CN106582593B - Synthetic method of rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancy - Google Patents
Synthetic method of rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancy Download PDFInfo
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- CN106582593B CN106582593B CN201611159000.1A CN201611159000A CN106582593B CN 106582593 B CN106582593 B CN 106582593B CN 201611159000 A CN201611159000 A CN 201611159000A CN 106582593 B CN106582593 B CN 106582593B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 22
- 239000001301 oxygen Substances 0.000 title claims abstract description 22
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000010189 synthetic method Methods 0.000 title claims abstract description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N Titanium isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 31
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 17
- 239000004698 Polyethylene (PE) Substances 0.000 claims abstract description 17
- 239000004743 Polypropylene Substances 0.000 claims abstract description 17
- -1 polyethylene Polymers 0.000 claims abstract description 17
- 229920000573 polyethylene Polymers 0.000 claims abstract description 17
- 229920001155 polypropylene Polymers 0.000 claims abstract description 17
- 229920000428 triblock copolymer Polymers 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N iso-propanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 15
- RLJWTAURUFQFJP-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O.CC(C)O.CC(C)O RLJWTAURUFQFJP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 238000000967 suction filtration Methods 0.000 claims abstract description 13
- 230000002194 synthesizing Effects 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000005712 crystallization Effects 0.000 claims description 7
- 239000002073 nanorod Substances 0.000 claims description 6
- 230000000875 corresponding Effects 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 abstract 1
- 238000006303 photolysis reaction Methods 0.000 abstract 1
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 5
- 230000004298 light response Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N TiO Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000003197 catalytic Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large scale production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000005298 paramagnetic Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000001235 sensitizing Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- 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
- B01J35/002—Catalysts characterised by their physical properties
- B01J35/004—Photocatalysts
-
- 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
Abstract
The invention discloses a synthetic method of a rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancies, belonging to the technical field of synthesis of titanium dioxide photocatalysts. The technical scheme provided by the invention has the key points that: dissolving a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and titanium tetraisopropoxide TTIP in a mixed solution of concentrated hydrochloric acid, isopropanol and deionized water; evaporating the obtained mixed solution in an evaporation dish at room temperature, transferring the mixed solution to a hydrothermal reaction kettle, and crystallizing for 12-48h at the temperature of 180 DEG and 230 ℃; and (4) carrying out suction filtration and natural airing on the crystallized product to obtain the rutile-phase titanium dioxide photocatalyst containing the bound electron oxygen vacancy. The preparation method has the advantages of simple preparation process, easily obtained raw materials and strong controllability of reaction conditions, and the prepared material has higher practical value and application prospect in the aspects of environmental management, photolysis water to produce hydrogen, dye-sensitized solar cells, photoelectric materials and the like.
Description
Technical Field
The invention belongs to the technical field of synthesis of titanium dioxide photocatalysts, and particularly relates to a synthetic method of a rutile-phase titanium dioxide photocatalyst containing bound electron oxygen vacancies.
Background
The semiconductor titanium dioxide material has the characteristics of high photocatalytic efficiency, stable structure, low price, no toxicity and the like, and becomes one of the most spotlighted materials in a plurality of photocatalysts. However, due to TiO2The band gap of the light-absorbing material is wide (the band gap energy is 3.0-3.2 ev), the light absorption wavelength is mainly limited in an ultraviolet region and can not be directly excited by visible light, and the ultraviolet light only accounts for 4% of the specific gravity of sunlight on the surface of the earth. Therefore, in order to utilize more visible light in sunlight, how to prepare titanium dioxide with visible light response becomes a great research hotspot in the field of photocatalysis at present.
At present, in order to prepare titanium dioxide with visible light response, researchers generally adopt methods such as ion doping, compounding with narrow bandgap semiconductors, fuel sensitization, transition metal doping, non-metal element doping and the like to make the titanium dioxide suitable for the visible light region. In addition, in TiO2The introduction of single electron-binding oxygen vacancies in the crystal lattice is also a cause of TiO2An important method with visible light response. TiO containing bound single electron oxygen vacancy reported at present2The synthesis methods of visible light catalysts mainly include two types: (1) radio frequency plasma treatment of TiO2(ii) a (2) In TiO2The crystal lattice is doped with nitrogen.However, the preparation process of the traditional synthetic method is too complex and the equipment cost and the production cost are too high, which seriously restricts the popularization of industrialization. It was therefore possible to propose a novel, simple and inexpensive process for preparing TiO with high visible light activity2Catalysts face major technical challenges.
