CN113277512B - Preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 Material, preparation method and application thereof - Google Patents
Preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 Material, preparation method and application thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C01G9/00—Compounds of zinc
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a method for preparing a Ti with a nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The material is subjected to wet ball milling, and physical and chemical reactions are induced by mechanical energy, and friction collision occurs under the action of a certain medium, so that the tissue structure of the material is changed to a certain extent. Compared with other preparation methods in the prior art, the method has the advantages of simple operation, simple process equipment, low production cost, and the like compared with the traditional method of introducing amorphous modification layers of other materials, such as coating amorphous carbon materials, sintering and annealing to obtain amorphous layers rich in defective active sites, and the like, thereby avoiding the inherent chemical energy barrier between the amorphous modification layers and the intrinsic lattice materials, and avoiding the problem that the collapse of the self structure of the materials after the sintering and annealing affects the chemical stability in the cyclic process.
Description
Technical Field
The invention relates to the technical field of synthesis of mixed sodium ion capacitor materials, in particular to a method for preparing nano-scale ultrathin amorphous oxide by wet ball millingLayer Ti 3 C 2 A preparation method of the material.
Background
With the development of the electronic information age, people are urgent to find sustainable energy sources, and the construction of clean and renewable energy storage devices is a problem to be solved urgently. Rechargeable batteries and capacitors are two complementary electrical energy storage devices that play a vital role in electric vehicles and electronics. As the most developed rechargeable battery, lithium ion batteries have a strong competitive advantage in terms of energy density. However, due to the unsatisfactory power density of lithium ion batteries and the limited and uneven distribution of lithium resource reserves. More and more researchers are turning to the development of other rechargeable batteries and capacitors. Compared to chargeable and dischargeable batteries, capacitors have a high power density, a fast charge and discharge process and a long cycle life, but are limited by their lower energy density. Hybrid ion capacitors have received great attention because they can combine the advantages of batteries and capacitors. Sodium ion hybrid capacitors have significant cost advantages over lithium ion hybrid capacitors.
The sodium ion mixed capacitor mainly comprises a battery type positive electrode, a capacitor type negative electrode and a sodium salt-containing electrolyte. Capacitive cathodes, e.g. Nb 2 O 5 、TiO 2 、V 2 O 5 MXene has been widely studied, wherein MXene has high conductivity and large surface area, and has wide prospect in application to pseudocapacitive electrodes. However, the form of MXene in which sodium ions are stored is primarily ion intercalation and has not been very satisfactory for ion-adsorption storage.
To address this problem, increasing the ionic adsorption storage of MXene is the most effective strategy. We propose a titanium alloy with a nanoscale ultra-thin amorphous oxide layer 3 C 2 Preparation method of material, ti after treatment 3 C 2 There still exist two-dimensional layered structures whose surfaces are coated with this layer of nanoscale ultrathin oxide, which is present in amorphous form. Therefore, the material structure can increase sodium without affecting ion embedded storageIon adsorption and storage are carried out, rapid charge transfer on the interface of the electrode and the electrolyte is accelerated, diffusion of sodium ions is facilitated, and pseudo capacitance of the capacitor is increased.
Disclosure of Invention
The invention aims to prepare Ti with a nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 A method of preparing a material that addresses one or more of the problems of the prior art described above.
In order to solve the technical problems of the invention, the technical proposal is as follows: preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 Preparation method of material by controlling Ti 3 C 2 The amount of the mixed solvent is ball milled for a period of time, and the oxide generated under the action of strong external force is tightly wrapped in a few-layer Ti 3 C 2 The surface of the tablet is distorted to a certain extent, after ball milling for a period of time, deionized water or absolute ethyl alcohol is used for ultrasonic washing, redundant solvents and oxides are washed off, and the tablet is dried; the Ti is 3 C 2 The material is less-layer (1-3 layers) Ti after stripping etching 3 C 2 The mass ratio of the grinding balls to the ball-milling substances is 1-100:1, and the ball-milling substances are Ti 3 C 2 The mixed solvent is a mixed solvent of a raw material solvent for synthesizing oxides and a dispersing agent; ti is mixed with 3 C 2 Slowly adding the stirred mixed solution; control of Ti 3 C 2 The mass ratio of the mixed solvent is 1:1-100.
