CN112939482A - TiO 22Nano needle film and preparation method thereof - Google Patents
TiO 22Nano needle film and preparation method thereof Download PDFInfo
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- CN112939482A CN112939482A CN202110057315.XA CN202110057315A CN112939482A CN 112939482 A CN112939482 A CN 112939482A CN 202110057315 A CN202110057315 A CN 202110057315A CN 112939482 A CN112939482 A CN 112939482A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
The invention belongs to the technical field of nano materials, and particularly relates to TiO2The preparation method of the nano needle film adopts high-activity titanium tetrachloride as a titanium source and obtains TiO by means of modification and other treatment means2A nano needle film, develops a new method for preparing TiO2The idea and the method of the nano needle film have simple preparation process and environment-friendly property, and the prepared TiO is2The nanoneedle film has controllable appearance, uniform height and good crystallinity of crystals, and provides a new material for the fields of photovoltaics, lithium batteries, biosensing and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to TiO2A nano needle film and a preparation method thereof.
Background
Titanium dioxide, also known as titanium white, can be used as a white inorganic pigment, has strong adhesion and is not easy to chemically change, and is widely applied to the industries of paint, plastics, papermaking, printing ink, chemical fiber, rubber, cosmetics and the like; the melting point is very high, and the method is also used for manufacturing refractory glass, glaze, enamel, pottery clay, high-temperature resistant experimental vessels and the like; it has good UV-screening effect, can be used as sunscreen agent to be added into textile fiber, and superfine titanium dioxide powder can be added into sunscreen cream to make sunscreen cosmetic.
TiO2The nano material has a plurality of excellent characteristics, for example, the nano titanium dioxide UG-T30D is an excellent lithium ion battery anode and cathode doped material, has the characteristics of low toxicity, low energy consumption, good stability, high rate, good lithium release reversibility and the like, has a good development prospect, and the synthesis and the morphology control of the titanium dioxide nano material become hot spots of current research.
At present, most titanium sources used for synthesizing titanium dioxide are esterified titanium, such as isopropyl titanate, butyl titanate and the like, and the hydrolysis process of the titanium sources is slow, and the reaction is mild, so that the titanium dioxide micro-nano material with controllable morphology can be obtained easily in the process of synthesizing titanium dioxide.
The research reports of titanium dioxide prepared by adopting titanium tetrachloride are more, but the titanium tetrachloride is very active, the reaction process is violent in the preparation process, the appearance is difficult to control, the prepared titanium dioxide material is mostly granular, and the preparation of the titanium dioxide nano material with controllable appearance by taking the titanium tetrachloride as a titanium source is a new challenge.
Disclosure of Invention
The present invention has been made to solve the above problems, and provides a TiO compound2The preparation method of the nano-needle film has simple preparation process and environment-friendly property, and the prepared TiO is2The nanoneedle film has controllable appearance, uniform height and good crystallinity of crystals, and provides a new material for the fields of photovoltaics, lithium batteries, biosensing and the like.
The invention is realized by adopting the following technical scheme:
s1, preparing low-activity titanate solution
Preparing titanium tetrachloride and ethylene glycol into a mixed solution according to a proportion, and stirring at room temperature to fully react and passivate the mixed solution to form a low-activity titanate solution;
preferably, in step S1, the ratio of titanium tetrachloride to ethanol is 1: 49.5-50.5;
in a further preferred embodiment, in step S1, the ratio of titanium tetrachloride to ethanol is 50 parts by volume;
s2, preparing titanium dioxide stock solution
Adding inorganic acid into the low-activity titanate solution, and fully stirring to prepare uniform titanium dioxide stock solution;
preferably, in step S2, the inorganic acid is hydrochloric acid;
in a further preferable scheme, the mass fraction of the hydrochloric acid is 18-22%; in a further preferable scheme, the mass fraction of the hydrochloric acid is 20-21%;
preferably, in the step S2, the stirring time is 15-20 min;
s3, adding an inducer
Adding selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding FTO conductive glass to obtain a reactant;
preferably, in step S3, the addition amount of selenourea is 30-50 mg per 1mL of the titanium dioxide stock solution.
