CN111082010A - Positive electrode material and preparation method and application thereof - Google Patents

Positive electrode material and preparation method and application thereof Download PDF

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CN111082010A
CN111082010A CN201911299377.0A CN201911299377A CN111082010A CN 111082010 A CN111082010 A CN 111082010A CN 201911299377 A CN201911299377 A CN 201911299377A CN 111082010 A CN111082010 A CN 111082010A
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precursor
lithium
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positive electrode
electrode material
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屈杨
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Hefei Guoxuan Kehong New Energy Technology Co ltd
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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 positive electrode material and a preparation method and application thereof, and the preparation method comprises the following steps: adding iron source, lithium source and carbon source into the mixture6H9Obtaining slurry in NO) n dispersion liquid, grinding the slurry and drying to obtain a precursor I, and mixing the precursor I with β -LiAl (SiO)3)2Mixing to obtain a precursor II; and carrying out solid-phase sintering on the precursor II under a protective atmosphere, and crushing and grading to obtain the anode material. The anode material prepared by the method has high compaction density and long cycle life.

Description

Positive electrode material and preparation method and application thereof
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a positive electrode material as well as a preparation method and application thereof.
Background
The lithium ion battery has the advantages of high specific energy, high power density, long cycle life, environmental friendliness, no pollution and the like, and is widely applied to electric vehicles, unmanned aerial vehicles, smart phones, notebook computers, camcorders, electronic cigarettes, intelligent wearable electronic products and other electric equipment. The performance of the lithium ion battery is determined by taking the anode material, the cathode material, the diaphragm and the electrolyte as four key materials of the lithium ion battery, wherein the performance of the lithium ion battery is also determined by taking the anode material as one of the most key materials in the lithium ion battery.
The common lithium ion battery anode material is generalThe lithium ion battery positive electrode material mainly comprises lithium cobaltate, lithium manganate, lithium nickel manganese oxide, lithium iron phosphate and the like. With the continuous upgrading and upgrading of electric automobiles and electronic products, the requirements on batteries are also continuously improved. In the manufacturing process of the lithium ion power battery, the compaction density has a great influence on the battery performance, generally, the greater the compaction density is, the higher the capacity of the battery with the same specification is, so the compaction density is also considered as one of the reference indexes of the energy density of the material. Generally, under the conditions of fixed specification and model of the battery and fixed process conditions, the higher the compaction density is, the higher the capacity of the single battery is, the higher the mass specific energy density is, and the lower the unit comprehensive cost of the battery is. However, most of lithium iron phosphate materials in the current market have low compaction density which can only reach 2.1-2.3 g/cm3And generally, the cycle life thereof shows a downward trend as the capacity of the battery increases.
Disclosure of Invention
In view of the above, the present invention is necessary to provide a positive electrode material, a preparation method and applications thereof, which are prepared by introducing (C)6H9NO) n to obtain a lithium iron phosphate precursor with uniform carbon coating, and then β -LiAl (SiO) is introduced3)2The prepared anode material has high compaction density and long cycle life, and solves the technical problems of low compaction density and poor cycle life of the conventional lithium iron phosphate material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a positive electrode material comprises the following steps:
adding an iron source, a lithium source and a carbon source (C)6H9NO) n dispersion liquid to obtain slurry;
grinding the slurry and then drying to obtain a precursor I;
mixing the precursor I with β -LiAl (SiO)3)2Mixing to obtain a precursor II;
and carrying out solid-phase sintering on the precursor II under a protective atmosphere, and crushing and grading to obtain the anode material.
Further, said (C)6H9NO) n dispersion is prepared by mixing (C)6H9NO) n in pure water, wherein (C) is a homogeneous dispersion6H9NO) n has a value of n of 3000-4000.
Further, the iron source is selected from at least one of ferric orthophosphate and ferric phosphate dihydrate, the lithium source is selected from at least one of lithium carbonate, lithium chloride and lithium sulfate, and the carbon source is selected from at least one of glucose, sucrose and citric acid.
Further, the iron source is FePO4The lithium source is Li2CO3The carbon source is C6H12O6Said FePO4、Li2CO3、C6H12O6In a molar ratio of 1.95:1:0.165, C6H12O6And (C) described6H9The mass ratio of NO) n is 1 (0.4-0.5).
Further, the particle size D50 of the ground slurry is 400 nm.
Further, the precursors I and β -LiAl (SiO)3)2The mass ratio of (A) to (B) is 1: 0.003.
Further, the protective atmosphere comprises one of nitrogen, argon and hydrogen; the sintering temperature of the solid phase sintering is 650-730 ℃, the sintering time is 8-10h, and the heating rate is 5 ℃/min.
Further, the particle size distribution of the pulverization classification was 0.28 μm in terms of D10, 1.0 μm in terms of D50, and 7.6 μm in terms of D100.
