CN111710839A - Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material - Google Patents

Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material Download PDF

Info

Publication number
CN111710839A
CN111710839A CN202010477633.7A CN202010477633A CN111710839A CN 111710839 A CN111710839 A CN 111710839A CN 202010477633 A CN202010477633 A CN 202010477633A CN 111710839 A CN111710839 A CN 111710839A
Authority
CN
China
Prior art keywords
sfac
lithium ion
ion battery
moo
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010477633.7A
Other languages
Chinese (zh)
Other versions
CN111710839B (en
Inventor
杜锐
石张延
余传柏
李靖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin University of Technology
Original Assignee
Guilin University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guilin University of Technology filed Critical Guilin University of Technology
Priority to CN202010477633.7A priority Critical patent/CN111710839B/en
Publication of CN111710839A publication Critical patent/CN111710839A/en
Application granted granted Critical
Publication of CN111710839B publication Critical patent/CN111710839B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • 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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 Fe3O4‑MoO2A preparation method of a @ SFAC lithium ion battery cathode material belongs to the technical field of lithium ion batteries. The preparation method comprises the following steps: 1) cleaning and shearing sisal fibers into small segments, and carrying out pretreatment on the sisal fibers, including carbonization and hydrothermal reaction to obtain SFAC; 2) weighing an iron source, a molybdenum source, a complexing agent, a buffering agent and sisal fiber activated carbon powder subjected to hydrothermal treatment, adding the obtained mixture into deionized water for dissolution, uniformly mixing, transferring the obtained product into a reaction kettle, and placing the reaction kettle in an air-blast drying oven for water treatmentCarrying out thermal reaction, filtering, cleaning, drying and calcining a sample obtained after the reaction is finished to obtain Fe3O4‑MoO2The material is a cathode material of a @ SFAC lithium ion battery. The lithium ion battery cathode material prepared by the invention has excellent electrochemical performance, higher specific capacity and good cycling stability.