In a further preferable scheme, in the step S3, the addition amount of the selenourea is 35-45 mg per 1mL of the titanium dioxide stock solution;
in a further preferable embodiment, in step S3, the addition amount of selenourea is 40mg per 1mL of the titanium dioxide stock solution;
in the invention, the existence of selenourea can modify the formed titanium dioxide nanocrystal, so that the titanium dioxide nanoarray forms a needle shape under the condition of low-concentration growth;
preferably, in step S3, the addition amount of the FTO conductive glass is 1-4 cm-2；
Further preferred embodimentsThe addition amount of the FTO conductive glass is 3cm-2；
In a further supplementary preferable scheme, the addition amount of the FTO conductive glass is 8-10 (+ -0.5) g;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle for reaction, collecting FTO conductive glass after the reaction is finished, annealing at high temperature, cooling, cleaning with absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film;
preferably, in the step S4, the reaction temperature in the high-pressure reaction kettle is 160-180 ℃;
in a further preferable scheme, in the step S4, the reaction temperature in the high-pressure reaction kettle is 170-175 ℃;
preferably, in step S4, the temperature of the high-temperature annealing is 450 to 500 ℃;
in a further preferable scheme, in the step S4, the temperature of the high-temperature annealing is 470-490 ℃;
in a further preferable embodiment, in the step S4, the high-temperature annealing time is 30 to 40 min.
The invention has the beneficial effects that:
1. the invention adopts high-activity titanium tetrachloride as a titanium source and obtains TiO by modification and other treatment means2A nano needle film, develops a new method for preparing TiO2The idea and the method of the nano needle film have simple preparation process and environment-friendly property, and the prepared TiO is2The nanoneedle film has controllable appearance, uniform height and good crystallinity of crystals, and provides a new material for the fields of photovoltaics, lithium batteries, biosensing and the like.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows rutile phase TiO prepared in example 1 of the present invention2Scanning electron microscope image of the section of the nano needle film.
FIG. 2 shows rutile phase TiO prepared in example 1 of the present invention2Nanoneedle thin film X-ray diffraction pattern.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
s1, preparing low-activity titanate solution
Mixing titanium tetrachloride and ethylene glycol according to the proportion of 1: 50mL of mixed solution is prepared according to the volume ratio of 50, and the mixed solution is stirred for 12 hours at room temperature to fully react and passivate to form low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding 30mL of hydrochloric acid with the mass fraction of 22% into the low-activity titanate solution, and stirring for 20min to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding 40mg/mL of selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding 1 piece of FTO conductive glass with the size of 3cm x 1cm to obtain a reactant;
optionally, in this embodiment, the weight of the FTO conductive glass is 8(± 0.5) g;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle at 180 DEG CReacting for 5h under the condition, collecting FTO conductive glass after the reaction is finished, annealing for 30min at the high temperature of 500 ℃, cooling, cleaning for 3 times by using absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film.
Example 2
s1, preparing low-activity titanate solution
Mixing titanium tetrachloride and ethylene glycol according to the proportion of 1: preparing 40mL of mixed solution according to the volume ratio of 49.5, and stirring for 12 hours at room temperature to fully react and passivate the mixed solution to form low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding 40mL of hydrochloric acid with the mass fraction of 18% into the low-activity titanate solution, and stirring for 15min to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding 30mg/mL of selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding 1 piece of FTO conductive glass with the size of 1cm x 1cm to obtain a reactant;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle, reacting for 6h at 160 ℃, collecting FTO conductive glass after the reaction is finished, annealing for 40min at 450 ℃, cooling, cleaning for 3 times by using absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film.
Example 3
TiO 22The preparation method of the nano needle film comprises the following steps:
s1, preparing low-activity titanate solution
Mixing titanium tetrachloride and ethylene glycol according to the proportion of 1: 50mL of mixed solution is prepared according to the volume ratio of 50.5, and the mixed solution is stirred for 12 hours at room temperature, so that the mixed solution is fully reacted and passivated to form low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding 30mL of hydrochloric acid with the mass fraction of 20% into the low-activity titanate solution, and stirring for 18min to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding 50mg/mL of selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding 1 piece of FTO conductive glass with the size of 3cm x 1cm to obtain a reactant;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle, reacting at 170 ℃ for 4h, collecting FTO conductive glass after the reaction is finished, annealing at 470 ℃ for 35min, cooling, cleaning with absolute ethyl alcohol for 3 times, and drying to obtain TiO2A nanoneedle film.
