CN107876034B - Ti2O@TiO2Composite photocatalyst and preparation method thereof - Google Patents
Ti2O@TiO2Composite photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000002131 composite material Substances 0.000 claims abstract description 47
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 36
- 239000011258 core-shell material Substances 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000010410 layer Substances 0.000 claims description 10
- 239000012792 core layer Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
- 238000002441 X-ray diffraction Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000969 carrier Substances 0.000 abstract description 2
- 239000000975 dye Substances 0.000 abstract description 2
- 230000004298 light response Effects 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 230000006798 recombination Effects 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 46
- 238000001354 calcination Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910009973 Ti2O3 Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- -1 titanium hydride Chemical compound 0.000 description 1
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/043—Titanium sub-oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
Abstract
The invention discloses a Ti2O@TiO2Composite photocatalyst, preparation method thereof and TiH2After heat treatment at different temperatures and time, gradually converting into Ti2O@TiO2The composite material has different product proportion due to different temperature and time. The optimal temperature and time parameters are obtained by analysis according to an X-ray diffraction spectrum (XRD), an ultraviolet-visible absorption spectrogram of a composite sample and a time-sharing chart of photocatalytic degradation methylene blue of different samples. The invention has the beneficial effect that Ti is used2O/TiO2The composite structure forms a core-shell structure, the visible light response capability is greatly enhanced, the recombination probability of photon-generated carriers is reduced, the photoelectric conversion efficiency is promoted, the rate of light degradation is further enhanced, the degradation speed of the composite structure on organic dyes such as methylene blue is greatly improved, the preparation process is simpler, and the time and the cost are greatly saved.
Description
Technical Field
The invention relates to the technical field of nano photocatalytic materials, in particular to Ti2O@TiO2A composite photocatalyst and a preparation method thereof.
Background
Since 1972 the discovery by Japanese scientists Fujishima and Honda on TiO2After photocatalytic water decomposition can be carried out on the electrode, people pay more and more attention to the photocatalysis by utilizing solar energy. TiO 22The photocatalyst has the advantages of high photocatalytic activity, high chemical stability, no toxicity, low cost and the like, and is widely applied to the research of low-cost thin-film solar cells and photocatalysts. At present, against TiO2The defects of only absorbing ultraviolet light and no response to visible light and the like are developed to TiO2Improving TiO by metal/nonmetal doping, semiconductor/noble metal compounding, crystal face morphology adjusting and the like2The photocatalytic efficiency of (c). Simple searching process, low cost and capability ofVisible light responsive catalytic composites have been the focus of research.
TiH2Is an industrial raw material and is always applied to the preparation of porous aluminum alloy and titanium alloy. Around TiH2Much research has been done on oxidation of (a). Research on TiH by thermal oxidation treatment2The influence of hydrogen evolution behavior confirms the formation of Ti xHOy, Ti during oxidation2O3And TiO2A variety of phases and structures. King-dazzling et al also studied the titanium hydride oxidation treatment and its thermal decomposition behavior Ti2O3+TiO2And Ti3O+TiO2]Powder metallurgy materials science and engineering 20 (2015) 1-6]. Many oxidation works are established under the condition of studying sufficient and continuous supplement of oxygen atmosphere, and low-oxygen Ti is not realized2O and pure phase Ti2O@TiO2And (3) preparing the composite material.
Disclosure of Invention
The invention provides a method for limited space oxidation, and obtains a novel Ti2O phase to form Ti2O@TiO2The composite photocatalyst solves the problem of the existing TiO2The catalytic material can not absorb visible light, photoproduction electrons are easy to compound, and the catalytic efficiency is low.
In order to solve the problems, the invention adopts the following technical scheme: ti2O@TiO2Composite photocatalyst, Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O。
Mix TiH2Ball-milling, placing in a closed quartz tube, and calcining at high temperature to obtain Ti2O@TiO2A composite photocatalyst is provided.
The TiH2The grain diameter after ball milling is 2-6 μm.
The temperature of the high-temperature calcination is 550-670 ℃, and the time is 2-10 h.
Each 20g of TiH2The container is placed in a 500mL quartz tube, and the air in the container is at the atmospheric pressure and has no gas exchange with the outside.
The invention has the beneficial effects that: prepared by the inventionThe visible light area of the composite material is obviously enhanced after 400 nm. Especially, the absorption between 400 and 500nm is strongly enhanced, and the electronic structure analysis shows that the forbidden band of the material is similar to a metal material, can effectively absorb visible light, and the absorption has the characteristic of SPR (surface plasmon resonance). Ti2O/TiO2The rate of the photocatalyst for photodegradation is enhanced, and the degradation rate of organic dyes such as methylene blue is greatly improved. The formed composite structure is a product obtained by in-situ oxidation, the interface bonding is good, and the interface impedance is favorably reduced. Compared with other semiconductor composite and metal composite, the material cost is low, and TiH2Is a cheap industrial raw material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an XRD pattern of materials prepared according to examples 1-7 of the present invention.
