CN102916179B - Method for manufacturing industrialized high-energy lithium iron phosphate material - Google Patents
Method for manufacturing industrialized high-energy lithium iron phosphate material Download PDFInfo
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- CN102916179B CN102916179B CN201210370420.XA CN201210370420A CN102916179B CN 102916179 B CN102916179 B CN 102916179B CN 201210370420 A CN201210370420 A CN 201210370420A CN 102916179 B CN102916179 B CN 102916179B
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for manufacturing lithium iron phosphate materials, in particular to the method for manufacturing an industrialized high-energy lithium iron phosphate material. The method is mainly used for solving the technical problems that the existing lithium iron phosphate materials in the prior art are manufactured in a laboratory, are manufactured in a complicated process and are converted into industrialized products difficultly; and high power capacity batteries are manufactured difficultly if the materials with poor particle size distribution and bad material compaction capacity are adopted because the materials are processed only after a primary ball-milling is performed. The method provided by the invention comprises the following steps: adding and mixing lithium salt, ferric salt and phosphor salt twice and performing a wet ball milling twice to obtain two groups of slurry materials with different particle sizes; mixing, drying and presintering the two groups of the slurry materials in different proportions, carrying out the third wet ball milling and sintering on the slurry materials; and finally obtaining the high-energy lithium iron phosphate material.
Description
Technical field
The present invention relates to a kind of preparation method of LiFePO 4 material, especially relate to a kind of preparation method of industrialization high-energy lithium iron phosphate material.
Background technology
Along with fossil resources is day by day deficient, crude oil price goes up again fast, and energy problem has obviously become the global common issue of puzzlement.Finding new forms of energy replaces crude oil extremely urgent as the power set of automobile.The appearance of anode material of lithium battery, makes pure electric automobile, the industrialized development of hybrid vehicle has welcome spring.
At present, lithium ion anode material mainly contains LiCoO
2, LiMn
2o
4, LiNi
xco
ymn
zo
2, LiFePO
4.Wherein LiCoO
2be current unique scale industrialization, commercial positive electrode, the lithium ion battery of commercially available more than 90% all adopts this kind of material.But cobalt acid lithium battery, gram volume is low, cycle life is poor (500 times), coefficient of safety is low and the raising of the rare and cost of cobalt resource, and market share presents the trend of successively decreasing year by year.The LiMn of spinel structure
2o
4cost is low, and fail safe is good, but capacity is low, and cycle performance is poor.LiNi
xco
ymn
zo
2ternary material and LiFePO
4the anode material for lithium-ion batteries of rising in recent years, with LiFePO
4compare LiNi
xco
ymn
zo
2ternary material cost is high, cycle performance is poor (800 times), poor stability.LiFePO
4its characteristic of positive electrode does not expect that price is low, lithium iron phosphorus resource rich content on earth, feed can not have problems containing precious metal element, source; Theoretical capacity high (170mAh/g), discharge power are large, working stability change without exception under have extended cycle life (2000 times), hot environment.LiFePO
4positive electrode has become the focus of positive electrode of new generation research with the advantage of its uniqueness.
But LiFePO4 electronic conductivity is low, ion diffuse speed is slow, improves its capacity to a certain extent by adopting Li position and Fe position doping techniques, in-situ carbon clad nano technology, metal nanoparticle coating technology etc.; But be mostly laboratory preparation, complex process, be difficult to be converted into industrialized product; Other manufacturers are just processed after mostly adopting a ball milling, and domain size distribution is poor, material compaction poor performance, is difficult to make high-capacity battery.
