CN103638915A - High-catalytic-property TiO2 nano powder/porous material as well as preparation method and application of high-catalytic-property TiO2 nano powder/porous material - Google Patents
High-catalytic-property TiO2 nano powder/porous material as well as preparation method and application of high-catalytic-property TiO2 nano powder/porous material Download PDFInfo
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Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to a high-catalytic-property TiO2 nano powder/porous material as well as a preparation method and an application of the high-catalytic-property TiO2 nano powder/porous material. The preparation method provided by the invention comprises the following steps: firstly, growing a TiO2 nano film on sponge by utilizing an atomic layer deposition method; then putting the sponge covered with the TiO2 nano film into an alumina crucible; putting the alumina crucible into a tube furnace for which a certain heating procedure is set up, and introducing proper gas for thermal treatment; and taking out after cooling, thereby obtaining the high-catalytic-property TiO2 nano powder/porous material. According to the invention, the process is simple; the preparation temperature is low; and anatase and rutile in the obtained TiO2 nano powder/porous material have a certain proportion, and the TiO2 nano powder/porous material has favorable photocatalytic degradation capability, thus being applied to the field of photocatalysis.
Description
Technical field
The invention belongs to photocatalysis technology field, be specifically related to a kind of TiO
2nanometer powder/porous material and preparation method thereof and its application in photocatalysis field.
Background technology
Along with the continuous progress of science and technology and industrial fast development; water resource limited on the earth is subject to serious pollution day by day; brought the potential danger side of body to the mankind's Health and Living; also make the mankind recognize gradually the importance [Chen Lin of water conservation; photocatalysis material of titanium dioxide and Research Advance in Modification Methods thereof, 2013].People are finding always and are attempting to administer the way of water environment pollution for many years, such as adopting Physical, chemical method and biological treatment etc.Physical comprises sedimentation, filtration etc., these class methods are mainly by being pollutant and the colloidal impurity of suspended state in physical action separation, recovery sewage, and for the dissolubility pollutant in water and metal ion, as widely used lead ion, mercury ion, cadmium ion, arsenic ion etc. in industrial production flow process, be all difficult to reach the object of effective removal; Take chemical method that stripping, stripping, ion-exchange etc. are representative mainly by chemical reaction and effect of mass transmitting come separated, remove the pollutant that is dissolved state in sewage, but this class methods processing cost is high, and inevitably brings secondary pollution; Bioanalysis is mainly that the metabolism by microorganism makes the organic pollution that is dissolving, colloid and fine suspended state in sewage be converted into stable, harmless material.This class methods treatment cycle is long and content of organics in treatment temperature, time and water body etc. is had to higher requirement.Therefore, research and develop novel advanced treatment method for sewage water and have very important meaning.
Photocatalysis oxidation technique is compared with aforementioned water pollutant improvement method, has that energy consumption is low, reaction condition is gentle, easy and simple to handle, non-secondary pollution, can directly utilize the advantages such as solar energy.Cleanliness without any pollution, inexhaustible solar energy are combined with water pollution control and protection, and the research that utilizes light-catalyzed reaction and reaction engineering equipment to carry out the pollutant in removal sewage has far-reaching strategic importance.
TiO
2(being commonly called as titanium dioxide) is a kind of important meals oxide semiconductor material, have that chemical stability is good, catalytic activity is strong, non-toxic inexpensive, fast light burn into be to the selective little and mineralization degree of organic pollution compared with high, its photocatalysis performance and chemical stability are better than ZnO, WO
3with other photochemical catalysts such as CdS.From [Fujishima A, Honda K. Nature. 1972] such as Fujishim in 1972, find TiO
2since can be used for decomposing aquatic products hydrogen as photochemical catalyst, about TiO
2research aspect organic matter degradation also gradually deeply, becomes the focus of environmental area research.
TiO
2there are brockite, rutile and three kinds of crystal formations of anatase, wherein for light-catalysed two kinds of crystal formations, i.e. Detitanium-ore-type and the rutile-type of mainly containing.Due to TiO
2energy gap is larger, and the Detitanium-ore-type bandwidth Eg of tool photocatalytic activity is 3.2～3.5 ev, only under wavelength is less than the UV-irradiation condition of 387 nm, shows good reactivity and stability.Ultraviolet light proportion in sunshine composition is only 3%～5%, thereby has greatly limited TiO
2utilization rate to solar energy.In addition, the simple composite rate that optical excitation produces electronics and hole is higher, causes quantum utilization rate low, is also restricting TiO
2the significantly raising of photocatalysis efficiency.In order to solve TiO
2the problems referred to above that photochemical catalyst exists, improve visible light catalytic efficiency, and except considering that semiconductor light-catalyst self property (as crystal formation, particle diameter and sintering temperature etc.) is on photocatalytic activity impact, people are to TiO
2photochemical catalyst has carried out a large amount of modified test research.For this reason, researcher mainly adopts and improves preparation technology, controls the technological means such as pattern and size, surface modification, for improving TiO
2the efficiency of catalysis material and performance, and then improve its photocatalytic activity and carried out various trial.But up to the present from the angle of practical application, various results of study are improving TiO
2photocatalysis performance aspect all desirable not enough.