Disclosure of Invention
The invention solves the technical problem of providing a synthetic method of rutile titanium dioxide photocatalyst containing bound electron oxygen vacancy, which has simple preparation process, strong controllability of reaction conditions and good reproducibility.
The invention adopts the following technical scheme for solving the technical problems, and the synthesis method of the rutile titanium dioxide photocatalyst containing the bound electron oxygen vacancy is characterized by comprising the following specific steps of:
(1) dissolving a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and titanium tetraisopropoxide TTIP in a mixed solution of concentrated hydrochloric acid, isopropanol and deionized water;
(2) evaporating the mixed solution obtained in the step (1) in an evaporation dish at room temperature, and then transferring the mixed solution to a hydrothermal reaction kettle for crystallization at the temperature of 180 ℃ and 230 ℃ for 12-48 h;
(3) and (3) carrying out suction filtration and natural airing on the crystallized product obtained in the step (2) to obtain the rutile-phase titanium dioxide photocatalyst containing the bound electron oxygen vacancy.
More preferably, the mass ratio of the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 to the titanium tetraisopropoxide TTIP in the step (1) is 1:6-12, the volumes of 1g of the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 corresponding to concentrated hydrochloric acid, isopropanol and deionized water are 3.5mL, 11.75mL and 0.75mL respectively, and the mass concentration of the concentrated hydrochloric acid is 36-38%.
Further preferably, the time of the room-temperature evaporation in the step (2) is 12 to 24 hours.
The invention relates to a synthetic method of a rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancies, which is characterized by comprising the following specific steps:
(1) dissolving 0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water;
(2) evaporating the mixed solution obtained in the step (1) in an evaporating dish at room temperature for 12-24h, and then transferring the mixed solution to a hydrothermal reaction kettle for crystallization at 180 ℃ for 12-48 h;
(3) and (3) carrying out suction filtration and natural airing on the product crystallized in the step (2) to obtain the rutile phase nano-rod titanium dioxide photocatalyst containing the bound electron oxygen vacancy.
Compared with the prior art, the invention has the following beneficial effects:
1. the titanium dioxide photocatalyst synthesized by the invention contains a large number of bound electron oxygen vacancies, so that the titanium dioxide photocatalyst has visible light catalytic performance;
2. the invention directly synthesizes the rutile phase titanium dioxide visible light catalyst which has strong thermal stability and contains bound electron oxygen vacancy;
3. the rutile phase titanium dioxide nanorod containing the bound electron oxygen vacancy, which is prepared by the invention, has uniform size and good crystallinity;
4. the preparation process is simple, the reaction condition controllability is strong, the reproducibility is good, other semiconductors or elements doped with visible light response are not required to be additionally introduced in the synthesis process, and the large-scale production is easy to carry out.
Drawings
FIG. 1 is an XRD spectrum of titanium dioxide produced in example 1 of the present invention;
FIG. 2 is an SEM photograph of titanium dioxide produced in example 2 of the present invention;
FIG. 3 is an EPR spectrum of titanium dioxide produced in example 4 of the present invention;
FIG. 4 is a UV-vis DRS spectrum of titanium dioxide prepared in example 7 of the present invention with P25 titanium dioxide.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, the mixed solution is evaporated in an evaporation dish at room temperature for 12h and then transferred to a hydrothermal reaction kettle to be crystallized at 180 ℃ for 12h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
From the X-ray (XRD) spectrum of the titanium dioxide photocatalyst of FIG. 1, it can be seen that the diffraction peaks are ascribed to the crystal structure of rutile phase titanium dioxide (JCPDS card No. 21-1276).
Example 2
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle for crystallization at 180 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
According to the Scanning Electron Microscope (SEM) of the titanium dioxide photocatalyst shown in FIG. 2, it can be seen that the prepared sample has a very regular nanorod shape with a length of about 200 nm and 250 nm.
Example 3
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle for crystallization at 180 ℃ for 48h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
Example 4
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle to be crystallized at 210 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
According to the paramagnetic resonance (EPR) spectrum of the titanium dioxide photocatalyst shown in fig. 3, a strong symmetric peak at g =2.0013 is attributed to the oxygen vacancy of the bound single electron, indicating that the rutile phase titanium dioxide photocatalyst prepared contains a large amount of oxygen vacancies of the bound single electron.
