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CN104701499B - A kind of preparation method of high-specific surface area LiFePO 4/C composite - Google Patents

A kind of preparation method of high-specific surface area LiFePO 4/C composite Download PDF

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CN104701499B
CN104701499B CN201310647936.9A CN201310647936A CN104701499B CN 104701499 B CN104701499 B CN 104701499B CN 201310647936 A CN201310647936 A CN 201310647936A CN 104701499 B CN104701499 B CN 104701499B
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surface area
specific surface
preparation
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composite
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CN104701499A (en
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叶丽光
郝德利
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Guizhou batian new energy materials Co.,Ltd.
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TIANJIN HEWEI TECHNOLOGY CO LTD
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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
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    • Y02E60/10—Energy storage using batteries

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Abstract

A kind of preparation method of high-specific surface area LiFePO 4/C composite, it is the step of preparation method：(1) take LITHIUM BATTERY nano ferric phosphate with battery-level lithium carbonate according to mol ratio Fe：Li=0.99:1 ratio mixes, and grinding, adds butanone, then grinds, and is uniformly dispersed, and adds 3% polyvinyl alcohol water solution, and stirring turns into uniform slurry, is then slowly added into active carbon with high specific surface area, is stirred for turning into uniform slurry；(2) the forced air drying 3~5 hours of 105 DEG C of slurry, blocks of solid is turned into；(3) blocks of solid under nitrogen protection, 600 DEG C of sintering are heated to 2 DEG C/min of speed, kept for 2 hours, 720 DEG C of sintering are heated to 2 DEG C/min of speed, is kept for 4 hours, is then stopped heating, naturally cool to room temperature；(4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite.