Researcher has also studied TiO
2the impact of crystal structure on photocatalysis performance.Early stage research [the .TiO such as Shen Hangyan
2organic pollution in fine catalyst catalytic degradation room air, 1998] show, pure anatase is better than rutile photocatalysis effect, and this is caused by rutile and anatase crystal architectural difference, rutile TiO
2micro-aobvious iris, band gap 3.0 eV, Detitanium-ore-type TiO
2be obvious iris distortion, band gap 3.2 eV, and the higher energy gap of anatase makes its electron-hole have corrigendum or more negative current potential, thereby have higher oxidability, anatase surface is to H
2o, O
2adsorption capacity is strong compared with rutile also, causes its photocatalytic activity higher.Therefore before, correlative study person often concentrates on notice the TiO that how to suppress anatase
2to Rutile Type, change.
Recent study person [Li G H, Gray K A. Chemistry of Materials. 2007] finds that resulting photocatalysis effect is better than single crystal form when two kinds of crystal formations mix with certain proportion, and this is mainly owing to two kinds of crystal formation TiO
2fermi level different, between two-phase interface, forming Schottky potential barrier (refer to form on metal-semiconductor border the region with rectified action), can promote transfer, the separation in electronics and hole and move to the surface of catalyst; Due to the close contact of two kinds of crystal formations, make the electron-hole separating effect of granule interior better.But along with the increase gradually of rutile-type ratio, electron-hole increases to migration path under particle surface, separation probability reduces, and recombination probability increases, and causes its photocatalytic activity not good, therefore by strict, controls two kinds of TiO
2the ratio of crystal formation, can realize the control to its photocatalysis effect.
The present invention has adopted following preparation method in line with principle with low cost, simple to operate: the method by ald has been prepared TiO on the sponge of porosity and looseness
2nano thin-film is for after increasing specific surface area, then film is annealed in best heat treatment temperature and suitable atmosphere, reasonably improved TiO
2surface state and crystalline condition, at utmost to TiO
2intrinsic shortcoming improve, thereby obtained a kind of more material of high light catalytic capability that has, made up existing TiO
2deficiency in the efficiency of light energy utilization.
Summary of the invention
The object of the present invention is to provide the TiO that a kind of photocatalysis efficiency is high, photo-catalysis capability is strong, cost is low
2nanometer powder/porous material and preparation method thereof, to solve some problem existing in present this field, improves TiO
2the photocatalysis performance of nanometer powder/porous material, the practical application of expanding such material.
High catalytic property matter TiO provided by the invention
2the preparation method of nanometer powder/porous material, concrete steps are as follows:
(1) utilize the Atomic layer deposition method TiO that grows on sponge
2nano thin-film:
In atomic layer deposition apparatus, using titanium source and water as presoma, it is 50 ~ 150 ℃ that titanium source temperature is controlled, it is 30 ~ 60 ℃ that coolant-temperature gage is controlled, reaction temperature is that substrate temperature is made as 120 ~ 220 ℃, carries out the growth of several circulations on clean sponge, obtains having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; Alumina crucible is put into tube furnace, with the flow velocity of 0.2 ~ 1 liter/min, pass into gas (oxygen or nitrogen or ozone or hydrogen), heat-treat, with the programming rates of 5 ~ 20 ℃/min, be warming up to 200 ~ 700 ℃, calcination, time is 1 ~ 5 hour, after naturally cooling, takes out, and obtains having the TiO of high catalytic performance
2nanometer powder/porous material.
Preparation flow schematic diagram as shown in Figure 1.
In step (1), described titanium source is selected from: four (dimethylamino) titanium Titanium tetrakis (dimethylamide) or titanium tetrachloride (TiCl
4) or butyl titanate (Ti (OBu)
4);
In step (1), the temperature of described presoma and substrate temperature can change as required; Preferably 100 ~ 110 ℃ of titanium source temperatures, coolant-temperature gage is preferably 50 ~ 55 ℃, and reaction temperature is that substrate temperature is preferably 140 ~ 160 ℃,
In step (1), in described atomic layer deposition process, the cycle-index of presoma can change as required;
In step (2), described gas can be O
2, N
2, O
3or H
2pure gas;
In step (2), described tube furnace heat treatment temperature program can change as required.Programming rate is preferably 15-18 ℃, preferably 500 ~ 600 ℃ of calcination temperatures, the preferred 3-4 hour of calcination time.
XRD test shows (as shown in Figure 3), TiO prepared by the inventive method
2there is the hybrid junctions crystalline phase of anatase and Rutile Type in nanometer powder/porous material.
Photocatalysis experimental result shows (as shown in Figure 4), the TiO that the inventive method prepares
2there is the experiment effect of good photo-catalytic degradation of methyl-orange in nanometer powder/porous material.So, the TiO being prepared by the inventive method
2nanometer powder/porous material has high activity in the process of photocatalytic degradation of dye, can aspect light degradation organic pollution especially water pollution processing, be used widely.