Summary of the invention
The present invention is to provide a kind of preparation method of industrialization high-energy lithium iron phosphate material, and its LiFePO 4 material mainly solving existing for prior art is mostly laboratory preparation, complex process, is difficult to be converted into industrialized product; And just processed after having plenty of employing ball milling, domain size distribution is poor, material compaction poor performance, is difficult to the technical problem making high-capacity battery etc.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
The preparation method of a kind of industrialization high-energy lithium iron phosphate material of the present invention, is characterized in that described method comprises:
A. in ball mill, add lithium salts, molysite, microcosmic salt mixing, wherein Li:Fe:P mol ratio is 1-1.2:1:1-1.1, then adds doping vario-property agent and carbon source, carries out first time wet ball grinding, and after ball milling completes, taking-up is for subsequent use;
B. after repeating to add in ball mill and mixing with the lithium salts of step a identical type, equal in quality, molysite, microcosmic salt, add again and the doping vario-property agent of step a identical type, equal in quality and carbon source, carry out second time wet ball grinding, after ball milling completes, taking-up is for subsequent use, and the particle diameter of twice wet ball grinding disposed slurry is different;
C. by the slurry of step a and step b milled, after the mixing of different ratios, formation presoma is dried; Or first by dry respectively for the slurry of step a and step b milled, after drying, be mixed to form presoma according to different ratios again;
D. the presoma obtained by step c carries out presintering in inertia or reducing atmosphere, cools to room temperature with the furnace after insulation, obtains presintering product;
E. presintering product is carried out third time wet ball grinding, be then dried;
F. the product obtained by step e sinters in inertia or protection of reducing atmosphere stove, cools to room temperature with the furnace, namely obtain high-energy lithium iron phosphate material after heat preservation sintering.
The method that the present invention adopts primary particle size to mix mutually, the presoma that obtained distribution of particles is good, in presoma, small particle diameter fills the gap of Large stone, improve the tap density of its precursor, the LiFePO4 of tap density height domain size distribution the best is obtained after sintering, inherently improve the compaction capacity of material, make the lithium iron phosphate positive material of high power capacity.
As preferably, described wet ball grinding take alcohol as medium ball milling 1-10h, and first time, ball milling size controlling was at 600nm-1200nm, and second time ball milling size controlling is at 50nm-500nm; Third time, ball milling size controlling was at 50nm-1200nm, and the solid content of mechanical milling process is 15-60wt%, and mill used is situated between for zirconium silicate ball, agate ball, zirconia ball, polyurethane ball, alumina balls, the one or more combination of sphere diameter in 0.1-10mm.
As preferably, in described step c, the slurry of step a milled is mixed according to the ratio of 0.5-1:1-5 with the slurry of step b milled.
As preferably, described steps d pre-sintering temperature is 280-450 DEG C, insulation 2-7h; Step f sintering temperature is 550-850 DEG C, heat preservation sintering 5-20h.
As preferably, described dry time adopt atomizer drying-granulating, its inlet temperature is 190-250 DEG C, and outlet temperature is 100 DEG C; Equipment for Heating Processing is sealed type or gas circulating type stove, and inertia or reducing atmosphere are one or more combination in nitrogen, argon gas, hydrogen.
As preferably, described lithium salts be lithia, lithium carbonate, lithium nitrate, lithium dihydrogen phosphate, lithium acetate, lithium hydroxide, lithium phosphate, lithium oxalate, lithium chloride, lithium vanadate, in one or more combinations.
As preferably, described phosphate is one or more combinations in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, phosphoric acid, lithium dihydrogen phosphate, ammonium phosphate, ferric phosphate, phosphorus pentoxide.
As preferably, described molysite is one or more combinations in ferric phosphate, di-iron trioxide, ferric acetate, ferric oxalate, ferric nitrate, iron chloride, ferric sulfate, ferrous sulfate, frerrous chloride.
As preferably, described doping vario-property agent is slaine or metal oxide, and wherein slaine is the one or more combination in nickel, zinc, magnesium, titanium, copper, chromium, manganese, niobium, the carbonate of vanadium, nitrate, acetate, oxalates; Metal oxide is the one or more combination in the oxide of nickel, zinc, magnesium, titanium, copper, chromium, manganese, niobium, vanadium; Doping vario-property agent accounts for the 0.5-20% of LiFePO 4 material gross mass.
As preferably, described carbon source is native graphite, Delanium, hard carbon, soft carbon, organic pyrolysis carbon source, one or more combinations of nanometer conductive material, and the mass ratio that carbon source accounts for LiFePO 4 material is 0.8-20%; Organic pyrolysis carbon source is cellulose acetate, vitamin C, glucose, polyvinyl alcohol, phenolic resins, CMC, polystyrene, sucrose, fructose, polytetrafluoroethylene, epoxy resin, starch, pitch, polyacrylonitrile, polyethylene glycol, one or more combinations of polyvinylpyrrolidone; Nanometer conductive material is conductive black, Graphene, one or more combinations of nano-sized carbon microballoon.
