CN103531793A - Method for preparing nanometer lithium iron phosphate for low temperature service - Google Patents

Method for preparing nanometer lithium iron phosphate for low temperature service Download PDF

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CN103531793A
CN103531793A CN201310504706.7A CN201310504706A CN103531793A CN 103531793 A CN103531793 A CN 103531793A CN 201310504706 A CN201310504706 A CN 201310504706A CN 103531793 A CN103531793 A CN 103531793A
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iron phosphate
source
lithium iron
temperature
ball milling
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张建新
姚斌
丁昭郡
冯小钰
路婷婷
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Shandong University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a method for preparing nanometer lithium iron phosphate for low temperature service. The method comprises the following steps of (1) weighing a lithium source, an iron source and a phosphoric acid source in the molar ratio of 1:1:1, adding a metal doped source, carrying out ball milling with acetone as a medium, and holding the temperature of the ball-milled sample for 10-14 hours in a vacuum environment at the temperature of 70-90 DEG C to fully dry the sample; (2) grinding and pelletizing the dried sample, holding the temperature for 1-5 hours in an inert gas at the temperature of 250-400 DEG C, nucleating and crystallizing lithium iron phosphate and cooling; (3) mixing the crystallized lithium iron phosphate with glucose, carrying out ball milling with the acetone as the medium, holding the temperature of the ball-milled sample for 10-14 hours in a vacuum environment at the temperature of 70-90 DEG C to fully dry the sample; (4) grinding the dried sample, carrying out in-situ graphitization for 2-4 hours in the inert gas at the temperature of 600-800 DEG C, and cooling to room temperature to obtain the nanometer lithium iron phosphate for the low temperature service. The obtained lithium iron phosphate material is a nanoscale crystal material; the grain size of the lithium iron phosphate is below 60nm; the lithium iron phosphate has excellent low temperature performance.

