CN112259718A - FeVO applied to lithium secondary battery4Preparation method of/C composite material - Google Patents

FeVO applied to lithium secondary battery4Preparation method of/C composite material Download PDF

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CN112259718A
CN112259718A CN202011137235.7A CN202011137235A CN112259718A CN 112259718 A CN112259718 A CN 112259718A CN 202011137235 A CN202011137235 A CN 202011137235A CN 112259718 A CN112259718 A CN 112259718A
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fevo
composite material
mesoporous carbon
preparation
lithium secondary
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司玉昌
张紫瑞
王卫国
尹吉庆
李惠惠
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MEDICAL COLLEGE OF CAPF
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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
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/58—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 FeVO applied to a lithium secondary battery4A preparation method of the/C composite material. The preparation method comprises the following steps: taking Fe (NO) with a certain concentration3)3The solution fully soaks the mesoporous carbon material to form a mixed solution. The mixture is then added dropwise with NH in the corresponding stoichiometric ratio4VO3Reacting the solution for a period of time, drying to obtain a material precursor, and calcining the precursor to obtain FeVO4a/C composite material. ByThe material has rich pore structure and large specific surface area, so that the adsorption capacity of the material is strong. In addition, the composite material is compounded with a carbon material with excellent conductivity, so that the conductivity of the material is effectively improved, and the composite material is a good electrode material applied to a lithium secondary battery.

