CN1837033A - Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell - Google Patents

Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell Download PDF

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Publication number
CN1837033A
CN1837033A CNA2006100433501A CN200610043350A CN1837033A CN 1837033 A CN1837033 A CN 1837033A CN A2006100433501 A CNA2006100433501 A CN A2006100433501A CN 200610043350 A CN200610043350 A CN 200610043350A CN 1837033 A CN1837033 A CN 1837033A
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lithium
ion
phosphate
aqueous solution
lithium ion
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CN100413781C (en
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谷亦杰
黄小文
崔洪芝
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Shandong University of Science and Technology
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Shandong University of Science and Technology
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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 Synthesis of lithium ferrous phosphate which is anode material of lithium ion battery. The material synthesis is as follows: geeting lithium salt, malysite and mammonium dihydrogen phosphate, according to the mole ratio of lithium ion: iron ion: phosphate radical ion is (0.8-1.2):(0.8-1.2):(0.8-1.2), getting compound A of equal proportion, joining some compound A in aqueous solution B which contains soluble salt and soluble organic species, putting it in high temperature furnace, then cooling naturely, compounding ferrous phosphate powder containing carbon and adulterating metal ion, milling the synthetical aqueous lithium solution powder, controllong the grain diameter between 1-50 mum. The synthetical material of this invention distribute equally, using this material as positive material can improve batteries' charging capacity effectively.