Description

A kind of method of preparing low temperature use nano-grade lithium iron phosphate
Technical field
The present invention relates to a kind of method of preparing nano-grade lithium iron phosphate, especially relate to a kind of method of nano-grade lithium iron phosphate for low temperature of preparing.
Background technology
Lithium iron phosphate positive material, as the promising lithium ion power battery cathode material of new generation of tool at present, first Shi You Goodenough group found in 1997.This material has stable by FePO 4the olivine structural skeleton forming, lithium ion can freely be deviate to embed from b direction of principal axis, very large distortion of lattice can not occur, therefore be a kind of desirable lithium iron phosphate positive material in process.LiFePO 4the high theoretical specific capacity with 170mAh/g, the high-energy-density of 550Wh/Kg, good cycling stability, environmental friendliness, cost is low, extensively had an optimistic view of, and the quantity research that has high input.
But the defect of LiFePO4 causes it so far can't large-scale application, is embodied in: (1) intrinsic conductivity is low, is difficult to high rate charge-discharge, has extended the charging interval; (2) intrinsic ion diffusion rate is low, has had a strong impact on the high rate performance of material; (3) poor performance at low temperatures, compares compared with commercialization cell positive materials such as LiMn2O4s, LiFePO4-40 ℃ can only the temperature remains within the normal range 15% of capacity, far below other positive electrodes.
For LiFePO4 is come into operation as early as possible, current research is mainly several is improving conductance and the ion proliferation of normal temperature.(1) by carbon, be coated and metal ion mixing, greatly improved the conductivity of material, make it can be 1C current charges (within 1 hour, being full of); (2) by preparing nano-grade lithium iron phosphate, shorten lithium ion the evolving path, improved the transmission channel of lithium ion.
Low Temperature Problems is the important subject of lithium rechargeable battery always, compare other positive electrodes, the Low Temperature Problems of LiFePO4 is more outstanding, and this respect does not have good way to solve at present, and current commercial material-40 ℃ capacity can only the temperature remains within the normal range 15%.And LiFePO4 is as current unique operable power battery anode material, and electrokinetic cell will inevitably run into low-temperature working in using, therefore low temperature is a difficult problem urgently to be resolved hurrily.The patent of invention occurring at present (application number: the preparation method who mentions 201210065013.8), comprise two step high energy Ultrafine Grindings and the processing of two step carbon sources, but result is comparatively loaded down with trivial details, the temperature and time of high-temperature process is longer,
Summary of the invention
The present invention is for solving the technical problem existing at present, provides the preparation method of the lithium iron phosphate positive material that a kind of low temperature uses, the little d of resulting lithium iron phosphate positive material particle diameter 50≤ 60nm, even particle size distribution, purity is high, has normal temperature high rate performance and the cycle performance more excellent than conventional business LiFePO4.-40 ℃ of capability retentions reach the more than 60% of normal temperature.
The technical solution adopted in the present invention is as follows:
Prepare a method for nano-grade lithium iron phosphate for low temperature, step comprises:
1) raw material lithium source, source of iron and source of phosphoric acid are carried out proportioning according to element mol ratio Li:Fe:P=1:1:1, and add metal-doped source, and the acetone of usining carries out ball milling as medium, and after ball milling, sample makes sample fully dry for 10-14 hour the vacuum environment insulation of 70-90 ℃;
2) dried sample grind, granulation, in inert gas 250-400 ℃ insulation 1-5 hour, LiFePO4 nucleation and crystallization, cooling subsequently;
3) LiFePO4 of crystallization mixes with glucose, and the acetone of usining carries out ball milling as medium, and after ball milling, sample makes sample fully dry for 10-14 hour in the vacuum environment insulation at 70-90 ℃;
4) dried sample, grinds, and in inert gas, 600-800 ℃ of original position graphitization bag carbon 2-4 hour, is cooled to room temperature and obtains low temperature nano-grade lithium iron phosphate.
Described lithium source is selected from Li 2cO 3or LiH 2pO 4a kind of.
Described source of iron is selected from FeC 2o 4or Fe 2o 3a kind of.
Described metal-doped source MnAc 2, ZnAc 2or NiAc 2a kind of.
It is the 0-15% of source of iron molal quantity that described metal-doped source adds molar ratio.
The step 1) of stating and 3) mechanical milling process in, wherein the mass ratio of ball milling ball material and material is 12-17:1, rotational speed of ball-mill is 200-300r/min, ball milling 3-14 hour.
Described step 2) and 4) heating rate is 5-20 ℃/min, and described inert gas is argon gas.
The proportioning that adds of the glucose in described step 3) is 5～8% of crystallization LiFePO4 quality, and the best proportioning that adds is 7%.
Advantage of the present invention and effect are as follows:
1) in the present invention, pass through twice ball milling, effectively reduced the granularity of particle, improved effective response area.
2) adopt the first nucleation and crystallization of LiFePO4, rear recycling glucose carries out the coated method of original position graphitization, make like this LiFePO4 forming in first step heat treatment carry out recrystallization in the coated process of glucose graphitization, guaranteed the perfect degree of LiFePO4 crystal, and coated carbon-coating while original position has limited growing up of LiFePO4 crystal, therefore can effectively prepare nano-scale lithium iron phosphate crystallite (monocrystalline, because polycrystalline has crystal boundary, affect ion diffusion), this method can guarantee that the normal temperature performance of LiFePO4 do not lose that (normal temperature capacity reaches 160mAh/g, 5C discharge capacity reaches 120mAh/g), promote the cryogenic property of LiFePO4 simultaneously.