Description

Fe3O4-MoO2@ SFAC lithium ionPreparation method of cell cathode material
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of lithium ion batteries, in particular to Fe3O4-MoO2A preparation method of a @ SFAC lithium ion battery cathode material.
[ background of the invention ]
In the modern society, with the development of microelectronic technology in the twenty-first century, the increasing number of miniaturized devices has put higher demands on energy storage devices. The lithium ion battery is an ideal energy storage device in the 21 st century due to the characteristics of small volume, light weight, small self-discharge and the like. However, the traditional negative electrode material graphite of the lithium ion battery cannot meet the increasing demands of people due to the defects of lower theoretical specific capacity, poorer rate capability and too low charge and discharge platform.
The biomass charcoal material is used as a novel lithium ion battery cathode material, has the characteristics of low price, easy obtaining and environmental friendliness, and the theoretical specific capacity of the material is higher than that of the traditional cathode material graphite.
Transition metal oxides (e.g. Fe)2O3、Fe4O3、CuO、NiO、MoO2、MoO3Etc.) are attracting more and more attention of researchers due to higher theoretical specific capacity and better safety. But the lithium ion battery is easy to generate fragmentation and pulverization due to larger volume change in the lithium extraction and insertion process, so that part of active substances lose effective electric contact in the circulation process, the capacity of the active substances is gradually attenuated, and the circulation stability is poor. Therefore, how to improve the cycling stability of the transition metal oxide negative electrode material while keeping the high specific capacity characteristic becomes the key point for realizing the practical application of the negative electrode material. At present, two methods can be mainly used for solving the problem, one is to prepare a nano active material, increase the specific surface area of the material and reduce a charge diffusion path. Secondly, the carbon material is compounded, so that the falling of the active substance is prevented, and the formed carbon coating layer can improve the conductivity of the material; but the increased capacity is not large. At present, no iron oxide or dioxygen is foundThe report of compounding molybdenum oxide and carbon material to obtain the lithium ion battery cathode material with good electrochemical performance.
[ summary of the invention ]
The invention aims at the problems and provides Fe3O4-MoO2A preparation method of a @ SFAC lithium ion battery cathode material. The lithium ion battery cathode material has excellent electrochemical performance, higher specific capacity and good cycling stability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
fe3O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material comprises the following steps:
(1) cleaning and cutting sisal fiber into small sections with the length of about 1-2cm, placing the small sections into a crucible, carbonizing the small sections in a tube furnace for 2-2.5 hours in an inert atmosphere, wherein the carbonization temperature is 700-; the resulting powder samples were further processed: putting the obtained powder sample into a forced air dryer, carrying out hydrothermal treatment for 5-6h at the temperature of 120-140 ℃, naturally cooling, washing and drying to obtain a sisal fiber activated carbon powder sample;
(2) weighing a certain amount of iron source, molybdenum source, complexing agent, buffering agent and sisal fiber activated carbon powder subjected to hydrothermal treatment, uniformly mixing, adding deionized water for dissolution, transferring into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, carrying out hydrothermal treatment for 14-18h at the temperature of 100-160 ℃, filtering, cleaning, drying and calcining a sample obtained after the reaction is finished to obtain a black powder sample, namely Fe3O4-MoO2The material is a cathode material of a @ SFAC lithium ion battery.
Preferably, the specific process of further processing the prepared powder sample in step (1) is as follows: putting 70mL of distilled water into a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying box, carrying out hydrothermal treatment at the temperature of 120-140 ℃ for 5-6h, filtering the solution after the solution is naturally cooled, washing the solution with absolute ethyl alcohol, and drying the solution in the air-blast drying box at the temperature of 80 ℃ for 12h to obtain a sisal fiber activated carbon powder sample.
Preferably, the iron source is one or more of ferric chloride, ferric nitrate, ferrous chloride and ferrous nitrate.
Preferably, the molybdenum source is one of ammonium dimolybdate, ammonium paramolybdate and ammonium tetramolybdate.
Preferably, the complexing agent is one of urea, ammonia water, citric acid, L-histidine and glycine.
Preferably, the buffer is ammonium chloride.
Preferably, the iron source, the molybdenum source, the complexing agent, the buffer and the hydrothermally treated sisal fiber activated carbon powder in the step (2) have the following mass respectively: 0.437-1.313g of iron source, 0.245-0.85g of molybdenum source, 0.2-0.6g or 3-5mL of complexing agent, 0.16-0.37g of buffering agent and 0.25-0.75g of sisal fiber activated carbon powder.
Preferably, step (2) further comprises sieving the black powder sample through a 200 mesh sieve after the calcination is completed.
Preferably, the inert atmosphere is one of nitrogen, argon and helium.
By adopting the technical scheme, the invention has the beneficial effects that:
in the present invention, iron oxide (Fe)3O4) And molybdenum dioxide (MoO)2) All have higher specific capacity and are Fe3O4The preparation method is environment-friendly, low in cost and rich in raw material source, and Fe, a molybdenum source and an SFAC material are prepared in one step by a hydrothermal method in the presence of a complexing agent and a buffering agent to ensure that Fe3O4、MoO2Compounding with SFAC to obtain a composite material in which Fe can be buffered by virtue of the abundant pore structure of the SFAC material3O4、MoO2Tension generated by volume change avoids structural collapse; on the other hand, the excellent conductivity of the SFAC material can improve Fe3O4、MoO2Thereby increasing the conductivity of Fe3O4、MoO2In the circulation ofFinally obtaining the novel lithium ion battery cathode material Fe with higher specific capacity3O4-MoO2@ SFAC composite.
