CN113957506B - Preparation method of rutile type titanium dioxide plate - Google Patents
Preparation method of rutile type titanium dioxide plate Download PDFInfo
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- CN113957506B CN113957506B CN202111475587.8A CN202111475587A CN113957506B CN 113957506 B CN113957506 B CN 113957506B CN 202111475587 A CN202111475587 A CN 202111475587A CN 113957506 B CN113957506 B CN 113957506B
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- titanium dioxide
- rutile type
- sheet
- titanium
- type titanium
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 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 16
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 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
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-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
- 239000003792 electrolyte Substances 0.000 claims description 5
- AAORDHMTTHGXCV-UHFFFAOYSA-N uranium(6+) Chemical compound [U+6] AAORDHMTTHGXCV-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004064 recycling 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 1
Classifications
-
- 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
Abstract
The invention provides a preparation method of a rutile type titanium dioxide plate, and belongs to the technical field of material preparation. The method comprises the following steps: (1) Taking a titanium sheet as an anode, taking an inert material as a cathode, and carrying out electrochemical oxidation to obtain a titanium sheet with a titanium dioxide film loaded on the surface; (2) And (3) annealing the titanium sheet with the titanium dioxide film on the surface, and then ultrasonically cleaning and drying the titanium sheet in deionized water to obtain the rutile type titanium dioxide plate. The method is simple to operate, good in controllability, and the formed rutile type titanium dioxide film is firmly combined with the titanium substrate, so that the method is suitable for being used in the field of photocatalysis or in 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 type 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. Titanium dioxide powder (titanium dioxide) has been widely used in the fields of solar cells, photocatalysis, photosensitive devices, sensors, and the like in recent years. However, titanium dioxide powder has limited applications due to its poor stability, difficulty in separation, difficulty in recycling, and the like.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a rutile type titanium dioxide board, so as to solve the problems existing in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the preparation method of the rutile type titanium dioxide plate comprises the following steps:
(1) Taking a titanium sheet as an anode, taking an inert material as a cathode, and carrying out electrochemical oxidation to obtain a titanium sheet with a titanium dioxide film loaded on the surface;
(2) And (3) annealing the titanium sheet with the titanium dioxide film 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 being used, and the specific steps are as follows: the titanium sheet was respectively placed in isopropyl alcohol, acetone, 5wt% nitric acid, and deionized water for ultrasonic cleaning for 15min.
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 anode and the cathode is 3cm, and the voltage is 10-30V by adopting a direct current power supply.
Further, the electrolyte solution for electrochemical oxidation in the step (1) is prepared by the following steps: ammonium fluoride and ammonium sulfate are used as solutes, water is used as a solvent, and the electrolyte is used in an amount which is as much as the cathode and anode are not used.
Further, the ammonium fluoride concentration was 0.15mol/L, and the ammonium sulfate concentration was 1mol/L.
Further, the annealing treatment in the step (2) is as follows: the heating rate is 2 ℃/min, and the temperature is raised to 900-950 ℃ for annealing for 30min.
The invention also provides the rutile type titanium dioxide board obtained by the preparation method.
The invention also provides application of the rutile type titanium dioxide plate in the field of photocatalysis or in photoelectric components.
Compared with the prior art, the invention has the beneficial effects that:
the process for in-situ anodic oxidation annealing by taking the titanium sheet as the substrate has the characteristics 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-redox desorption of reaction products deposited on the surface of 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, easiness in operation and low cost, and is beneficial to being used in photocatalysis and photoelectric equipment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope picture of a rutile titanium dioxide board prepared in example 1 of the present invention;
FIG. 2 is a graph showing the result of X-ray diffraction characterization of the rutile titanium dioxide board prepared in example 1 of the present invention;
fig. 3 is a diagram of a reaction system for removing uranium (VI) in water by photocatalysis using the rutile type titanium dioxide sheet prepared in example 1 of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions 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. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 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 invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
A preparation process of a rutile type titanium dioxide plate comprises the following steps: the titanium sheet is sequentially ultrasonically cleaned by isopropanol, acetone, 5wt% nitric acid and deionized water, and dried for standby.
Preparing an electrolyte: the solute is ammonium fluoride, ammonium sulfate and the solvent is water.
Preparing a two-electrode system electrolytic cell, wherein a titanium sheet is used as an anode, an inert material is used as a cathode, a direct current power supply is connected to perform electrochemical anodic oxidation, a titanium dioxide film can be generated on the anode titanium sheet, and the titanium sheet is annealed at 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 substrate into the size of 3cm x 3.5 cm.
(2) Sequentially ultrasonically cleaning the surface of a titanium sheet with isopropanol, acetone, 5wt% nitric acid and deionized water for 15min, removing impurities such as oxides and organic matters 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 electrolyte is used in an amount which is based on the condition that the electrode is not used.