3) utilize the resulting LiFePO 4 material of this method for nanoscale crystalline material, crystallite dimension, below 60nm, and can reach 30nm.The battery that this material is prepared as positive electrode, its cryogenic property is remarkable, and-40 ℃ of capacitances are at least 50% of normal temperature electric capacity, and can reach 67%.
4) this method adopts low temperature LiFePO4 nucleation, thereby has greatly shortened the time of second step high-temperature heat treatment, can reduce costs like this, shortens technique consuming time.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of embodiment 1 sample
Fig. 2 is the scanning electron microscope diagram of embodiment 4 samples
Fig. 3 is the normal temperature high rate performance of embodiment 2 samples
Fig. 4 is the normal temperature capacity curve of embodiment 3 samples
Fig. 5 is embodiment 3 sample-40 ℃ test curves
Embodiment
Specifically the present invention is further illustrated in conjunction with the embodiments.
Embodiment 1
Take 0.7192gLi 2cO 3, 3.4987FeC 2o 4, 2.2827gNH 4h 2pO 4join in 100mL agate jar, control ratio of grinding media to material is 15:1, pour the high pure acetone of 15mL into as decentralized medium, with 200r/min ball milling 12 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 80 ℃ of vacuumize 12 hours, dried sample is ground, use 10t pressure to be pressed into disk, pack ceramic boat into, with 10 ℃/min heating rate, heat up, in tube furnace, 250 ℃ are incubated 5 hours, cool to room temperature with the furnace, LiFePO4 after sintering and 0.6873g glucose are mixed, be poured in 100mL agate jar, add the high pure acetone of 10mL as ball-milling medium 250r/min ball milling 3 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 80 ℃ of vacuumize 12 hours, by dried sample, grind, pack ceramic boat into, with 5 ℃/min heating rate, heat up, in tube furnace, 700 ℃ are incubated 3 hours, cool to room temperature with the furnace, obtain low temperature nano-grade lithium iron phosphate.The particle diameter d for preparing LiFePO4 50=58nm, normal temperature specific capacity can reach 160mAh/g, and the specific capacity conservation rate of-40 ℃ reaches 51% of normal temperature.
Embodiment 2
Take 0.7192gLi 2cO 3, 1.6582gFe 2o 3, 2.2827gNH 4h 2pO 4, 0.1717gMnAc 2join in 100mL agate jar, control ratio of grinding media to material is 12:1, pour the high pure acetone of 15mL into as decentralized medium, with 300r/min ball milling 14 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 70 ℃ of vacuumize 10 hours, dried sample is ground, use 10t pressure to be pressed into disk, pack ceramic boat into, with 5 ℃/min heating rate, heat up, in tube furnace, 250 ℃ are incubated 5 hours, cool to room temperature with the furnace, LiFePO4 after sintering and 0.6873g glucose are mixed, be poured in 100mL agate jar, add the high pure acetone of 10mL as ball-milling medium 250r/min ball milling 3 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 70 ℃ of vacuumize 10 hours, by dried sample, grind, pack ceramic boat into, with 10 ℃/min heating rate, heat up, in tube furnace, 600 ℃ are incubated 2 hours, cool to room temperature with the furnace, obtain low temperature nano-grade lithium iron phosphate.The particle diameter d for preparing LiFePO4 50=51nm, normal temperature specific capacity can reach 160mAh/g, and the specific capacity conservation rate of-40 ℃ reaches 57% of normal temperature.
Embodiment 3
Take 2.0233gLiH 2pO 4, 3.1489gFeC 2o 4, 0.3508gNiAc 2join in 100mL agate jar, control ratio of grinding media to material is 17:1, pour the high pure acetone of 15mL into as decentralized medium, with 250r/min ball milling 12 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 90 ℃ of vacuumize 14 hours, dried sample is ground, use 10t pressure to be pressed into disk, pack ceramic boat into, with 10 ℃/min heating rate, heat up, in tube furnace, 400 ℃ are incubated 1 hour, cool to room temperature with the furnace, LiFePO4 after sintering and 0.6873g glucose are mixed, be poured in 100mL agate jar, add the high pure acetone of 10mL as ball-milling medium 250r/min ball milling 3 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 80 ℃ of vacuumize 12 hours, by dried sample, grind, pack ceramic boat into, with 10 ℃/min heating rate, heat up, in tube furnace, 800 ℃ are incubated 4 hours, cool to room temperature with the furnace, obtain low temperature nano-grade lithium iron phosphate.The particle diameter d for preparing LiFePO4 50=30nm, normal temperature specific capacity can reach 160mAh/g, and the specific capacity conservation rate of-40 ℃ reaches 67% of normal temperature.
Embodiment 4
Take 2.0233gLiH 2pO 4, 2.9739gFeC 2o 4, 0.5461gZnAc 2join in 100mL agate jar, control ratio of grinding media to material is 16:1, pour the high pure acetone of 15mL into as decentralized medium, with 250r/min ball milling 15 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 80 ℃ of vacuumize 12 hours, dried sample is ground, use 10t pressure to be pressed into disk, pack ceramic boat into, with 10 ℃/min heating rate, heat up, in tube furnace, 400 ℃ are incubated 2 hours, cool to room temperature with the furnace, LiFePO4 after sintering and 0.6873g glucose are mixed, be poured in 100mL agate jar, add the high pure acetone of 10mL as ball-milling medium 250r/min ball milling 3 hours, use the high pure acetone of extra 10mL to disperse in the material of thickness, be poured in culture dish, 80 ℃ of vacuumize 12 hours, by dried sample, grind, pack ceramic boat into, with 20 ℃/min heating rate, heat up, in tube furnace, 700 ℃ are incubated 3 hours, cool to room temperature with the furnace, obtain low temperature nano-grade lithium iron phosphate.The particle diameter d for preparing LiFePO4 50=45nm, normal temperature specific capacity can reach 160mAh/g, and the specific capacity conservation rate of-40 ℃ reaches 63% of normal temperature.

