CN112599762A - TiO 22Negative electrode material of CNF battery and preparation method thereof - Google Patents
TiO 22Negative electrode material of CNF battery and preparation method thereof Download PDFInfo
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 TiO 22a/CNF battery cathode material and a preparation method thereof, relating to the technical field of lithium ion battery cathode materials, wherein the TiO is2The negative electrode material of CNF battery is prepared by using carbon nano-cellulose as matrix and loading layered TiO on the matrix2A hybrid; the layered TiO2The hybrid being a multilayer Ti3C2TxThe material is prepared from a precursor; the preparation of the anode material comprises the following steps: a plurality of layers of Ti3C2TxDispersing the material in an ethanol solution, adding nano-cellulose, performing ultrasonic dispersion, aging, centrifugally washing, performing vacuum drying, calcining in an inert atmosphere, cooling, washing, and drying to obtain the nano-cellulose/nano-cellulose composite material. The invention utilizes Ti3C2TxObtaining TiO by heat treatment2Hybrid and first mixing CNF with TiO2The lithium ion battery cathode material prepared by compounding the hybrid solves the problems of low specific capacity and poor layered stability of a single carbon-based material, obtains good cycle stability and reversibility, realizes improvement of the electrochemical characteristics of the carbon-based material, and is an ideal choice of the cathode material.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to TiO2A CNF battery negative electrode material and a preparation method thereof.
Background
With the wide application of electronic products and new energy automobiles, lithium ion batteries have been permeated in various fields, and meanwhile, commercial graphite negative electrode materials have been difficult to meet the development of green energy and low-carbon economy, so that the development of high-specific-capacity negative electrode materials has a very important significance for the research of lithium ion batteries. The excellent negative electrode material ensures that the battery has high energy, good cycling stability and longer service life, and also ensures safety so as to adapt to the development of novel negative electrode materials.
The carbon-based material has been favored by researchers because of its advantages of low density, simple synthesis, designable structure, and good stability. However, research on negative electrode materials is mainly focused on graphite-based and non-graphite-based carbons, and although these materials have good cycle performance and safety performance, they have low lithium intercalation capacity and are easy to precipitate lithium, and are not suitable for large-current discharge, so that practical applications thereof are limited.
At present, titanium dioxide (TiO)2) The lithium ion battery is environment-friendly, low in cost, stable in structure in the process of lithium ion intercalation/deintercalation, capable of avoiding deposition of metal lithium, high in safety and high in development potential in high-energy storage. But TiO 22The poor electronic conductivity and poor lithium ion diffusion of the material affect the use effect of the material, and other materials are compounded to solve the problems.
Patent CN108448073A discloses C @ TiO with adjustable proportion2The composite negative electrode material is prepared by adding tetrabutyl titanate into ethylene glycol, forming a precursor through hydrolysis, and calcining the precursor in inert gas to form C @ TiO2And (3) compounding the negative electrode material. The C in the composite material is wrapped with TiO2The cathode material has a stable structure in the charging and discharging processes, and the conductivity of the material is improved by introducing carbon base, so that the C @ TiO is2The composite negative electrode material not only has high capacity, but also has good rate performance. However, the above-mentioned C @ TiO2The composite material takes ethylene glycol as a carbon source, and has the problems of small specific surface area, high cost, deficient source and the like.
Disclosure of Invention
Based on the technical problems in the background art, the invention providesProduce a TiO2CNF battery negative electrode material and preparation method thereof, CNF and TiO are firstly mixed2The hybrid is compounded, and the obtained composite material is used as the lithium ion battery cathode material, so that the problems of low specific capacity and poor layered stability of a single carbon-based material are solved, and good cycle stability and reversibility are obtained.
The invention provides TiO2The negative electrode material of CNF battery is prepared by using carbon nano-cellulose as matrix and loading layered TiO on the matrix2A hybrid; the layered TiO2The hybrid being a multilayer Ti3C2TxThe material is prepared by a precursor.
