CN113264514A - Preparation method of lithium ion battery anode material lithium iron phosphate - Google Patents
Preparation method of lithium ion battery anode material lithium iron phosphate Download PDFInfo
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- CN113264514A CN113264514A CN202110533193.7A CN202110533193A CN113264514A CN 113264514 A CN113264514 A CN 113264514A CN 202110533193 A CN202110533193 A CN 202110533193A CN 113264514 A CN113264514 A CN 113264514A
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- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- 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
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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
- 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
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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
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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
Abstract
The invention discloses a preparation method of lithium iron phosphate as a lithium ion battery cathode material, which comprises the steps of adding a lithium source, an iron source, a phosphorus source and a carbon source into deionized water according to a molar ratio, ultrasonically dissolving, adding a complexing agent to obtain a gel substance, freeze-drying in a liquid nitrogen environment, adding the gel substance into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing a cleaned copper plate into the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate with a film coated in a certain thickness; and placing the obtained coated copper plate in a tubular furnace, introducing nitrogen, heating to 400-450 ℃, keeping the temperature for 1-2 h, heating to 700-800 ℃, keeping the temperature for 2-3 h, cooling, dropwise adding N-methyl pyrrolidone, carrying out vacuum drying, placing the product obtained in the step S3 in a magnetron sputtering device, sputtering the product on the coated copper plate obtained in the step S3 by using a conductive agent Super-C and a binder PVDF as magnetron sputtering targets, dropwise adding N-methyl pyrrolidone again after sputtering is finished, and carrying out vacuum drying to obtain the cathode material lithium iron phosphate.
Description
Technical Field
The invention belongs to the technical field of lithium ion secondary battery materials, and particularly relates to a preparation method of a lithium ion battery anode material lithium iron phosphate.
Background
Lithium ion batteries have been rapidly developed since their advent as new green batteries. The development and application of the anode material of the lithium ion battery at present mainly comprise lithium cobaltate, lithium manganate, ternary materials and lithium iron phosphate, wherein the lithium iron phosphate has the characteristics of good safety, excellent cycle performance, low cost and the like, and meanwhile, the material has wide raw material sources,environment-friendly, stable material structure, outstanding cycling stability and the like, thereby being widely applied in the fields of electric vehicles, energy storage, standby power supplies and the like. LiFePO is synthesized at present4The method mainly comprises a high-temperature solid-phase synthesis method, a hydrothermal synthesis method, a liquid-phase precipitation method, a sol-gel method and the like. The lithium iron phosphate material prepared by the high-temperature solid phase method has the advantages that due to the irregular shape of the raw materials and the limitation of reaction conditions, the particle morphology of the synthesized material is difficult to control, the particle size is large, the particle size distribution of the material is uneven, and the influence on the consistency of the material is large. The hydrothermal synthesis method, the liquid-phase precipitation method, the sol-gel method and other liquid-phase methods have the advantages that the raw materials are mixed at a molecular level, the synthesis temperature is low, the roasted product particles are fine and uniform in size, the size distribution range is narrow, and the method is incomparable to a solid-phase method. But has the following disadvantages: the preparation process is complex, the raw materials are generally applied excessively, so that the resource waste is caused, the cost is increased, the environmental protection problem is caused, and meanwhile, the problems of lattice defects and the like are easily caused due to low temperature.
Disclosure of Invention
The invention aims to provide a preparation method of lithium iron phosphate serving as a lithium ion battery cathode material, which comprises the following steps:
s1: adding a lithium source, an iron source, a phosphorus source and a carbon source into deionized water according to a molar ratio of (1-2) to (0.96-2.12) to (1.15-2.45) to (1.85-3.96), carrying out ultrasonic stirring to fully dissolve the lithium source, the iron source, the phosphorus source and the carbon source, then adding a complexing agent, carrying out magnetic stirring for 5-10 hours, and standing for 20-30 hours to obtain a gel substance for later use.
S2: and (5) freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate into the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain the copper plate with a film coated at a certain thickness.
S3: and (4) placing the coated copper plate obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 400-450 ℃ at a speed of 2-3 ℃/min, preserving heat at the temperature for 1-2 h, heating to 700-800 ℃ at a speed of 5-10 ℃/min, preserving heat for 2-3 h, cooling, dropwise adding N-methylpyrrolidone, and drying in vacuum for later use.
S4: and (3) placing the product obtained in the step (S3) into a magnetron sputtering device, sputtering the product on the copper plate with the coating obtained in the step (S3) by using a conductive agent Super-C and a binder PVDF in a mass ratio of 1 (0.65-1) as a magnetron sputtering target material, dropwise adding N-methylpyrrolidone again after the sputtering is finished, and drying in vacuum to obtain the cathode material lithium iron phosphate.