Electrochemical tests show that the Fe prepared by the invention3O4-MoO2The @ SFAC lithium ion battery cathode material has higher specific capacity and good cycling stability. The highest first discharge specific capacity of the composite material can reach 961mAh/g, the first coulombic efficiency is 67.4%, the specific capacity can still reach over 380mAh/g after 30 cycles, and the capacity retention rate is 40%, which shows that Fe3O4-MoO2The @ SFAC composite material has higher specific capacity and good cycling stability.
[ description of the drawings ]
FIG. 1 is a graph of electrochemical cycle performance of composite materials obtained at different hydrothermal temperatures according to example 1 of the present invention;
FIG. 2 is a graph showing the first charge and discharge curves of the composite materials obtained in examples 2 to 4 of the present invention;
FIG. 3 is a graph comparing electrochemical cycle performance of the composite materials obtained in examples 2 to 4 of the present invention with that of SFAC materials.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Cleaning and cutting sisal fiber into small sections with the length of about 2cm, placing the small sections into a crucible, carbonizing the small sections for 2 hours in a tube furnace by taking nitrogen as protective gas, wherein the carbonizing temperature is 900 ℃, the heating rate is 3 ℃/min, after the furnace temperature is naturally cooled to the room temperature, ball-milling the obtained carbon material for 5 hours in a planetary ball mill at the rotating speed of 35r/s, and preparing a powder sample.
(2) The prepared powder samples were further processed: putting 70mL of distilled water in a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying oven, carrying out hydrothermal treatment for 6h at 140 ℃, filtering and washing the powder sample with absolute ethyl alcohol after the powder sample is naturally cooled, and drying the powder sample in the air-blast drying oven for 12h at 80 ℃ to obtain the sisal fiber activated carbon powder sample.
(3) Weighing 0.875g of ferric chloride, 0.56g of ammonium tetramolybdate, 0.4g of complexing agent urea, 0.24g of buffering agent ammonium chloride and 0.5g of hydrothermally treated sisal fiber activated carbon powder, uniformly mixing, adding the mixture into 70mL of deionized water for dissolving, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, placing the reaction kettle into the forced air drying box for hydrothermal reaction for 18h at the temperature of 100 ℃, 120 ℃, 140 ℃ and 160 ℃, naturally cooling, filtering and cleaning a sample obtained by the reaction, and drying the sample in a vacuum drying box at the temperature of 80 ℃ to obtain Fe with different hydrothermal temperatures3O4-MoO2The material is a cathode material of a @ SFAC lithium ion battery.
Preparing a battery: mixing 0.4g of the negative electrode material obtained in the step (3), 0.05g of acetylene black and 0.05g of PVDF (polyvinylidene fluoride), adding NMP (N-methyl-2-pyrrolidone) as a solvent, stirring to paste, uniformly coating on a copper foil with the thickness of 10 mu m, then putting the copper foil into an air-blowing drying oven to dry for 4h at 60 ℃, then transferring the copper foil into a vacuum drying oven to dry for 12h at 110 ℃, punching the copper foil into a 16mm circular pole piece by using a manual punching machine, taking the circular pole piece as a negative electrode, a lithium piece as a positive electrode, a microporous polypropylene film as a diaphragm, 1mol/L of LiPF6/EC (ethylene carbonate) + DMC (dimethyl carbonate) + DEC (diethyl carbonate) as an electrolyte (in which LiPF6 is a solute, the volume ratio of the solvent EC + DMC + DEC is 1:1:1), assembling a simulated button cell with the model CR2025 in a glove box filled with argon gas, after sealing, the mixture is placed in a ventilated place and kept stand for 12 hours.
Electrochemical tests were performed at room temperature using a battery tester. The current density is set to 50mA/g, and the voltage testing range is 0.01-3V.
Electrochemical tests show that as shown in figure 1, under the condition that the current density is 50mA/g, the first discharge specific volume of sisal fiber activated carbon prepared by hydrothermal method at 100 ℃ as a negative electrode materialThe highest amount, but the fastest its capacity decays. And Fe prepared by hydrothermal method at 120 DEG C3O4-MoO2The initial coulombic efficiency of the @ SFAC lithium ion battery negative electrode material is highest (58.26%), the specific capacity can still reach more than 400mAh/g after 30 cycles, and the capacity retention rate is 80.62%, which shows that Fe prepared by hydrothermal method at 120 DEG C3O4-MoO2The @ SFAC lithium ion battery cathode material has higher specific capacity and good cycling stability.
Example 2
Fe3O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material comprises the following steps:
(1) cleaning sisal fiber, cutting into small segments with the length of about 1-2cm, placing in a crucible, carbonizing for 2h in a tube furnace under nitrogen atmosphere at 900 deg.C and the heating rate of 3 deg.C/min, naturally cooling to room temperature, and ball-milling the obtained carbon material in a planetary ball mill at the rotation speed of 35r/s for 5h to obtain a powder sample;
(2) the prepared powder samples were further processed: putting 70mL of distilled water in a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying oven, carrying out hydrothermal treatment for 6h at 140 ℃, filtering and washing the powder sample with absolute ethyl alcohol after the powder sample is naturally cooled, and drying the powder sample for 12h at 80 ℃ in the air-blast drying oven to obtain a sisal fiber activated carbon powder sample (SFAC material).
(3) Weighing 0.437g of ferric chloride, 0.245g of ammonium tetramolybdate, 0.2g of complexing agent urea, 0.16g of buffering agent ammonium chloride and 0.75g of hydrothermally treated sisal fiber activated carbon powder, uniformly mixing, adding the mixture into 70mL of deionized water for dissolving, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, performing hydrothermal reaction for 18h again at 120 ℃, filtering, cleaning and drying a sample obtained after the reaction is finished, calcining the sample in air at 500 ℃ for 3 h, and sieving a black powder sample with a 200-mesh sieve after the calcination is finished to obtain a black powder sample, namely Fe3O4-MoO2The @ SFAC lithium ion battery negative electrode material is named as C-75(C-75 composite material).
