CN112442688B - Anatase phase TiO prepared by titanium substrate2Method for nanotube film - Google Patents
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Abstract
The invention relates to the technical field of preparation of inorganic materials, in particular to a method for preparing anatase phase TiO by using a titanium substrate2Nanotube film methods; the method sequentially comprises the steps of pretreatment, oxidation, hydrothermal treatment, acid washing and heat treatment, and specifically comprises the following steps: (1) pretreatment: cutting a titanium sheet, grinding the titanium sheet by using sand paper, carrying out ultrasonic cleaning, and finally carrying out chemical polishing treatment; (2) and (3) oxidation reaction: putting the pretreated titanium sheet into hydrogen peroxide for oxidation reaction, washing the titanium sheet with water after the reaction is finished, and drying the titanium sheet for later use; (3) hydrothermal reaction: putting the oxidized titanium sheet into a NaOH solution for hydrothermal reaction, taking out the titanium sheet after the reaction is finished, and cooling the titanium sheet to room temperature for later use; (4) acid washing: soaking the titanium sheet obtained in the step (3) in a hydrochloric acid solution, taking out, washing, and drying for later use; (5) and (3) heat treatment: roasting the titanium sheet obtained in the step (4) by using a muffle furnace, cooling to room temperature, and taking out to obtain anatase-phase TiO2A nanotube film.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic materials, in particular to a method for preparing anatase phase TiO by using a titanium substrate2A method of nanotube film.
Background
TiO2As a catalyst, the catalyst can fully utilize solar energy, and is widely applied to the fields of solar cells, wastewater treatment and the like because the catalyst is nontoxic, low in manufacturing cost and good in stability, and products are relatively clean and pollution-free in the process of chemical reaction. One-dimensional TiO2The nanotube structure has higher specific surface area and faster electron transmission channel, can greatly reduce the recombination rate of photo-generated electron-hole pairs, and is expected to improve TiO2Photoelectric conversion and photocatalytic efficiency. At present TiO2The preparation method of the nanotube comprises a template method, an anodic oxidation method and a hydrothermal synthesis method. Compared with the former two methods, the hydrothermal method does not need a reaction template and an external electric field, and has the advantages of simple process, controllable appearance, low manufacturing cost and the like. The invention uses pure titanium sheet as titanium source, first generates a layer of TiO on the titanium substrate by hydrogen peroxide2Oxidizing the film, and preparing TiO with high length-diameter ratio by hydrothermal method2A nanotube film. TiO prepared by the method2The nanotube film takes a titanium sheet as a substrate, has high conductivity, and the nanotubes grow in situ on the titanium substrate, have good associativity with the substrate, are not easy to fall off, have large specific surface area and have higher photoelectrochemical properties.
Disclosure of Invention
The invention aims to provide a method for preparing anatase phase TiO by using a titanium substrate2The method for preparing the nanotube film uses pure titanium sheets as a titanium source, and utilizes hydrogen peroxide to oxidize the titanium sheets at a certain temperature to generate a layer of TiO2Oxide film, and then formed TiO2Is a precursor, hydrothermal synthesis of a nanotube structure is carried out in a strong alkali solution under the conditions of high temperature and high pressure, and the TiO of anatase phase is obtained by acid washing and water washing processes and final roasting in a muffle furnace2A nanotube film.
The preparation method specifically comprises the following steps: anatase phase TiO prepared by titanium substrate2A method of nanotube film comprising the steps of:
(1) pretreatment: cutting a titanium sheet, grinding the titanium sheet by using sand paper, carrying out ultrasonic cleaning, and finally carrying out chemical polishing treatment;
(2) and (3) oxidation reaction: putting the pretreated titanium sheet into hydrogen peroxide for oxidation reaction, washing the titanium sheet with water after the reaction is finished, and drying the titanium sheet for later use;
(3) hydrothermal reaction: putting the oxidized titanium sheet into a NaOH solution for hydrothermal reaction, taking out the titanium sheet after the reaction is finished, and cooling the titanium sheet to room temperature for later use;
(4) acid washing: soaking the titanium sheet obtained in the step (3) in a hydrochloric acid solution, taking out, washing, and drying for later use;
(5) and (3) heat treatment: will step withRoasting the titanium sheet in the step (4) by using a muffle furnace, cooling to room temperature, and taking out to obtain anatase-phase TiO2A nanotube film.
