CN109004207B - Composite lithium iron phosphate cathode material and preparation method thereof - Google Patents

Composite lithium iron phosphate cathode material and preparation method thereof Download PDF

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CN109004207B
CN109004207B CN201810713326.7A CN201810713326A CN109004207B CN 109004207 B CN109004207 B CN 109004207B CN 201810713326 A CN201810713326 A CN 201810713326A CN 109004207 B CN109004207 B CN 109004207B
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iron phosphate
lithium iron
nitrogen
composite lithium
doped carbon
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CN109004207A (en
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李磊
张祥功
周思思
吴军
代化
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
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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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • 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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  • Electrochemistry (AREA)
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Abstract

The invention discloses a compositeThe lithium iron phosphate anode material is characterized in that the surface of the lithium iron phosphate material is modified with nitrogen-doped carbon, and the molecular formula of the lithium iron phosphate anode material is represented as LiFePO4(iii)/NC; the invention also discloses a preparation method of the composite lithium iron phosphate anode material, which is prepared by mixing LiFePO4Adding the solid into dilute hydrochloric acid for ultrasonic dispersion, and then cleaning for multiple times by using ultrapure water; to the ultrasonically dispersed LiFePO4Adding resorcinol, cysteine, ethanol and ammonia water into the aqueous solution; adding formaldehyde solution, washing the precipitate with deionized water and ethanol, and drying; calcining for 3-10 hours at 500-800 ℃ under the protection of nitrogen to obtain a final finished product of the nitrogen-doped carbon composite lithium iron phosphate cathode material; the method is simple and feasible, and finished products are saved; the introduction of the nitrogen-doped carbon can greatly improve the stability of the lithium iron phosphate anode material in the using process and solve the problem of low conductivity so as to meet the performance requirements of the current electric automobile and energy source direction on the lithium ion battery.

