CN111554913B - Multilayer titanium dioxide mesoporous film electrode material and preparation method and application thereof - Google Patents
Multilayer titanium dioxide mesoporous film electrode material and preparation method and application thereof Download PDFInfo
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- CN111554913B CN111554913B CN202010430036.9A CN202010430036A CN111554913B CN 111554913 B CN111554913 B CN 111554913B CN 202010430036 A CN202010430036 A CN 202010430036A CN 111554913 B CN111554913 B CN 111554913B
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- H01M4/00—Electrodes
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
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- 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
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention discloses a multilayer titanium dioxide mesoporous film electrode material and a preparation method and application thereof, and relates to the field of electrode material preparation, wherein cyclodextrin and a composite template formed by surfactant self-assembly are combined, a hydrothermal method is adopted to prepare the multilayer titanium dioxide mesoporous film electrode material at one time, post crystallization treatment is not needed, the prepared titanium dioxide mesoporous electrode material has a multilayer mesoporous structure with 5-6 layers, and the titanium dioxide mesoporous film electrode material is applied to the electrode material, so that higher specific capacity and good cycle performance can be realized. The preparation method is simple in preparation process, remarkably shortened in time and more suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a multilayer titanium dioxide mesoporous film electrode material and a preparation method and application thereof.
Background
As a novel photocatalyst, an ultraviolet resistant agent, a photoelectric effect agent and the like, the nano titanium dioxide shows wide application prospects in the fields of antibiosis and mildew prevention, exhaust purification, deodorization, water treatment, pollution prevention, weather resistance and ageing resistance, automobile finish and the like, and plays an unappreciable role in the fields of environment, information, materials, energy, medical treatment, sanitation and the like along with the gradual maturity of the industrial production and functional application development of products.
The specific surface area of the nano-scale titanium dioxide is directly determined by the grain size of the nano-scale titanium dioxide, the smaller the grain size is, the larger the specific surface area is, the transmission rate of surface active centers and surface charges is increased therewith, the reaction activity is improved therewith, and the nano-scale titanium dioxide used as a lithium ion battery material has the excellent characteristics of high theoretical specific capacity, good cycle performance and low price, and has very wide application prospect. However, the pure titanium dioxide nano powder has the defect that 1, the oversize is difficult to achieve the ideal effect, and the oversize is easy to agglomerate; 2. small specific surface area and is not easy to combine with other elements.
According to the definition of IUPAC, the pore material with the pore diameter less than 2 nanometers is microporous material, the pore material with the pore diameter between 2 and 50 nanometers is mesoporous material, and the pore material with the pore diameter more than 50 nanometers is called macroporous material. Compared with nano titanium dioxide, the mesoporous titanium dioxide material is an inorganic biological material with the advantages of high specific surface area, large pore volume, controllable morphology and size and the like, has the dual characteristics of the mesoporous material and the nano material, and has very high chemical stability and biocompatibility. In recent years, with the development of mesoporous material synthesis technology, the preparation of mesoporous titanium dioxide materials with rich morphology and structure has become a current research hotspot. The multilayer structure is formed on the basis of the original mesoporous morphology of the mesoporous titanium dioxide material, the specific surface area can be obviously improved, and the material can realize higher specific capacity and good cycle performance when being used as a battery material.
At present, precipitation method, peptization method and hydrothermal method are mostly adopted for preparing mesoporous titanium dioxide. The mesoporous titanium dioxide material is prepared by a precipitation method, the process is simple, the operation is convenient, but the local concentration of a precipitator is easily overhigh, a large amount of fine precipitates are promoted to be rapidly formed, and crystals are often incomplete due to fast particle formation, have large surface area and are difficult to grow and precipitate; the peptization method has many influencing factors when preparing the mesoporous titanium dioxide, is difficult to form a multilayer stable structure, has long reaction time which is usually more than 50 hours, and is difficult to realize stable large-scale production; the hydrothermal method is carried out under the unlimited condition, so that the method has certain superiority in the aspect of preparing mesoporous titanium dioxide compared with other liquid-phase preparation methods, but when the hydrothermal method is adopted to prepare the mesoporous titanium dioxide material, a multilayer structure with an excellent structure cannot be prepared, the multilayer mesoporous structure is limited to 2-3 layers, and the multilayer mesoporous titanium dioxide material still has the limitation in performance when used as an electrode material.
Disclosure of Invention
The invention aims to provide a multilayer titanium dioxide mesoporous film electrode material, and a preparation method and application thereof, so as to solve the problems in the prior art, and the titanium dioxide mesoporous material can realize a multilayer mesoporous structure with 5-6 layers, and can realize higher specific capacity and good cycle performance when being used in the electrode material.