Description

The synthetic method of lithium ferrous phosphate as anode material of lithium ion battery
Technical field
The present invention relates to anode material for lithium-ion batteries, especially refer to the synthetic method of lithium ferrous phosphate as anode material of lithium ion battery.
Background technology
Lithium ion battery is being subjected to extensive attention for over ten years as the green high-capacity power supply, characteristics such as it has the energy density height, cyclicity is good and self-discharge rate is low.Battery circle generally believes LiFePO 4 (molecular formula: LiFePO in recent years 4) be one of best novel anode material of high-energy power battery, in order to improve the capacity of LiFePO 4, generally take in building-up process, to add carbon and doped metal ion.Chinese patent publication number (the patent No.: 200410039176.4) disclose a kind of preparation method of lithium ferrous phosphate as anode material of lithium ion battery; it is with lithium salts; ferrous salt; phosphoric acid salt and additive are put into Equipment for Heating Processing behind the uniform mixing in proportion; flow velocity be the 0.01-50 liter/minute inert gas protection in zone heating handle; temperature rise rate is 1-20 ℃/mi; when temperature to be heated rises to 200-400 ℃; holding temperature is constant; thermostatically heating 1-30 hour; continue then to heat up; carry out pyroprocessing; at 500-850 ℃ of constant temperature 10-48 hour, be cooled to room temperature then, make ferrous phosphate doping lithium anode material.This preparation method is simple to operate, be easy to control, prepared product has good conductivity, weak point is: because the carbon that adds adds with the solid form, the amount of mingling is fewer, so be not easy to mix, mix not thorough, thereby make in the synthetic ferrous phosphate positive electrode material inhomogeneous, can not improve the capacity of material effectively.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide that a kind of generated time is short, the synthetic method of the uniform heavy body ferrous phosphate lithium battery anode material of synthetic materials.
Technical scheme of the present invention is
1, get lithium salts, molysite, primary ammonium phosphate, in lithium ion: iron ion: the phosphate anion mol ratio is (0.8-1.2): (0.8-1.2): ratio uniform mixing (0.8-1.2) obtains mixture A, wherein:
Lithium salts is wherein a kind of of Quilonum Retard, lithium hydroxide, phosphoric acid hydrogen two lithiums, Lithium Sulphate, Lithium Acetate, lithium nitrate and lithium oxalate.
Molysite is ferrous acetate or Ferrox.
2, above-mentioned a certain amount of mixture A is put into a certain amount of aqueous solution B that contains solubility salt and the organic class of solubility, after evenly stirring, put into High Temperature Furnaces Heating Apparatus, in non-air or non-oxidizing atmosphere, temperature rise rate heating with 1-30 ℃/min, the insulation 0-100h time when temperature rises to the 50-200 ℃ of left and right sides, the high more time of temperature is short more, carry out pyroprocessing according to existing one section or zone heating method then, naturally cooling, the synthetic ferrous phosphate powder that contains carbon simple substance (representing with C) and doped metal ion (representing with M) (is used Li xFe yM zPO 4Expression), the x in the formula, y, z value are decided according to respective substance addition content under the following conditions;
(1) mass ratio of aqueous solution B and mixture A be=(0.1-10): 1;
(2) comprise at least in the solubility salt among the aqueous solution B: a kind of in nitrate, acetate, vitriol and the hydrochloride of metallic elements such as aluminium, titanium, magnesium, zirconium, vanadium, manganese, nickel, cobalt, niobium, rhodium, barium, chromium, its addition content must meet following condition: molar ratio≤0.3 of lithium ion in the metal ion in the solubility salt (M) and the lithium salts;
(3) the organic class material of the solubility among the aqueous solution B comprises at least: sucrose, glucose and can be decomposed into a kind of in the soluble high-molecular compound with good electric conductivity carbon class material through pyrolysis, its addition content must meet following condition: carbon simple substance and Li in the final synthetics xFe yM zPO 4Quality ratio≤10;
3, above synthetic ferrous phosphate lithium powder is levigate, particle diameter is controlled between the 1-50um.
The present invention is owing to adopt above-mentioned solution blending means, so mix easily, blended is thorough, thereby makes the distribution of material after synthetic more even, when adopting this material as the positive electrode material of lithium ion battery, can improve the charging capacity of battery effectively.
Embodiment
In order to be illustrated more clearly in the present invention, enumerate following examples, but it there is not any restriction to the present invention.
Embodiment one:
(1) at first lithium oxalate, Ferrox and three kinds of materials of primary ammonium phosphate in lithium ion: iron ion: the phosphate anion mol ratio is that 1: 1: 1 ratio uniform mixing obtains mixture A
(2) getting mixture A 1kg puts into the aqueous solution B that 1kg contains glucose and zirconium nitrate and stirs, under nitrogen atmosphere, temperature rise rate heating with 20 ℃/min, insulation 5h when temperature reaches 100 ℃ of left and right sides, continue to heat up then, in 700 ℃ of constant temperature 10 hours, naturally cooling, the synthetic ferrous phosphate lithium powder that contains carbon simple substance and doping metals zirconium ion, wherein:
Contain glucose 10g, zirconium nitrate (Zr (NO among the aqueous solution B of requirement 1kg 3) 4) 1g (about 0.003 mole);
According to step (1) as can be known 1kg mixture A contain 1.62 moles lithium oxalate (Li 2C 2O 4Molecular weight 102), 3.24 moles of Ferrox (FeC 2O 4143) and 3.24 mole of phosphoric acid ammonium dihydrogen (NH molecular weight: 4H 2PO 4Molecular weight: 115), so last synthetic contains the ferrous phosphate doping lithium anode material LiFeZr of carbon simple substance and doping metals zirconium ion 0.0009PO 4Expression;
(3) synthetic LiFePO 4 powder art is levigate, particle diameter is controlled between the 1-50um.
Embodiment two:
(1) at first with Quilonum Retard, Ferrox and three kinds of materials of primary ammonium phosphate in lithium ion: iron ion: the phosphate anion mol ratio is that 1: 1: 1 ratio uniform mixing obtains mixture A
(2) getting 1kg mixture A puts into the aqueous solution B that 1kg contains polyvinyl alcohol and magnesium nitrate and stirs, under nitrogen atmosphere, temperature rise rate heating with 30 ℃/min, insulation 4h continues heat temperature raising when temperature is raised to 110 ℃ of left and right sides, and constant temperature is 5 hours when temperature reaches 300 ℃, continued to be warming up to 700 ℃ of constant temperature then 5 hours, naturally cooling, the synthetic ferrous phosphate lithium powder that contains carbon simple substance and doping metals magnesium ion, wherein:
Contain polyvinyl alcohol 10g, magnesium nitrate 1g (about 0.004 mole) among the aqueous solution B of requirement 1kg;
According to step (1) as can be known 1kg mixture A contain 1.70 moles Quilonum Retard (Li 2CO 3Molecular weight 74), 3.48 moles of Ferrox (FeC 2O 4143) and 3.4 mole of phosphoric acid ammonium dihydrogen (NH molecular weight: 4H 2PO 4Molecular weight: 115), so the ferrous phosphate doping lithium anode material that last synthetic contains carbon simple substance and doping metals magnesium ion can be used LiFeMg 0.0013PO 4Expression;
(3) synthetic ferrous phosphate lithium powder is levigate, particle diameter is controlled between the 1-50um.
Embodiment three:
(1) at first phosphoric acid hydrogen two lithiums, Ferrox and three kinds of materials of primary ammonium phosphate in lithium ion: iron ion: the phosphate anion mol ratio is that 1: 1: 1 ratio uniform mixing obtains mixture A;
(2) getting 1kg mixture A puts into the aqueous solution B that 1kg contains sucrose and magnesium nitrate and evenly stirs, under nitrogen atmosphere, temperature rise rate heating with 5 ℃/min, insulation 6h continues heating when temperature reaches 90 ℃ of left and right sides, and constant temperature is 5 hours when temperature reaches 300 ℃, continued to be warming up to 700 ℃ of constant temperature then 5 hours, naturally cooling, the synthetic ferrous phosphate lithium powder that contains carbon simple substance and doping metals magnesium ion, wherein:
Contain sucrose 10g, magnesium nitrate 1g (about 0.004 mole) among the aqueous solution B of requirement 1kg;
According to step (1) as can be known 1kg mixture A contain 1.6 moles phosphoric acid hydrogen two lithium (Li 2HPO 4Molecular weight 110), 3.2 moles of Ferrox (FeC 2O 4143) and 3.2 mole of phosphoric acid ammonium dihydrogen (NH molecular weight: 4H 2PO 4Molecular weight: 115), so the ferrous phosphate doping lithium anode material that last synthetic contains carbon simple substance and doping metals magnesium ion can be used LiFeMg 0.0011PO 4Expression;
(3) synthetic ferrous phosphate lithium powder is levigate, particle diameter is controlled between the 1-50um.
For the ease of calculating, when three kinds of materials of the lithium salts in the embodiment of the invention, molysite, primary ammonium phosphate mix all in lithium ion: iron ion: the phosphate anion mol ratio is that 1: 1: 1 ratio is carried out, thereby makes last synthetic ferrous phosphate lithium powder molecular formula LiFeMg 0.0013PO 4In X, Y, Z value equate that but this can not be as the restriction to technical solution of the present invention.