The products obtained in the above steps are specifically described with reference to fig. 1 to 7, that is: FIG. 1 shows that the product obtained in step (2) is TiO2Thin film, indicating that a dense, uniform oxide film was formed on the titanium substrate. FIG. 2 illustrates the anatase phase TiO obtained after the heat treatment of step (5)2. FIG. 3 shows that TiO is obtained in step (2)2Oxide film, FIG. 4 shows TiO obtained in step (3)2Typical morphology of nanotube films. FIG. 5 shows the dense TiO obtained in step (2)2And (3) film appearance. FIG. 6 shows TiO in example 12The transient photocurrent of the nanotube film is tested under the condition of simulating solar illumination, and the electrolyte is a KOH solution with the concentration of 1mol/L, so that the obtained product has good photoelectric response characteristics. FIG. 7 shows TiO in example 32The transient photocurrent of the nanotube film measured under the condition of simulating solar illumination is tested, and the electrolyte is a KOH solution with the concentration of 1mol/L, which shows that the obtained product has good photoelectrochemical properties.
As a preferable mode of the present invention, the titanium sheet in the step (1) of the above production method is cut to 5cm x 1 cm.
As a preferable embodiment of the present invention, the ultrasonic cleaning in step (1) in the preparation method specifically includes: ultrasonic cleaning with acetone and anhydrous ethanol for 15 min.
As a preferable embodiment of the present invention, the chemical polishing in step (1) of the above preparation method specifically includes: at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
As a preferable embodiment of the present invention, in the step (2) of the preparation method, the hydrogen peroxide concentration is 30%.
As a preferable scheme of the invention, the temperature of the oxidation reaction in the step (2) in the preparation method is 80 ℃, and the reaction time is 1-24 h.
In a preferred embodiment of the present invention, the NaOH solution in step (3) of the above-mentioned production method has a concentration of 5 to 10mol/L.
As a preferable scheme of the invention, the temperature of the hydrothermal reaction in the step (3) in the preparation method is 140-180 ℃ and the time is 1-6 h.
The concentration of the hydrochloric acid solution in the step (4) is 0.1mol/L, and the acid washing time is 12 h.
And (5) roasting at the temperature of 400-550 ℃ for 1-3 h.
Compared with the prior art, the invention has the following advantages:
1. simple formula, scientific design and low cost.
2. The product takes a titanium sheet as a substrate, has good conductivity, and the nanotube film grows in situ on a titanium substrate, and has good associativity.
3. The obtained product has high specific surface area and high photoelectrochemical property.
Drawings
FIG. 1 shows TiO after oxydol oxidation in example 12Scanning electron microscope pictures of the thin film;
FIG. 2 shows TiO prepared in example 12An X-ray diffraction pattern of the nanotube film;
FIG. 3 shows TiO oxidized with hydrogen peroxide in example 22Scanning electron microscope pictures of the thin film;
FIG. 4 shows TiO prepared after hydrothermal reaction in example 22Scanning electron microscope pictures of nanotube films;
FIG. 5 shows TiO after oxydol oxidation in example 32Scanning electron microscope pictures of the thin film;
FIG. 6 shows TiO prepared in example 12Nanotube film transient photocurrent diagram;
FIG. 7 shows TiO prepared in example 32Nanotube film transient photocurrent diagrams.
