CN110624527A - Preparation method of three-dimensional colored titanium dioxide photocatalytic material, product and application thereof - Google Patents
Preparation method of three-dimensional colored titanium dioxide photocatalytic material, product and application thereof Download PDFInfo
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- CN110624527A CN110624527A CN201910973646.0A CN201910973646A CN110624527A CN 110624527 A CN110624527 A CN 110624527A CN 201910973646 A CN201910973646 A CN 201910973646A CN 110624527 A CN110624527 A CN 110624527A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 42
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004098 Tetracycline Substances 0.000 claims abstract description 13
- 229960002180 tetracycline Drugs 0.000 claims abstract description 13
- 229930101283 tetracycline Natural products 0.000 claims abstract description 13
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 13
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 13
- 230000007547 defect Effects 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 230000002950 deficient Effects 0.000 claims abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910003081 TiO2−x Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention provides a preparation method of a three-dimensional colored titanium dioxide photocatalytic material, which prepares three-dimensional colored titanium dioxide TiO by a hydrothermal auxiliary high-temperature solid phase method2‑x(0<x is less than or equal to 1), and the oxygen-deficient defects play an important role in improving the photocatalytic performance of the material. The three-dimensional colored titanium dioxide photocatalytic material firstly balances the adsorption of the three-dimensional colored titanium dioxide to the tetracycline in the dark, and then degrades the tetracycline to 96.9 percent after 60min under the ultraviolet light catalysis condition. The preparation process is relatively simple and easy to operate.
Description
Technical Field
The invention belongs to the field of photocatalytic materials and preparation and application thereof, and particularly relates to a preparation method of a three-dimensional colored titanium dioxide photocatalytic material, a product and application thereof.
Background
With the development of chemical industry, environmental pollution is becoming more serious. The discharge of printing and dyeing wastewater is one of the important causes of water pollution. Every year, a large amount of commercial dyes are discharged, and the dyes are stable in chemical property and cause great damage to the ecological environment. By utilizing the characteristic that the semiconductor oxide material can be activated under the irradiation of sunlight, organic matters can be effectively oxidized and degraded into carbon dioxide, water and other small molecules. Compared with the traditional purification method, the semiconductor photocatalysis technology has the advantages of mild reaction conditions, no secondary pollution, simple operation, obvious degradation effect and the like. Titanium dioxide is one of the most interesting photocatalysts, which is low-toxic, low-cost, durable, superhydrophilic and has excellent photochemical stability.
Titanium dioxide (TiO)2) The TiO is attracted attention as a photocatalytic material under the condition of illumination2Can oxidize organic pollutants in water, and makes the photocatalysis technology have great breakthrough in the field of treating organic pollutants in water phase and gas phase. Since then, photocatalytic degradation of organic pollutants has become one of the hot areas.
To improve TiO2As the catalytic efficiency of the photocatalyst, various means have been used to modify the material. Wherein, the surface oxygen defect generates lower state density at the top of the valence band, which increases the top of the valence band, leads to the broadening of the valence band and the reduction of forbidden bandwidth, thereby improving the ultraviolet light catalytic activity and generating visible light activity (the titanium dioxide with the surface oxygen defect is called as colored titanium dioxide).
The invention provides a preparation method of a three-dimensional colored titanium dioxide photocatalytic material, which prepares three-dimensional colored titanium dioxide TiO by a hydrothermal auxiliary high-temperature solid phase method2-x(0<x is less than or equal to 1), and the oxygen-deficient defects play an important role in improving the photocatalytic performance of the material. The preparation process is relatively simple and easy to operate.
Disclosure of Invention
Aiming at the defect that the existing titanium dioxide photocatalysis performance is not high enough, the invention aims to provide a preparation method of a three-dimensional colored titanium dioxide photocatalysis material.
Yet another object of the present invention is to: provides a three-dimensional colored titanium dioxide photocatalytic material product obtained by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a three-dimensional colored titanium dioxide photocatalytic material is characterized in that a hydrothermal auxiliary high-temperature solid phase method is used for preparing three-dimensional colored titanium dioxide TiO2-x(0<x is less than or equal to 1), the oxygen-deficient defect plays an important role in improving the photocatalytic performance of the material, and the method comprises the following specific steps:
(1) placing the titanium mesh in 20 mL of 1-2 mol/L aqueous alkali, standing for 0.5-1 h, then transferring the titanium mesh into a reaction kettle for reaction at 180 ℃ for 6-8 h to obtain A, washing the A for a plurality of times by using ethanol and deionized water, and drying the A in an oven at 80-100 ℃;
(2) soaking the A in 1-2 mol/L acid solution, standing for 10-30 min, taking out the titanium mesh from the acid solution, washing with ethanol and deionized water for several times, and drying in an oven at 80-100 deg.C to obtain B;
(3) calcining the B in a muffle furnace at the temperature rise rate of 2-5 ℃/min of 400-3+Of TiO 22;
(4) Will be doped with Ti3+Of TiO 22Calcining the mixture in a muffle furnace at the temperature of 400 ℃ and 500 ℃ for 2 to 5 hours to obtain pure TiO2;
(5) Mixing pure TiO2Calcining the mixture in a hydrogen atmosphere at the temperature rise and temperature drop speed of 1-2 ℃/min at the temperature of 300-400 ℃ for 1-2 h to obtain TiO2-x(0<x≤1)。
The alkali solution is one or the combination of a sodium hydroxide solution and a potassium hydroxide solution.