Preferably, the mixed solvent is ammonia water and Tetraethoxysilane (TEOS).
Preferably, the mixed solvent is Mn (CH 3 COO) 2 ·4H 2 O and deionized water.
Preferably, the dispersant is an inorganic dispersant or an organic dispersant.
Preferably, the oxide in the amorphous oxide layer is silicon dioxide, zinc oxide, aluminum oxide, manganese oxide, vanadium oxide.
Preferably, the ball milling speed is 100-1800r/min, and the ball milling reaction time is 1-24h.
Preferably, the stirring speed is 500-1000r/min, and the reaction time is 1-24h.
Preferably, the drying means may be air-dried at room temperature, air-dried in a blast oven at 60-100deg.C for 12-24 hr, and freeze-dried for 24-72 hr.
In order to solve the technical problem of the invention, another technical proposal is that: the Ti with the nanoscale ultrathin amorphous oxide layer prepared by the method 3 C 2 A material.
In order to solve the technical problem of the invention, another technical proposal is that: the Ti with the nano-scale ultrathin amorphous oxide layer 3 C 2 Material application, preparing Ti with nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The material can be used as a sodium ion capacitor, and the method can be applied to electrode materials of other batteries or amorphous modification layers of solid electrolyte.
The invention provides a method for preparing a Ti with a nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The material comprises specific oxide and a corresponding treatment method, and the thickness, the lattice distortion degree and the like of the nanoscale ultrathin amorphous oxide layer are regulated and controlled by controlling the proportion and the concentration of various solvents for ball milling, the ball milling time, the surfactant and the like.
Amorphous layer cathode materials with different thicknesses and lattice distortion degrees are prepared by controlling the proportion and concentration of various solvents, the ball milling time and the surfactant. Wherein, the regulation and control variation range of thickness is tens nanometers to a few nanometers, the amorphous oxide layer refers to the typical interplanar spacing of oxide, and the lattice stripes show disordered arrangement or even no lattice stripes.
By controlling Ti 3 C 2 Ball milling with various solvents for a period of time, and tightly wrapping oxide generated under the action of strong external force on the less-layer Ti 3 C 2 The surface of the sheet is distorted to a certain extent in the crystal structure, and after ball milling for a period of time, deionized water or absolute ethyl alcohol is used for ultrasonic washing to remove redundant solvents and oxides.
In an embodiment, ti 3 C 2 Etching Ti with HF 3 AlC 2 The Al layer in the alloy is washed and dried by deionized water through ultrasonic insertion of dimethyl sulfoxide (DMSO) to obtain a few (1-3) layers of Ti 3 C 2 。
In some embodiments, the synthesized oxide is one or more of silica, zinc oxide, aluminum oxide, manganese oxide, vanadium oxide, and the like.
In some embodiments, the dispersant is an inorganic dispersant, an organic dispersant, water. The inorganic dispersant is sodium pyrophosphate, sodium hexametaphosphate, and the organic dispersant is one or more of ethanol, polyacrylamide, F127, polyethylene glycol and the like.
In some embodiments, the ball milling conditions are a ball milling rate of 100 to 1800r/min and a mass ratio of grinding balls to ball milled material of 1 to 100:1, the reaction time is 1-24h.
In some embodiments, the stirring rate is 500-1000r/min and the reaction time is 1-24 hours.
In some embodiments, ti 3 C 2 The mass ratio of the solvent to the solvent is 1:1-100.
In some embodiments, the drying means may be air-dried at room temperature, air-oven-dried at 60-100deg.C for 12-24 hours, and freeze-dried for 24-72 hours.
Preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 The material may be a sodium ion capacitor, but is not limited to use in sodium ion capacitors, and the method may also be extended for application to electrode materials for other batteries or to amorphous modification layers of solid state electrolytes.
