CN113957506A - Preparation method of rutile type titanium dioxide plate - Google Patents
Preparation method of rutile type titanium dioxide plate Download PDFInfo
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- CN113957506A CN113957506A CN202111475587.8A CN202111475587A CN113957506A CN 113957506 A CN113957506 A CN 113957506A CN 202111475587 A CN202111475587 A CN 202111475587A CN 113957506 A CN113957506 A CN 113957506A
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- titanium dioxide
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- titanium
- rutile type
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 33
- 239000010936 titanium Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 8
- 230000001699 photocatalysis Effects 0.000 claims abstract description 7
- 238000007146 photocatalysis Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003792 electrolyte Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000005693 optoelectronics Effects 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 6
- AAORDHMTTHGXCV-UHFFFAOYSA-N uranium(6+) Chemical compound [U+6] AAORDHMTTHGXCV-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Hybrid Cells (AREA)
Abstract
The invention provides a preparation method of a rutile type titanium dioxide plate, belonging to the technical field of material preparation. The method comprises the following steps: (1) carrying out electrochemical oxidation by taking a titanium sheet as an anode and an inert material as a cathode to obtain the titanium sheet with the surface loaded with the titanium dioxide film; (2) and annealing the titanium sheet with the titanium dioxide film loaded on the surface, and then ultrasonically cleaning and drying in deionized water to obtain the rutile type titanium dioxide plate. The method has the advantages of simple operation and good controllability, and the formed rutile type titanium dioxide film is firmly combined with the titanium substrate and is suitable for being used in the field of photocatalysis or photoelectric components.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of a rutile titanium dioxide plate.
Background
Titanium dioxide is an important semiconductor material, and has the characteristics of stable chemical property, safety, no toxicity, high redox capability, low cost and the like, which are widely regarded. In recent years, titanium dioxide powder (titanium dioxide) is widely applied to the fields of solar cells, photocatalysis, photosensitive devices, sensors and the like. However, the titanium dioxide powder has the defects of poor stability, difficulty in separation, difficulty in recovery and the like, so that the application of the titanium dioxide powder is limited.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a rutile titanium dioxide plate, so as to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a rutile type titanium dioxide plate comprises the following steps:
(1) carrying out electrochemical oxidation by taking a titanium sheet as an anode and an inert material as a cathode to obtain the titanium sheet with the surface loaded with the titanium dioxide film;
(2) and annealing the titanium sheet with the titanium dioxide film loaded on the surface, then ultrasonically cleaning in deionized water, and drying to obtain the rutile type titanium dioxide plate.
Further, the titanium sheet in the step (1) is pretreated before use, and the method specifically comprises the following steps: and (3) respectively placing the titanium sheet in isopropanol, acetone, 5 wt% nitric acid and deionized water, and ultrasonically cleaning for 15 min.
Further, the inert material in the step (1) comprises one of graphite, platinum sheet and titanium sheet.
Further, the electrochemical oxidation time in the step (1) is 2 hours, the distance between the cathode and the anode is 3cm, a direct current power supply is adopted, and the voltage is 10-30V.
Further, the preparation method of the electrolyte used in the electrochemical oxidation in the step (1) comprises the following steps: ammonium fluoride and ammonium sulfate are used as solutes, water is used as a solvent, and the use amount of the electrolyte is based on that the electrolyte submerges the cathode and the anode.
Further, the concentration of the ammonium fluoride is 0.15mol/L, and the concentration of the ammonium sulfate is 1 mol/L.
Further, the annealing treatment in the step (2) is as follows: the heating rate is 2 ℃/min, and the annealing is carried out for 30min when the temperature is increased to 900 ℃ and 950 ℃.
The invention also provides a rutile type titanium dioxide plate obtained by the preparation method.
The invention also provides the application of the rutile type titanium dioxide plate in the field of photocatalysis or photoelectric components.
Compared with the prior art, the invention has the beneficial effects that:
the process for carrying out in-situ anodic oxidation annealing by using the titanium sheet as the substrate has the characteristic of simple preparation process, and the obtained titanium dioxide film is tightly combined with the titanium sheet substrate, is not easy to peel off and has good stability. The titanium sheet is used as a substrate, has good conductivity, and provides conditions for electro-oxidation-reduction desorption of reaction products deposited on the surface of the titanium dioxide. The rutile type titanium dioxide plate is prepared by in-situ oxidation annealing on the titanium plate substrate, and the implementation method has the characteristics of simplicity, easy operation and low cost, and is favorable for being used in photocatalysis and photoelectric devices.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described 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 without creative efforts.
FIG. 1 is a scanning electron microscope image of a rutile titanium dioxide plate prepared in example 1 of the present invention;
FIG. 2 is a photograph showing the results of X-ray diffraction characterization of rutile titanium dioxide plate prepared in example 1 of the present invention;
FIG. 3 is a diagram of a reaction system for removing uranium (VI) from water by photocatalysis using rutile type titanium dioxide plates prepared in example 1 of the invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
A preparation process of a rutile type titanium dioxide plate comprises the following steps: and ultrasonically cleaning the titanium sheet by using isopropanol, acetone, 5 wt% nitric acid and deionized water in sequence, and drying for later use.