Example 5
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 1.8g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle to be crystallized at 210 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
Example 6
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 1.8g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle to be crystallized at 230 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
Example 7
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 1.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle for crystallization at 180 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
According to the ultraviolet-visible absorption (UV-vis DRS) spectrum of the titanium dioxide photocatalyst shown in figure 4, it can be seen that the product prepared by the invention has obvious absorption on visible light with the wavelength of more than 400nm compared with P25 titanium dioxide, which is attributed to the function of binding single electron oxygen vacancies.
Example 8
0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 1.3g of titanium tetraisopropoxide TTIP are dissolved in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water, then the mixed solution is evaporated in an evaporation dish at room temperature for 24h and then transferred to a hydrothermal reaction kettle to be crystallized at 210 ℃ for 24h, and after the reaction is finished, the crystallized product is subjected to suction filtration and natural airing to obtain the target product.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (2)
1. A synthetic method of rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancy is characterized by comprising the following specific steps:
(1) dissolving a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and titanium tetraisopropoxide TTIP in a mixed solution of concentrated hydrochloric acid, isopropanol and deionized water, wherein the mass ratio of the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 to the titanium tetraisopropoxide TTIP is 1:6-12, the volumes of the concentrated hydrochloric acid, the isopropanol and the deionized water corresponding to 1g of the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 are respectively 3.5mL, 11.75mL and 0.75mL, and the mass concentration of the concentrated hydrochloric acid is 36-38%;
(2) evaporating the mixed solution obtained in the step (1) in an evaporation dish at room temperature for 12-24h, and then transferring the mixed solution to a hydrothermal reaction kettle for crystallization at the temperature of 180-;
(3) and (3) carrying out suction filtration and natural air drying on the crystallized product obtained in the step (2) to obtain the rutile titanium dioxide photocatalyst containing bound electron oxygen vacancies, wherein the morphology of the rutile titanium dioxide photocatalyst is very regular nanorods, and the length of the nanorods is 200-250 nm.
2. The method for synthesizing the rutile titanium dioxide photocatalyst containing bound electron oxygen vacancies as claimed in claim 1, which is characterized by comprising the following steps:
(1) dissolving 0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 and 2.3g of titanium tetraisopropoxide TTIP in a mixed solution of 0.7mL of concentrated hydrochloric acid, 2.35mL of isopropanol and 0.15mL of deionized water;
(2) evaporating the mixed solution obtained in the step (1) in an evaporating dish at room temperature for 12-24h, and then transferring the mixed solution to a hydrothermal reaction kettle for crystallization at 180 ℃ for 12-48 h;
(3) and (3) carrying out suction filtration and natural airing on the product crystallized in the step (2) to obtain the rutile phase nano-rod titanium dioxide photocatalyst containing the bound electron oxygen vacancy.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037226A (en) * | 2007-03-23 | 2007-09-19 | 河南大学 | Novel Titanium dioxide, preparation method and application thereof |
| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN104162427A (en) * | 2014-08-12 | 2014-11-26 | 河南大学 | Metal ion-grafted TiO2 high-efficiency photocatalyst containing restriction single electron oxygen vacancy as well as preparation and application thereof |
| CN106145184A (en) * | 2016-06-21 | 2016-11-23 | 河南师范大学 | One has the high activity { TiO of 111} exposure high preferred orientation2the preparation method of microsphere |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037226A (en) * | 2007-03-23 | 2007-09-19 | 河南大学 | Novel Titanium dioxide, preparation method and application thereof |
| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN104162427A (en) * | 2014-08-12 | 2014-11-26 | 河南大学 | Metal ion-grafted TiO2 high-efficiency photocatalyst containing restriction single electron oxygen vacancy as well as preparation and application thereof |
| CN106145184A (en) * | 2016-06-21 | 2016-11-23 | 河南师范大学 | One has the high activity { TiO of 111} exposure high preferred orientation2the preparation method of microsphere |
Non-Patent Citations (1)
| Title |
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| "Preparation of Highly Ordered Mesoporous Al2O3/TiO2 and Its Application in Dye-Sensitized Solar Cells";Jae-Yup Kim et al;《Langmuir》;20091016;第26卷(第4期);第2864-2870页 * |
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