CN111634942B - Preparation method of titanium dioxide nanowire array with slender branches - Google Patents
Preparation method of titanium dioxide nanowire array with slender branches Download PDFInfo
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- CN111634942B CN111634942B CN202010449585.0A CN202010449585A CN111634942B CN 111634942 B CN111634942 B CN 111634942B CN 202010449585 A CN202010449585 A CN 202010449585A CN 111634942 B CN111634942 B CN 111634942B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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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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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- 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
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses a preparation method of a titanium dioxide nanowire array with slender branches. Firstly, preparing sodium titanate nanowire array, and obtaining TiO through acid exchange and heat treatment2A nanowire array; then, using TiF4In solution in TiO2Depositing a layer of TiO on the surface of the nanowire array through a chemical bath2Particles; finally, carrying out hydrothermal reaction to obtain TiO2Sodium titanate branched nanowire arrays followed by acid exchange and thermal treatment to convert the sodium titanate branches to TiO2Branching to obtain TiO2And (3) branching the nanowire array. Compared with the existing method for preparing TiO2Compared with the technology of branching nanowire arrays, the method disclosed by the invention utilizes' utilizing TiO2The obtained material can be simultaneously combined with the new synthesis idea of' difference of reactivity and speed caused by the difference of the number of surface defects, crystallinity and surface area2The structural characteristics of the main body and the superfine branch of the nanowire are realized, and the length of the branch is larger, so that the performance of the nanowire serving as a photocatalyst is improved.
Description
Technical Field
The invention relates to a preparation method of a titanium dioxide nanowire array with a long and thin branch, which is hopeful to be applied to the fields of photocatalysis, dye-sensitized solar cells, lithium ion batteries, gas sensors and the like.
Background
TiO2Nano material in photocatalysis and lightThe method has potential application prospect in the fields of electric conversion, lithium ion batteries, gas sensors and the like. TiO 22Depending on its composition and microstructure. Single crystal TiO 22The nanowire array has excellent charge transfer performance; TiO 22Two-dimensional nanostructures (e.g., nanobelts) have a thin thickness and a high specific surface area. Growing TiO with fine branch structure on the surface of the nanowire array2The hierarchical structure array is formed, the advantages of the single crystal nanowire trunk and the high specific surface area branch can be combined, and the hierarchical structure array is expected to become a high-performance functional material.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium dioxide nanowire array with elongated branches.
The invention relates to a titanium dioxide nanowire array (TiO for short) with slender branches2Branched nanowire arrays) comprising the steps of:
1) carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array;
2) soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array;
3) subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in an acidic aqueous solution at 60 ℃ for 1-3 h to obtain TiO2nanowire/TiO2An array of particle branches;
4) adding TiO into the mixture2nanowire/TiO2Carrying out hydrothermal reaction on the particle branch array in NaOH aqueous solution with the concentration of 2.5-5.0 mol/L for 6h at 140 ℃ to obtain TiO2A sodium titanate branched nanowire array;
5) adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO2And (3) branching the nanowire array.
The invention has the beneficial effects that:
compared with the existing method for preparing TiO2Compared with the technology of branching nanowire arrays, the method disclosed by the invention utilizes' utilizing TiO2The obtained material combines the new synthesis idea of' difference of reactivity and speed caused by the difference of the number of surface defects, crystallinity and surface area2The structural characteristics of the main body and the superfine branch of the nanowire are realized, and the length of the branch is larger, so that the performance of the nanowire serving as a photocatalyst is improved.
Drawings
FIG. 1 is a scanning electron micrograph of a branched nanowire array of titanium dioxide prepared in example 1;
FIG. 2 is a Raman spectrum of a branched nanowire array of titanium dioxide prepared in example 1;
FIG. 3 is a scanning electron micrograph of a branched nanowire array of titanium dioxide prepared in example 2;
FIG. 4 is a SEM photograph of branched titania nanowire array prepared in example 3;
FIG. 5 is a SEM photograph of branched titania nanowire array prepared in example 4;
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
Carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array; soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array; subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in acid aqueous solution at 60 ℃ for 1h to obtain TiO2nanowire/TiO2An array of particle branches; adding TiO into the mixture2nanowire/TiO2The particle branch array is dissolved in NaOH water with the concentration of 2.5mol/LCarrying out hydrothermal reaction for 6h at 140 ℃ in the solution to obtain TiO2A sodium titanate branched nanowire array; adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO2And (3) branching the nanowire array.