The invention provides a method for preparing a Ti with a nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The material comprises specific oxide and a corresponding treatment method, and the thickness, the lattice distortion degree and the like of the nanoscale ultrathin amorphous oxide layer are regulated and controlled by controlling the proportion and the concentration of various solvents for ball milling, the ball milling time, the surfactant and the like.
The ball mill with different solvent ratio and concentration, ball milling time and surfactant can be preparedNanoscale ultrathin amorphous oxide layer Ti with thickness and degree of lattice distortion 3 C 2 A material. Wherein, the regulation and control variation range of thickness is tens nanometers to a few nanometers, the amorphous oxide layer refers to the typical interplanar spacing of oxide, and the lattice stripes show disordered arrangement or even no lattice stripes.
By controlling Ti 3 C 2 Ball milling with various solvents for a period of time, and tightly wrapping oxide generated under the action of strong external force on the less-layer Ti 3 C 2 The surface of the sheet is distorted to a certain extent in the crystal structure, and after ball milling for a period of time, deionized water or absolute ethyl alcohol is used for ultrasonic washing to remove redundant solvents and oxides.
The invention has the beneficial effects that:
1) The preparation method of the embodiment of the invention is wet ball milling of Ti with a nanoscale ultrathin amorphous oxide layer 3 C 2 Compared with other preparation methods in the prior art, the material has the advantages of simple operation, simple process equipment, low production cost, and the like compared with the traditional method of introducing amorphous modification layers of other materials, such as coating amorphous carbon materials, sintering and annealing to obtain amorphous layers rich in defective active sites, and the like, thereby avoiding the inherent chemical energy barrier between the amorphous modification layers and the intrinsic lattice materials, and avoiding the problem that the collapse of the self structure of the material after the sintering and annealing affects the chemical stability in the battery cycle process.
2) The invention prepares the Ti with the nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The material may be a sodium ion capacitor, but is not limited to use in sodium ion capacitors, and the method may also be extended for application to electrode materials for other batteries or to amorphous modification layers of solid state electrolytes.
3) The invention prepares the Ti with the nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 Material, treated Ti 3 C 2 There still exist two-dimensional layered structures whose surfaces are coated with this layer of nanoscale ultrathin oxide, which is present in amorphous form. The material structure is therefore in advance of storage without affecting ion intercalationUnder the premise, sodium ion adsorption storage is increased, rapid charge transfer on the interface of the electrode and the electrolyte is accelerated, diffusion of sodium ions is facilitated, and pseudocapacitance of the capacitor is increased.
4) By controlling ball milling Ti 3 C 2 The ratio and concentration of the material and the raw material solvent of the synthetic oxide, the ball milling time and the surfactant are used for preparing the nano-scale ultrathin amorphous oxide layer Ti with different thickness and lattice distortion degree 3 C 2 A material.
Drawings
FIG. 1 is a raw material Ti as a raw material of example 1 of the present invention 3 C 2 SEM image of (2)
FIG. 2 is O-Ti film obtained in example 1 of the present invention 3 C 2 SEM image of (2)
Detailed Description
The invention is further described below with reference to examples. The following examples are only for the purpose of more clearly illustrating the properties of the present invention and are not limited to the following examples.