Further, the lithium source is selected from any one of lithium carbonate, lithium hydroxide, lithium acetate, lithium sulfate, lithium chloride or lithium nitrate.
Further, the iron source is selected from any one of ferric nitrate, ferric sulfate, ferric acetate, ferric chloride, ferric phosphate or ferrous oxalate.
Further, the phosphorus source is selected from any one of ammonium dihydrogen phosphate, ammonium phosphate and phosphoric acid.
Further, the carbon source is selected from any one of sucrose, citric acid and glucose.
Further, the thickness of the coating film on the copper plate in the step S2 is 0.2-1.6 mm.
Further, in the step S2, the sputtering power of magnetron sputtering is 350-400W, the sputtering time is 3-8 h, the local vacuum degree is 5.2-6 Pa, and the target-substrate distance is 40-50 mm.
Further, the sputtering power of the magnetron sputtering in the step S4 is 300-340W, the sputtering time is 2-3 h, the local vacuum degree is 4.5-4.9 Pa, and the target-substrate distance is 35-40 mm; the thickness of the magnetron sputtering coating is 0.1-0.5 mm.
Further, the complexing agent is oxalic acid or ammonia water.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, firstly, a lithium source, an iron source, a phosphorus source and a carbon source are prepared into a gel substance, a powder obtained after freeze drying is coated on a copper plate through magnetron sputtering, a binder and a conductive agent are sputtered after calcination by a two-stage method, and finally the obtained lithium iron phosphate as the lithium ion battery anode material has the advantages of uniform granularity, small particle size, good crystallinity, and good discharge capacity and cycle stability after testing.
Drawings
Fig. 1 is an SEM image of the cathode material lithium iron phosphate prepared in example 1 of the present invention;
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of lithium iron phosphate as a positive material of a lithium ion battery specifically comprises the following steps:
s1: adding lithium carbonate, ferric nitrate, ammonium dihydrogen phosphate and sucrose into deionized water according to the molar ratio of 1:0.96:1.15:1.85, performing ultrasonic stirring to fully dissolve the lithium carbonate, the ferric nitrate, the ammonium dihydrogen phosphate and the sucrose, then adding oxalic acid, performing magnetic stirring for 5 hours, and standing for 20 hours to obtain a gel substance for later use.
S2: freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate in the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate coated with a certain thickness, wherein the thickness of the coating film formed on the copper plate by magnetron sputtering is 0.2 mm; the sputtering power of magnetron sputtering is 350W, the sputtering time is 3h, the local vacuum degree is 5.2Pa, and the target-substrate distance is 40 mm.
S3: and (4) placing the copper plate subjected to film coating obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 400 ℃ at a speed of 2 ℃/min, preserving heat at the temperature for 1h, heating to 700 ℃ at a speed of 5 ℃/min, preserving heat for 2h, cooling, dropwise adding N-methyl pyrrolidone, and drying in vacuum for later use.
S4: placing the product obtained in the step S3 into a magnetron sputtering device, sputtering the product on the copper plate with the coating film obtained in the step S3 by taking a conductive agent Super-C and a binder PVDF in a mass ratio of 1:0.65 as magnetron sputtering targets, dropwise adding N-methylpyrrolidone again after sputtering, and drying in vacuum to obtain the cathode material lithium iron phosphate; wherein the sputtering power of magnetron sputtering is 300W, the sputtering time is 2h, the local vacuum degree is 4.5Pa, and the target-substrate distance is 35 mm; the thickness of the magnetron sputtering coating is 0.1 mm.
Example 2
A preparation method of lithium iron phosphate as a positive material of a lithium ion battery specifically comprises the following steps:
s1: adding lithium hydroxide, ferric sulfate, ammonium phosphate and citric acid into deionized water according to the molar ratio of 1.3:1.36:1.54:2.38, carrying out ultrasonic stirring to fully dissolve the lithium hydroxide, the ferric sulfate, the ammonium phosphate and the citric acid, then adding ammonia water, carrying out magnetic stirring for 8h, and standing for 25h to obtain a gelatinous substance for later use.
S2: freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate in the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate coated with a certain thickness, wherein the thickness of the coating film formed on the copper plate by magnetron sputtering is 0.6 mm; the sputtering power of magnetron sputtering is 380W, the sputtering time is 5h, the local vacuum degree is 5.5Pa, and the target-substrate distance is 45 mm.
S3: and (4) placing the copper plate subjected to film coating obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 420 ℃ at a speed of 2.5 ℃/min, preserving heat at the temperature for 1.5h, heating to 700-800 ℃ at a speed of 6 ℃/min, preserving heat for 2.5h, cooling, dropwise adding N-methyl pyrrolidone, and drying in vacuum for later use.