Claims (9)

1. prepare a method for nano-grade lithium iron phosphate for low temperature, it is characterized in that, step comprises:
1) raw material lithium source, source of iron and source of phosphoric acid are carried out proportioning according to element mol ratio Li:Fe:P=1:1:1, and add metal-doped source, and the acetone of usining carries out ball milling as medium, and after ball milling, sample makes sample fully dry for 10-14 hour the vacuum environment insulation of 70-90 ℃;
2) dried sample grind, granulation, in inert gas 250-400 ℃ insulation 1-5 hour, LiFePO4 nucleation and crystallization, cooling subsequently;
3) LiFePO4 of crystallization mixes with glucose, and the acetone of usining carries out ball milling as medium, and after ball milling, sample makes sample fully dry for 10-14 hour in the vacuum environment insulation at 70-90 ℃;
4) dried sample, grinds, and in inert gas, 600-800 ℃ of original position graphitization bag carbon 2-4 hour, is cooled to room temperature and obtains low temperature nano-grade lithium iron phosphate.
2. the method for claim 1, is characterized in that: described lithium source is selected from Li 2cO 3or LiH 2pO 4a kind of.
3. the method for claim 1, is characterized in that: described source of iron is selected from FeC 2o 4or Fe 2o 3a kind of.
4. the method for claim 1, is characterized in that: described metal-doped source MnAc 2, ZnAc 2or NiAc 2a kind of.
5. the method for claim 1, is characterized in that: it is the 0-15% of source of iron molal quantity that described metal-doped source adds metal-doped source to add molar ratio.
6. the method for claim 1, is characterized in that: the mechanical milling process described step 1) and 3), and wherein the mass ratio of ball milling ball material and material is 12-17:1, rotational speed of ball-mill is 200-350r/min, ball milling 10-14 hour.
7. the method for claim 1, is characterized in that: heating rate described step 2) and 4) is 5-20 ℃/min, and described inert gas is argon gas.
8. the method for claim 1, is characterized in that: the proportioning that adds of the glucose in described step 3) is 5～8% of crystallization LiFePO4 quality.
9. method as claimed in claim 8, is characterized in that: the proportioning that adds of described glucose is 7% of crystallization LiFePO4 quality.
CN201310504706.7A 2013-10-23 2013-10-23 Method for preparing nanometer lithium iron phosphate for low temperature service Pending CN103531793A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112349965A (en) * 2020-10-14 2021-02-09 双登集团股份有限公司 Lithium iron phosphate lithium ion battery with improved low-temperature performance and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101339995A (en) * 2008-08-12 2009-01-07 中国兵器工业第二一三研究所 Preparation of lithium iron phosphate positive electrode material for lithium ion power cell
CN101930453A (en) * 2010-07-23 2010-12-29 百度在线网络技术（北京）有限公司 Method and equipment for realizing updating of embedded block of webpage
CN102623707A (en) * 2012-04-02 2012-08-01 湘潭大学 Cobalt-doped carbon-coated ferric fluoride anode material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101339995A (en) * 2008-08-12 2009-01-07 中国兵器工业第二一三研究所 Preparation of lithium iron phosphate positive electrode material for lithium ion power cell
CN101930453A (en) * 2010-07-23 2010-12-29 百度在线网络技术（北京）有限公司 Method and equipment for realizing updating of embedded block of webpage
CN102623707A (en) * 2012-04-02 2012-08-01 湘潭大学 Cobalt-doped carbon-coated ferric fluoride anode material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112349965A (en) * 2020-10-14 2021-02-09 双登集团股份有限公司 Lithium iron phosphate lithium ion battery with improved low-temperature performance and preparation method thereof

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Application publication date: 20140122