CN110963473A - Preparation method of carbon/titanium nitride nanotube composite material - Google Patents
Preparation method of carbon/titanium nitride nanotube composite material Download PDFInfo
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- CN110963473A CN110963473A CN201911339637.2A CN201911339637A CN110963473A CN 110963473 A CN110963473 A CN 110963473A CN 201911339637 A CN201911339637 A CN 201911339637A CN 110963473 A CN110963473 A CN 110963473A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0765—Preparation by carboreductive nitridation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C—CHEMISTRY; METALLURGY
- 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
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a method for preparing carbon/titanium nitride nanotube composite material, which comprises the steps of putting nano titanium dioxide into sodium hydroxide solution, and fully stirring until the solution is in an emulsion state; putting the mixture into a polytetrafluoroethylene container, putting the polytetrafluoroethylene container into a high-pressure reaction kettle, performing hydrothermal reaction, cooling, pouring out supernatant, taking white sediment at the bottom, repeatedly washing the white sediment with water, and performing acid washing for three times by using 1M nitric acid; then filtering and drying to obtain a titanium dioxide nanotube; and then, fully and uniformly mixing the titanium dioxide nanotube and guanidine hydrochloride together, calcining under inert gas, putting the obtained product into 1M nitric acid for ultrasonic treatment for 1 hour, washing and filtering by distilled water, and drying to obtain the carbon/titanium nitride nanotube composite material product. The prepared material is provided with the carbon coating layer, so that direct contact between titanium nitride and electrolyte is avoided, and the carbon coating layer effectively improves the conductivity of the titanium nitride material.
Description
Technical Field
The invention relates to a preparation method of a composite material, in particular to a preparation method of a carbon/titanium nitride nanotube composite material.
Technical Field
The super capacitor is a novel green energy storage element developed in the last decade and is widely applied in many aspects. Supercapacitors have received much attention from researchers due to their faster energy storage characteristics, higher power density, and cycling stability.
Currently, electrode materials for supercapacitors include graphene-based materials, biomass carbon materials, nanostructured metal oxides, conductive polymers, transition metal disulfides, metal-organic framework-based materials, carbide/nitride materials, and the like. Among these materials, carbide/nitride materials are receiving attention because of their high conductivity, high density, excellent chemical stability and excellent capacitance properties. More importantly, the presence of these materials also changed the poor cyclability characteristics of previous pseudocapacitive supercapacitors. The metal carbide/nitride and the composite material thereof are considered to be the electrode materials of the super capacitor with the highest high power density performance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a carbon/titanium nitride nanotube composite material.
The invention aims to provide the following scheme for realization: a preparation method of a carbon/titanium nitride nanotube composite material comprises the following steps of preparing a titanium dioxide nanotube by hydrothermal reaction by using nano titanium dioxide as a raw material and guanidine hydrochloride as a carbon/nitrogen source, and calcining the titanium dioxide nanotube and the guanidine hydrochloride under inert gas to prepare the carbon-coated titanium nitride nanotube composite material:
1) placing nano titanium dioxide into a sodium hydroxide solution, fully stirring until the solution is in an emulsion state, placing the solution into a polytetrafluoroethylene container, placing the solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 150-200 ℃, cooling, removing supernatant, taking white sediment at the bottom, repeatedly washing the white sediment with water, carrying out acid washing for three times by using 1M nitric acid, filtering, and drying at 80 ℃ to obtain a titanium dioxide nanotube;
2) mixing titanium dioxide nanotubes and guanidine hydrochloride in a mass ratio of 1: (5-10), fully and uniformly mixing, calcining at 900 ℃ under inert gas, putting the obtained product into 1M nitric acid for cleaning, cleaning and filtering by distilled water, and drying at 80 ℃ to obtain the product C @ TiN.
In the step 1), 2g of nano titanium dioxide is put into 100ml of 10M sodium hydroxide solution, and the hydrothermal reaction is carried out after the solution is fully stirred to be in an emulsion state, wherein the hydrothermal reaction time is 24-48 h.
The inert gas is nitrogen.
Calcining conditions are as follows: heating to 900 ℃ at the heating rate of 5-10 ℃/min, preserving the heat for 2h, and then naturally cooling to room temperature.
Compared with the prior patent, the invention has the advantages that: the preparation condition is simple, and the titanium nitride nanotube material can be prepared at relatively low temperature. The prepared material is provided with the carbon coating layer, so that direct contact between titanium nitride and electrolyte is avoided, and the carbon coating layer effectively improves the conductivity of the titanium nitride material.
Drawings
FIG. 1 is a scanning electron micrograph of the carbon/titanium nitride nanotube composite prepared in example 1;
FIG. 2 is a cyclic voltammogram of the carbon/titanium nitride nanotube composite prepared in example 1.
Detailed Description
The invention will be further elucidated by means of specific embodiments, without being limited thereto, in conjunction with the accompanying drawings.