The invention also provides a positive electrode material prepared by the preparation method.
The third purpose of the invention is to provide the application of the cathode material in the preparation of lithium ion batteries.
Compared with the prior art, the invention has the following beneficial effects:
the invention introduces (C) in the preparation process of precursor6H9NO)n，(C6H9NO) n performs the dual functions of a dispersant and a coating carbon source, so that the prepared phosphorusThe iron lithium precursor has uniform carbon coating and excellent coating quality, and β -LiAl (SiO) is introduced before the precursor is sintered3)2，β-LiAl(SiO3)2Has dual functions of sintering aid and surface coating, and the precursor is mixed with β -LiAl (SiO)3)2After mixing, on one hand, the grain size growth during sintering is promoted, and the material compaction density is improved; and on the other hand, the material is coated on the surface, so that the structure of the material is stabilized to prolong the cycle life of the material.
In addition, the invention introduces β -LiAl (SiO)3)2The lithium iron phosphate anode material is modified, so that the high-temperature solid phase sintering temperature and the high-temperature solid phase sintering time in the preparation process of the lithium iron phosphate material are reduced, the energy consumption is reduced, the production efficiency is improved, and the production cost is greatly reduced.
Drawings
FIG. 1 is a charge and discharge curve of a battery made of a positive electrode material according to an example of the present invention and a comparative example;
FIG. 2 is a cycle curve of a battery made of the positive electrode material according to the example of the present invention and the comparative example;
fig. 3 is SEM images of the positive electrode materials prepared in example 1 of the present invention and comparative example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description of specific embodiments. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention firstly discloses a preparation method of a positive electrode material, which comprises the following steps:
adding an iron source, a lithium source and a carbon source (C)6H9NO) n dispersion liquid to obtain slurry;
grinding the slurry and then drying to obtain a precursor I;
mixing the precursor I with β -LiAl (SiO)3)2Mixing to obtain a precursor II;
and carrying out solid-phase sintering on the precursor II under a protective atmosphere, and crushing and grading to obtain the anode material.
Lithium iron phosphate is one of the most studied lithium ion anode materials at present, and is generally prepared by mixing an iron source, a lithium source and a carbon source to prepare a precursor, and sintering the precursor. In the present invention, by adding an iron source, a lithium source, a carbon source to (C)6H9NO) n dispersion, grinding and drying to obtain carbon-coated precursor I, and (C)6H9NO) n dispersion liquid plays a role of a dispersing agent, so that a carbon coating layer on the surface of the precursor I is uniform and excellent in quality, and further, the precursor I and β -LiAl (SiO)3)2After mixing, precursor II is obtained, which is then subjected to solid phase sintering, β -LiAl (SiO)3)2On one hand, the precursor I can be coated again, and on the other hand, the sintering aid also has the function of promoting the grain size growth during sintering and improving the material compaction density. The iron source may be at least one selected from iron orthophosphate and iron phosphate dihydrate, the lithium source may be at least one selected from lithium carbonate, lithium chloride and lithium sulfate, and the carbon source may be at least one selected from glucose, sucrose and citric acid, and it is understood that the selection of the iron source, the lithium source and the carbon source is a conventional choice for preparing lithium iron phosphate cathode materials in the art, and the above is only used for example, and the selection includes but is not limited to the above.
Further aspect, said (C)6H9NO) n dispersion is prepared by mixing (C)6H9NO) n in pure water, and in some embodiments of the invention, the (C) is6H9NO) n has a value of n of 3000-4000.
Further, in some embodiments of the present invention, the iron source is selected from at least one of ferric orthophosphate and ferric phosphate dihydrate, the lithium source is selected from at least one of lithium carbonate, lithium chloride and lithium sulfate, and the carbon source is selected from at least one of glucose, sucrose and citric acid.
It can be understood that the selection of the proportional relationship can be adjusted according to the composition of the lithium iron phosphate cathode material to be finally prepared, and therefore, the selection is not particularly limited. In some embodiments of the invention, the iron source is FePO4The lithium source is Li2CO3The carbon source is C6H12O6Said FePO4、Li2CO3、C6H12O6In a molar ratio of 1.95:1:0.165, C6H12O6And (C) described6H9The mass ratio of NO) n is 1 (0.4-0.5).
Preferably, the particle size D50 of the slurry after grinding is 400 nm.
Further, in some embodiments of the present invention, the precursors I and β -LiAl (SiO)3)2The mass ratio of (A) to (B) is 1: 0.003.
In a further aspect, the precursor ii is subjected to solid-phase sintering in a protective atmosphere, where the protective atmosphere is mainly used to enable the precursor ii to be sintered under the condition of isolating oxygen, so as to ensure the performance of the finally prepared cathode material.
Further, in some embodiments of the present invention, the sintering temperature of the solid phase sintering is 650-730 ℃, the sintering time is 8-10h, and the temperature rising rate is 5 ℃/min.