S4: placing the product obtained in the step S3 into a magnetron sputtering device, sputtering the product on the copper plate with the coating film obtained in the step S3 by taking a conductive agent Super-C and a binder PVDF in a mass ratio of 1:0.8 as a magnetron sputtering target material, dropwise adding N-methylpyrrolidone again after sputtering is finished, and drying in vacuum to obtain the anode material lithium iron phosphate; wherein the sputtering power of magnetron sputtering is 320W, the sputtering time is 2.5h, the local vacuum degree is 4.7Pa, and the target-substrate distance is 38 mm; the thickness of the magnetron sputtering coating is 0.2 mm.
Example 3
A preparation method of lithium iron phosphate as a positive material of a lithium ion battery specifically comprises the following steps:
s1: adding lithium acetate, iron acetate, phosphoric acid and glucose into deionized water according to the molar ratio of 1.7:2.05:2.36:3.85, carrying out ultrasonic stirring to fully dissolve the lithium acetate, the iron acetate, the phosphoric acid and the glucose, then adding oxalic acid, carrying out magnetic stirring for 8 hours, and standing for 25 hours to obtain a gelatinous substance for later use.
S2: freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate in the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate coated with a certain thickness, wherein the thickness of the coating film formed on the copper plate by magnetron sputtering is 0.8 mm; the sputtering power of magnetron sputtering is 390W, the sputtering time is 7h, the local vacuum degree is 5.8Pa, and the target-substrate distance is 45 mm.
S3: and (4) placing the copper plate subjected to film coating obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 430 ℃ at a rate of 3 ℃/min, preserving heat at the temperature for 1.5h, heating to 750 ℃ at a rate of 8 ℃/min, preserving heat for 3h, cooling, dropwise adding N-methylpyrrolidone, and drying in vacuum for later use.
S4: placing the product obtained in the step S3 into a magnetron sputtering device, sputtering the product on the copper plate with the coating film obtained in the step S3 by taking a conductive agent Super-C and a binder PVDF in a mass ratio of 1:0.9 as a magnetron sputtering target material, dropwise adding N-methylpyrrolidone again after sputtering is finished, and drying in vacuum to obtain the anode material lithium iron phosphate; wherein the sputtering power of magnetron sputtering is 330W, the sputtering time is 2.5h, the local vacuum degree is 4.8Pa, and the target-substrate distance is 38 mm; the thickness of the magnetron sputtering coating is 0.3 mm.
Example 4
A preparation method of lithium iron phosphate as a positive material of a lithium ion battery specifically comprises the following steps:
s1: adding lithium sulfate, ferric chloride, ammonium dihydrogen phosphate and citric acid into deionized water according to the molar ratio of 2:2.12:2.45:3.96, performing ultrasonic stirring to fully dissolve the lithium sulfate, the ferric chloride, the ammonium dihydrogen phosphate and the citric acid, then adding ammonia water, performing magnetic stirring for 10 hours, and standing for 30 hours to obtain a gel substance for later use.
S2: freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate in the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate coated with a certain thickness, wherein the thickness of the coating film formed on the copper plate by magnetron sputtering is 1.6 mm; the sputtering power of magnetron sputtering is 400W, the sputtering time is 8h, the local vacuum degree is 6Pa, and the target-substrate distance is 50 mm.
S3: and (4) placing the coated copper plate obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 450 ℃ at a rate of 3 ℃/min, preserving the heat at the temperature for 1-2 h, then heating to 700-800 ℃ at a rate of 10 ℃/min, preserving the heat for 3h, cooling, dropwise adding N-methylpyrrolidone, and carrying out vacuum drying for later use.
S4: placing the product obtained in the step S3 into a magnetron sputtering device, sputtering the product on the copper plate with the coating obtained in the step S3 by taking a conductive agent Super-C and a binder PVDF in a mass ratio of 1:1 as magnetron sputtering targets, dropwise adding N-methylpyrrolidone again after sputtering is finished, and drying in vacuum to obtain the cathode material lithium iron phosphate; wherein the sputtering power of magnetron sputtering is 340W, the sputtering time is 3h, the local vacuum degree is 4.9Pa, and the target-substrate distance is 40 mm; the thickness of the magnetron sputtering coating is 0.5 mm.
And (3) performance testing: the button cell assembled by the lithium iron phosphate as the positive electrode material obtained in examples 1-4 was tested for electrochemical performance with a current density of 1C, wherein the test results are shown in Table 1,
table 1. test results:
as can be seen from table 1, the first discharge specific capacities of the lithium iron phosphate as the cathode material prepared in embodiments 1 to 4 of the present invention at a current density of 0.1C are all above 168.3mAh/g, the coulombic efficiency is still above 98.8%, the lowest charge transfer resistance can reach 65.7 Ω, the discharge specific capacity is still 158.9mAh/g after 100 cycles of cycling, and the coulombic efficiency is 83.8%, which indicates that the lithium iron phosphate as the cathode material prepared in the present invention has good discharge specific capacity and cycling stability.