Claims (1)

1, a kind of synthetic method of lithium ferrous phosphate as anode material of lithium ion battery, its concrete synthetic method is as follows:
(1) get lithium salts, molysite, primary ammonium phosphate, in lithium ion: iron ion: the phosphate anion mol ratio is (0.8-1.2): (0.8-1.2): ratio uniform mixing (0.8-1.2), obtain mixture A, wherein:
Lithium salts is wherein a kind of of Quilonum Retard, lithium hydroxide, phosphoric acid hydrogen two lithiums, Lithium Sulphate, Lithium Acetate, lithium nitrate and lithium oxalate,
Molysite is ferrous acetate or Ferrox;
(2) above-mentioned a certain amount of mixture A is put into a certain amount of aqueous solution B that contains solubility salt and the organic class of solubility, after evenly stirring, put into High Temperature Furnaces Heating Apparatus, in non-air or non-oxidizing atmosphere, temperature rise rate heating with 1-30 ℃/min, the insulation 0-100h time when temperature rises to the 50-200 ℃ of left and right sides, the high more time of temperature is short more, carry out pyroprocessing according to existing heating means then, naturally cooling, the synthetic ferrous phosphate lithium powder that contains carbon simple substance (representing with C) and doped metal ion (representing with M) (is used Li xFe yM zPO 4Expression), the x in the formula, y, z value are decided according to respective substance addition content under the following conditions;
1. the mass ratio of aqueous solution B and mixture A is (0.1-10): 1;
2. comprise at least in the solubility salt among the aqueous solution B: a kind of in nitrate, acetate, vitriol and the hydrochloride of aluminium, titanium, magnesium, zirconium, vanadium, manganese, nickel, cobalt, niobium, rhodium, barium, chromium metallic element, its addition content must meet following condition: molar ratio≤0.3 of lithium ion in the metal ion in the solubility salt (M) and the lithium salts;
3. the organic class material of the solubility among the aqueous solution B comprises at least: sucrose, glucose and can be decomposed into a kind of in the soluble high-molecular compound with good electric conductivity carbon class material through pyrolysis, its addition content must meet following condition: carbon simple substance and Li in the final synthetics xFe yM zPO 4Quality ratio≤10;
(3) above synthetic ferrous phosphate lithium powder is levigate, particle diameter is controlled between the 1-50um.
CNB2006100433501A 2006-03-24 2006-03-24 Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell Expired - Fee Related CN100413781C (en)