The acid solution is one or the combination of hydrochloric acid, nitric acid and sulfuric acid.
The invention provides a three-dimensional colored titanium dioxide photocatalytic material prepared by any one of the methods.
The invention provides an application of a three-dimensional colored titanium dioxide photocatalytic material in tetracycline wastewater treatment.
The three-dimensional colored titanium dioxide photocatalytic material firstly balances the adsorption of the three-dimensional colored titanium dioxide to the tetracycline in the dark, and then degrades the tetracycline to 96.9 percent after 60min under the ultraviolet light catalysis condition. The preparation process is relatively simple and easy to operate.
Has the advantages that:
the invention provides a preparation method of a three-dimensional colored titanium dioxide photocatalytic material, which prepares three-dimensional colored titanium dioxide TiO by a hydrothermal auxiliary high-temperature solid phase method2-x(0<x is less than or equal to 1), and the oxygen-deficient defects play an important role in improving the photocatalytic performance of the material. The preparation process is relatively simple and easy to operate, and the degradation rate of the tetracycline reaches over 96 percent.
Drawings
FIG. 1 is a diagram of the UV photocatalytic degradation of a three-dimensional colored titanium dioxide photocatalytic material of example 1;
FIG. 2 is a diagram showing the ultraviolet photocatalytic degradation of the three-dimensional colored titanium dioxide photocatalytic material of example 2;
FIG. 3 is a diagram of the UV photocatalytic degradation of the three-dimensional colored titanium dioxide photocatalytic material of example 3.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A three-dimensional colored titanium dioxide photocatalytic material is prepared by a hydrothermal-assisted high-temperature solid phase method2-x(0<x is less than or equal to 1), the oxygen-deficient defect plays an important role in improving the photocatalytic performance of the material, and the method comprises the following steps:
(1) placing the titanium mesh in 20 mL of 1mol/L sodium hydroxide alkali solution, standing for 0.5-1 h, then transferring into a reaction kettle for reaction for 8 h at 160 ℃ to obtain a titanium mesh A, washing the titanium mesh A with ethanol and deionized water for several times, and drying in an oven at 80 ℃;
(2) soaking the titanium mesh A in a hydrochloric acid solution with the concentration of 1mol/L, standing for 20min, taking the titanium mesh out of the hydrochloric acid solution, washing the titanium mesh A with ethanol and deionized water for a plurality of times, and drying the titanium mesh A in an oven at 80 ℃ to obtain a titanium mesh B;
(3) calcining the titanium mesh B in a muffle furnace at the temperature rise rate of 2 ℃/min and the temperature of 500 ℃ for 3h to obtain the doped materialHetero Ti3+Of TiO 22;
(4) Will be doped with Ti3+Of TiO 22Placing in a muffle furnace, calcining for 3h at 500 ℃ to obtain pure TiO2;
(5) Mixing pure TiO2Calcining at 300 deg.C for 2 h at 2 deg.C/min in hydrogen atmosphere to obtain TiO2-x(0<x is less than or equal to 1). Fig. 1 is a graph of ultraviolet light catalyzed degradation of the three-dimensional colored titanium dioxide photocatalytic material in this example 1, in which in the dark, the adsorption of the three-dimensional colored titanium dioxide to tetracycline is balanced, and then under the ultraviolet light catalysis condition, after 60min, the degradation of tetracycline is 97.3%.
Example 2
A three-dimensional colored titanium dioxide photocatalytic material, similar to example 1, comprising the following steps:
(1) placing the titanium mesh in 20 mL of 1mol/L potassium hydroxide alkali solution, standing for 1h, then transferring the solution into a reaction kettle for reaction at 180 ℃ for 6h to obtain a titanium mesh A, washing the titanium mesh A with ethanol and deionized water for a plurality of times, and drying in an oven at 80 ℃;
(2) soaking the titanium mesh A in a nitric acid solution with the concentration of 1mol/L, standing for 20min, taking the titanium mesh out of the nitric acid solution, washing the titanium mesh A with ethanol and deionized water for a plurality of times, and drying the titanium mesh A in an oven at 80 ℃ to obtain a titanium mesh B;
(3) calcining the titanium mesh B in a muffle furnace at the temperature rise rate of 5 ℃/min and the temperature of 400 ℃ for 5 h to obtain doped Ti3+Of TiO 22;
(4) Will be doped with Ti3+Of TiO 22Placing in a muffle furnace, calcining for 5 h at 400 ℃ to obtain pure TiO2;
(5) Mixing pure TiO2Calcining at 300 deg.C for 2 h at 1 deg.C/min in hydrogen atmosphere to obtain TiO2-x(0<x is less than or equal to 1). Fig. 2 is a graph of ultraviolet photocatalytic degradation of the three-dimensional colored titanium dioxide photocatalytic material of this embodiment 2, in which in the dark, the adsorption of the three-dimensional colored titanium dioxide to tetracycline is balanced, and then under the ultraviolet photocatalytic condition, after 60min, the degradation of tetracycline is 96.9%.