The invention provides a preparation method of a multilayer titanium dioxide mesoporous film electrode material, which comprises the following steps:
(1) dissolving octadecyl trimethyl ammonium chloride and dimethyl benzyl dodecyl ammonium bromide in water, self-assembling the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide to form a composite template under the stirring condition, adding cyclodextrin, and continuously stirring uniformly;
(2) mixing Ti (SO)4)2Adding the solution into the solution obtained in the step (1), and uniformly stirring;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the cleaned glass substrate into the solution, heating to 60-80 ℃ for reaction, and naturally cooling to room temperature after the reaction is finished;
(4) and taking out the glass substrate, washing with water and alcohol, and drying to obtain the multilayer titanium dioxide mesoporous film electrode material.
Further, the concentration of the octadecyl trimethyl ammonium chloride is 0.005-0.095 mol/L; the concentration of the dimethyl benzyl dodecyl ammonium bromide is 0.003 to 0.005 mol/L.
Further, the molar ratio of the cyclodextrin to the octadecyl trimethyl ammonium chloride is (1-1.2): 1.
Further, the stirring temperature in the step (1) is 25-30 ℃, and the stirring time is 2-3 h.
Further, the Ti (SO)4)2The concentration of the solution is 0.02-0.025 mol/L.
Further, in the step (3), the heating rate is 3-5 ℃/min, and the reaction time is 3-5 h; the cleaning treatment of the glass substrate is acetone ultrasonic cleaning and drying.
Further, the film thickness of the multilayer titanium dioxide mesoporous film electrode material is 0.2-0.3 mm.
Further, in the step (4), the drying temperature is 45-55 ℃, and the drying time is 2.5-3 h.
The invention provides a multilayer titanium dioxide mesoporous film electrode material prepared by the preparation method of the multilayer titanium dioxide mesoporous film electrode material.
The invention also provides application of the multilayer titanium dioxide mesoporous film electrode material prepared by the preparation method of the multilayer titanium dioxide mesoporous film electrode material in an electrode.
The invention discloses the following technical effects:
1. the multilayer titanium dioxide mesoporous film electrode material can be directly obtained at the temperature of 60-80 ℃, and the heat treatment at higher temperature is not needed, so that the hard agglomeration which may be formed is avoided.
2. The cyclodextrin is a truncated cone-shaped cyclic oligosaccharide with axial symmetry, the molecular cavity of the cyclodextrin is hydrophobic, the outer surface of the cyclodextrin is hydrophilic, and the cyclodextrin and guest molecules such as surfactants and the like can form aggregates with different morphologies. According to the invention, cyclodextrin and a composite template formed by surfactant self-assembly are combined to form an aggregate with a multilayer structure, then a hydrothermal method is adopted to prepare the multilayer titanium dioxide mesoporous film electrode material once, no post crystallization treatment is needed, and the prepared titanium dioxide mesoporous electrode material has a multilayer mesoporous structure with 5-6 layers, and can realize higher specific capacity and good cycle performance when being applied to the electrode material.
3. The preparation method is simple, the time is obviously shortened, and the multilayer glass substrates can be placed in the hydrothermal reaction kettle at intervals at one time, so that the batch production of the multilayer titanium dioxide mesoporous film electrode material is realized, and the preparation method is more suitable for industrialization.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
Example 1
(1) Dissolving 0.005mol of octadecyl trimethyl ammonium chloride and 0.003mol of dimethyl benzyl dodecyl ammonium bromide in lL deionized water, carrying out self-assembly on the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide under the stirring condition to form a composite template, adding 0.006mol of cyclodextrin, and continuously stirring uniformly;
(2) 50ml of 0.02mol/L Ti (SO)4)2Adding the solution into the solution in the step (1), and stirring for 2 hours at the temperature of 30 ℃;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the glass substrate subjected to ultrasonic cleaning and drying by acetone into the solution, controlling the heating rate to be 5 ℃/min, heating to 80 ℃ for reaction for 5h, and naturally cooling to room temperature after the reaction is finished;
(4) and taking out the glass substrate, washing with deionized water and ethanol, and drying at 55 ℃ for 2.5h to obtain the multilayer titanium dioxide mesoporous film electrode material.
The thickness of the obtained multilayer titanium dioxide mesoporous film electrode material is 0.2mm, and the multilayer titanium dioxide mesoporous film electrode material has a multilayer mesoporous structure with 6 layers.