Detailed Description
The present invention is further illustrated by the following specific embodiments. The following examples are only some embodiments of the present invention, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
Example 1
(1) Pretreatment of titanium sheets
Cutting a high-purity titanium sheet into a size of 5cm x 1cm, then respectively polishing the titanium sheet by using coarse and fine abrasive paper, and then cleaning the titanium sheet by using deionized water;
ultrasonically cleaning the polished titanium sheet for 15 minutes by using acetone and absolute ethyl alcohol respectively, removing an oxide layer and grease on the surface of the titanium sheet, and cleaning the titanium sheet by using deionized water;
at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
(2) Hydrogen peroxide titanium oxide sheet
The treated titanium sheet is put into a culture dish filled with 30ml of hydrogen peroxide (with the concentration of 30 percent), and the heat preservation reaction is carried out for 6 hours in a drying oven at the temperature of 80 ℃. And taking out after the reaction is finished, washing with deionized water, and drying for later use.
(3) Hydrothermal reaction
And (3) putting the titanium sheet after the reaction into a hydrothermal reaction kettle filled with 30ml of NaOH solution (with the concentration of 10mol/L), putting the hydrothermal reaction kettle into a drying oven, and heating to 140 ℃ for reaction for 6 hours.
(4) Acid pickling process
And taking out the reaction kettle after the hydrothermal reaction is finished, cooling to room temperature, and taking out the titanium sheet. And (3) soaking the titanium sheet in 0.1mol/L hydrochloric acid solution for 12 hours, taking out, washing with deionized water, and drying for later use.
(5) Thermal treatment
Roasting the dried titanium sheet in a muffle furnace at 450 ℃ for 1 hour, cooling the titanium sheet to room temperature along with the furnace, and taking out the titanium sheet to obtain anatase-phase TiO2A nanotube film.
FIG. 1 shows that the product obtained in step (2) is TiO2Thin film, indicating that a dense, uniform oxide film was formed on the titanium substrate. FIG. 2 illustrates the anatase phase TiO obtained after the heat treatment of step (5)2. FIG. 6 shows TiO in example 12Nanotube film strip for simulating sun illuminationAnd (3) testing the transient photocurrent under the test condition, wherein the electrolyte is a 1mol/L KOH solution, and the obtained product has good photoelectric response characteristics.
Example 2
(1) Pretreatment of titanium sheets
Cutting a high-purity titanium sheet into a size of 5cm x 1cm, then respectively polishing the titanium sheet by using coarse and fine abrasive paper, and then cleaning the titanium sheet by using deionized water;
ultrasonically cleaning the polished titanium sheet for 15 minutes by using acetone and absolute ethyl alcohol respectively, removing an oxide layer and grease on the surface of the titanium sheet, and cleaning the titanium sheet by using deionized water;
at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
(2) Hydrogen peroxide titanium oxide sheet
The treated titanium sheet is put into a culture dish filled with 30ml of hydrogen peroxide (with the concentration of 30 percent), and the heat preservation reaction is carried out for 4 hours in a drying oven at the temperature of 80 ℃. And taking out after the reaction is finished, washing with deionized water, and drying for later use.
(3) Hydrothermal reaction
And (3) putting the titanium sheet after the reaction into a hydrothermal reaction kettle filled with 30ml of NaOH solution (with the concentration of 10mol/L), putting the hydrothermal reaction kettle into a drying oven, and heating to 140 ℃ for reaction for 6 hours.
(4) Acid pickling process
And taking out the reaction kettle after the hydrothermal reaction is finished, cooling to room temperature, and taking out the titanium sheet. And (3) soaking the titanium sheet in 0.1mol/L hydrochloric acid solution for 12 hours, taking out, washing with deionized water, and drying for later use.
(5) Thermal treatment
Roasting the dried titanium sheet in a muffle furnace at 450 ℃ for 1 hour, cooling the titanium sheet to room temperature along with the furnace, and taking out the titanium sheet to obtain anatase-phase TiO2A nanotube film.
FIG. 3 shows that TiO is obtained in step (2)2Oxide film, FIG. 4 shows TiO obtained in step (3)2Typical morphology of nanotube films.