(4) Preparing a two-electrode system electrolytic cell, taking a titanium sheet as an anode, taking the titanium sheet as a cathode, setting the interval between the anode and the cathode to be 3cm, setting the voltage to be 15V, switching on a direct current power supply to perform electrochemical oxidation, and forming a titanium dioxide film on the surface of the titanium sheet for 2 hours.
(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 picture of the rutile type titanium dioxide sheet prepared in example 1. As can be seen from FIG. 1, the flaky rutile type titanium dioxide is formed, is tightly coated on the surface of a titanium sheet, is not easy to peel off, and has good stability.
FIG. 2 is a graph showing the result of X-ray diffraction characterization of the rutile titanium dioxide slab prepared in example 1. As can be seen from fig. 2, characteristic diffraction peaks of the rutile titanium dioxide are obtained at 2θ=27.4, 36.0, 39.2, 41.2, 54.3, 56.6, 62.7, 64.0, 69.0, indicating that the synthesized material is a rutile titanium dioxide nano-array.
Example 2
The difference is that the annealing temperature is 950℃as in example 1.
It can be found that the rutile type titanium dioxide nano-array can be stably synthesized by adjusting the temperature.
Example 3
The difference from example 1 is that a platinum sheet electrode is used as the cathode.
It was found that the rutile titanium dioxide nanoarray could be stably synthesized as well by substitution of the cathode material.
Test example 1
The rutile type titanium dioxide plate prepared in the example 1 is applied to the field of photocatalysis to remove uranium (VI) in water, uranium (VI) solution is prepared by uranyl nitrate, the concentration is 0.05mmol/L, the volume is 60ml, an ultraviolet lamp is adopted as a light source, the initial pH=5.2 is adopted, the reaction is carried out for 12 hours, and the graph of a reaction system is shown in FIG. 3. The removal rate of the rutile type titanium dioxide plate to uranium (VI) in water is 98.7%.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (2)
1. The application of the rutile type titanium dioxide plate in the field of photocatalysis or photoelectric components is characterized in that uranium (VI) in water is removed by adopting the rutile type titanium dioxide plate;
the preparation method of the rutile type titanium dioxide plate comprises the following steps:
(1) Taking a titanium sheet as an anode, taking an inert material as a cathode, and carrying out electrochemical oxidation to obtain a titanium sheet with a titanium dioxide film loaded on the surface;
(2) Annealing the titanium sheet with the titanium dioxide film on the surface, then ultrasonically cleaning in deionized water, and drying to obtain a rutile type titanium dioxide plate;
the titanium sheet in the step (1) is pretreated before being used, and the specific steps are as follows: respectively placing the titanium sheet in isopropanol, acetone, 5wt% nitric acid and deionized water for ultrasonic cleaning for 15min;
the electrolyte solution for electrochemical oxidation in the step (1) is prepared by the following steps: ammonium fluoride and ammonium sulfate are used as solutes, water is used as a solvent, and the use amount of electrolyte is based on the condition that the cathode and the anode are not used;
the annealing treatment in the step (2) is as follows: heating to 900-950 ℃ at a heating rate of 2 ℃/min, and annealing for 30min;
the electrochemical oxidation time in the step (1) is 2 hours, the distance between the anode and the cathode is 3cm, a direct current power supply is adopted, and the voltage is 10-15V;
the concentration of ammonium fluoride is 0.15mol/L, and the concentration of ammonium sulfate is 1mol/L.
2. The use of claim 1, wherein the inert material of step (1) comprises one of graphite, platinum sheet, titanium sheet.
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|---|---|---|---|---|
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| JP2017222892A (en) * | 2016-06-13 | 2017-12-21 | 新日鐵住金株式会社 | Titanium material and manufacturing method of titanium material |
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| CN110747451A (en) * | 2019-11-04 | 2020-02-04 | 浙江工业大学 | Method for in-situ preparation of high-energy crystal face preferred rutile type titanium dioxide film |
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| JP5584923B2 (en) * | 2008-06-27 | 2014-09-10 | 国立大学法人東北大学 | Rutile type titanium dioxide photocatalyst |
| US20110303552A1 (en) * | 2009-01-12 | 2011-12-15 | Rajeshkumar Shankar Hyam | One step electrochemical process for the synthesis of pure rutile titanium dioxide nanoneedles |
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2021
- 2021-12-06 CN CN202111475587.8A patent/CN113957506B/en active Active
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| CN101307479A (en) * | 2008-01-31 | 2008-11-19 | 上海交通大学 | TiO2 nanometer pore array material preparation method and uses thereof |
| JP2017222892A (en) * | 2016-06-13 | 2017-12-21 | 新日鐵住金株式会社 | Titanium material and manufacturing method of titanium material |
| CN110230084A (en) * | 2019-04-15 | 2019-09-13 | 清华大学 | Titanium surface polycrystalline structure forming method and system based on femtosecond laser annealing |
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