Description

FeVO applied to lithium secondary battery4Preparation method of/C composite material
Technical Field
The invention belongs to the technical field of preparation of electrode materials of lithium secondary batteries, and particularly relates to in-situ filling of FeVO in mesoporous carbon4Form FeVO4A preparation method of the/C composite material.
Background
With the further development of the scientific and technical level, the requirements of various devices on energy sources are continuously increased. Lithium ion batteries, as a new generation energy system, are widely used in many areas of life due to their characteristics of cleanliness, portability, high specific energy, long cycle life, etc.: military, traffic, electronic products, etc. The excellent characteristics of lithium ion batteries are mainly related to electrode materials. Usually, the specific capacity of the anode material is smaller than that of the cathode material, so that the capacities of the anode and the cathode of the lithium ion battery are not matched, and therefore, the improvement of the whole capacity of the lithium ion battery is restricted by the anode material. The development of high capacity positive electrode materials is imperative. The iron vanadium oxide is used as the anode material of the lithium secondary battery, and has potential high specific capacity due to changeable valence states of Fe and V.
Amorphous FeVO4The first discharge specific capacity of the lithium ion battery anode material is about 220mAh/g, which is more than that of the prior common lithium battery anode material (LiCoO)2About 150mAh/g, LiFePO4About 170 mAh/g) has higher specific energy. But FeVO4As an electrode material, the electrochemical property and the cycling stability are poor due to low conductivity.
Disclosure of Invention
The invention aims to solve the problem of FeVO in the prior art4Low conductivity, resulting in FeVO4The preparation method of the FeVO4/C composite material with good conductivity is provided as the electrode material with poor electrochemical property and poor cycling stability.
The preparation method of the FeVO4/C composite material applied to the lithium secondary battery comprises the steps of fully mixing the treated mesoporous carbon with a ferric nitrate solution with a certain concentration, and dropwise adding an ammonium metavanadate solution according to the stoichiometric ratio of 1:1 of the molar ratio of Fe to VCarrying out reaction to obtain a precursor material, and calcining the obtained precursor material to prepare FeVO applied to the lithium secondary battery4a/C composite material.
The preparation method comprises the following specific steps:
1) and (3) treating the mesoporous carbon material: placing 0.5-2 g of mesoporous carbon in a mortar, fully grinding into powder of 200 meshes, placing the powder into a container, vacuumizing, and draining water in gaps of the mesoporous carbon to completely open holes;
2) preparing a precursor material: 2mol/L of Fe (NO)3)3Transferring the solution into a container of a standby mesoporous carbon material, performing ultrasonic oscillation, uniformly mixing, and simultaneously turning on a vacuum pump so as to facilitate Fe (NO)3)3The solution is immersed into the pores of the mesoporous carbon as much as possible, and NH with corresponding stoichiometric ratio is added dropwise4VO3The molar ratio of Fe to V in the reaction is 1:1, the reaction is continued until the reaction is complete, the mixed solution is taken out, and the mixed solution is evaporated to dryness at the temperature of 60-120 ℃ to obtain a precursor material;
3) finally FeVO is carried out4Preparation of the/C composite material: placing the precursor material obtained in the step 2) in a vacuum environment, heating to 300-550 ℃ at a heating rate of 3 ℃/min, calcining at high temperature for 24 hours, washing with ethanol and deionized water, and drying to obtain a product FeVO4a/C composite material.
The invention has the advantages and beneficial effects that:
1) the method adopts an in-situ growth mode to fill FeVO into mesoporous carbon4Form FeVO4The electrochemical performance of the/C composite material is improved by improving the conductivity of the/C composite material, and the FeVO is prepared by in-situ infiltration, mixing and calcination of mesoporous carbon, ferric nitrate and ammonium metavanadate serving as raw materials4the/C composite material is FeVO generated in situ in mesoporous carbon4The nano-grade is realized, and the high conductivity of the mesoporous carbon is beneficial to improving the conductivity of the mesoporous carbon so as to improve the cycle performance of the mesoporous carbon.
2)FeVO4the/C composite material has rich pore structure and large specific surface area (144 m)2/g) to make it stronger in adsorption capacity and able to accommodate more lithiumIons, FeVO4The first discharge specific capacity of the/C composite material is 249 mAh/g. In addition, the introduction of the mesoporous carbon can improve the conductivity of the material, and FeVO can be obtained after 40-week circulation4The capacity of the/C composite material can still reach 228 mAh/g.
3) The material prepared by the invention has rich pore structures and larger specific surface area, so that the adsorption capacity of the material is stronger. The composite material is compounded with carbon material with excellent conductivity, so that the conductivity of the material is effectively improved, and the composite material is a good electrode material applied to a lithium secondary battery.
Drawings