Example 3
(1) Pretreatment of titanium sheets
Cutting a high-purity titanium sheet into a size of 5cm x 1cm, then respectively polishing the titanium sheet by using coarse and fine abrasive paper, and then cleaning the titanium sheet by using deionized water;
ultrasonically cleaning the polished titanium sheet for 15 minutes by using acetone and absolute ethyl alcohol respectively, removing an oxide layer and grease on the surface of the titanium sheet, and cleaning the titanium sheet by using deionized water;
at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
(2) Hydrogen peroxide titanium oxide sheet
The treated titanium sheet is put into a culture dish filled with 30ml of hydrogen peroxide (with the concentration of 30 percent), and the heat preservation reaction is carried out for 2 hours in a drying oven at the temperature of 80 ℃. And taking out after the reaction is finished, washing with deionized water, and drying for later use.
(3) Hydrothermal reaction
And (3) putting the titanium sheet after the reaction into a hydrothermal reaction kettle filled with 30ml of NaOH solution (with the concentration of 10mol/L), putting the hydrothermal reaction kettle into a drying oven, and heating to 140 ℃ for reaction for 6 hours.
(4) Acid pickling process
And taking out the reaction kettle after the hydrothermal reaction is finished, cooling to room temperature, and taking out the titanium sheet. And (3) soaking the titanium sheet in 0.1mol/L hydrochloric acid solution for 12 hours, taking out, washing with deionized water, and drying for later use.
(5) Thermal treatment
Roasting the dried titanium sheet in a muffle furnace at 450 ℃ for 1 hour, cooling the titanium sheet to room temperature along with the furnace, and taking out the titanium sheet to obtain anatase-phase TiO2A nanotube film.
FIG. 5 shows the dense TiO obtained in step (2)2And (3) film appearance. FIG. 7 shows TiO in example 32The transient photocurrent of the nanotube film measured under the condition of simulating solar illumination is tested, and the electrolyte is a KOH solution with the concentration of 1mol/L, which shows that the obtained product has good photoelectrochemical properties.
Example 4
(1) Pretreatment of titanium sheets
Cutting a high-purity titanium sheet into a size of 5cm x 1cm, then respectively polishing the titanium sheet by using coarse and fine abrasive paper, and then cleaning the titanium sheet by using deionized water;
ultrasonically cleaning the polished titanium sheet for 15 minutes by using acetone and absolute ethyl alcohol respectively, removing an oxide layer and grease on the surface of the titanium sheet, and cleaning the titanium sheet by using deionized water;
at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
(2) Hydrogen peroxide titanium oxide sheet
The treated titanium sheet is put into a culture dish filled with 30ml of hydrogen peroxide (with the concentration of 30 percent), and the heat preservation reaction is carried out for 10 hours in a drying oven at the temperature of 80 ℃. And taking out after the reaction is finished, washing with deionized water, and drying for later use.
(3) Hydrothermal reaction
And (3) putting the titanium sheet after the reaction into a hydrothermal reaction kettle filled with 30ml of NaOH solution (with the concentration of 10mol/L), putting the hydrothermal reaction kettle into a drying box, and heating to 150 ℃ for reaction for 1 hour.
(4) Acid pickling process
And taking out the reaction kettle after the hydrothermal reaction is finished, cooling to room temperature, and taking out the titanium sheet. And (3) soaking the titanium sheet in 0.1mol/L hydrochloric acid solution for 12 hours, taking out, washing with deionized water, and drying for later use.
(5) Thermal treatment
Roasting the dried titanium sheet in a muffle furnace at 400 ℃ for 2 hours, cooling the titanium sheet to room temperature along with the furnace, and taking out the titanium sheet to obtain anatase-phase TiO2A nanotube film.
Example 5
(1) Pretreatment of titanium sheets
Cutting a high-purity titanium sheet into a size of 5cm x 1cm, then respectively polishing the titanium sheet by using coarse and fine abrasive paper, and then cleaning the titanium sheet by using deionized water;
ultrasonically cleaning the polished titanium sheet for 15 minutes by using acetone and absolute ethyl alcohol respectively, removing an oxide layer and grease on the surface of the titanium sheet, and cleaning the titanium sheet by using deionized water;
at volume ratio of HNO3∶HF∶H2Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
(2) Hydrogen peroxide titanium oxide sheet
The treated titanium sheet is put into a culture dish filled with 30ml of hydrogen peroxide (with the concentration of 30 percent), and the heat preservation reaction is carried out for 15 hours in a drying oven at the temperature of 80 ℃. And taking out after the reaction is finished, washing with deionized water, and drying for later use.