Example 3
Fe3O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material comprises the following steps:
(1) cleaning sisal fiber, cutting into small segments with the length of about 1-2cm, placing in a crucible, carbonizing for 2h in a tube furnace under nitrogen atmosphere at 900 deg.C and the heating rate of 3 deg.C/min, naturally cooling to room temperature, and ball-milling the obtained carbon material in a planetary ball mill at the rotation speed of 35r/s for 5h to obtain a powder sample;
(2) the prepared powder samples were further processed: putting 70mL of distilled water in a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying oven, carrying out hydrothermal treatment for 6h at 140 ℃, filtering and washing the powder sample with absolute ethyl alcohol after the powder sample is naturally cooled, and drying the powder sample for 12h at 80 ℃ in the air-blast drying oven to obtain a sisal fiber activated carbon powder sample (SFAC material);
(3) weighing 0.875g of ferric chloride, 0.56g of ammonium tetramolybdate, 0.4g of complexing agent urea, 0.24g of buffering agent ammonium chloride and 0.5g of hydrothermally treated sisal fiber activated carbon powder, uniformly mixing, adding the mixture into 70mL of deionized water for dissolving, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, performing hydrothermal reaction for 18h again at 120 ℃, filtering, cleaning and drying a sample obtained after the reaction is finished, calcining the sample in air at 500 ℃ for 3 h, and sieving a black powder sample with a 200-mesh sieve after the calcination is finished to obtain a black powder sample, namely Fe3O4-MoO2The @ SFAC lithium ion battery negative electrode material is named as C-50(C-50 composite material).
Example 4
Fe3O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material comprises the following steps:
(1) cleaning sisal fiber, cutting into small segments with the length of about 1-2cm, placing in a crucible, carbonizing for 2h in a tube furnace under nitrogen atmosphere at 900 deg.C and the heating rate of 3 deg.C/min, naturally cooling to room temperature, and ball-milling the obtained carbon material in a planetary ball mill at the rotation speed of 35r/s for 5h to obtain a powder sample;
(2) the prepared powder samples were further processed: putting 70mL of distilled water into a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying oven, carrying out hydrothermal treatment for 6h at 140 ℃, filtering and washing the powder sample with absolute ethyl alcohol after the powder sample is naturally cooled, and drying the powder sample for 12h at 80 ℃ in the air-blast drying oven to obtain a sisal fiber activated carbon powder sample (SFAC material)
(3) Weighing 1.313g of ferric chloride, 0.85g of ammonium tetramolybdate, 0.6g of complexing agent urea, 0.37g of buffering agent ammonium chloride and 0.25g of hydrothermally treated sisal fiber activated carbon powder, uniformly mixing, adding the mixture into 70mL of deionized water for dissolving, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, performing hydrothermal reaction for 18h again at 120 ℃, filtering, cleaning and drying a sample obtained after the reaction is finished, calcining the sample in air at 500 ℃ for 3 h, and sieving a black powder sample with a 200-mesh sieve after the calcination is finished to obtain a black powder sample, namely Fe3O4-MoO2The @ SFAC lithium ion battery negative electrode material is named as C-25(C-25 composite material).
Example 5
The procedure was as in example 4 except that the complexing agent used in step (3) was changed to 3mL of aqueous ammonia.
Fe obtained in examples 2 to 4 were separately added3O4-MoO2The @ SFAC material was used as a negative electrode material to prepare an electrode, and the preparation of the electrode, the assembly of the battery and the electrochemical test were the same as those in example 1.
Electrochemical tests were performed on the electrodes assembled in examples 2 to 4, respectively. Electrochemical tests show that the three samples have excellent electrochemical performance under the condition of the current density of 50mA/g, and Fe is increased along with the increase of the content of the ferric oxide, as shown in figures 2 and 33O4-MoO2The specific capacity of the @ SFAC lithium ion battery negative electrode material is increased, and the initial coulombic efficiency is improved. Wherein the first discharge specific capacity of the C-25 composite materialThe highest specific capacity is 961mAh/g, the first coulombic efficiency is 67.4%, the specific capacity can still reach over 380mAh/g after 30 cycles, and the capacity retention rate is 40%, which shows that the C-25 composite material has higher specific capacity and good cycle stability.
Comparative example
The applicant also prepared the SFAC material separately and tested it separately as a lithium ion battery negative electrode material for battery performance to compare with the battery data of the composite materials obtained in examples 2 to 4 above.
In this comparative example, the preparation of the SFAC material was the same as that of example 2.
FIG. 3 for SFAC material and Fe3O4-MoO2The @ SFAC composite was subjected to a charge-discharge cycle performance test under the same test conditions, and it can be seen from the figure that Fe was used3O4、MoO2Compounded with SFAC materials, on the one hand, Fe can be buffered by virtue of abundant pore structure of the SFAC materials3O4、MoO2Tension generated by volume change avoids structural collapse; on the other hand, the excellent conductivity of the SFAC material can improve the conductivity of the ferric oxide, thereby improving the Fe3O4、MoO2The cycling stability of the lithium ion battery is improved, and finally the novel lithium ion battery cathode material Fe with higher specific capacity is obtained3O4-MoO2@ SFAC composite, Fe as can be seen in the figure3O4-MoO2The cycling performance of the @ SFAC composite is far superior to that of the SFAC material.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.