Description

Composite lithium iron phosphate cathode material and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery anodes, and particularly relates to a nitrogen-doped carbon layer modified lithium iron phosphate anode material and a preparation method thereof.
Background
Lithium ion batteries are widely used in electronic devices in daily life due to their excellent energy density, good rate performance and cycle life. As an important component of the lithium ion battery, the research and development of the anode material largely determine the performance of the lithium ion battery.
Therefore, the development of a lithium ion battery cathode material with high specific capacity, good cycle performance and high safety is the focus of the current lithium ion battery research. Lithium ion anode material mostly adopts lithium intercalation transition metalCompared with other similar anode materials, the olivine type lithium iron phosphate material has great advantages in the aspects of safety, cycle life and the like. But the electron conductivity and Li of pure lithium iron phosphate material+The diffusion coefficient is poor, the electrochemical performance of the composite material is seriously influenced, and the further application of the composite material is limited. The electrochemical performance of the lithium iron phosphate material is improved mainly by nano preparation, cation doping and carbon compounding of the lithium iron phosphate material. Among them, carbon recombination is the most effective means. The carbon compounding can not only improve the conductivity of the lithium iron phosphate material, but also avoid the agglomeration of the lithium iron phosphate material in the circulation process. More importantly, through the compounding of the carbon material, lithium ions can be more easily removed and embedded from the lithium iron phosphate material in the using process.
And researches show that the carbon material doped with nitrogen can obviously improve the active site of electrochemical reaction and break through the energy barrier of ion migration, thereby effectively improving the electrical property of the material.
Disclosure of Invention
The invention aims to solve the problems of poor conductivity and easy agglomeration of a lithium iron phosphate material in the using process, and designs a composite lithium iron phosphate positive electrode material and a preparation method thereof. The method is characterized in that resorcinol and formaldehyde are used as a carbon source, cysteine is used as a nitrogen source, and the lithium iron phosphate material is modified and modified. The method is simple and feasible, and saves finished products; the introduction of the nitrogen-doped carbon can greatly improve the stability of the lithium iron phosphate anode material in the using process, solve the problem of low conductivity and meet the performance requirements of the current electric automobile and energy direction on the lithium ion battery.
The technical scheme adopted by the invention for solving the technical problems is as follows: a composite lithium iron phosphate anode material and a preparation method thereof are provided, wherein nitrogen-doped carbon is modified on the surface of the lithium iron phosphate material by a coating means, and the molecular formula of the nitrogen-doped carbon is represented as LiFePO4/NC。
The invention also discloses a preparation method of the composite lithium iron phosphate anode material, which comprises the following steps:
(1) mixing LiFePO4Adding the solid into dilute hydrochloric acid for ultrasonic dispersion, and then washing with ultrapure water for multiple times；
(2) To the ultrasonically dispersed LiFePO4Adding resorcinol, cysteine, ethanol and ammonia water into the aqueous solution, heating to 25-60 ℃, and stirring for 8-12 hours;
(3) adding a formaldehyde solution, keeping the temperature, continuously stirring for 6-20 hours, cleaning the precipitate with deionized water and ethanol, and drying;
(4) and (4) calcining the material obtained in the step (3) for 3-10 hours at 500-800 ℃ under the protection of nitrogen to obtain a final nitrogen-doped carbon composite lithium iron phosphate cathode material finished product.
The concentration of the dilute hydrochloric acid in the step (1) is 0.01 mol/L.
The volume ratio of distilled water to ethanol in the ultrasonic dispersion in the step (2) is 2: 1, the mass ratio of resorcinol to cysteine is 2: 1; the reactant is put into a water bath kettle for temperature adjustment.
The stirring mode in the step (2) and the step (3) is magnetic stirring.
The step (3) comprises the following steps:
(31) adding the reaction solution obtained in the step (2) into a formaldehyde solution, keeping the temperature, continuously stirring for 6-20 hours, and naturally cooling the precipitate to room temperature after the reaction is finished;
(32) then, washing and centrifuging the precipitate for multiple times by using deionized water and ethanol;
(33) the obtained material was placed in a vacuum drying oven and vacuum dried at 60 ℃ for 24 hours.
The step (4) comprises the following steps:
(41) grinding the material obtained in the step (3);
(42) then transferring the ceramic boat into a ceramic boat, placing the ceramic boat into a tube furnace, introducing nitrogen for half an hour, heating the ceramic boat to 500-800 ℃ at a speed of 5 ℃/min under the protection of the nitrogen, and calcining the material for 3-10 hours;
(43) and after the calcination is finished, cooling to room temperature under the nitrogen protection condition, and grinding the obtained material again to obtain a finished product of the nitrogen-doped carbon composite lithium iron phosphate cathode material.
The invention has the beneficial effects that:
compared with the existing preparation process of the lithium iron phosphate cathode material, the preparation method provided by the invention is simple to operate, strong in implementability and good in repeatability. The nitrogen-doped carbon layer compounded on the lithium iron phosphate material is an amorphous carbon material, and the introduction of the nitrogen-doped carbon material can effectively reduce the dissolution of electrolyte to the lithium iron phosphate anode material, improve the stability of the lithium iron phosphate material in the circulation process, effectively accelerate the electron conduction rate of the lithium iron phosphate material, reduce the ion migration distance, improve the rate capability of the anode material and reduce the internal resistance of the material. Meanwhile, the carbon material is doped with nitrogen elements, so that active sites of electrochemical reaction can be obviously improved, energy barriers of ion migration can be reduced, and the electrical property of the material is further improved. The high-performance lithium ion battery anode material prepared by the invention is expected to be widely applied to the field of automobile power batteries.