The invention also provides the TiO2The preparation method of the negative electrode material of the CNF battery comprises the following steps:
s1, forming a multilayer Ti3C2TxDispersing the material in ethanol solution, adding carbon nano-cellulose, performing ultrasonic dispersion, aging, centrifugally washing, and vacuum drying to obtain Ti3C2TxA nanocellulose composite;
s2, mixing Ti3C2TxCalcining the/nano-cellulose composite material in inert atmosphere, cooling, washing and drying to obtain TiO2a/CNF composite material.
Preferably, in S1, multiple layers of Ti3C2TxThe material is Ti3AlC2Is prepared by acid etching reaction of raw materials; the specific operation is as follows: under the condition of stirring, adding Ti3AlC2Adding into acid etching agent, sealing, stirring, reacting, centrifuging, washing, and vacuum drying to obtain multilayer Ti3C2TxA material; wherein the etchant is hydrofluoric acid aqueous solution.
Preferably, in S1, multiple layers of Ti3C2TxThe weight-volume ratio g/mL of the material to the ethanol solution is 0.1-0.3: 20-40 parts of; preferably, a plurality of layers of Ti3C2TxThe weight ratio of the material to the carbon nanocellulose is 1-3: 3.
preferably, in S1, ultrasonic dispersion is carried out for 5-10 min, and standing and aging are carried out for 12-24 h.
Preferably, in S2, the calcining temperature is 600-800 ℃, and the calcining time is 6-8 h; preferably, the temperature rise speed of the calcination is 1-3 ℃/min.
Preferably, Ti is added3AlC2Adding the mixture into an acid etching agent, and carrying out sealed stirring reaction at a stirring speed of 100-300 rpm for 24-72 h.
Preferably, the etchant is 40 wt% aqueous hydrofluoric acid, Ti3AlC2And the weight volume ratio g/mL of the etching agent is 1.0-3.0: 10 to 15.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
1.TiO2in the preparation of the/CNF composite material, the carbon nano-cellulose has larger contact area and strong van der Waals force, so that Ti3C2TxCan be well dispersed on the surface of the CNF-loaded layered TiO and is calcined in inert atmosphere to prepare the CNF-loaded layered TiO2Composite structures of hybrids. In the invention, TiO is mixed with2The nano particles are well dispersed and loaded on the CNF, and the electrochemical performance of the negative electrode material is effectively improved.
2. The carbon-based negative electrode material prepared by taking the nano-cellulose as the raw material has higher specific surface area, lower cost and abundant sources, and becomes a battery material with potential application value.
3. The invention utilizes Ti3C2TxObtaining TiO by heat treatment2Hybrid and first mixing CNF with TiO2The obtained composite material is used as the lithium ion battery cathode material, so that the problems of low specific capacity and poor layered stability of a single carbon-based material are solved, good cycle stability and reversibility are obtained, and the electrochemical characteristics of the carbon-based material are improved due to the improvement of the conductivity and the increase of the surface area, so that the composite material is an ideal choice of the cathode material.