Therefore, the method that the present invention utilizes wet ball grinding particle diameter to mix mutually, makes its particle size distribution reach optimum proportioning, adopts the method for double sintering simultaneously, improve the compaction capacity of material, thus enters the capacity that is improved material.
Accompanying drawing explanation
Accompanying drawing 1 is the XRD diffraction spectrogram of the embodiment of the present invention 4;
Accompanying drawing 2 is first charge-discharge curves of the IFR 26650 type battery 0.2C of the embodiment of the present invention 1,2,3,4 sample;
Accompanying drawing 3 is curve of double curvature of the embodiment of the present invention 4;
Accompanying drawing 4 is IFR 26650 type battery 1C charge and discharge cycles curves of the embodiment of the present invention 4 sample.
Embodiment
Below by embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment 1(comparative example): after lithium salts, molysite, microcosmic salt are 1.01:1:1 mixing according to mol ratio, then add the nickel nitrate of 10% polyethylene glycol and 1%, solution gross mass is 400kg.In ball mill first time wet ball grinding, survey its particle diameter 600nm-1200nm by MalvernMS2000 laser particle analyzer; Adopt atomizer granulating and drying machine, inlet temperature is 240 DEG C, and outlet temperature is 100 DEG C, obtains spherical precursor; Sinter under precursor being put into the nitrogen protection of gas circulating type stove, 400 DEG C of pre-burning constant temperature 5h; By the presoma that burns down in advance again after ball milling, spraying dry, under nitrogen protection, sinter 700 DEG C of constant temperature 5h.
The preparation of negative material: with MCMB: acetylene black: the ratio of polyvinylidene fluoride=92wt%:3wt%:7wt%, and 1-METHYLPYRROLIDONE stirring is sized mixing, and is uniformly coated on by slurry on Copper Foil, 120 DEG C of oven dryings.
The preparation of positive electrode: with LiFePO4: acetylene black: the ratio of polyvinylidene fluoride=92wt%:4wt%:4wt%, and 1-METHYLPYRROLIDONE stirring is sized mixing, and is uniformly coated on by slurry on Copper Foil, 120 DEG C of oven dryings.
The assembling of battery: roll battery by winding method, circular winding pin diameter 4mm, effective length is greater than 100mm; With 1mol/L LiPF
6/ (EC+DEC) (volume ratio 1:1) is electrolyte, take polypropylene film as barrier film, assembled battery.
Cell tester: charge and discharge cycles test is carried out in Shenzhen new prestige (CT-3008W-5V3A).
Fig. 1 is the first charge-discharge curve making IFR 26650 type battery 0.2C.
Embodiment 2(comparative example): after lithium salts, molysite, microcosmic salt are 1.01:1:1 mixing according to mol ratio, then add the nickel nitrate of 10% polyethylene glycol and 1%, solution gross mass is 400kg.In ball mill, second time wet ball grinding, surveys its particle diameter 50nm ~ 500nm by MalvernMS2000 laser particle analyzer; Adopt atomizer granulating and drying machine, inlet temperature is 240 DEG C, and outlet temperature is 100 DEG C, obtains spherical precursor; Sinter under precursor being put into the nitrogen protection of gas circulating type stove, 400 DEG C of pre-burning constant temperature 5h; By the presoma that burns down in advance again through third time ball milling, after spraying dry, under nitrogen protection, sinter 700 DEG C of constant temperature 5h.Battery makes identical with embodiment 1.
Fig. 1 is the first charge-discharge curve making IFR 26650 type battery 0.2C.