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CN101209821B (en) * 2006-12-31 2010-05-19 比亚迪股份有限公司 Preparation method for lithium ion secondary battery positive pole active substance lithium iron phosphate
CN101807697A (en) * 2010-04-29 2010-08-18 江苏中欧材料研究院有限公司 Method for synthesizing lithium iron phosphate with full substitute structure
CN101315981B (en) * 2008-06-16 2010-12-08 合肥工业大学 Lithium iron phosphate anode material for lithium ion battery and modification method
CN101314463B (en) * 2007-05-28 2011-04-06 上海比亚迪有限公司 Method of producing active compound lithium iron phosphate of lithium ion secondary battery anode
CN102084524A (en) * 2008-05-22 2011-06-01 株式会社杰士汤浅国际 Positive electrode active material for lithium secondary battery and lithium secondary battery
CN102339987A (en) * 2011-11-02 2012-02-01 中北大学 Method for preparing anode of magnesium ion battery
CN102439767A (en) * 2009-05-22 2012-05-02 夏普株式会社 Positive pole active material, positive pole, and nonaqueous secondary cell
CN102616764A (en) * 2011-10-10 2012-08-01 山东科技大学 Preparation method of porous LiFePO4 powder
CN101673823B (en) * 2009-09-24 2012-09-26 福建师范大学 Method for preparing lithium iron phosphate cathode material simultaneously blended with nickel and iodine by sintering method
CN103069624A (en) * 2010-07-01 2013-04-24 夏普株式会社 Cathode active material, cathode and non-aqueous secondary battery
WO2013056543A1 (en) * 2011-10-20 2013-04-25 四川天齐锂业股份有限公司 Complete cycle preparation method for producing lithium iron phosphate by using lithium ore as lithium source
CN103296276A (en) * 2012-02-28 2013-09-11 珠海银通新能源有限公司 Carbon coating precursor of lithium ion battery anode material and preparation method thereof
CN102034962B (en) * 2009-09-30 2013-11-06 清华大学 Preparation method of anode material of lithium-ion battery
US9083046B2 (en) 2011-03-23 2015-07-14 Sharp Kabushiki Kaisha Cathode active material, cathode electrode and non-aqueous secondary battery
US9293234B2 (en) 2010-07-12 2016-03-22 Sharp Kabushiki Kaisha Positive electrode active material, positive electrode, and nonaqueous-electrolyte secondary battery
US9373844B2 (en) 2010-07-01 2016-06-21 Sharp Kabushiki Kaisha Positive electrode active substance containing lithium-containing metal oxide
CN107834028A (en) * 2017-07-16 2018-03-23 郑观情 A kind of combination electrode material for adulterating vanadium
CN107834029A (en) * 2017-07-17 2018-03-23 郑观情 A kind of doping Cr combination electrode material and its preparation technology
CN107834030A (en) * 2017-07-17 2018-03-23 郑观情 One kind addition nano titanium oxide prepares combination electrode material and technique
CN107834027A (en) * 2017-07-16 2018-03-23 郑观情 A kind of combination electrode material and technique for adulterating aluminium element

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JP4225859B2 (en) * 2003-07-29 2009-02-18 日本化学工業株式会社 Method for producing lithium iron phosphorus composite oxide carbon composite containing Mn atom
US7348100B2 (en) * 2003-10-21 2008-03-25 Valence Technology, Inc. Product and method for the processing of precursors for lithium phosphate active materials
CN1255887C (en) * 2004-03-25 2006-05-10 浙江大学 Method of preparing positive electrode composite material of lithium ion cell contg, ferrous phosphate lithium salt-carbon
CN100336247C (en) * 2004-03-30 2007-09-05 中国科学院物理研究所 Method for preparing phosphate positive-pole material of lithium-ion cell