4. The invention can enhance the electrochemical performance of the cathode material by the synergistic effect among the multi-component, and reasonably uses TiO with high lithium intercalation potential2To improve the problem of dendritic lithium formation of carbon-based negative electrode material, and simultaneouslyThe nano-cellulose can meet the development of green energy and low-carbon economy. Therefore, compared with the traditional graphite material, the prepared composite negative electrode material has a novel structure, and provides a certain technical reference and theoretical basis for the carbon-based negative electrode material.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention;
FIG. 2 shows TiO prepared in example 1 of the present invention2XRD pattern of/CNF composite material;
FIG. 3 shows TiO prepared in example 1 of the present invention2Raman spectra of/CNF composites;
FIG. 4 is a diagram showing the preparation of TiO in example 1 of the present invention2SEM images of the raw materials and products of the/CNF composite; wherein (a) Ti3C2TxCarbon nanocellulose, (b) TiO 30 μm in scale2TiO 5 μm on scale of/CNF (d)2/CNF;
FIG. 5 is a diagram showing the preparation of TiO in example 1 of the present invention2TEM images of the starting materials and products of the/CNF composite; wherein (a) is 1 μm TiO2CNF transmission diagram, (b) TiO scale 100nm2CNF transmission diagram, (c) 50nm TiO scale2CNF transmission diagram, (d) TiO2A CNF transmission diffraction analysis chart;
FIG. 6 shows TiO prepared in example 1 of the present invention2BET and XPS profiles of/CNF composites; wherein (a) TiO2Specific surface area of the/CNF (b) TiO2CNF pore size distribution plot, (c) TiO2X-ray photoelectron spectrum of/CNF, and (d) valence diagram of Ti element.
Detailed Description
Referring to FIG. 1, the present invention provides a TiO compound2The preparation process flow chart of the/CNF battery negative electrode material is that carbon nano-cellulose and a plurality of layers of Ti are mixed3C2TxMixing the solutions to obtain Ti-loaded surface3C2TxNano carbon fiber composite material Ti3C2TxThe TiO is obtained by heat treatment and carbonization of the/nano-cellulose composite material2a/CNF composite material.
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Weighing 10mL of 40% HF aqueous solution in a polytetrafluoroethylene reaction kettle, and weighing Ti3AlC2Precursor 1.0g, stirring Ti at room temperature under the condition of magnetic stirring rotation speed of 100r/min3AlC2Slowly adding HF aqueous solution into the precursor within 1.0min, sealing the reaction kettle, and keeping the stirring time for 24 h. Deionized water is added into the obtained product, and centrifugal separation is carried out at the rotating speed of 3500rpm for 3min each time. At the final centrifugation, the supernatant had a pH around 7.0. The obtained product is dried in a vacuum drying oven at 60 ℃.
At room temperature, the Ti prepared in the step 1 is added3C2Tx0.1g of the solution is weighed and evenly dispersed in 20mL of ethanol solution, 0.3g of carbon nano-cellulose is added, ultrasonic dispersion is carried out, and standing and aging are carried out for 12 hours. And finally, centrifugally washing the mixture by using distilled water and absolute ethyl alcohol for 3-5 times respectively, and drying the mixture in vacuum at the temperature of 60 ℃.
Preparing Ti by the step 23C2TxThe/nanocellulose composite is transferred to a tube furnace in N2The calcination was carried out for 8h at 600 ℃ under a stream-protecting atmosphere. Cooling to room temperature to obtain TiO2a/CNF composite material.
For the prepared TiO2the/CNF composite was characterized and tested.
FIG. 2 shows TiO prepared in example 12XRD pattern of/CNF composite material; in TiO2In the/CNF sample, in addition to the carbon peaks at 22 DEG and 44 DEG, other main diffraction peaks were associated with TiO2The JCPDS cards are consistent.
FIG. 3 shows TiO prepared in example 1 of the present invention2Raman spectra of/CNF composites; in the figure, D represents amorphous carbon, G represents graphitic graphitized carbon, and the strong peak at G can be seenThe degree is greater than the peak intensity at D, indicating that TiO2the/CNF negative electrode material has high graphitization degree.
FIG. 4 is a diagram showing the preparation of TiO in example 1 of the present invention2SEM images of the raw materials and products of the/CNF composite; as can be seen from a comparison of FIG. b with FIGS. c and d, TiO was added2Loaded on the CNF backbone.
FIG. 5 is a diagram showing the preparation of TiO in example 1 of the present invention2TEM images of the starting materials and products of the/CNF composite; TiO as shown in the figures (a) and (b)2The particles are surrounded by carbon, indicating TiO2The formation of the particle structure and CNF; (c) is TiO2CNF high resolution TEM; (d) SAED confirmed TiO2The lattice characteristics of the nanoparticles.