FIG. 1 is a scanning electron micrograph of the material obtained, from which it can be seen that the product is a branched nanowire structure. The branches are mutually staggered nanowires with larger length, and form an integral structure of the branch nanowires under the supporting action of the main nanowire. FIG. 2 shows the Raman spectrum of the obtained material, and it can be seen that the phase of the material is anatase TiO2。
Example 2
Carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array; soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array; subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in acid aqueous solution at 60 ℃ for 3h to obtain TiO2nanowire/TiO2An array of particle branches; adding TiO into the mixture2nanowire/TiO2Carrying out hydrothermal reaction on the particle branch array in 2.5mol/L NaOH aqueous solution at 140 ℃ for 6h to obtain TiO2A sodium titanate branched nanowire array; adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO2And (3) branching the nanowire array.
Fig. 3 is a scanning electron micrograph of the resulting product, which can be seen as a branched nanowire structure. The branches are mutually staggered nanowires with larger length, and form an integral structure of the branch nanowires under the supporting action of the main nanowire.
Example 3
Carrying out hydrothermal reaction on a titanium sheet in NaOH aqueous solution with the concentration of 1.25mol/L at 220 DEG CObtaining a sodium titanate nanowire array after 20 hours; soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array; subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in acid aqueous solution at 60 ℃ for 3h to obtain TiO2nanowire/TiO2An array of particle branches; adding TiO into the mixture2nanowire/TiO2Carrying out hydrothermal reaction on the particle branch array in NaOH aqueous solution with the concentration of 3.2mol/L at 140 ℃ for 6h to obtain TiO2A sodium titanate branched nanowire array; adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO2And (3) branching the nanowire array.
Fig. 4 is a scanning electron micrograph of the resulting product, which can be seen as a branched nanowire structure.
Example 4
Carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array; soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array; subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in acid aqueous solution at 60 ℃ for 3h to obtain TiO2nanowire/TiO2An array of particle branches; adding TiO into the mixture2nanowire/TiO2Carrying out hydrothermal reaction on the particle branch array in NaOH aqueous solution with the concentration of 5mol/L at 140 ℃ for 6h to obtain TiO2A sodium titanate branched nanowire array; adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO2And (3) branching the nanowire array.
Fig. 5 is a scanning electron micrograph of the resulting product, which can be seen as a branched nanowire structure.
Claims (1)
1. A method for preparing a titanium dioxide nanowire array with slender branches is characterized by comprising the following steps:
1) carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array;
2) soaking the sodium titanate nanowire array in a hydrochloric acid aqueous solution with the concentration of 0.1mol/L for 2 hours, and carrying out an acid exchange reaction to obtain a titanic acid nanowire array; performing heat treatment on the titanic acid nanowire array for 3h at 550 ℃ to obtain single crystal anatase TiO2A nanowire array;
3) subjecting single crystal anatase TiO2Placing the nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in an acidic aqueous solution at 60 ℃ for 1-3 h to obtain TiO2nanowire/TiO2An array of particle branches;
4) adding TiO into the mixture2nanowire/TiO2Carrying out hydrothermal reaction on the particle branch array in NaOH aqueous solution with the concentration of 2.5-5.0 mol/L at 140 ℃ for 6h to obtain TiO2A sodium titanate branched nanowire array;
5) adding TiO into the mixture2Soaking the sodium titanate branched nanowire array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then carrying out heat treatment at 450 ℃ for 1h to obtain TiO with slender branches2And (4) nanowire arrays.
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| US8440162B1 (en) * | 2006-12-18 | 2013-05-14 | The Research Foundation Of State University Of New York | Titanate and titania nanostructures and nanostructure assemblies, and methods of making same |
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