FIG. 2 is a graph of the UV-VIS absorption spectrum of the composite material.
Fig. 3 is a photoluminescence spectrum (PL spectrum) of the composite.
Fig. 4 is an exploded view of photocatalytic degradation of methylene blue of a composite sample under different conditions.
Figure 5 is a high resolution TEM of the composite catalyst.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing the mixture in a 500ml closed quartz tube furnace for heating, calcining and high-temperature calcining at the temperature of 550 ℃ for 6 hours to obtain Ti2O@TiO2A composite photocatalyst is provided.
Example 2
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 580 ℃, and the time is 2 hours, thus obtaining Ti2O@TiO2A composite photocatalyst is provided.
Example 3
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 580 ℃, the time is 6 hours, and Ti is obtained2O@TiO2A composite photocatalyst is provided.
Example 4
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of the particlesOf TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 580 ℃, and the time is 10 hours, thus obtaining Ti2O@TiO2A composite photocatalyst is provided.
Example 5
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 610 ℃, and the time is 6h, thus obtaining Ti2O@TiO2A composite photocatalyst is provided.
Example 6
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 640 ℃, and the time is 6 hours, thus obtaining Ti2O@TiO2A composite photocatalyst is provided.
Example 7
Example Ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O, the preparation method is as follows:
by TiH2As raw material, ball-milled TiH2Obtaining particles of 2-6 microns, and ball-milling 20g of TiH2Placing in a 500ml sealed quartz tube furnace for heating and calcining, wherein the air in the container is one atmosphere, no gas exchange is carried out with the outside, the temperature of high-temperature calcining is 670 ℃, and the time is 10 hours, thus obtaining Ti2O@TiO2Composite photocatalysisAnd (3) preparing.
As shown in FIG. 1, Ti prepared for examples 1-72O@TiO2XRD pattern of composite photocatalyst, standard reference phase is TiO respectively2,Ti2O and TiH2. As can be seen from the figure, Rutile-TiO increases with the heating temperature in the same heating time (6 h)2The (R) phase is present in an increasing amount, Ti2The O (T) phase then gradually decreases after 580 ℃ for TiH2(TH) phase, the content is maximum at 550 ℃, the content decreases sharply when the temperature is raised to 580 ℃, and is almost absent at 610 ℃ and 640 ℃. TiH2Stable at low temperature, and is oxidized after reaching a certain temperature.
The phase ratios of the respective substances are shown in table 1.
Table 1 proportions of the phases in the catalysts of examples 1 to 7.
FIG. 2 illustrates Ti2O is compared with TiO2Has obvious visible light response. A certain amount of Ti2O recombination forms an effective light absorption band peak in the region of 400-500nm, and the absorption peak and Ti2The O content is in close correlation with each other. Known as Ti2The capture capability of O to visible light is better than that of TiO2Is strong.
FIG. 4 is a degradation curve of the catalyst for degrading organic methylene blue, wherein the degradation performance of the obtained pure rutile phase is poor, and the visible light capturing capacity is too small and is lower than 10%. And Ti2O/TiO2The composite phase shows better photocatalytic performance, shows the best photocatalytic activity at 610 ℃ for 6h, and illustrates that Ti2O/TiO2The composite material structure and visible light absorption enhance the photocatalytic performance, thereby improving the degradation rate. Meanwhile, fig. 3 shows that the composite material also has a significant enhancement effect on the separation of photon-generated carriers.
FIG. 5 shows Ti2O/TiO2The image of the composite photocatalyst is approximately regular granular overall. Transmission electron microscope height markThe image-resolved image shows TiO with rutile phase as the outer layer2The interior is Ti2And O. The different areas have high resolution lattice images as the basis.
Invention by TiH2A unique Ti is prepared by oxidation reaction2O/TiO2Composite structure of Ti2The O content depends only on the heat treatment conditions. The absorption spectrum centered at 420 nm shows the typical visible response of the composite, the formation of a composite structure and the heterojunction contribute to the carrier separation. And in the optimal sample, the degradation rate of the optimized composite material to methylene blue aqueous solution is about 90% under the irradiation of visible light for 2 hours.
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, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. Ti2O@TiO2The composite photocatalyst is characterized in that: ti2O@TiO2The composite photocatalyst is of a core-shell structure, and the shell layer is TiO2The core layer is Ti2O；
The Ti2O@TiO2A preparation method of the composite photocatalyst, which is to mix TiH2Ball-milling, placing in a sealed quartz tube, and placing TiH2Ball-milled to obtain Ti with particle size of 2-6 microns and high-temperature calcination2O@TiO2The high-temperature calcination temperature of the composite photocatalyst is 550-670 ℃, and the time is 2-10 h.
2. The Ti of claim 12O@TiO2The composite photocatalyst is characterized in that: each 20g of TiH2Placed in a 500mL quartz tube.
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