FIG. 6 shows TiO prepared in example 1 of the present invention2BET and XPS profiles of/CNF composites; FIG. A is TiO2The CNF sample has a representative IV-type isothermal curve at a relative pressure of 0.4-1.0, has an obvious hysteresis loop and represents a mesoporous structure of the composite material. The specific surface area of the sample was 251.59m2(ii) in terms of/g. (b) The pore diameter is mainly distributed below 5 nm. (c) TiO 22XPS scanning spectrum of/CNF shows the existence of Ti, C, O and F elements in the composite material, (d) Ti 2p has two main peaks at 459.2eV and 464.9eV, which respectively correspond to Ti-O (2p3/2) and Ti-O (2p 1/2). This fact confirms the use of Ti3C2Tx to TiO2Complete phase transition of the phases.
Example 2
Weighing 12mL of 40% HF aqueous solution in a polytetrafluoroethylene reaction kettle, and weighing Ti3AlC2Precursor 1.0g, stirring Ti at room temperature under the condition of magnetic stirring rotation speed of 200r/min3AlC2The precursor is slowly added with HF aqueous solution within 2.0min, the reaction kettle is sealed, and the stirring time lasts 24 h. Deionized water is added into the obtained product, and centrifugal separation is carried out at the rotating speed of 3500rpm for 3min each time. At the final centrifugation, the supernatant had a pH around 7.0. The obtained product is dried in a vacuum drying oven at 60 ℃.
At room temperature, the Ti prepared in the step 1 is added3C2Tx0.2g of the solution is weighed and evenly dispersed in 30mL of ethanol solution, 0.3g of carbon nano-cellulose is added, ultrasonic dispersion is carried out, and standing and aging are carried out for 12 hours. And finally, centrifugally washing the mixture by using distilled water and absolute ethyl alcohol for 3-5 times respectively, and drying the mixture in vacuum at the temperature of 60 ℃.
Preparing Ti by the step 23C2TxThe/nanocellulose composite is transferred to a tube furnace in N2The calcination was carried out at 700 ℃ for 7h under a stream-protecting atmosphere. Cooling to room temperature to obtain TiO2a/CNF composite material.
Example 3
Weighing 15mL of 40% HF aqueous solution in a polytetrafluoroethylene reaction kettle, and weighing Ti3AlC2Precursor 2.0g, stirring Ti at room temperature under the condition of magnetic stirring rotation speed of 300r/min3AlC2Slowly adding HF aqueous solution into the precursor within 3.0min, sealing the reaction kettle, and keeping the stirring time for 48 h. Deionized water is added into the obtained product, and centrifugal separation is carried out at the rotating speed of 3500rpm for 3min each time. At the final centrifugation, the supernatant had a pH around 7.0. The obtained product is dried in a vacuum drying oven at 60 ℃.
At room temperature, the Ti prepared in the step 1 is added3C2Tx0.3g of the solution is weighed and evenly dispersed in 40mL of ethanol solution, 0.3g of carbon nano-cellulose is added, ultrasonic dispersion is carried out, and standing and aging are carried out for 12 hours. And finally, centrifugally washing the mixture by using distilled water and absolute ethyl alcohol for 3-5 times respectively, and drying the mixture in vacuum at the temperature of 60 ℃.
Preparing Ti by the step 23C2TxThe/nanocellulose composite is transferred into a tube furnace in whichN2The calcination was carried out at 800 ℃ for 6h under a stream-protecting atmosphere. Cooling to room temperature to obtain TiO2a/CNF composite material.
Example 4
Weighing 12mL of 40% HF aqueous solution in a polytetrafluoroethylene reaction kettle, and weighing Ti3AlC2Precursor 3.0g, stirring Ti at room temperature under the condition of magnetic stirring rotation speed of 300r/min3AlC2Slowly adding HF aqueous solution into the precursor within 3.0min, sealing the reaction kettle, and keeping the stirring time for 48 h. Deionized water is added into the obtained product, and centrifugal separation is carried out at the rotating speed of 3500rpm for 3min each time. At the final centrifugation, the supernatant had a pH around 7.0. The obtained product is dried in a vacuum drying oven at 60 ℃.