Claims (9)

1. Fe3O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material is characterized by comprising the following steps of:
(1) cleaning and cutting sisal fiber into small sections with the length of about 1-2cm, placing the small sections into a crucible, carbonizing the small sections in a tube furnace for 2-2.5 hours in an inert atmosphere, wherein the carbonization temperature is 700-; the resulting powder samples were further processed: putting the obtained powder sample into a forced air dryer, carrying out hydrothermal treatment for 5-6h at the temperature of 120-140 ℃, naturally cooling, washing and drying to obtain a sisal fiber activated carbon powder sample;
(2) weighing a certain amount of iron source, molybdenum source, complexing agent, buffering agent and sisal fiber activated carbon powder subjected to hydrothermal treatment, uniformly mixing, adding deionized water for dissolution, transferring into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into a forced air drying box, carrying out hydrothermal treatment for 14-18h at the temperature of 100-160 ℃, filtering, cleaning, drying and calcining a sample obtained after the reaction is finished to obtain a black powder sample, namely Fe2O3-MoO2The material is a cathode material of a @ SFAC lithium ion battery.
2. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery anode material is characterized in that the specific process of further processing the prepared powder sample in the step (1) is as follows: putting 70mL of distilled water into a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying box, carrying out hydrothermal treatment at the temperature of 120-140 ℃ for 5-6h, filtering the solution after the solution is naturally cooled, washing the solution with absolute ethyl alcohol, and drying the solution in the air-blast drying box at the temperature of 80 ℃ for 12h to obtain a sisal fiber activated carbon powder sample.
3. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery cathode material is characterized in that the iron source is one or more of ferric chloride, ferric nitrate, ferrous chloride and ferrous nitrate.
4. Root of herbaceous plantFe according to claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery cathode material is characterized in that the molybdenum source is one of ammonium dimolybdate, ammonium paramolybdate and ammonium tetramolybdate.
5. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery cathode material is characterized in that the complexing agent is one of urea, ammonia water, citric acid, L-histidine and glycine.
6. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery negative electrode material is characterized in that the buffering agent is ammonium chloride.
7. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery cathode material is characterized in that the mass of the iron source, the molybdenum source, the complexing agent, the buffering agent and the sisal fiber activated carbon powder subjected to hydrothermal treatment in the step (2) are respectively as follows: 0.437-1.313g of iron source, 0.245-0.85g of molybdenum source, 0.2-0.6g or 3-5mL of complexing agent, 0.16-0.37g of buffering agent and 0.25-0.75g of sisal fiber activated carbon powder.
8. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery negative electrode material is characterized in that the step (2) further comprises the step of sieving a black powder sample by a 200-mesh sieve after calcination is completed.
9. Fe of claim 13O4-MoO2The preparation method of the @ SFAC lithium ion battery cathode material is characterized in that the inert atmosphere is one of nitrogen, argon and helium.
CN202010477633.7A 2020-05-29 2020-05-29 Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material Active CN111710839B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010477633.7A CN111710839B (en) 2020-05-29 2020-05-29 Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010477633.7A CN111710839B (en) 2020-05-29 2020-05-29 Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material