FIG. 1 shows FeVO generated in situ under different atmospheres according to example 1 of the present invention4C and Fe2VO4XRD of the/C composite material, wherein curve a is FeVO generated in situ in air atmosphere4a/C composite material, b, generating Fe in situ under Ar atmosphere2VO4a/C composite material.
FIG. 2(a), FIG. 2(b), FIG. 2(c), FIG. 2(d), FIG. 2(e) and FIG. 2(f) are FeVO obtained in example 2 of the present invention4Scanning electron microscope and transmission electron microscope images of the/C composite material and the mesoporous carbon, wherein, figure 2(a) is a low-power Scanning Electron Microscope (SEM) image of the mesoporous carbon, and figure 2(b) is FeVO4Scanning Electron Microscope (SEM) of low magnification of/C composite material, Transmission Electron Microscope (TEM) of mesoporous carbon in FIG. 2(C), and FeVO in FIG. 2(d)4Transmission electron micrograph (SEM) of/C composite, FIG. 2(e) high-magnification transmission electron micrograph (HR-TEM) of mesoporous carbon, FIG. 2(f) FeVO4High power transmission electron microscopy (HR-TEM) of the/C composite.
FIGS. 3(a) and 3(b) show FeVO obtained in example 2 of the present invention4Pore diameter distribution diagram of/C composite material and mesoporous carbon and N2Absorption/desorption curve, in which, FIG. 3(a) FeVO4The pore diameter distribution diagram of the/C composite material and the mesoporous carbon is shown in FIG. 3(b) FeVO4N of/C composite material and mesoporous carbon2Adsorption/desorption curves.
FIG. 4 shows FeVO obtained in example 3 of the present invention4AC impedance spectrum and equivalent circuit diagram of the/C composite material.
FIG. 5 shows FeVO obtained in example 3 of the present invention4Comparative graph of cycle performance of the/C composite.
Detailed Description
To better illustrate the invention, the following examples are given to further illustrate the invention without limiting its scope.
Example 1
1) Treating a mesoporous carbon material: 2g of mesoporous carbon is placed in an agate mortar and fully ground into 200-mesh powder, and the powder is placed in a flat-bottomed flask for vacuum-pumping treatment. And (4) pumping water in the mesoporous carbon gaps to completely open the pores.
2) Preparing a precursor: 2mol/L of Fe (NO)3)3Transferring the solution into a flat-bottomed flask of a standby mesoporous carbon material, carrying out ultrasonic oscillation, and uniformly mixing. At the same time, the vacuum pump is turned on, so that Fe (NO)3)3The solution is immersed into the pores of the mesoporous carbon as much as possible. Dropwise adding 2mol/L NH4VO3And (4) continuing the reaction until the reaction is completed. Taking out the mixed solution, and evaporating to dryness at 60 ℃ to obtain a precursor material. Wherein the atomic ratio of Fe to V is 1: 1.
3)FeVO4preparation of the/C composite material: respectively heating the precursor obtained in the step 2) to 550 ℃ at the heating rate of 3 ℃/min in vacuum and air environments, calcining the precursor at high temperature for 24 hours, washing the calcined precursor with ethanol and deionized water, and drying the washed precursor overnight to obtain a product FeVO4a/C composite material.
FIG. 1 is the in situ generation of FeVO4And calcining the/C composite material at 550 ℃ for 24 hours, wherein a is calcining under an air atmosphere, and b is calcining under the protection of an Ar atmosphere. Firstly FeVO4the/C composite material is burned for 24 hours at 550 ℃ in the air, the product is a, and the product a in the figure is consistent with a standard card JCPDS 38-1372 and corresponds to a triclinic FeVO4(C reacts with oxygen in the air at about 350 ℃ to generate gas to escape). The synthesized composite material is considered to be FeVO4A composite material of/C. If FeVO is to be added4Calcining the/C composite material at 550 ℃ for 24 hours under the protection of inert gas, wherein the product is b in the figure, and the product b is consistent with the JCPDS 75-1519 standard card and corresponds to cubic Fe2VO4Crystal (C and FeVO)4A reduction reaction is carried out at a high temperature to convert Fe3+Reduction ofIs Fe2 +，V5+Reduction to V4+). Therefore, too high temperature is not favorable for FeVO4And (4) generating.
Example 2
1) Treating a mesoporous carbon material: 0.5g of mesoporous carbon is placed in an agate mortar and fully ground into 200-mesh powder, and the powder is placed in a flat-bottomed flask for vacuum-pumping treatment. And (4) pumping water in the mesoporous carbon gaps to completely open the pores.
2) Preparing a precursor: 2mol/L of Fe (NO)3)3Transferring the solution into a flat-bottomed flask of a standby mesoporous carbon material, carrying out ultrasonic oscillation, and uniformly mixing. At the same time, the vacuum pump is turned on, so that Fe (NO)3)3The solution is immersed into the pores of the mesoporous carbon as much as possible. Dropwise adding 2mol/L NH4VO3And (4) continuing the reaction until the reaction is completed. And taking out the mixed solution, and evaporating to dryness at the temperature of 60-120 ℃ to obtain a precursor material. Wherein the atomic ratio of Fe to V is 1: 1.
3)FeVO4preparation of the/C composite material: heating the precursor obtained in the step 2) to 300-550 ℃ at a heating rate of 3 ℃/min in a vacuum environment, calcining the precursor at a high temperature for 24 hours, washing the calcined precursor with ethanol and deionized water, and drying the washed precursor overnight to obtain a product FeVO4a/C composite material.