At room temperature, the Ti prepared in the step 1 is added3C2Tx0.2g of the solution is weighed and evenly dispersed in 40mL of ethanol solution, 0.3g of carbon nano-cellulose is added, ultrasonic dispersion is carried out, and standing and aging are carried out for 12 hours. And finally, centrifugally washing the mixture by using distilled water and absolute ethyl alcohol for 3-5 times respectively, and drying the mixture in vacuum at the temperature of 60 ℃.
Preparing Ti by the step 23C2TxThe/nanocellulose composite is transferred to a tube furnace in N2The calcination was carried out for 8h at 600 ℃ under a stream-protecting atmosphere. Cooling to room temperature to obtain TiO2a/CNF composite material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. TiO 22/CNF batteryThe negative electrode material is characterized in that carbon nano-cellulose is taken as a substrate, and layered TiO is loaded on the substrate2A hybrid; the layered TiO2The hybrid being a multilayer Ti3C2TxThe material is prepared by a precursor.
2. The TiO of claim 12The preparation method of the negative electrode material of the CNF battery is characterized by comprising the following steps:
s1, forming a multilayer Ti3C2TxDispersing the material in ethanol solution, adding carbon nano-cellulose, performing ultrasonic dispersion, aging, centrifugally washing, and vacuum drying to obtain Ti3C2TxA nanocellulose composite;
s2, mixing Ti3C2TxCalcining the/nano-cellulose composite material in inert atmosphere, cooling, washing and drying to obtain TiO2a/CNF composite material.
3. The TiO of claim 22The preparation method of the negative electrode material of the CNF battery is characterized in that in S1, multiple layers of Ti3C2TxThe material is Ti3AlC2Is prepared by acid etching reaction of raw materials; the specific operation is as follows: under the condition of stirring, adding Ti3AlC2Adding into acid etching agent, sealing, stirring, reacting, centrifuging, washing, and vacuum drying to obtain multilayer Ti3C2TxA material; wherein the etchant is hydrofluoric acid aqueous solution.
4. The TiO of claim 22The preparation method of the negative electrode material of the CNF battery is characterized in that in S1, multiple layers of Ti3C2TxThe weight-volume ratio g/mL of the material to the ethanol solution is 0.1-0.3: 20-40 parts of; preferably, a plurality of layers of Ti3C2TxThe weight ratio of the material to the carbon nanocellulose is 1-3: 3.
5. according to claim2 said TiO2The preparation method of the negative electrode material of the CNF battery is characterized in that in S1, ultrasonic dispersion is carried out for 5-10 min, and standing and aging are carried out for 12-24 h.
6. The TiO of claim 22The preparation method of the CNF battery negative electrode material is characterized in that in S2, the calcining temperature is 600-800 ℃, and the calcining time is 6-8 h; preferably, the temperature rise speed of the calcination is 1-3 ℃/min.
7. The TiO of claim 32The preparation method of the negative electrode material of the CNF battery is characterized in that Ti is added3AlC2Adding the mixture into an acid etching agent, and carrying out sealed stirring reaction at a stirring speed of 100-300 rpm for 24-72 h.
8. The TiO of claim 32The preparation method of the negative electrode material of the CNF battery is characterized in that the etching agent is 40 wt% hydrofluoric acid aqueous solution and Ti3AlC2And the weight volume ratio g/mL of the etching agent is 1.0-3.0: 10 to 15.
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CN113559920A (en) * | 2021-07-05 | 2021-10-29 | 青岛科技大学 | ZSM-5 molecular sieve/titanium dioxide composite material and preparation method thereof |
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