Example 3
A three-dimensional colored titanium dioxide photocatalytic material, similar to example 1, comprising the following steps:
(1) placing the titanium mesh in 20 mL of 1mol/L sodium hydroxide alkali solution, standing for 1h, then transferring the solution into a reaction kettle for reaction at 180 ℃ for 6h to obtain a titanium mesh A, washing the titanium mesh A with ethanol and deionized water for a plurality of times, and drying in an oven at 80 ℃;
(2) soaking the titanium mesh A in a nitric acid solution with the concentration of 1mol/L, standing for 20min, taking the titanium mesh out of the nitric acid solution, washing the titanium mesh A with ethanol and deionized water for a plurality of times, and drying the titanium mesh A in an oven at 80 ℃ to obtain a titanium mesh B;
(3) calcining the titanium mesh B in a muffle furnace at the temperature rise rate of 3 ℃/min and the temperature of 400 ℃ for 5 h to obtain doped Ti3+Of TiO 22;
(4) Will be doped with Ti3+Of TiO 22Placing in a muffle furnace, calcining for 5 h at 400 ℃ to obtain pure TiO2;
(5) Mixing pure TiO2Calcining at 400 deg.C for 1h at 2 deg.C/min in hydrogen atmosphere to obtain TiO2-x(0<x is less than or equal to 1). Fig. 3 is a graph of ultraviolet photocatalytic degradation of the three-dimensional colored titanium dioxide photocatalytic material of example 3, in which the adsorption of the three-dimensional colored titanium dioxide to tetracycline is balanced in the dark, and then the degradation of tetracycline is 94% after 60min under the ultraviolet photocatalytic condition.
Claims (5)
1. The preparation method of the three-dimensional colored titanium dioxide photocatalytic material is characterized in that the three-dimensional colored titanium dioxide TiO is prepared by a hydrothermal-assisted high-temperature solid phase method2-x(0<x is less than or equal to 1), the oxygen-deficient defects play an important role in improving the photocatalytic performance of the material, and the method comprises the following steps:
(1) placing the titanium mesh in 20 mL of 1-2 mol/L aqueous alkali, standing for 0.5-1 h, then transferring the solution into a reaction kettle for reaction at 180 ℃ for 6-8 h to obtain a titanium mesh A, washing the titanium mesh A for a plurality of times by using ethanol and deionized water, and drying the titanium mesh A in an oven at 80-100 ℃;
(2) soaking the titanium mesh A in an acid solution with the concentration of 1-2 mol/L, standing for 10-30 min, taking the titanium mesh out of the acid solution, washing with ethanol and deionized water for several times, and drying in an oven at 80-100 ℃ to obtain a titanium mesh B;
(3) calcining the titanium mesh B in a muffle furnace at the temperature rise rate of 2-5 ℃/min of 400-3+Of TiO 22;
(4) Will be doped with Ti3+Of TiO 22Calcining the mixture in a muffle furnace at the temperature of 400 ℃ and 500 ℃ for 2 to 5 hours to obtain pure TiO2;
(5) Mixing pure TiO2Calcining the mixture in a hydrogen atmosphere at the temperature rise and temperature drop speed of 1-2 ℃/min at the temperature of 300-400 ℃ for 1-2 h to obtain TiO2-x(0<x≤1)。
2. The method for preparing a three-dimensional colored titanium dioxide photocatalytic material according to claim 1, wherein the alkali solution is one or a combination of a sodium hydroxide solution and a potassium hydroxide solution.
3. The method for preparing a three-dimensional colored titanium dioxide photocatalytic material according to claim 1, wherein the acid solution is one or a combination of hydrochloric acid, nitric acid and sulfuric acid.
4. A three-dimensional colored titanium dioxide photocatalytic material characterized by being prepared according to the method of any one of claims 1 to 3.
5. Use of the three-dimensional colored titanium dioxide photocatalytic material according to claim 4 in tetracycline wastewater treatment.
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Cited By (3)
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CN112591792A (en) * | 2020-12-30 | 2021-04-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Simple preparation method of colored titanium dioxide for photocatalysis |
CN113617347A (en) * | 2021-08-19 | 2021-11-09 | 生工生物工程(上海)股份有限公司 | Photocatalytic filter screen, air purifier and preparation method of photocatalytic filter screen |
CN116078366A (en) * | 2022-12-20 | 2023-05-09 | 济南大学 | Aluminum-based oxide doped titanium dioxide and preparation method and application thereof |
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