Embodiment 3: the preparation method of a kind of industrialization high-energy lithium iron phosphate material of this example, is characterized in that described method comprises:
A. in ball mill, add lithium salts, molysite, microcosmic salt mixing, wherein Li:Fe:P mol ratio is 1.01:1:1, add the polyethylene glycol of mass percent 10% and the nickel nitrate of 1% again, solution gross mass is 400kg, carry out first time wet ball grinding, survey its particle diameter 600nm-1200nm by MalvernMS2000 laser particle analyzer, after ball milling completes, taking-up is for subsequent use;
B. after repeating to add in ball mill and mixing with the lithium salts of step a identical type, equal in quality, molysite, microcosmic salt, add again and the polyethylene glycol of step a identical type, equal in quality and nickel nitrate, solution gross mass is 400kg, carry out second time wet ball grinding, survey its particle diameter 50nm-500nm by MalvernMS2000 laser particle analyzer, after ball milling completes, taking-up is for subsequent use;
C. by the slurry of step a and step b milled, mix according to mass ratio 1:1, adopt atomizer granulating and drying machine, inlet temperature is 240 DEG C, and outlet temperature is 100 DEG C, obtains spherical precursor;
D. sinter under step c being put into the nitrogen protection of gas circulating type stove, 400 DEG C of pre-burning constant temperature 5h, cool to room temperature with the furnace, obtain presintering product;
E. presintering product is carried out third time wet ball grinding, be then dried;
F. the product obtained by step e sinters 700 DEG C under nitrogen protection, and constant temperature 5h, cools to room temperature with the furnace, namely obtains high-energy lithium iron phosphate material.
Battery makes identical with embodiment 1.
Fig. 1 is the first charge-discharge curve making IFR 26650 type battery 0.2C.
Embodiment 4: the preparation method of a kind of industrialization high-energy lithium iron phosphate material of this example, is characterized in that described method comprises:
A. in ball mill, add lithium salts, molysite, microcosmic salt mixing, wherein Li:Fe:P mol ratio is 1.01:1:1, add the polyethylene glycol of mass percent 10% and the nickel nitrate of 1% again, solution gross mass is 400kg, carry out first time wet ball grinding, survey its particle diameter 600nm-1200nm by MalvernMS2000 laser particle analyzer, after ball milling completes, taking-up is for subsequent use;
B. after repeating to add in ball mill and mixing with the lithium salts of step a identical type, equal in quality, molysite, microcosmic salt, add again and the polyethylene glycol of step a identical type, equal in quality and nickel nitrate, solution gross mass is 400kg, carry out second time wet ball grinding, survey its particle diameter 50nm-500nm by MalvernMS2000 laser particle analyzer, after ball milling completes, taking-up is for subsequent use;
C. by the slurry of step a and step b milled, mix according to mass ratio 1:1.5, adopt atomizer granulating and drying machine, inlet temperature is 240 DEG C, and outlet temperature is 100 DEG C, obtains spherical precursor;
D. sinter under step c being put into the nitrogen protection of gas circulating type stove, 400 DEG C of pre-burning constant temperature 5h, cool to room temperature with the furnace, obtain presintering product;
E. presintering product is carried out third time wet ball grinding, be then dried;
F. the product obtained by step e sinters 700 DEG C under nitrogen protection, and constant temperature 5h, cools to room temperature with the furnace, namely obtains high-energy lithium iron phosphate material.
Battery makes identical with embodiment 1.
Fig. 1 is the first charge-discharge curve making IFR 26650 type battery 0.2C.
Fig. 2 is the XRD diffraction spectrogram of the present embodiment;
Fig. 3 is the curve of double curvature of the present embodiment;
Fig. 4 is the 1C charge and discharge cycles curve of the present embodiment sample IFR 26650 type battery.
The foregoing is only specific embodiments of the invention, but architectural feature of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and the change done or modification are all encompassed among the scope of the claims of the present invention.