And (3) carrying out performance test on the prepared multilayer titanium dioxide mesoporous film electrode material:
preparing a mixture according to the mass ratio of the multilayer titanium dioxide mesoporous film electrode material to PVDF to KS6 of 60:10:30, adding NMP as a solvent, and stirring for 2 hours to prepare the lithium ion battery electrode slurry. And (3) coating the electrode viscous slurry on a copper foil with the thickness of 12 microns, wherein the coating thickness is 50 microns, and drying at 100 ℃ for 12 hours to obtain the lithium ion battery electrode. The negative pole piece of the lithium ion battery is cut into a circular pole piece with the diameter of 14mm, and the counter electrode of the lithium ion battery adopts a metal lithium piece with the diameter of 15 m. The electrolyte is as follows: 1mol/L LiPF6The button cell was assembled in a 2032 type glove box filled with argon gas, dissolved in a solvent of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (molar ratio EC: DMC 1: 1).
The prepared button cell is subjected to charge and discharge tests, and the first discharge specific capacity of the multilayer titanium dioxide mesoporous film electrode material can reach 1526mAh/g under the current density of 0.01V-3V and 100 mA/g; under the current density of 0.01V-3V and 100mA/g, the specific capacity of the 50 th discharge can still reach 610 mAh/g.
Under the current density of 100mA/g, the capacity retention rate of the multilayer titanium dioxide mesoporous film electrode material after 50 cycles is 82 percent calculated from the second discharge capacity.
Under the current density of 800mA/g, after the multilayer titanium dioxide mesoporous film electrode material is circulated for 500 times, the capacity retention rate is 92.4%, and the cycle stability is excellent.
Example 2
(1) Dissolving 0.095mol of octadecyl trimethyl ammonium chloride and 0.005mol of dimethyl benzyl dodecyl ammonium bromide in lL deionized water, performing self-assembly on the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide under the stirring condition to form a composite template, adding 0.095mol of cyclodextrin, and continuously stirring uniformly;
(2) 50ml of 0.025mol/L Ti (SO)4)2Adding the solution into the solution in the step (1), and stirring for 3 hours at the temperature of 25 ℃;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the glass substrate subjected to ultrasonic cleaning and drying by acetone into the solution, controlling the heating rate to be 3 ℃/min, heating to 60 ℃ for reaction for 3h, and naturally cooling to room temperature after the reaction is finished;
(4) and taking out the glass substrate, washing with deionized water and ethanol, and drying at 45 ℃ for 3h to obtain the multilayer titanium dioxide mesoporous film electrode material.
The thickness of the obtained multilayer titanium dioxide mesoporous film electrode material is 0.3mm, and the multilayer titanium dioxide mesoporous film electrode material has a multilayer mesoporous structure with 5 layers.
The performance test of the prepared multilayer titanium dioxide mesoporous film electrode material is carried out by adopting the same method as the embodiment 1:
the first discharge specific capacity of the multilayer titanium dioxide mesoporous film electrode material can reach 1530mAh/g under the current density of 0.01V-3V and 100 mA/g; under the current density of 0.01V-3V and 100mA/g, the specific capacity of the 50 th discharge can still reach 686 mAh/g.
Under the current density of 100mA/g, the capacity retention rate of the multilayer titanium dioxide mesoporous film electrode material after 50 cycles is 91 percent calculated from the second discharge capacity.
Under the current density of 800mA/g, after the multilayer titanium dioxide mesoporous film electrode material is circulated for 500 times, the capacity retention rate is 90.2%, and the electrode material has excellent circulation stability.
Example 3
(1) Dissolving 0.026mol of octadecyl trimethyl ammonium chloride and 0.004mol of dimethyl benzyl dodecyl ammonium bromide in lL deionized water, self-assembling the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide to form a composite template under the stirring condition, adding 0.026mol of cyclodextrin, and continuously stirring uniformly;
(2) 50ml of 0.023mol/L Ti (SO)4)2Adding the solution into the solution in the step (1), and stirring for 2.5h at the temperature of 28 ℃;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the glass substrate subjected to ultrasonic cleaning and drying by acetone into the solution, controlling the heating rate to be 4 ℃/min, heating to 65 ℃ for reaction for 4h, and naturally cooling to room temperature after the reaction is finished;
(4) and taking out the glass substrate, washing with deionized water and ethanol, and drying at 50 ℃ for 2.8h to obtain the multilayer titanium dioxide mesoporous film electrode material.
The thickness of the obtained multilayer titanium dioxide mesoporous film electrode material is 0.25mm, and the multilayer titanium dioxide mesoporous film electrode material has a multilayer mesoporous structure with 6 layers.
The performance test of the prepared multilayer titanium dioxide mesoporous film electrode material is carried out by adopting the same method as the embodiment 1:
the first discharge specific capacity of the multilayer titanium dioxide mesoporous film electrode material can reach 1510mAh/g under the current density of 0.01V-3V and 100 mA/g; under the current density of 0.01V-3V and 100mA/g, the specific capacity of the 50 th discharge can still reach 612 mAh/g.