Description

A kind of preparation method of high-specific surface area LiFePO 4/C composite
Technical field
The invention belongs to new chemical energy storage field, more particularly to a kind of high-specific surface area LiFePO 4/C composite Preparation method.
Background technology
Ferrousphosphate lithium material is a kind of positive electrode of lithium ion battery, has cheap, abundant raw materials, nothing Poison, heat endurance it is good, it is higher than energy, have extended cycle life, usage time is long, security performance is prominent and environmentally safe spy Point, its theoretical specific capacity are 170mAh/, and theoretical work voltage is about 3.45V, are a kind of most potential new type lithium ion electricity Pond positive electrode.But in place of lithium iron phosphate positive material still suffers from some shortcomings, as electrical conductivity is low, ionic diffusion coefficient is low, The shortcomings of poor performance at low temperatures, multiplying power discharging ability, its application aspect is caused to receive many limitations.Ultracapacitor is one The new chemical device of kind, its capacitance is higher than the traditional capacitance of same volume 100,000 times, has high power charging-discharging ability good, follows The good advantage of performance in terms of ring long lifespan and low temperature, but it is lower than energy, the energy that unit mass is stored well below lithium from The level of sub- battery.In recent years, domestic-developed has gone out the product lithium ion battery and ultracapacitor combination, turns into electric capacity electricity Pond, than 3~5 times that energy is ultracapacitor, discharge-rate is 10~20 times of conventional lithium-ion battery for it, is had good Application prospect.Capacitor batteries are generally mixed with active carbon with high specific surface area from LiFePO 4 and are used as positive electrode, and both Mixing uniformity and be tightly combined degree and some problems be present, the invention discloses a kind of high-specific surface area LiFePO 4/C The preparation method of composite, activated carbon is imported in ferrousphosphate lithium material preparation process, so that activated carbon and phosphoric acid are sub- Iron lithium more combines, and is advantageous to improve the performance of capacitor batteries.
The content of the invention
It is an object of the invention to provide a kind of preparation method of LiFePO 4/C of high-specific surface area composite, The existing high-specific surface area of material of preparation, has the high gram volume of comparison, and charge-discharge magnification is strong again.
The present invention realizes that the technical scheme of purpose is：
A kind of preparation method of high-specific surface area LiFePO 4/C composite, it is the step of preparation method：
(1) take LITHIUM BATTERY nano ferric phosphate with battery-level lithium carbonate according to mol ratio Fe：Li=0.99:1 ratio mixes, and puts Enter in mortar and be ground, added according to the 10% of mixture quality and analyze pure butanone, then grind 30 minutes, mixture is poured into Small-sized scattered pan mixer, 3% polyvinyl alcohol water solution with ferric phosphate homogenous quantities is added, with 300 revs/min of rotating speed Stirring turns into uniform slurry in 2 hours, is then slowly added into the active carbon with high specific surface area of phosphoric acid weight of iron 10%, then with 800 Rev/min rotating speed stir and turn into uniform slurry in 2 hours；
(2) the forced air drying 3~5 hours of 105 DEG C of slurry, blocks of solid is turned into；
(3) blocks of solid under nitrogen protection, 600 DEG C of sintering are heated to 2 DEG C/min of speed, kept for 2 hours, 720 DEG C of sintering are heated to 2 DEG C/min of speed, is kept for 4 hours, is then stopped heating, naturally cool to room temperature；
(4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite；
(5) polyvinyl alcohol described in step (1) is characterized in that molecular weight is 5000~10000；Described nanometer phosphoric acid Iron contains 2 crystallizations water；
(6) specific surface area of the active carbon with high specific surface area described in step (1) is in 1000~1500m2/g。
It is an advantage of the invention that process is simple, high-specific surface area LiFePO 4/C composite gram volume of preparation exists More than 110mAh/g, specific surface area is up to 400m2/ g, and can be charged with 40C, 60C electric discharges.
Embodiment
With reference to embodiment, the present invention is further described, and following embodiments are illustrative, be not it is limited, Protection scope of the present invention can not be limited with following embodiments.
Embodiment 1
(1) LITHIUM BATTERY nano ferric phosphate 18.6g is taken（99% purity, molecular formula FePO4·2H2O）With LITHIUM BATTERY micro mist carbonic acid Lithium 3.79g（Shanghai China Lithium Industrial Co., Ltd., purity 99.9%）Mixing, is put into mortar and is ground, and adds and analyzes pure butanone 2.24g, then grind 30 minutes, mixture is poured into small-sized scattered pan mixer, adds the polyvinyl alcohol of 18.6g 3%（Molecule Measure as 5000）The aqueous solution, being stirred 2 hours with 300 revs/min of rotating speed turns into uniform slurry, then slowly adds while stirring Enter 1.86g active carbon with high specific surface area（South Korea produces, the m of specific surface area 10002/g）, then it is small with the rotating speed stirring 2 of 800 turns of minutes The uniform slurries of Shi Chengwei；
(2) the forced air drying 5 hours of 105 DEG C of slurry, blocks of solid is turned into；
(3) blocks of solid in the case where purity is the protection of 99.99% nitrogen, 600 DEG C of burnings are heated to 2 DEG C/min of speed Knot, kept for 2 hours, 720 DEG C of sintering are heated to 2 DEG C/min of speed, is kept for 4 hours, then stops heating, natural cooling To room temperature；
(4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite；
It is an advantage of the invention that process is simple, high-specific surface area LiFePO 4/C composite gram volume of preparation exists More than 111mAh/g, specific surface area is up to 405m2/ g, and can be charged with 40C, 60C electric discharges.
Embodiment 2
(1) LITHIUM BATTERY nano ferric phosphate 18.6g is taken（99% purity, molecular formula FePO4·2H2O）With LITHIUM BATTERY micro mist carbonic acid Lithium 3.79g（Shanghai China Lithium Industrial Co., Ltd., purity 99.9%）Mixing, is put into mortar and is ground, and adds and analyzes pure butanone 2.24g, then grind 30 minutes, mixture is poured into small-sized scattered pan mixer, adds the polyvinyl alcohol of 18.6g 3%（Molecule Measure as 10000）The aqueous solution, being stirred 2 hours with 300 revs/min of rotating speed turns into uniform slurry, then slowly adds while stirring Enter 1.86g active carbon with high specific surface area（South Korea produces, the m of specific surface area 15002/g）, then it is small with the rotating speed stirring 2 of 800 turns of minutes The uniform slurries of Shi Chengwei；
(2) the forced air drying 3 hours of 105 DEG C of slurry, blocks of solid is turned into；
(3) blocks of solid in the case where purity is the protection of 99.99% nitrogen, 600 DEG C of burnings are heated to 2 DEG C/min of speed Knot, kept for 2 hours, 720 DEG C of sintering are heated to 2 DEG C/min of speed, is kept for 4 hours, then stops heating, natural cooling To room temperature；
(4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite；
It is an advantage of the invention that process is simple, high-specific surface area LiFePO 4/C composite gram volume of preparation exists More than 111mAh/g, specific surface area is up to 410m2/ g, and can be charged with 43C, 66C electric discharges.
Embodiment 3
(1) LITHIUM BATTERY nano ferric phosphate 18.6g is taken（99% purity, molecular formula FePO4·2H2O）With LITHIUM BATTERY micro mist carbonic acid Lithium 3.79g（Shanghai China Lithium Industrial Co., Ltd., purity 99.9%）Mixing, is put into mortar and is ground, and adds and analyzes pure butanone 2.24g, then grind 30 minutes, mixture is poured into small-sized scattered pan mixer, adds the polyvinyl alcohol of 18.6g 3%（Molecule Measure as 8000）The aqueous solution, being stirred 2 hours with 300 revs/min of rotating speed turns into uniform slurry, then slowly adds while stirring Enter 1.86g active carbon with high specific surface area（South Korea produces, the m of specific surface area 12002/g）, then it is small with the rotating speed stirring 2 of 800 turns of minutes The uniform slurries of Shi Chengwei；
(2) the forced air drying 4 hours of 105 DEG C of slurry, blocks of solid is turned into；
(3) blocks of solid in the case where purity is the protection of 99.99% nitrogen, 600 DEG C of burnings are heated to 2 DEG C/min of speed Knot, kept for 2 hours, 720 DEG C of sintering are heated to 2 DEG C/min of speed, is kept for 4 hours, then stops heating, natural cooling To room temperature；
(4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite；
It is an advantage of the invention that process is simple, high-specific surface area LiFePO 4/C composite gram volume of preparation exists More than 112mAh/g, specific surface area is up to 410m2/ g, and can be charged with 41C, 60C electric discharges.