Publications (2)

Publication Number Publication Date
CN111710839A true CN111710839A (en) 2020-09-25
CN111710839B CN111710839B (en) 2021-07-20

Family

ID=72538482

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010477633.7A Active CN111710839B (en) 2020-05-29 2020-05-29 Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material

Country Status (1)

Country Link
CN (1) CN111710839B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102820465A (en) * 2012-06-20 2012-12-12 中南大学 Application of polyacrylic acid in preparation of lithium ion battery anode material nano-sized iron oxide/carbon composite material
CN104078656A (en) * 2014-07-09 2014-10-01 桂林理工大学 Preparation method for cathode material of nano ferroferric oxide/sisal hemp carbon lithium ion battery
CN104157857A (en) * 2014-08-04 2014-11-19 桂林理工大学 Preparation method for nano-Fe2O3/SFC lithium ion battery composite anode material
CN104269535A (en) * 2014-09-15 2015-01-07 南京工业大学 Preparation method of carbon-coated metal oxide-graphene composite electrode material
CN111193015A (en) * 2020-01-09 2020-05-22 桂林理工大学 MoSe2-MoO2Preparation method of @ sisal fiber activated carbon lithium ion battery negative electrode material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102820465A (en) * 2012-06-20 2012-12-12 中南大学 Application of polyacrylic acid in preparation of lithium ion battery anode material nano-sized iron oxide/carbon composite material
CN104078656A (en) * 2014-07-09 2014-10-01 桂林理工大学 Preparation method for cathode material of nano ferroferric oxide/sisal hemp carbon lithium ion battery
CN104157857A (en) * 2014-08-04 2014-11-19 桂林理工大学 Preparation method for nano-Fe2O3/SFC lithium ion battery composite anode material
CN104269535A (en) * 2014-09-15 2015-01-07 南京工业大学 Preparation method of carbon-coated metal oxide-graphene composite electrode material
CN111193015A (en) * 2020-01-09 2020-05-22 桂林理工大学 MoSe2-MoO2Preparation method of @ sisal fiber activated carbon lithium ion battery negative electrode material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SHAN-SHAN CHEN 等: "Molybdenum oxide-iron oxide/graphene composite as anode materials for lithium ion batteries", 《J.SOLID STATE ELECTROCHEM》 *