Example 1:
preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 Preparation of the Material
Ti 3 C 2 The material is few-layer (1-3-layer) Ti after purchased stripping etching 3 C 2 (gallop, ving technology), 0.1g of Ti 3 C 2 Dispersing in 2mL absolute ethanol, ultrasonic treating for half an hour, adding 0.25mL ammonia water while stirring, mixing 0.025mL Tetraethoxysilane (TEOS) uniformly, stirring at 800rmp, ball milling at 800r/min for 12h, and grinding to obtain the final product 3 C 2 Mass ratio of the mixture with the mixed solvent is 100:1, grinding the balls into agate balls with the diameter of 12mm, repeatedly washing and centrifuging for 3-5 times by using deionized water under the centrifugation condition of 8000rmp for 5min, and freeze-drying for 48h until the supernatant is neutral, thus obtaining the final product with the nanoscale ultrathin amorphous oxide layer Ti 3 C 2 Material, denoted O-Ti 3 C 2 。
Assembling and testing of the battery:
to O-Ti 3 C 2 Uniformly mixing the powder, conductive carbon black Super P and polyvinylidene fluoride PVDF according to the formula mass ratio of 8:1:1, and then dropwise adding the mixture into an N-methyl-2-pyrrolidone solvent. Stirring fully to form slurry, and scraping and coating the slurry on carbon-coated aluminum foil by using a coating machine to obtain the pole piece. The coated pole piece was placed in an oven and dried overnight at 120 ℃. Then cutting the pole piece into a round pole piece with the diameter of 11 mm. The electrode is used as a working electrode plate, sodium metal is used as a counter electrode, a glass fiber membrane is used as a diaphragm, and the electrode comprises 1.0MNAPF 6 DMC EMC solution as electrolyte A button cell was assembled in an argon glove box and then activated and left to stand for 24h to test cell performance on a cell test system.
FIG. 1 is a raw material Ti as a raw material of example 1 of the present invention 3 C 2 SEM image of (2)
FIG. 2 is O-Ti film obtained in example 1 of the present invention 3 C 2 SEM image of (2)
O-Ti 3 C 2 Ultra-thin amorphous oxide layer SiO with thickness of 5nm 2 As can be seen from XRD test, the XRD of the layer has a broad peak without crystal form, namely, the transition amorphous modification layer O-Ti with specific thickness 3 C 2 The material exposes more ion channels, accelerates rapid charge transfer on the interface of the electrode and the electrolyte, is favorable for diffusion of sodium ions, and increases the pseudo capacitance of the capacitor on the premise of not affecting intercalation of the sodium ions.
Example 2:
preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 Material
0.1g Ti 3 C 2 0.034mg Mn (CH) was added to 0.2mL polyethylene glycol with stirring 3 COO) 2 ·4H 2 O1.5 mL deionized water, and ultrasonic treatment for 1h to make Ti 3 C 2 Modification of some Mn 2+ Further adding 0.0145KMnO 4 After stirring and mixing uniformly, the stirring speed is 800rmp, the ball milling rotating speed is 800r/min, ball milling is carried out for 18 hours, and the grinding balls and Ti are mixed 3 C 2 Mass ratio of the mixture with the mixed solvent is 100:1, the grinding ball is agate small ball with diameter of 12mm, and the grinding ball and the Ti are 3 C 2 The quality of the mixture with the mixed solventThe weight ratio is 150:1, grinding the balls into agate balls with the diameter of 12mm, repeatedly washing and centrifuging for 3-5 times by using deionized water under the centrifugation condition of 8000rmp for 5min, and freeze-drying for 48h until the supernatant is neutral, thus obtaining the final product with the nanoscale ultrathin amorphous oxide layer Ti 3 C 2 Material, designated M-Ti 3 C 2 。
Assembling and testing of the battery:
M-Ti 3 C 2 Uniformly mixing the powder, conductive carbon black Super P and polyvinylidene fluoride PVDF according to the formula mass ratio of 8:1:1, and then dropwise adding the mixture into an N-methyl-2-pyrrolidone solvent. Stirring fully to form slurry, and scraping and coating the slurry on carbon-coated aluminum foil by using a coating machine to obtain the pole piece. The coated pole piece was placed in an oven and dried overnight at 120 ℃. Then cutting the pole piece into a round pole piece with the diameter of 11 mm. The electrode is used as a working electrode plate, sodium metal is used as a counter electrode, a glass fiber membrane is used as a diaphragm, and the electrode comprises 1.0MNAPF 6 DMC EMC solution as electrolyte A button cell was assembled in an argon glove box and then activated and left to stand for 24h to test cell performance on a cell test system.