As can be seen from the SEM image 2(a) of the mesoporous carbon in fig. 2, the pore distribution of the mesoporous carbon is uniform and regular, and the black part in the TEM image 2(c) is the pore wall, and the gray part is the large mesopores. The carbon material has large and medium pores of dozens of nanometers, the surface of particles has rich large pores of about 100nm, the thickness of the pore wall is about 10nm, and a plurality of small through holes exist on mesoporous carbon particles, thereby being beneficial to the filling of substances and the charging and discharging. FeVO prepared in situ from 300 DEG C4As can be seen in SEM2(b) and TEM2(d) of the/C composite, the pores of the carbon particles became blurred, and FeVO was not seen4Agglomeration and growth of particles, possibly prepared FeVO4Has been embedded into mesoporous carbon to form FeVO4a/C composite material. Fig. 2(e) in fig. 2 is a high power transmission electron microscope (HR-TEM) image of the mesoporous carbon, and the one-dimensional pore structure of the mesoporous carbon can be clearly seen. From the comparison between FIG. 2(e) and FIG. 2(f) of the high power transmission electron microscopeTo see that the in situ generated FeVO4Black due to the density greater than that of carbon, highly dispersed in the mesoporous matrix, further proving the in-situ generated FeVO4Is uniformly embedded into the mesoporous carbon.
FIG. 3(a) shows mesoporous carbon and FeVO measured by the BET method, in addition to SEM and TEM4The pore diameter distribution diagram of the/C composite material is shown by comparison, when FeVO4After the mesoporous carbon is filled, the aperture of the material is obviously reduced. The specific surface area of the mesoporous carbon material is 645m calculated from the adsorption and desorption curve of FIG. 3(b)2Per g, total pore volume of 0.47cm3(ii) in terms of/g. While the specific surface area of the composite material is reduced to 144m2(g), total pore volume decreased to 0.28cm3(ii) in terms of/g. And analysis of fig. 3(b) shows that the amount of micropores and mesopores of the composite material is significantly reduced. This indicates that FeVO4Better deposited in the mesoporous carbon in the in-situ generation process. The newly generated nano FeVO is enabled to be rich in mesoporous carbon pore structure, large in specific surface area and strong in adsorption capacity4The particles enter the interior of the mesoporous carbon material, so that the specific surface area of the mesoporous carbon is reduced, and the aperture is reduced. The above results show that: FeVO4the/C composite material has rich pore structure and large specific surface area (144 m)2/g) to make it stronger in adsorption capacity.
Example 3
1) Treating a mesoporous carbon material: weighing 10% and 0% of mesoporous carbon by mass, fully grinding the mesoporous carbon into 200-mesh powder in an agate mortar, and putting the powder into a flat-bottomed flask for vacuumizing treatment. And (4) pumping water in the mesoporous carbon gaps to completely open the pores.
2) Preparing a precursor: 1mol/L of Fe (NO)3)3Transferring the solution into a flat-bottomed flask of the standby mesoporous carbon, carrying out ultrasonic oscillation, and uniformly mixing. At the same time, the vacuum pump is turned on, so that Fe (NO)3)3The solution is immersed into the pores of the mesoporous carbon as much as possible. Adding 1mol/L NH dropwise4VO3And (4) continuing the reaction until the reaction is completed. And taking out the mixed solution, and evaporating to dryness at the temperature of 80 ℃ to obtain a precursor material. Preferably, the atomic ratio of Fe to V is 1: 1.
3)FeVO4preparation of the/C composite material:heating the precursor obtained in the step 2) to 300 ℃ at a heating rate of 3 ℃/min in an air environment, calcining the precursor at a high temperature for 24 hours, washing the calcined precursor with ethanol and deionized water, and drying the washed precursor to obtain a product FeVO4a/C composite material.
FIG. 4 is FeVO4And FeVO4Electrochemical impedance spectroscopy and equivalent circuit diagrams of the/C composite. As can be seen from the figure, the impedance spectrum consists of a semicircle and a diagonal line. FeVO4The intercept obtained by the intersection point of the semicircle and the real axis of the high-frequency region of the/C composite material is due to Li+The impedance produced during migration in the electrolyte solution is expressed as solution resistance Rs; the semi-circular arc radius of the high-frequency region is smaller, so that very small charge transfer impedance is indicated, the conductivity of the composite material is increased, the charge transfer is facilitated, and the electrochemical performance is better indicated.
FIG. 5 is FeVO at 300 ℃4And FeVO4And the electrochemical performance of the/C composite material is compared. As can be seen from the figure, FeVO is observed at 300 DEG C4The specific capacity and the cycling stability of the/C composite material are both obvious advantages. The first discharge specific capacity is 249mAh/g, the second cycle is 248mAh/g, and the capacity after 40-week circulation is 228 mAh/g. The specific capacity remained substantially stable from cycle 30. FeVO4the/C composite material utilizes the template effect of the large mesoporous carbon to realize the nanocrystallization of filler particles, and simultaneously, the high conductivity of the mesoporous carbon is beneficial to improving the conductivity, thereby increasing the utilization rate of active substances.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. While the invention has been described with respect to the above embodiments, it will be understood by those skilled in the art that the invention is not limited to the above embodiments, which are described in the specification and illustrated only to illustrate the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (4)