Example 4
TiO 22The preparation method of the nano needle film comprises the following steps:
s1, preparing low-activity titanate solution
Mixing titanium tetrachloride and ethylene glycol according to the proportion of 1: 50mL of mixed solution is prepared according to the volume ratio of 50, and the mixed solution is stirred for 12 hours at room temperature to fully react and passivate to form low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding 30mL of hydrochloric acid with the mass fraction of 21% into the low-activity titanate solution, and stirring for 20min to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding 35mg/mL of selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding 1 piece of FTO conductive glass with the size of 3cm x 1cm to obtain a reactant;
optionally, in this embodiment, the weight of the FTO conductive glass is 10(± 0.5) g;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle, reacting for 6h at 175 ℃, collecting FTO conductive glass after the reaction is finished, annealing for 40min at 490 ℃, cooling, cleaning for 3 times by using absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film.
Example 5
TiO 22The preparation method of the nano needle film comprises the following steps:
s1, preparing low-activity titanate solution
Mixing titanium tetrachloride and ethylene glycol according to the proportion of 1: 50mL of mixed solution is prepared according to the volume ratio of 50, and the mixed solution is stirred for 12 hours at room temperature to fully react and passivate to form low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding 30mL of hydrochloric acid with the mass fraction of 20% into the low-activity titanate solution, and stirring for 20min to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding 45mg/mL of selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding 1 piece of FTO conductive glass with the size of 4cm x 1cm to obtain a reactant;
optionally, in this embodiment, the weight of the FTO conductive glass is 10(± 0.5) g;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle, reacting for 6h at 175 ℃, collecting FTO conductive glass after the reaction is finished, annealing for 40min at 500 ℃, cooling, cleaning for 3 times by using absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film.
TiO prepared in the above examples2Nanoneedle films with similar property profiles to the TiO produced in example 12The nanoneedle films were tested as follows:
FIG. 1 shows rutile phase TiO prepared in example 1 of the present invention2The sectional scanning electron microscope image of the nano-needle film can be seen from figure 1, and the prepared TiO2The nano needle thin film is densely grown on the FTO conductive glass and is uniform in height, the tail end of a single nano rod becomes thin and is in an embroidered needle shape, the diameter of the nano rod is 80-100 nm, and the length of the nano rod is about 1 um;
FIG. 2 shows rutile phase TiO prepared in example 1 of the present invention2X-ray diffraction pattern of nano needle film, FIG. 2 shows that obtained by the present inventionThe titanium dioxide nanoneedle is in a rutile phase, the crystallinity of the crystal is good as shown by the intensity of an X-ray diffraction peak, and the growth direction tends to grow towards a (101) crystal face.
The invention is not limited to the above-described examples, and various modifications or alterations without inventive work may be made by those skilled in the art within the scope of the invention defined by the claims appended hereto.
Claims (10)
1. TiO 22The preparation method of the nano needle film is characterized by comprising the following steps:
s1, preparing low-activity titanate solution
Preparing titanium tetrachloride and ethylene glycol into a mixed solution according to a proportion, and stirring at room temperature to fully react and passivate the mixed solution to form a low-activity titanate solution;
s2, preparing titanium dioxide stock solution
Adding inorganic acid into the low-activity titanate solution, and fully stirring to prepare uniform titanium dioxide stock solution;
s3, adding an inducer
Adding selenourea into the titanium dioxide stock solution, fully stirring to completely dissolve the selenourea to form a uniform solution, and adding FTO conductive glass to obtain a reactant;
s4 preparation of TiO2Nanoneedle film
Placing the reactant in a high-pressure reaction kettle for reaction, collecting FTO conductive glass after the reaction is finished, annealing at high temperature, cooling, cleaning with absolute ethyl alcohol, and drying to obtain TiO2A nanoneedle film.
2. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S1, the ratio of titanium tetrachloride to ethanol is 1: 49.5 to 50.5.
3. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S2, the inorganic acid is hydrochloric acid, and the mass fraction of the hydrochloric acid isThe amount is 18-22%.
4. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S2, the stirring time is 15-20 min.
5. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in the step S3, the addition amount of the selenourea is that 30-50 mg of selenourea is added into every 1mL of the titanium dioxide stock solution.
6. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S3, the addition amount of the FTO conductive glass is 8-10 (+ -0.5) g.
7. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S3, the area of the FTO conductive glass is 1-4 cm-2。
8. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S4, the reaction temperature in the high-pressure reaction kettle is 160-180 ℃.
9. The TiO of claim 12The preparation method of the nano needle film is characterized by comprising the following steps: in step S4, the temperature of the high-temperature annealing is 450-500 ℃, and the time of the high-temperature annealing is 30-40 min.
10. TiO 22The nanoneedle film is characterized in that: the compound is prepared by any one method of the claims 1 to 9.
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