Claims (10)
1. a preparation method for industrialization high-energy lithium iron phosphate material, is characterized in that described method comprises:
A. in ball mill, add lithium salts, molysite, phosphate mixing, wherein Li:Fe:P mol ratio is 1-1.2:1:1-1.1, then adds doping vario-property agent and carbon source, carries out first time wet ball grinding, and after ball milling completes, taking-up is for subsequent use;
B. after repeating to add in ball mill and mixing with the lithium salts of step a identical type, equal in quality, molysite, microcosmic salt, add again and the doping vario-property agent of step a identical type, equal in quality and carbon source, carry out second time wet ball grinding, after ball milling completes, taking-up is for subsequent use, and the particle diameter of twice wet ball grinding disposed slurry is different;
C. by the slurry of step a and step b milled, after the mixing of different ratios, formation presoma is dried; Or first by dry respectively for the slurry of step a and step b milled, after drying, be mixed to form presoma according to different ratios again;
D. the presoma obtained by step c carries out presintering in inertia or reducing atmosphere, cools to room temperature with the furnace after insulation, obtains presintering product;
E. presintering product is carried out third time wet ball grinding, be then dried;
F. the product obtained by step e sinters in inertia or protection of reducing atmosphere stove, cools to room temperature with the furnace, namely obtain high-energy lithium iron phosphate material after heat preservation sintering.
2. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, it is characterized in that described wet ball grinding take alcohol as medium ball milling 1-10h, first time, ball milling size controlling was at 600nm-1200nm, and second time ball milling size controlling is at 50nm-500nm; Third time, ball milling size controlling was at 50nm-1200nm, and the solid content of mechanical milling process is 15-60wt%, and mill used is situated between for zirconium silicate ball, agate ball, zirconia ball, polyurethane ball, alumina balls, the one or more combination of sphere diameter in 0.1-10mm.
3. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, is characterized in that being mixed according to the ratio of 0.5-1:1-5 with the slurry of step b milled by the slurry of step a milled in described step c.
4. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, is characterized in that described steps d pre-sintering temperature is 280-450 DEG C, insulation 2-7h; Step f sintering temperature is 550-850 DEG C, heat preservation sintering 5-20h.
5. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, it is characterized in that described dry time adopt atomizer drying-granulating, its inlet temperature is 190-250 DEG C, and outlet temperature is 100 DEG C; Equipment for Heating Processing is sealed type or gas circulating type stove, and inertia or reducing atmosphere are one or more combination in nitrogen, argon gas, hydrogen.
6. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, is characterized in that described lithium salts is one or more combinations in lithium carbonate, lithium nitrate, lithium dihydrogen phosphate, lithium acetate, lithium hydroxide, lithium phosphate, lithium oxalate, lithium chloride, lithium vanadate.
7. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, is characterized in that described phosphate is one or more combinations in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate, ammonium phosphate, ferric phosphate, phosphorus pentoxide.
8. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, is characterized in that described molysite is one or more combinations in ferric phosphate, di-iron trioxide, ferric acetate, ferric oxalate, ferric nitrate, iron chloride, ferric sulfate, ferrous sulfate, frerrous chloride.
9. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, it is characterized in that described doping vario-property agent is slaine or metal oxide, wherein slaine is the one or more combination in nickel, zinc, magnesium, titanium, copper, chromium, manganese, niobium, the carbonate of vanadium, nitrate, acetate, oxalates; Metal oxide is the one or more combination in the oxide of nickel, zinc, magnesium, titanium, copper, chromium, manganese, niobium, vanadium; Doping vario-property agent accounts for the 0.5-20% of LiFePO 4 material gross mass.
10. the preparation method of a kind of industrialization high-energy lithium iron phosphate material according to claim 1, it is characterized in that described carbon source is native graphite, Delanium, hard carbon, soft carbon, organic pyrolysis carbon source, one or more combinations of nanometer conductive material, the mass ratio that carbon source accounts for LiFePO 4 material is 0.8-20%; Organic pyrolysis carbon source is cellulose acetate, vitamin C, glucose, polyvinyl alcohol, phenolic resins, CMC, polystyrene, sucrose, fructose, polytetrafluoroethylene, epoxy resin, starch, pitch, polyacrylonitrile, polyethylene glycol, one or more combinations of polyvinylpyrrolidone; Nanometer conductive material is conductive black, Graphene, one or more combinations of nano-sized carbon microballoon.
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| CN101081696A (en) * | 2007-05-15 | 2007-12-05 | 深圳市贝特瑞电子材料有限公司 | Ferric phosphate lithium material for lithium ion powder cell and preparation method thereof |
| CN101222038A (en) * | 2008-01-31 | 2008-07-16 | 东北师范大学 | Production method of lithium ion power cell ferrous phosphate lithium composite material |
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