1. FeVO applied to lithium secondary battery4The preparation method of the/C composite material is characterized by comprising the following specific preparation steps:
1) processing the mesoporous carbon material;
2) preparing a precursor material; mixing the treated mesoporous carbon with ferric nitrate (Fe (NO)3)3) The solution is fully mixed, then ammonium metavanadate solution is dropwise added according to the stoichiometric ratio of Fe to V of 1:1 for reaction to obtain precursor material,
3) finally FeVO is carried out4Preparation of the/C composite material: preparing FeVO applied to lithium secondary battery by calcining precursor material4a/C composite material.
2. FeVO for lithium secondary battery according to claim 14The preparation method of the/C composite material is characterized in that the treatment method of the mesoporous carbon comprises the following steps: the mesoporous carbon is placed in an agate mortar and fully ground into powder of 200 meshes, the powder is placed in a container for vacuumizing treatment, moisture in gaps of the mesoporous carbon is pumped to dryness, and the holes are completely opened.
3. FeVO for lithium secondary battery according to claim 14The preparation method of the/C composite material is characterized in that the specific preparation method of the precursor material comprises the following steps: 2mol/L of Fe (NO)3)3Transferring the solution into a container of a standby mesoporous carbon material, performing ultrasonic oscillation, uniformly mixing, and simultaneously turning on a vacuum pump so as to facilitate Fe (NO)3)3The solution is immersed into the pores of the mesoporous carbon as much as possible, and NH with corresponding stoichiometric ratio is added dropwise4VO3And (3) the molar ratio of Fe to V in the reaction is 1:1, the reaction is continued until the reaction is completed, the mixed solution is taken out, and the mixed solution is evaporated to dryness at the temperature of 60-120 ℃ to obtain a precursor material.
4. FeVO for lithium secondary battery according to claim 14The preparation method of the/C composite material is characterized in that the calcination method of the precursor material comprises the following steps: putting the obtained precursor material in a vacuum ringIn the environment, the temperature is raised to 300-550 ℃ at the heating rate of 3 ℃/min for high-temperature calcination for 12-24 hours, and the product FeVO is obtained after washing and drying by ethanol and deionized water4a/C composite material.
CN202011137235.7A 2020-10-22 2020-10-22 FeVO applied to lithium secondary battery4Preparation method of/C composite material Pending CN112259718A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102891300A (en) * 2012-09-24 2013-01-23 上海锦众信息科技有限公司 Method for manufacturing mesoporous carbon composite material of lithium battery
CN106356510A (en) * 2016-10-13 2017-01-25 中南大学 Preparation method for Li-ion anode material FeVO4/C
CN111689524A (en) * 2020-04-28 2020-09-22 青海民族大学 Lithium ion battery material FeVO4Process for producing microparticles

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102891300A (en) * 2012-09-24 2013-01-23 上海锦众信息科技有限公司 Method for manufacturing mesoporous carbon composite material of lithium battery
CN106356510A (en) * 2016-10-13 2017-01-25 中南大学 Preparation method for Li-ion anode material FeVO4/C
CN111689524A (en) * 2020-04-28 2020-09-22 青海民族大学 Lithium ion battery material FeVO4Process for producing microparticles

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RJ01 Rejection of invention patent application after publication

Application publication date: 20210122

RJ01 Rejection of invention patent application after publication