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CN101209821B (en) * 2006-12-31 2010-05-19 比亚迪股份有限公司 Preparation method for lithium ion secondary battery positive pole active substance lithium iron phosphate
CN101314463B (en) * 2007-05-28 2011-04-06 上海比亚迪有限公司 Method of producing active compound lithium iron phosphate of lithium ion secondary battery anode
US8431271B2 (en) 2008-05-22 2013-04-30 Gs Yuasa International Ltd. Positive active material for lithium secondary battery and lithium secondary battery
CN102084524A (en) * 2008-05-22 2011-06-01 株式会社杰士汤浅国际 Positive electrode active material for lithium secondary battery and lithium secondary battery
CN101315981B (en) * 2008-06-16 2010-12-08 合肥工业大学 Lithium iron phosphate anode material for lithium ion battery and modification method
US9350022B2 (en) 2009-05-22 2016-05-24 Sharp Kabushiki Kaisha Cathode active material, cathode and nonaqueous secondary battery
US8999576B2 (en) 2009-05-22 2015-04-07 Sharp Kabushiki Kaisha Cathode active material, cathode and nonaqueous secondary battery
CN102439767A (en) * 2009-05-22 2012-05-02 夏普株式会社 Positive pole active material, positive pole, and nonaqueous secondary cell
US9419280B2 (en) 2009-05-22 2016-08-16 Sharp Kabushiki Kaisha Cathode active material, cathode and nonaqueous secondary battery
CN102439767B (en) * 2009-05-22 2014-06-18 夏普株式会社 Positive pole active material, positive pole, and nonaqueous secondary cell
US9337489B2 (en) 2009-05-22 2016-05-10 Sharp Kabushiki Kaisha Cathode active material, cathode and nonaqueous secondary battery
CN101673823B (en) * 2009-09-24 2012-09-26 福建师范大学 Method for preparing lithium iron phosphate cathode material simultaneously blended with nickel and iodine by sintering method
US8795550B2 (en) 2009-09-30 2014-08-05 Tsinghua University Method for preparing cathode active material
CN102034962B (en) * 2009-09-30 2013-11-06 清华大学 Preparation method of anode material of lithium-ion battery
CN101807697A (en) * 2010-04-29 2010-08-18 江苏中欧材料研究院有限公司 Method for synthesizing lithium iron phosphate with full substitute structure
CN103069624A (en) * 2010-07-01 2013-04-24 夏普株式会社 Cathode active material, cathode and non-aqueous secondary battery
US9005810B2 (en) 2010-07-01 2015-04-14 Sharp Kabushiki Kaisha Cathode active material, cathode and non-aqueous secondary battery
US9373844B2 (en) 2010-07-01 2016-06-21 Sharp Kabushiki Kaisha Positive electrode active substance containing lithium-containing metal oxide
CN103069624B (en) * 2010-07-01 2016-06-22 夏普株式会社 Positive electrode active materials, positive pole and non-aqueous secondary batteries
US9293234B2 (en) 2010-07-12 2016-03-22 Sharp Kabushiki Kaisha Positive electrode active material, positive electrode, and nonaqueous-electrolyte secondary battery
US9083046B2 (en) 2011-03-23 2015-07-14 Sharp Kabushiki Kaisha Cathode active material, cathode electrode and non-aqueous secondary battery
CN102616764B (en) * 2011-10-10 2014-04-02 山东科技大学 Preparation method of porous LiFePO4 powder
CN102616764A (en) * 2011-10-10 2012-08-01 山东科技大学 Preparation method of porous LiFePO4 powder
WO2013056543A1 (en) * 2011-10-20 2013-04-25 四川天齐锂业股份有限公司 Complete cycle preparation method for producing lithium iron phosphate by using lithium ore as lithium source
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CN103296276A (en) * 2012-02-28 2013-09-11 珠海银通新能源有限公司 Carbon coating precursor of lithium ion battery anode material and preparation method thereof
CN107834028A (en) * 2017-07-16 2018-03-23 郑观情 A kind of combination electrode material for adulterating vanadium
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