Claims (9)
1. A preparation method of lithium iron phosphate as a positive material of a lithium ion battery is characterized by comprising the following steps:
s1: adding a lithium source, an iron source, a phosphorus source and a carbon source into deionized water according to a molar ratio of (1-2): (0.96-2.12): (1.15-2.45): (1.85-3.96), carrying out ultrasonic stirring to fully dissolve the lithium source, the iron source, the phosphorus source and the carbon source, then adding a complexing agent, carrying out magnetic stirring for 5-10 h, and standing for 20-30 h to obtain a gel substance for later use;
s2: freeze-drying the gel-like substance in the step S1 in a liquid nitrogen environment, adding the dried powder into a sputtering magnetron sputtering device to be used as a magnetron sputtering target material, placing the cleaned copper plate into the sputtering magnetron sputtering device, and sputtering under the protection of argon to obtain a copper plate with a film coated at a certain thickness;
s3: placing the coated copper plate obtained in the step S2 in a tube furnace, introducing nitrogen, starting to heat to 400-450 ℃ at a speed of 2-3 ℃/min, preserving heat at the temperature for 1-2 h, then heating to 700-800 ℃ at a speed of 5-10 ℃/min, preserving heat for 2-3 h, cooling, dropwise adding N-methylpyrrolidone, and drying in vacuum for later use;
s4: and (3) placing the product obtained in the step (S3) into a magnetron sputtering device, sputtering the product on the copper plate with the coating obtained in the step (S3) by using a conductive agent Super-C and a binder PVDF in a mass ratio of 1 (0.65-1) as a magnetron sputtering target material, dropwise adding N-methylpyrrolidone again after the sputtering is finished, and drying in vacuum to obtain the cathode material lithium iron phosphate.
2. The method for preparing lithium iron phosphate as a positive electrode material of a lithium ion battery according to claim 1, wherein the lithium source is selected from any one of lithium carbonate, lithium hydroxide, lithium acetate, lithium sulfate, lithium chloride and lithium nitrate.
3. The method for preparing the lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the iron source is selected from any one of ferric nitrate, ferric sulfate, ferric acetate, ferric chloride, ferric phosphate or ferrous oxalate.
4. The method for preparing the lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the phosphorus source is selected from any one of ammonium dihydrogen phosphate, ammonium phosphate and phosphoric acid.
5. The method for preparing the lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the carbon source is selected from any one of sucrose, citric acid and glucose.
6. The method for preparing lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the thickness of the coating film formed on the copper plate by magnetron sputtering in the step S2 is 0.2-1.6 mm.
7. The method for preparing lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the sputtering power of the magnetron sputtering in the step S2 is 350-400W, the construction time is 3-8 h, the local vacuum degree is 5.2-6 Pa, and the target-substrate distance is 40-50 mm.
8. The method for preparing lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the sputtering power of the magnetron sputtering in the step S4 is 300-340W, the sputtering time is 2-3 h, the local vacuum degree is 4.5-4.9 Pa, and the target-substrate distance is 35-40 mm; the thickness of the magnetron sputtering coating is 0.1-0.5 mm.
9. The method for preparing the lithium iron phosphate as the positive electrode material of the lithium ion battery according to claim 1, wherein the complexing agent is oxalic acid or ammonia water.
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| CN104409734A (en) * | 2014-12-26 | 2015-03-11 | 北京化工大学 | Lithium iron phosphate battery positive material prepared by using microwave-assisted sol-gel method |
| CN106898733A (en) * | 2017-03-24 | 2017-06-27 | 安庆师范大学 | A kind of preparation method of lithium iron phosphate cathode material pole piece |
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| WO2009003093A1 (en) * | 2007-06-26 | 2008-12-31 | Tiax, Llc | Metal phosphate compounds and batteries containing the same |
| US20110229764A1 (en) * | 2010-03-19 | 2011-09-22 | Semiconductor Energy Laboratory Co., Ltd. | Power storage device and manufacturing method thereof |
| CN102306777A (en) * | 2011-08-30 | 2012-01-04 | 广州市云通磁电有限公司 | Positive electrode sheet of lithium iron phosphate type lithium ion battery, and preparation method thereof |
| CN103579623A (en) * | 2013-11-12 | 2014-02-12 | 上海冠旗电子新材料股份有限公司 | Preparation method of nano-level lithium iron phosphate electrode material |
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