M-Ti 3 C 2 Ultra-thin amorphous oxide layer MnO with thickness of 12nm 2 Such a transitional amorphous modification layer M-Ti having a specific thickness 3 C 2 The material exposes more ion channels, accelerates rapid charge transfer on the interface of the electrode and the electrolyte, is favorable for diffusion of sodium ions, and increases the pseudo capacitance of the capacitor on the premise of not affecting intercalation of the sodium ions.
Embodiments of the present invention provide for the preparation of ultra-thin amorphous oxide layers Ti having nanoscale by wet ball milling 3 C 2 The material, such as thickness of an amorphous layer, lattice distortion degree and the like, is subjected to wet ball milling, physical and chemical reactions are induced by mechanical energy, and friction collision occurs under the action of a certain medium, so that the tissue structure of the material is changed to a certain extent. Compared with other preparation methods in the prior art, the method has the advantages of simple operation, simple process equipment, low production cost, and the like compared with the traditional method for introducing amorphous modification layers of other materials, such as coating amorphous carbon materials, sintering and annealing to obtain amorphous layers rich in defective active sitesThe method not only avoids the inherent chemical energy barrier between the amorphous modification layer and the intrinsic lattice material, but also avoids the problem that the collapse of the structure of the material after sintering and annealing affects the chemical stability in the battery cycle process.
The above description is only of a preferred form of the invention, it being understood that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the inventive concept, which shall be regarded as being within the scope of the invention.
Claims (3)
1. Preparation of Ti with nanoscale ultrathin amorphous oxide layer by wet ball milling 3 C 2 The preparation method of the material is characterized by comprising the following steps:
Ti 3 C 2 the material is 1-3 layers of Ti after purchased stripping etching 3 C 2 0.1g of Ti 3 C 2 Dispersing in 2mL absolute ethanol, ultrasonic treating for half an hour, adding 0.25mL ammonia water and 0.025mL tetraethoxysilane under stirring, mixing, stirring at 800 rpm, ball milling at 800r/min for 12h, and grinding to obtain the final product 3 C 2 Mass ratio of the mixture with the mixed solvent is 100:1, grinding the balls into agate balls with the diameter of 12mm, repeatedly washing and centrifuging with deionized water for 3-5 times under the centrifugation condition of 8000 rpm for 5min, and freeze-drying for 48h until the supernatant is neutral, thus obtaining the final product with the nanoscale ultrathin amorphous oxide layer Ti 3 C 2 Material, denoted O-Ti 3 C 2 ；
By controlling Ti 3 C 2 Ball milling with various solvents for a period of time according to the mass proportion, and tightly wrapping the oxide generated in situ under the action of strong mechanical force and friction heat on the few-layer Ti 3 C 2 The surface of the sheet, the crystal structure is distorted to a certain extent;
ti with nanoscale ultrathin amorphous oxide layer prepared by wet ball milling 3 C 2 Material, treated Ti 3 C 2 Two-dimensional layered structure still exists and the surface is coated with a nanoscale ultrathin oxide layerThe nanoscale ultrathin oxide layer exists in an amorphous form; the amorphous oxide layer has typical interplanar spacings, but its lattice fringes exhibit a disordered arrangement or even no lattice fringes.
2. Ti with nanoscale ultra-thin amorphous oxide layer prepared according to the method of claim 1 3 C 2 A material.
3. Ultra-thin amorphous oxide layer Ti with nanoscale according to claim 2 3 C 2 The material application is characterized in that: preparation of ultra-thin amorphous oxide layer Ti with nanometer level by wet ball milling 3 C 2 The material is used for sodium ion capacitors, and extends to electrode materials or solid electrolyte amorphous modification layers applied to other batteries.
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| JP2007084351A (en) * | 2005-09-20 | 2007-04-05 | Tdk Corp | METHOD FOR PRODUCING TiC AND TiCN |
| CN102060535A (en) * | 2010-04-02 | 2011-05-18 | 陕西理工学院 | Method for preparing high-purity Ti3AlC2 ceramics |
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