Drawings
Fig. 1 shows an X-ray diffraction pattern of the nitrogen-doped carbon composite lithium iron phosphate positive electrode material.
Fig. 2 shows scanning electron microscope and transmission electron microscope photographs of the nitrogen-doped carbon composite lithium iron phosphate cathode material.
Fig. 3 is an energy spectrum analysis diagram of the nitrogen-doped carbon composite lithium iron phosphate cathode material.
Fig. 4 is a charge-discharge curve diagram of a nitrogen-doped carbon composite lithium iron phosphate positive electrode material 1C.
Fig. 5 is a graph showing the multiplying power performance of the nitrogen-doped carbon composite lithium iron phosphate positive electrode material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention discloses a composite lithium iron phosphate anode material, wherein nitrogen-doped carbon is modified on the surface of the lithium iron phosphate material by a coating means, and the molecular formula of the material is represented as LiFePO4/NC。
The invention also discloses a preparation method of the composite lithium iron phosphate anode material, which comprises the following steps:
(1) mixing LiFePO4Adding the solid into a dilute solution with the concentration of 0.01mol/LIn a hydrochloric acid solution, the materials are uniformly dispersed through ultrasonic treatment; and then, centrifuging, washing with ultrapure water for multiple times until the solution is neutral, modifying with dilute hydrochloric acid to increase active functional groups on the surfaces of the lithium iron phosphate particles, and dispersing the material obtained by centrifuging into 50mL of ultrapure water.
(2) To the ultrasonically dispersed LiFePO4Adding absolute ethyl alcohol into the aqueous solution (ultrasonic dispersion is carried out in the aqueous solution), adding resorcinol, cysteine and ammonia water under magnetic stirring, placing the beaker into a water bath kettle, adjusting the temperature of the water bath, heating to 25-60 ℃, and carrying out magnetic stirring for 8-12 hours.
(3) Adding the reaction solution obtained in the step (2) into a formaldehyde solution, keeping the temperature, continuing to magnetically stir for 6-20 hours, and naturally cooling the precipitate to room temperature after the reaction is finished; collecting black precipitates, then washing and centrifuging for multiple times by using deionized water and absolute ethyl alcohol; the obtained material was placed in a vacuum drying oven and vacuum dried at 60 ℃ for 24 hours.
(4) Grinding the material obtained in the step (3); then transferring the ceramic boat into a ceramic boat, placing the ceramic boat into a tube furnace, introducing nitrogen for half an hour, heating the ceramic boat to 500-800 ℃ at a speed of 5 ℃/min under the protection of the nitrogen, and calcining the material for 3-10 hours; and after the calcination is finished, cooling to room temperature under the nitrogen protection condition, and grinding the obtained material again to obtain a finished product of the nitrogen-doped carbon composite lithium iron phosphate cathode material.
The volume ratio of the ammonia water to the ethanol in the step (2) is 2: 1, the mass ratio of resorcinol to cysteine is 2: 1; adding resorcinol as carbon source of nitrogen-doped carbon, adding cysteine as nitrogen source of nitrogen-doped carbon, and placing the reactant in a water bath for temperature adjustment.
And (3) the formaldehyde added in the step (3) is also used as a carbon source of nitrogen-doped carbon.
The X-ray diffraction pattern, the scanning electron microscope and the transmission electron microscope photo of the nitrogen-doped carbon composite lithium iron phosphate anode material obtained by the preparation method disclosed by the invention are shown in the figures 1 and 2. The XRD spectrogram shows that the obtained sample is single homogeneous olivine structure LiFePO4(JCPDs number 83-2092). And no other impurity peak appears in the XRD spectrogram, which indicates that the nitrogen-doped carbon has an amorphous structure. As can be seen from FIG. 2, the prepared material is mostly spherical, the particle size distribution of the particles is wide, and the outer surface of the composite is very smooth by modification with nitrogen-doped carbon. From fig. 3, the EDS spectrum can see the presence of Fe, O, C, P, N elements, indicating that N elements can enter the carbon layer by doping through this synthesis method.
The obtained nitrogen-doped carbon composite lithium iron phosphate anode material is analyzed through XRD, SEM and EDS respectively, and is assembled with a lithium sheet to form a half cell for testing and analyzing the electrochemical performance of the material. The method comprises the following steps of uniformly mixing a synthesized nitrogen-doped carbon composite lithium iron phosphate material serving as an active substance of a positive electrode of a test battery, SP serving as a conductive agent and PVDF serving as a binder according to a ratio of 8:1:1 to prepare a positive plate; taking a metal lithium sheet as a negative electrode sheet, a diaphragm as a Celgard 2400 polypropylene microporous membrane, and electrolyte as 1mol/LiPF6V (EC + DME) (volume ratio 1: 1). And assembling the process CR 2025 button cell in an inert gas glove box, and performing electrical performance test by using Land CT2001, wherein the test voltage range is 2.4-4V, and the rate performance test is performed for five weeks at 0.1C, 0.5C, 1C, 2C and 0.1C respectively.
And (3) preparing the obtained nitrogen-doped carbon composite lithium iron phosphate anode material into a button cell, and charging and discharging at the rate of 1C between 2.4V and 4V. As shown in fig. 4, during charging, the voltage plateau appears at around 3.5V; during discharging, the platform appears near 3.4V, and the charging and discharging platform is very flat, and the corresponding capacity is 134 mAh/g. As shown in fig. 5, the specific capacities of the materials at 0.1C, 0.5C, 1C and 2C were 152.9 mAh/g, 147.1mAh/g, 134mAh/g and 127.6 mAh/g, respectively, showing good discharge rate performance. After the discharge at a large rate, the discharge capacity returns to 0.1C for charge and discharge, and the discharge capacity returns to the initial value and good stability can be maintained. Therefore, the nitrogen-doped carbon composite lithium iron phosphate cathode material has good electrochemical performance and can be used as a novel lithium ion battery cathode material.
Comparative example 1
The comparative example is similar to the procedure of example 1 except that no cysteine was added in step 2.
The test result shows that the obtained material has good structural stability and dimensional consistency. Electrochemical performance tests show that the gram capacity and rate capability of the material are reduced compared with those of the samples obtained in the examples.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.