Claims (4)

  1. A kind of 1. preparation method of high-specific surface area LiFePO 4/C composite, it is characterised in that：The step of preparation method It is：
    (1) take LITHIUM BATTERY nano ferric phosphate with battery-level lithium carbonate according to mol ratio Fe：Li=0.99:1 ratio mixes, and is put into and grinds It is ground in alms bowl, is added according to the 10% of mixture quality and analyze pure butanone, then ground 30 minutes, mixture is poured into small-sized Scattered pan mixer, adds 3% polyvinyl alcohol water solution with ferric phosphate homogenous quantities, and 2 are stirred with 300 revs/min of rotating speed Hour turns into uniform slurry, is then slowly added into the active carbon with high specific surface area of phosphoric acid weight of iron 10%, then with 800 turns of minutes Rotating speed stir and turn into uniform slurry in 2 hours；
    (2) the forced air drying 3~5 hours of 105 DEG C of slurry, blocks of solid is turned into；
    (3) blocks of solid under nitrogen protection, 600 DEG C of sintering are heated to 2 DEG C/min of speed, kept for 2 hours, with 2 DEG C/min speed be heated to 720 DEG C sintering, keep 4 hours, then stop heating, naturally cool to room temperature；
    (4) sintered product is ground, crosses 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite.
  2. A kind of 2. preparation method of high-specific surface area LiFePO 4/C composite described in claim 1, it is characterised in that： Described polyvinyl alcohol is characterized in that molecular weight is 5000~10000.
  3. A kind of 3. preparation method of high-specific surface area LiFePO 4/C composite described in claim 1, it is characterised in that： Described nano ferric phosphate contains 2 crystallizations water.
  4. A kind of 4. preparation method of high-specific surface area LiFePO 4/C composite described in claim 1, it is characterised in that： The specific surface area of described active carbon with high specific surface area is in 1000~1500m2/g。
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CN110970608A (en) * 2019-12-19 2020-04-07 湖南裕能新能源电池材料有限公司 Lithium iron battery material and preparation method thereof

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CN101330141A (en) * 2008-07-18 2008-12-24 清华大学 Method for preparing lithium ionic battery anode material spherical LiFePO4 /C
WO2009117871A1 (en) * 2008-03-28 2009-10-01 Byd Company Limited A method of preparing a lithium iron phosphate cathode material for lithium secondary batteries
CN102299319A (en) * 2011-07-20 2011-12-28 彩虹集团公司 Preparation method of lithium ion battery anode material LiFePO4
CN102610819A (en) * 2012-04-05 2012-07-25 宁波力邦新能源科技有限公司 Preparing method of high-activity material
CN103258995A (en) * 2013-06-06 2013-08-21 郑州瑞普生物工程有限公司 Preparation method of lithium iron phosphate material

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CN100420074C (en) * 2006-11-23 2008-09-17 武汉大学 A method to manufacture anode material of LiFePO4/C for lithium ion cell
CN100546077C (en) * 2007-11-12 2009-09-30 成都中科来方能源科技有限公司 Composite positive pole, battery-super electric capacity energy storage means and preparation method
CN101714627A (en) * 2008-10-08 2010-05-26 中国科学院金属研究所 Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof
CN101944588B (en) * 2010-09-14 2012-07-11 哈尔滨工业大学 Preparation method of capacitor carbon/lithium iron phosphate composite material
CN102306783A (en) * 2011-09-14 2012-01-04 哈尔滨工业大学 Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material

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WO2009117871A1 (en) * 2008-03-28 2009-10-01 Byd Company Limited A method of preparing a lithium iron phosphate cathode material for lithium secondary batteries
CN101330141A (en) * 2008-07-18 2008-12-24 清华大学 Method for preparing lithium ionic battery anode material spherical LiFePO4 /C
CN102299319A (en) * 2011-07-20 2011-12-28 彩虹集团公司 Preparation method of lithium ion battery anode material LiFePO4
CN102610819A (en) * 2012-04-05 2012-07-25 宁波力邦新能源科技有限公司 Preparing method of high-activity material
CN103258995A (en) * 2013-06-06 2013-08-21 郑州瑞普生物工程有限公司 Preparation method of lithium iron phosphate material

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Address after: 550400 Weng'an Economic Development Zone, Yinzhan Town, Weng'an county, Qiannan Buyei and Miao Autonomous Prefecture, Guizhou Province

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Patentee before: TIANJIN HEWEI TECHNOLOGY Co.,Ltd.

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