Preparing an electrolyte: the solute is ammonium fluoride and ammonium sulfate, and the solvent is water.
Preparing an electrolytic cell with a two-electrode system, taking a titanium sheet as an anode and an inert material as a cathode, connecting a direct current power supply to perform electrochemical anodic oxidation, generating a titanium dioxide film on the anode titanium sheet, and annealing the titanium sheet at the temperature of 900-950 ℃ to obtain the rutile titanium dioxide plate.
Example 1
(1) Selecting a titanium sheet with the thickness of 0.3mm and the purity of 99.9% as a substrate, and cutting the titanium sheet into 3cm by 3.5 cm.
(2) And ultrasonically cleaning the surface of the titanium sheet for 15min by using isopropanol, acetone, 5 wt% nitric acid and deionized water in sequence, removing impurities such as oxides, organic matters and the like on the surface, and drying the cleaned titanium sheet for later use.
(3) Preparing an electrolyte: the solute is ammonium fluoride and ammonium sulfate, and the solvent is water. The concentration of ammonium fluoride is 0.15mol/L, the concentration of ammonium sulfate is 1mol/L, and the amount of electrolyte is based on the electrode.
(4) Preparing a two-electrode system electrolytic cell, taking a titanium sheet as an anode and a titanium sheet as a cathode, setting the distance between the cathode and the anode to be 3cm, setting the voltage to be 15V, switching on a direct current power supply to carry out electrochemical oxidation for 2h, and forming a titanium dioxide film on the surface of the titanium sheet.
(5) And (3) placing the titanium sheet with the titanium dioxide film on the surface in a muffle furnace, heating to 900 ℃ at a speed of 2 ℃/min, annealing for 30min, finally ultrasonically cleaning in deionized water, and drying to obtain the rutile type titanium dioxide plate.
FIG. 1 is a scanning electron microscope image of the rutile titanium dioxide plate prepared in example 1. As can be seen from figure 1, the rutile type titanium dioxide which forms the sheet shape is tightly coated on the surface of the titanium sheet, is not easy to strip and has good stability.
FIG. 2 is a photograph showing the X-ray diffraction characterization results of the rutile titanium dioxide plate prepared in example 1. As can be seen from fig. 2, characteristic diffraction peaks of rutile titanium dioxide were obtained at 2 θ of 27.4, 36.0, 39.2, 41.2, 54.3, 56.6, 62.7, 64.0, and 69.0, indicating that the synthesized material is a rutile titanium dioxide nanoarray.
Example 2
The difference from example 1 is that the annealing temperature is 950 ℃.
It can be found that the rutile type titanium dioxide nano-array can be stably synthesized through temperature adjustment.
Example 3
The difference from example 1 is that the cathode employs a platinum sheet electrode.
It can be found that the rutile type titanium dioxide nano-array can be stably synthesized through the replacement of the cathode material.
Test example 1
The rutile titanium dioxide plate prepared in example 1 is applied to the field of photocatalysis to remove uranium (VI) in water, a uranium (VI) solution is prepared from uranyl nitrate, the concentration is 0.05mmol/L, the volume is 60ml, an ultraviolet lamp is used as a light source, the initial pH is 5.2, the reaction is carried out for 12h, and fig. 3 is a reaction system diagram. The rutile titanium dioxide plate has a uranium (VI) removal rate of 98.7% in water.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a rutile type titanium dioxide plate is characterized by comprising the following steps:
(1) carrying out electrochemical oxidation by taking a titanium sheet as an anode and an inert material as a cathode to obtain the titanium sheet with the surface loaded with the titanium dioxide film;
(2) and annealing the titanium sheet with the titanium dioxide film loaded on the surface, then ultrasonically cleaning in deionized water, and drying to obtain the rutile type titanium dioxide plate.
2. The preparation method according to claim 1, wherein the titanium sheet in the step (1) is pretreated before use, and the method comprises the following specific steps: and (3) respectively placing the titanium sheet in isopropanol, acetone, 5 wt% nitric acid and deionized water, and ultrasonically cleaning for 15 min.
3. The method of claim 1, wherein the inert material of step (1) comprises one of graphite, platinum sheet, and titanium sheet.
4. The preparation method of claim 1, wherein the electrochemical oxidation time in step (1) is 2h, the distance between the cathode and the anode is 3cm, and a direct current power supply is adopted, and the voltage is 10-30V.
5. The preparation method according to claim 1, wherein the electrolyte for the electrochemical oxidation in step (1) is prepared by: ammonium fluoride and ammonium sulfate are used as solutes, water is used as a solvent, and the use amount of the electrolyte is based on that the electrolyte submerges the cathode and the anode.
6. The method according to claim 5, wherein the ammonium fluoride concentration is 0.15mol/L and the ammonium sulfate concentration is 1 mol/L.
7. The method according to claim 1, wherein the annealing treatment of step (2) is: the heating rate is 2 ℃/min, and the annealing is carried out for 30min when the temperature is increased to 900 ℃ and 950 ℃.
8. A rutile titanium dioxide plate produced by the production process as claimed in any one of claims 1 to 7.
9. The rutile titanium dioxide plate of claim 8, in the field of photocatalysis or in optoelectronic devices.
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|---|---|---|---|---|
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-
2021
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