Under the current density of 100mA/g, the capacity retention rate of the multilayer titanium dioxide mesoporous film electrode material after 50 cycles is 90.8 percent calculated from the second discharge capacity.
Under the current density of 800mA/g, after the multilayer titanium dioxide mesoporous film electrode material is circulated for 500 times, the capacity retention rate is 91.2%, and the electrode material has excellent circulation stability.
Example 4
(1) Dissolving 0.056mol of octadecyl trimethyl ammonium chloride and 0.003mol of dimethyl benzyl dodecyl ammonium bromide in lL deionized water, carrying out self-assembly on the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide under the stirring condition to form a composite template, adding 0.056mol of cyclodextrin, and continuously stirring uniformly;
(2) 50ml of 0.024mol/L Ti (SO)4)2Adding the solution into the solution in the step (1), and stirring for 2.8h at the temperature of 27 ℃;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the glass substrate subjected to ultrasonic cleaning and drying by acetone into the solution, controlling the heating rate to be 3.5 ℃/min, heating to 70 ℃ for reaction for 3.5h, and naturally cooling to room temperature after the reaction is finished;
(4) and taking out the glass substrate, washing with deionized water and ethanol, and drying at 50 ℃ for 2.9h to obtain the multilayer titanium dioxide mesoporous film electrode material.
The thickness of the obtained multilayer titanium dioxide mesoporous film electrode material is 0.28mm, and the multilayer titanium dioxide mesoporous film electrode material has a multilayer mesoporous structure with 6 layers.
The performance test of the prepared multilayer titanium dioxide mesoporous film electrode material is carried out by adopting the same method as the embodiment 1:
the first discharge specific capacity of the multilayer titanium dioxide mesoporous film electrode material can reach 1586mAh/g under the current density of 0.01V-3V and 100 mA/g; under the current density of 0.01V-3V and 100mA/g, the specific capacity of the 50 th discharge can still reach 652 mAh/g.
Under the current density of 100mA/g, the capacity retention rate of the multilayer titanium dioxide mesoporous film electrode material after 50 cycles is 92.1 percent calculated from the second discharge capacity.
Under the current density of 800mA/g, after the multilayer titanium dioxide mesoporous film electrode material is circulated for 500 times, the capacity retention rate is 93.2%, and the electrode material has excellent circulation stability.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (6)
1. The preparation method of the multilayer titanium dioxide mesoporous film electrode material is characterized by comprising the following steps:
(1) dissolving octadecyl trimethyl ammonium chloride and dimethyl benzyl dodecyl ammonium bromide in water, self-assembling the octadecyl trimethyl ammonium chloride and the dimethyl benzyl dodecyl ammonium bromide to form a composite template under the stirring condition, adding cyclodextrin, and continuously stirring uniformly;
(2) mixing Ti (SO)4)2Adding the solution into the solution obtained in the step (1), and uniformly stirring;
(3) adding the solution obtained in the step (2) into a hydrothermal reaction kettle, placing the cleaned glass substrate into the solution, heating to 60-80 ℃ for reaction, and naturally cooling to room temperature after the reaction is finished;
(4) taking out the glass substrate, washing with water and alcohol, and drying to obtain the multilayer titanium dioxide mesoporous film electrode material;
the concentration of the octadecyl trimethyl ammonium chloride is 0.005-0.095 mol/L; the concentration of the dimethyl benzyl dodecyl ammonium bromide is 0.003 to 0.005 mol/L;
the molar ratio of the cyclodextrin to the octadecyl trimethyl ammonium chloride is (1-1.2) to 1;
in the step (1), the stirring temperature is 25-30 ℃, and the stirring time is 2-3 h;
in the step (3), the heating rate is 3-5 ℃/min, and the reaction time is 3-5 h;
the multilayer titanium dioxide mesoporous film electrode material is of a 5-6-layer mesoporous structure; the Ti (SO)4)2The concentration of the solution is 0.02-0.025 mol/L.
2. The method for preparing the multilayer titanium dioxide mesoporous thin film electrode material as claimed in claim 1, wherein the cleaning treatment of the glass substrate is acetone ultrasonic cleaning and drying.
3. The method for preparing a multilayer titanium dioxide mesoporous thin film electrode material according to claim 1, wherein the thickness of the multilayer titanium dioxide mesoporous thin film electrode material is 0.2-0.3 mm.
4. The preparation method of the multilayer titanium dioxide mesoporous thin film electrode material according to claim 1, wherein the drying temperature in the step (4) is 45-55 ℃, and the drying time is 2.5-3 h.
5. A multilayer titanium dioxide mesoporous thin film electrode material prepared by the preparation method of the multilayer titanium dioxide mesoporous thin film electrode material according to any one of claims 1 to 4.
6. The application of the multilayer titanium dioxide mesoporous film electrode material of claim 5 in an electrode.
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