Further, the particle size distribution of the pulverization classification was 0.28 μm in terms of D10, 1.0 μm in terms of D50, and 7.6 μm in terms of D100.
The embodiment of the invention also provides a positive electrode material prepared by the preparation method. The positive electrode material has high compaction density and long cycle life, so that the lithium ion battery prepared from the positive electrode material has high energy density and good cycle performance, the lithium ion battery mainly comprises the positive electrode material, the positive electrode material is prepared by the preparation method, and the specific preparation process and other materials of the lithium ion battery are not specifically limited.
The technical scheme of the invention is further clearly and completely explained by combining specific embodiments.
Example 1
Mixing 116g (C)6H9NO)4000Adding into 5kg pure water, stirring to obtain dispersion, adding 3kg FePO into the dispersion4、0.74kg Li2CO3And 0.29kg of C6H12O6Fully and uniformly stirring and grinding to obtain mixed slurry with D50 being 400 nm;
drying the mixed slurry to obtain a precursor I of the lithium iron phosphate, and mixing the precursor I with β -LiAl (SiO)3)2The mass ratio of the precursor I to 12.5g of β -LiAl (SiO)3)2Uniformly mixing to obtain a precursor II, and placing the precursor II in N2Solid-phase sintering at 700 deg.C for 9h under atmosphere, pulverizing and grading to obtain LFP/C/β -LiAl (SiO)3)2The particle size distribution of the lithium iron phosphate positive electrode material is D10 ═ 0.28 μm, D50 ═ 1.0 μm, and D100 ═ 7.6 μm.
Example 2
140g of (C)6H9NO)3000Adding into 5kg pure water, stirring to obtain dispersion, and adding 2.9kg FePO into the dispersion4、0.74kg Li2CO3And 0.28kg of C6H12O6Fully and uniformly stirring and grinding to obtain mixed slurry with D50 being 433 nm;
drying the mixed slurry to obtain a precursor I of the lithium iron phosphate, and mixing the precursor I with β -LiAl (SiO)3)2The mass ratio of the precursor I to 13.8g of β -LiAl (SiO)3)2Uniformly mixing to obtain a precursor II, and placing the precursor II in N2Solid-phase sintering at 700 ℃ under atmosphere 9Pulverizing and grading after h to obtain the product with the composition of LFP/C/β -LiAl (SiO)3)2The particle size distribution of the lithium iron phosphate positive electrode material is 0.33 μm in D10, 1.2 μm in D50, and 8.4 μm in D100.
Comparative example 1
3kg FePO4、0.74kg Li2CO3And 0.3kg of C6H12O6Adding 5kg of pure water, fully stirring uniformly, and grinding to obtain mixed slurry with D50 being 503 nm;
drying the mixed slurry to obtain a precursor of the lithium iron phosphate, and placing the precursor in N2Solid-phase sintering at 770 deg.C for 12h in atmosphere, pulverizing and grading to obtain LFP/C/β -LiAl (SiO)3)2The particle size distribution of the lithium iron phosphate positive electrode material is 0.24 μm in terms of D10, 1.61 μm in terms of D50, and 8.7 μm in terms of D100.
Comparative example 2
Mixing 116g (C)6H9NO)4000Adding into 5kg pure water, stirring to obtain dispersion, adding 3kg FePO into the dispersion4、0.74kgLi2CO3And 0.29kg of C6H12O6Fully and uniformly stirring and grinding to obtain mixed slurry with D50 being 400 nm;
drying the mixed slurry to obtain a precursor of the lithium iron phosphate, and placing the precursor in N2After solid-phase sintering at 700 ℃ for 9h in the atmosphere, the lithium iron phosphate positive electrode material with the composition of LFP/C is prepared by crushing and grading, and the particle size distribution is that D10 is 0.28 mu m, D50 is 1.0 mu m, and D100 is 7.6 mu m.
Comparative example 3
3kg of FePO were added4、0.74kg Li2CO3And 0.29kg of C6H12O6Adding 5kg of pure water, fully stirring uniformly, and grinding to obtain mixed slurry with D50 being 400 nm;
drying the mixed slurry to obtain a precursor I of the lithium iron phosphate, and mixing the precursor I with β -LiAl (SiO)3)2The mass ratio of the precursor I to 12.5g of β -LiAl (SiO)3)2Uniformly mixing to obtain a precursor II, and mixing the precursor IIIn N2Solid-phase sintering at 700 deg.C for 9h under atmosphere, pulverizing and grading to obtain LFP/β -LiAl (SiO)3)2The particle size distribution of the lithium iron phosphate positive electrode material is D10 ═ 0.28 μm, D50 ═ 1.0 μm, and D100 ═ 7.6 μm.