Also Published As

Publication number Publication date
CN111710839B (en) 2021-07-20

Similar Documents

Publication Publication Date Title
CN102790217B (en) Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof
CN109004199B (en) Preparation method of biomass hard carbon material for negative electrode of sodium-ion battery
CN102231435B (en) Method for preparing electrode material CuO (cupric oxide) film of lithium ion battery on copper substrate
CN108777294B (en) Carbon-supported porous spherical MoN composed of nanosheets and application of carbon-supported porous spherical MoN as negative electrode material in lithium battery
CN102339982A (en) Anode of lithium ion battery, preparation method and battery using anode
CN109461906B (en) Preparation method of lithium-sulfur battery positive electrode material
CN103050694B (en) A kind of positive electrode active materials and preparation method thereof, battery
CN112885985B (en) Positive pole piece and preparation method thereof, electrochemical energy storage device and pre-metallization method of electrochemical energy storage device
CN112133909B (en) Antimony sulfide-based negative electrode material for lithium ion battery and preparation method thereof
CN109286002B (en) Multi-bark biomass carbon-loaded red phosphorus sodium ion battery negative electrode material and preparation method thereof
CN112054174A (en) Potassium ion battery negative electrode material and preparation method and application thereof
CN112615005A (en) Method for preparing lithium iron phosphate anode composite material with good electrochemical performance based on waste bagasse
CN113871611B (en) Preparation method of high-entropy oxide material composite ternary material
CN111952553B (en) Preparation method of sulfur/sisal fiber activated carbon lithium-sulfur battery positive electrode material
CN114843459B (en) Antimony pentasulfide-based material and preparation method and application thereof
CN114709398B (en) Sulfur-containing fast ion conductor coated graphite composite material and preparation method thereof
CN107785559B (en) Graphene-lithium titanate composite material, preparation method thereof, lithium-supplementing graphene-lithium titanate film and lithium battery
CN116216746A (en) Preparation method and application of Prussian blue material with high thermal stability
CN111710839B (en) Fe3O4-MoO2Preparation method of @ SFAC lithium ion battery anode material
CN109256547A (en) A kind of preparation method of porous graphene-lithium iron phosphate positive material
CN112086629B (en) Si @ C/ZnNb2O6Preparation method and application of negative electrode composite material
CN111883746B (en) Modified lithium-rich manganese-based oxide positive electrode material and preparation method and application thereof
CN111193015A (en) MoSe2-MoO2Preparation method of @ sisal fiber activated carbon lithium ion battery negative electrode material
CN109378470B (en) Preparation method of vanadium-doped tungsten disulfide negative electrode material
CN117317200B (en) Positive electrode material, preparation method thereof and sodium ion battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20200925

Assignee: Guangxi Zaifa Energy Technology Co.,Ltd.

Assignor: GUILIN University OF TECHNOLOGY

Contract record no.: X2022450000526

Denomination of invention: A preparation method of Fe3O4- MoO2@ SFAC lithium ion battery cathode material

Granted publication date: 20210720

License type: Common License

Record date: 20221229

EE01 Entry into force of recordation of patent licensing contract
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20200925

Assignee: GUANGXI YANGSHENG NEW ENERGY CO.,LTD.

Assignor: GUILIN University OF TECHNOLOGY

Contract record no.: X2022450000636

Denomination of invention: A preparation method of Fe3O4- MoO2@ SFAC lithium ion battery anode material

Granted publication date: 20210720

License type: Common License

Record date: 20221230

EE01 Entry into force of recordation of patent licensing contract