(3) Hydrothermal reaction
And (3) putting the titanium sheet after the reaction into a hydrothermal reaction kettle filled with 30ml of NaOH solution (with the concentration of 10mol/L), putting the hydrothermal reaction kettle into a drying box, and heating to 170 ℃ for reaction for 3 hours.
(4) Acid pickling process
And taking out the reaction kettle after the hydrothermal reaction is finished, cooling to room temperature, and taking out the titanium sheet. And (3) soaking the titanium sheet in 0.1mol/L hydrochloric acid solution for 12 hours, taking out, washing with deionized water, and drying for later use.
(5) Thermal treatment
Roasting the dried titanium sheet in a muffle furnace at the temperature of 420 ℃ for 3 hours, cooling the titanium sheet to room temperature along with the furnace, and taking out the titanium sheet to obtain anatase-phase TiO2A nanotube film.
In conclusion, the titanium substrate of the invention is used for preparing anatase phase TiO2The preparation method of the nanotube film takes pure titanium sheets as a titanium source, and utilizes hydrogen peroxide to oxidize the titanium sheets at a certain temperature to generate a layer of TiO2Oxide film, and then formed TiO2Is a precursor, hydrothermal synthesis of a nanotube structure is carried out in a strong alkali solution under the conditions of high temperature and high pressure, and the TiO of anatase phase is obtained by acid washing and water washing processes and final roasting in a muffle furnace2A nanotube film.
Claims (7)
1. Anatase phase TiO prepared by titanium substrate2 A method of nanotube film, comprising the steps of:
(1) pretreatment: cutting a titanium sheet, grinding the titanium sheet by using sand paper, carrying out ultrasonic cleaning, and finally carrying out chemical polishing treatment;
(2) and (3) oxidation reaction: putting the pretreated titanium sheet into hydrogen peroxide for oxidation reaction, washing the titanium sheet with water after the reaction is finished, and drying the titanium sheet for later use, wherein the concentration of the hydrogen peroxide is 30%;
(3) hydrothermal reaction: putting the oxidized titanium sheet into a NaOH solution for hydrothermal reaction, taking out after the reaction is finished, cooling to room temperature for later use, wherein the concentration of the NaOH solution is 5-10 mol/L, the temperature of the hydrothermal reaction is 140-180 ℃, and the time is 1-6 h;
(4) acid washing: soaking the titanium sheet obtained in the step (3) in a hydrochloric acid solution, taking out, washing, and drying for later use;
(5) and (3) heat treatment: roasting the titanium sheet obtained in the step (4) by using a muffle furnace, cooling to room temperature, and taking out to obtain anatase-phase TiO2 A nanotube film.
2. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the titanium sheet obtained in the step (1) is cut to 5cm multiplied by 1 cm.
3. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the ultrasonic cleaning in the step (1) specifically comprises the following steps: ultrasonic cleaning with acetone and anhydrous ethanol for 15 min.
4. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the chemical polishing in the step (1) is specifically as follows: at volume ratio of HNO3 ∶HF∶H2 Chemical polishing treatment is carried out in a polishing solution with O being 1: 1 for 12 seconds, and the polishing solution is rinsed by a large amount of deionized water.
5. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the temperature of the oxidation reaction in the step (2) is 80 ℃, and the reaction time is 1-24 h.
6. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the concentration of the hydrochloric acid solution in the step (4) is 0.1mol/L, and the acid washing time is 12 hours.
7. Preparation of anatase phase TiO on a titanium substrate according to claim 12 The method for preparing the nanotube film is characterized in that the roasting temperature in the step (5) is 400-550 ℃, and the roasting time is 1-3 h.
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| CN112442688A (en) | 2021-03-05 |
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