Example 1
A carbon/titanium nitride nanotube composite material is prepared by taking nano titanium dioxide as a raw material and guanidine hydrochloride as a carbon/nitrogen source, preparing a titanium dioxide nanotube through a hydrothermal reaction, and then calcining the titanium dioxide nanotube and the guanidine hydrochloride under inert gas to prepare the carbon-coated titanium nitride nanotube composite material, wherein the carbon-coated titanium nitride nanotube composite material is prepared through the following steps:
1) putting 2g of nano titanium dioxide into 100ml of 10M sodium hydroxide solution, fully stirring until the solution is in an emulsion state, putting the solution into a polytetrafluoroethylene container by adopting a traditional simple hydrothermal reaction, putting the polytetrafluoroethylene container into a high-pressure reaction kettle, carrying out hydrothermal reaction for 48 hours at 150 ℃, cooling, removing supernatant, taking white sediment at the bottom, repeatedly washing the white sediment with water, carrying out acid washing for three times by using 1M nitric acid, filtering, and drying at 80 ℃ to obtain a titanium dioxide nanotube;
2) and (2) taking 1g of titanium dioxide nanotube and 5g of guanidine hydrochloride, fully and uniformly mixing, heating to 900 ℃ at a speed of 10 ℃/min in a tube furnace in a nitrogen atmosphere, then preserving heat for two hours, putting the obtained product into 1M nitric acid for ultrasonic treatment for 1 hour, cleaning and filtering with distilled water, and drying at a temperature of 80 ℃ to obtain a product C @ TiN. The scanning electron microscope is shown in figure 1, which is a TiN composite material with a carbon coating layer.
FIG. 2 is a cyclic voltammogram of the carbon/titanium nitride nanotube composite material prepared in this example. The carbon coating layer effectively improves the conductivity of the titanium nitride material.
Example 2
A carbon/titanium nitride nanotube composite material, similar to example 1, prepared by the following steps:
1) putting 2g of nano titanium dioxide into 100ml of 10M sodium hydroxide solution, fully stirring until the solution is in an emulsion state, putting the solution into a polytetrafluoroethylene container, putting the polytetrafluoroethylene container into a high-pressure reaction kettle, carrying out a traditional simple hydrothermal reaction at 180 ℃ for 24 hours, cooling, removing a supernatant, taking a white deposit at the bottom, repeatedly washing the white deposit with water, carrying out acid washing for three times by using 1M nitric acid, filtering, and drying at 80 ℃ to obtain a titanium dioxide nanotube;
2) the preparation method comprises the following steps of fully and uniformly mixing 1g of titanium dioxide nanotube and 10g of guanidine hydrochloride together, heating to 900 ℃ at a heating rate of 5 ℃/min in a tube furnace in a nitrogen atmosphere, calcining for 2 hours, putting the obtained product into 1M nitric acid, carrying out ultrasonic treatment for 1 hour, cleaning and filtering with distilled water, and drying at 80 ℃ to obtain the product C @ TiN.
Example 3
A carbon/titanium nitride nanotube composite material, similar to example 1, prepared by the following steps:
1) putting 2g of nano titanium dioxide into 100ml of 10M sodium hydroxide solution, fully stirring until the solution is in an emulsion state, putting the solution into a polytetrafluoroethylene container, putting the polytetrafluoroethylene container into a high-pressure reaction kettle, carrying out hydrothermal reaction for 12 hours at 200 ℃, cooling, removing supernatant, taking white sediment at the bottom, repeatedly washing the white sediment with water, carrying out acid washing for three times by using 1M nitric acid, filtering, and drying at 80 ℃ to obtain a titanium dioxide nanotube;
2) and (2) fully and uniformly mixing 1g of titanium dioxide nanotube and 10g of guanidine hydrochloride, calcining for two hours at the temperature of 5 ℃/min to 900 ℃ in a tube furnace in the nitrogen atmosphere, putting the obtained product into 1M nitric acid, carrying out ultrasonic treatment for 1 hour, cleaning and filtering by using distilled water, and drying at the temperature of 80 ℃ to obtain the product C @ TiN.
Claims (4)
1. A preparation method of a carbon/titanium nitride nanotube composite material is characterized in that nano titanium dioxide is used as a raw material, a carbon/nitrogen source is guanidine hydrochloride, a hydrothermal reaction is firstly carried out to prepare a titanium dioxide nanotube, and then the titanium dioxide nanotube and the guanidine hydrochloride are calcined under inert gas to prepare the carbon-coated titanium nitride nanotube composite material, and the preparation method comprises the following steps:
1) placing nano titanium dioxide into a sodium hydroxide solution, fully stirring until the solution is in an emulsion state, placing the solution into a polytetrafluoroethylene container, placing the solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 150-200 ℃, cooling, removing supernatant, taking white sediment at the bottom, repeatedly washing the white sediment with water, carrying out acid washing for three times by using 1M nitric acid, filtering, and drying at 80 ℃ to obtain a titanium dioxide nanotube;
2) mixing titanium dioxide nanotubes and guanidine hydrochloride in a mass ratio of 1: (5-10), fully and uniformly mixing, calcining at 900 ℃ under inert gas, putting the obtained product into 1M nitric acid for cleaning, cleaning and filtering by distilled water, and drying at 80 ℃ to obtain the product C @ TiN.
2. The method for preparing carbon/titanium nitride nanotube composite material as claimed in claim 1, wherein in step 1), 2g of nano-titania is put into 100ml of 10M sodium hydroxide solution, and the hydrothermal reaction is performed after the solution is fully stirred to be in an emulsion state, wherein the hydrothermal reaction time is 24-48 h.
3. The method of claim 1, wherein the inert gas is nitrogen.
4. The method for preparing a carbon/titanium nitride nanotube composite material as set forth in claim 1, wherein the calcination conditions are: heating to 900 ℃ at the heating rate of 5-10 ℃/min, preserving the heat for 2h, and then naturally cooling to room temperature.
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