The positive electrode materials obtained in examples 1-2 and comparative examples 1-3 were mixed with SP, KS-6 and PVDF in a proportion of 96%: 1.5%: 0.5%: after 2% of slurry is mixed, the slurry is coated on a carbon-coated aluminum foil current collector and matched with the same graphite cathode to prepare a full battery with the same specification and model, and the anode materials in the embodiment and the comparative example and the full battery prepared from the anode materials are respectively subjected to correlation performance tests, and the results are shown in table 1, fig. 1 and fig. 2. The cathode materials in example 1 and comparative example 1 were subjected to SEM characterization at the same time, and the results are shown in fig. 3.
TABLE 1 results of the related tests
Figure BDA0002321477740000061
Figure BDA0002321477740000071
From the test results in table 1 and fig. 1 and 2, it can be seen that the lithium iron phosphate materials with high specific energy and long service life prepared in examples 1 and 2 have higher 1C specific discharge capacity and higher compaction density, and in combination with fig. 3, it can be seen that the positive electrode material in example 1 has a larger grain size, so that a full battery with the same model has higher capacity and energy density, the energy density of the battery reaches above 185.5Wh/kg, and the capacity retention rate of the battery after 3000 cycles is greater than 88.5%, while the energy density and cycle performance of the battery prepared from the ordinary lithium iron phosphate material not prepared by the present invention are relatively poor.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The preparation method of the cathode material is characterized by comprising the following steps of:
adding an iron source, a lithium source and a carbon source (C)6H9NO) n dispersion liquid to obtain slurry;
grinding the slurry and then drying to obtain a precursor I;
reacting the precursor I withβ-LiAl(SiO3)2Mixing to obtain a precursor II;
and carrying out solid-phase sintering on the precursor II under a protective atmosphere, and crushing and grading to obtain the anode material.
2. The method according to claim 1, wherein (C) is6H9NO) n dispersion is prepared by mixing (C)6H9NO) n in pure water, wherein (C) is a homogeneous dispersion6H9NO) n has a value of n of 3000-4000.
3. The method according to claim 1, wherein the iron source is at least one selected from the group consisting of iron orthophosphate and iron phosphate dihydrate, the lithium source is at least one selected from the group consisting of lithium carbonate, lithium chloride and lithium sulfate, and the carbon source is at least one selected from the group consisting of glucose, sucrose and citric acid.
4. The method of claim 1, wherein the iron source is FePO4The lithium source is Li2CO3The carbon source is C6H12O6Said FePO4、Li2CO3、C6H12O6In a molar ratio of 1.95:1:0.165, C6H12O6And (C) described6H9The mass ratio of NO) n is 1 (0.4-0.5).
5. The method of claim 1, wherein the particle size D50 of the slurry after grinding is 400 nm.
6. The method of claim 1, wherein the precursor I is mixed withβ-LiAl(SiO3)2The mass ratio of (A) to (B) is 1: 0.003.
7. The method of claim 1, wherein the protective atmosphere comprises one of nitrogen, argon, hydrogen; the sintering temperature of the solid phase sintering is 650-730 ℃, the sintering time is 8-10h, and the heating rate is 5 ℃/min.
8. The method of claim 1, wherein the size distribution of the comminuted fraction is D10=0.28 μm, D50=1.0 μm, D100=7.6 μm.
9. A positive electrode material produced by the production method according to any one of claims 1 to 8.
10. Use of the positive electrode material according to claim 9 for the preparation of lithium ion batteries.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101955175A (en) * 2010-07-15 2011-01-26 北京中新联科技股份有限公司 Industrial preparation method for lithium iron phosphate
CN102148367A (en) * 2010-02-08 2011-08-10 江西省金锂科技有限公司 Method for preparing lithium-ion battery anode material of lithium iron phosphate
CN103531794A (en) * 2013-10-28 2014-01-22 金瑞新材料科技股份有限公司 Lithium ion battery positive material lithium ferrous phosphate and preparation method
CN108878799A (en) * 2018-04-24 2018-11-23 广东邦普循环科技有限公司 A kind of doping type monocrystalline tertiary cathode material and preparation method thereof of mesoporous lithium aluminosilicate cladding

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102148367A (en) * 2010-02-08 2011-08-10 江西省金锂科技有限公司 Method for preparing lithium-ion battery anode material of lithium iron phosphate
CN101955175A (en) * 2010-07-15 2011-01-26 北京中新联科技股份有限公司 Industrial preparation method for lithium iron phosphate
CN103531794A (en) * 2013-10-28 2014-01-22 金瑞新材料科技股份有限公司 Lithium ion battery positive material lithium ferrous phosphate and preparation method
CN108878799A (en) * 2018-04-24 2018-11-23 广东邦普循环科技有限公司 A kind of doping type monocrystalline tertiary cathode material and preparation method thereof of mesoporous lithium aluminosilicate cladding

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