Claims (5)

1. The preparation method of the composite lithium iron phosphate anode material is characterized in that nitrogen-doped carbon is modified on the surface of the lithium iron phosphate material by a coating means to obtain the lithium iron phosphate anode material with the molecular formula of LiFePO4The positive electrode material of/NC comprises the following steps:
(1) mixing LiFePO4Adding the solid into dilute hydrochloric acid for ultrasonic dispersion, and then cleaning for multiple times by using ultrapure water;
(2) to the ultrasonically dispersed LiFePO4Adding resorcinol, cysteine, ethanol and ammonia water into the aqueous solution, heating to 25-60 ℃, and stirring for 8-12 hours;
(3) adding a formaldehyde solution, keeping the temperature, continuously stirring for 6-20 hours, cleaning the precipitate with deionized water and ethanol, and drying;
(4) and (4) calcining the material obtained in the step (3) for 3-10 hours at 500-800 ℃ under the protection of nitrogen to obtain a final nitrogen-doped carbon composite lithium iron phosphate cathode material finished product.
2. The method for preparing the composite lithium iron phosphate cathode material according to claim 1, wherein the concentration of the dilute hydrochloric acid in the step (1) is 0.01 mol/L.
3. The preparation method of the composite lithium iron phosphate cathode material according to claim 1, wherein the stirring manner in the steps (2) and (3) is magnetic stirring.
4. The preparation method of the composite lithium iron phosphate positive electrode material according to claim 1, wherein the step (3) comprises the following steps:
(31) adding the reaction solution obtained in the step (2) into a formaldehyde solution, keeping the temperature, continuously stirring for 6-20 hours, and naturally cooling the precipitate to room temperature after the reaction is finished;
(32) then, washing and centrifuging the precipitate for multiple times by using deionized water and ethanol;
(33) the obtained material was placed in a vacuum drying oven and vacuum dried at 60 ℃ for 24 hours.
5. The preparation method of the composite lithium iron phosphate positive electrode material according to claim 1, wherein the step (4) comprises the following steps:
(41) grinding the material obtained in the step (3);
(42) then transferring the ceramic boat into a ceramic boat, placing the ceramic boat into a tube furnace, introducing nitrogen for half an hour, heating the ceramic boat to 500-800 ℃ at a speed of 5 ℃/min under the protection of the nitrogen, and calcining the material for 3-10 hours;
(43) and after the calcination is finished, cooling to room temperature under the nitrogen protection condition, and grinding the obtained material again to obtain a finished product of the nitrogen-doped carbon composite lithium iron phosphate cathode material.
CN201810713326.7A 2018-06-29 2018-06-29 Composite lithium iron phosphate cathode material and preparation method thereof Active CN109004207B (en)

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CN115050945B (en) * 2022-07-15 2023-09-22 湖北工业大学 Preparation method of biomass nitrogen-doped carbon-coated lithium-rich lithium iron phosphate positive electrode material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106129337A (en) * 2016-06-27 2016-11-16 华中农业大学 A kind of preparation method of cathode of lithium iron phosphate lithium ion battery electrode
CN106207169A (en) * 2016-08-05 2016-12-07 宁波江东仑斯福环保科技有限公司 A kind of preparation method of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106129337A (en) * 2016-06-27 2016-11-16 华中农业大学 A kind of preparation method of cathode of lithium iron phosphate lithium ion battery electrode
CN106207169A (en) * 2016-08-05 2016-12-07 宁波江东仑斯福环保科技有限公司 A kind of preparation method of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode

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