying gained promptly obtains ferrousphosphate lithium material behind 900 ℃ of thermal treatment 6hr under the high pure nitrogen protection, the weight content that records carbon in the ferrousphosphate lithium material is 3.5%.
Carry out charge-discharge performance test with embodiment one: carry out charge-discharge test with continuous current, charging/discharging voltage is 2.5-4.2V, and room temperature records under the 0.1C multiplying power first that reversible specific capacity is 150mAh/g, reversible specific capacity 133mAh/g under the 2C multiplying power.
Claims (4)
1. the preparation method of a lithium ferrous phosphate as anode material of lithium ion battery is characterized in that this method carries out according to the following steps:
(1) hypophosphite monohydrate iron was dewatered 2～12 hours 200～600 ℃ of following roastings, obtain the anhydrous phosphoric acid iron powder body;
(2) according to mol ratio Li: C: Fe=(1～1.05): (1～1.2): 1 takes by weighing the anhydrous iron phosphate in Li source compound, carbon-source cpd and the step (1), add pure water, the high speed ball milling mixes, obtain solid content and be 20～50% slurry, the median size D50 of suspended solids is 0.1～1 micron in the slurry;
(3) the prepared slurry of step (2) is carried out spraying drying, the powder that obtains mixing;
(4) with 700～900 ℃ of thermal treatment 6～24 hours under protection of inert gas of the resulting powder of step (3), promptly obtain ferrousphosphate lithium material of the present invention.
2. the preparation method of LiFePO 4 according to claim 1 is characterized in that in the step (2), and described Li source compound is a kind of in Quilonum Retard, lithium hydroxide, Lithium Acetate and the lithium oxalate.
3. the preparation method of LiFePO 4 according to claim 1 is characterized in that in the step (2), described carbon-source cpd is one or more in sucrose, glucose, citric acid, tetramethylolmethane, vitamins C, polyoxyethylene glycol and the polyethers.
4. the preparation method of LiFePO 4 according to claim 1 is characterized in that the carbon content in the described ferrousphosphate lithium material is 2～10%.
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| CN102139870A (en) * | 2010-12-03 | 2011-08-03 | 清华大学 | Nanocrystal microsphere lithium iron phosphate material with high tap density and preparation method thereof |
| CN102306791A (en) * | 2011-08-18 | 2012-01-04 | 合肥国轩高科动力能源有限公司 | Method for preparing carbon-cladding non-stoichiometric lithium iron phosphorous oxide material |
| CN102623695A (en) * | 2012-03-29 | 2012-08-01 | 天津巴莫科技股份有限公司 | Phosphate lithium ion battery cathode material and preparation method thereof |
| CN102664257A (en) * | 2012-04-05 | 2012-09-12 | 扬州奇峰纳米材料有限公司 | Low-temperature solid-phase synthesis method of nanoscale LiFePO4 |
| CN102683698A (en) * | 2012-05-16 | 2012-09-19 | 中国地质大学（武汉） | Preparation method of conductive modified lithium iron phosphate |
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| CN106981645A (en) * | 2017-05-26 | 2017-07-25 | 广东海洋大学 | Modified phosphate iron lithium anode material and preparation method thereof |
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| CN108011102A (en) * | 2017-10-31 | 2018-05-08 | 昆明理工大学 | A kind of method for preparing olivine-type lithium iron phosphate positive material |
| CN108011102B (en) * | 2017-10-31 | 2020-02-07 | 昆明理工大学 | Method for preparing olivine type lithium iron phosphate anode material |
| CN109786744A (en) * | 2019-01-24 | 2019-05-21 | 中南大学 | A method of phosphoric acid ferrisodium electrode is prepared using industrial by-product ferrous sulfate |
| CN112331846A (en) * | 2019-08-27 | 2021-02-05 | 万向一二三股份公司 | Preparation method of high-rate positive electrode material lithium iron phosphate |
| CN110620227A (en) * | 2019-10-22 | 2019-12-27 | 桑顿新能源科技(长沙)有限公司 | Lithium ion battery positive electrode material, preparation method and application thereof |
| CN111115610A (en) * | 2019-12-26 | 2020-05-08 | 李冬 | Dry mixing preparation method of lithium iron phosphate |
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| WO2023109020A1 (en) * | 2021-12-16 | 2023-06-22 | 中国科学院宁波材料技术与工程研究所 | Method for preparing phosphate positive electrode material |
| CN114604841A (en) * | 2022-02-09 | 2022-06-10 | 北京泰丰先行新能源科技有限公司 | Lithium iron phosphate cathode material and preparation method thereof |
| CN114604841B (en) * | 2022-02-09 | 2023-09-26 | 北京泰丰先行新能源科技有限公司 | Lithium iron phosphate positive electrode material and preparation method thereof |
| EP4345061A1 (en) * | 2022-09-05 | 2024-04-03 | Advanced Lithium Electrochemistry Co., Ltd. | Preparation method of battery composite material and precursor thereof |
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