Utilize the method for ald on clean sponge, to deposit the nano-TiO of different-thickness
2film, then can obtain the TiO with fine photocatalysis performance through simple annealing in process
2nanometer powder/porous material.The advantages such as therefore to have equipment simple, with low cost in the present invention, with short production cycle, have the prospect of the good commercialization of production, are TiO
2aspect light degradation organic pollution especially water pollution processing, be used widely a practicable approach is provided.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of nanometer powder/porous material of the present invention.Wherein, 1 is clean sponge blocks; 2 is the method for the utilizing ald TiO that grown
2the sponge of nano thin-film; 3 for having removed the TiO of sponge by Technology for Heating Processing
2nanometer powder/porous material; 4 is the network structure of sponge; 5 is the TiO of ald
2nano thin-film.
Fig. 2 is the TiO that utilizes the method for ald to grow on clean sponge in embodiment 1
2the in kind photo of the blocks of nano thin-film after annealing.
Fig. 3 is the prepared TiO of scheme in embodiment 1
2the XRD picture of nanometer powder/porous material is annealed 3 hours for 550 ℃ under oxygen atmosphere, the TiO obtaining
2the mixing crystal formation that has occurred anatase and rutile in nanometer powder/porous material, this is also the main reason that good photocatalysis performance appears in this product.
Curve in Fig. 4 be methyl orange solution under ultraviolet lighting concentration with the change curve of light application time.Wherein, the TiO that utilizes the method for ald to grow on clean sponge in the corresponding embodiment 1 of sample a
2nano thin-film, unannealed; The prepared TiO of scheme in the corresponding embodiment 1 of sample b
2nanometer powder/porous material; Two groups of samples have all been considered not the concentration compensation of blank methyl orange solution containing the sample light degradation effect under ultraviolet lighting.
Fig. 5 is the prepared TiO of scheme in embodiment 1
2the electron scanning micrograph of nanometer powder/porous material, wherein a is macrograph, b is high power photo.
The specific embodiment
Below in conjunction with embodiment, be intended to further illustrate the present invention, but these embodiment only for being described, do not form limitation of the scope of the invention in the present invention.
(1) utilize the method for the ald TiO that grows on clean sponge
2nano thin-film;
The method of described ald, usings four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, and it is 105 ℃ and 55 ℃ that its temperature is controlled respectively.Reaction temperature is that substrate temperature is made as 150 ℃, and 1000 the rear taking-ups of circulation of growing on clean sponge obtain having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, and pass into oxygen, heat-treat.With the programming rates of 18 ℃/min, heat up, calcination temperature is 550 ℃, and temperature retention time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; After sample is naturally cooling, take out, obtain having the TiO of high catalytic performance
2nanometer powder/porous material (accompanying drawing 5 is shown in by its electron micrograph);
Gained sample utilizes ultraviolet specrophotometer to test its photocatalysis performance, and result as shown in Figure 4.Using methyl orange as target degradation of dye.By the sample after annealing, (area is 3 cm
2) put into the methyl orange solution that 6 ml concns are 10 mg/litre, shading makes dyestuff and catalyst reach adsorption equilibrium standing half an hour.It is the xenon lamp of 350 W that ultraviolet source is selected power, apart from methyl orange (MO) liquid level 50 cm place vertical irradiations.Utilize spectrophotometer to measure its solution concentration at methyl orange maximum absorption wavelength 464 nm places.This example annealing specimen degradation experiment result as shown in Figure 4.By accompanying drawing 4, can be found out the TiO preparing by method provided by the invention
2nanometer powder/porous material possesses good photocatalysis performance.
Gained sample has been done to XRD test (as accompanying drawing 3), and XRD result shows, the mixing crystal formation of anatase and rutile has appearred in gained sample, the reason of Here it is product has better photocatalysis performance: two kinds of crystal formation TiO of anatase and rutile
2fermi level different, between two-phase interface, forming Schottky potential barrier (refer to form on metal-semiconductor border the region with rectified action), can promote transfer, the separation in electronics and hole and move to the surface of catalyst; Due to the close contact of two kinds of crystal formations, make the electron-hole separating effect of granule interior better.Thereby effectively suppressed the compound of electron-hole, thereby improved the photocatalysis performance of prepared sample.
(1) utilize the method for the ald TiO that grows on clean sponge
2nano thin-film;
The method of described ald, with titanium tetrachloride (TiCl
4) and water as presoma, it is 115 ℃ and 60 ℃ that its temperature is controlled respectively.Reaction temperature is that substrate temperature is made as 160 ℃.800 the rear taking-ups of circulation of growing on clean sponge obtain having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, and pass into oxygen, heat-treat.With the programming rates of 16 ℃/min, heat up, calcination temperature is 600 ℃, and temperature retention time is 4 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; After sample is naturally cooling, take out, can obtain TiO
2nanometer powder/porous material.
(1) utilize the method for the ald TiO that grows on clean sponge
2nano thin-film;
The method of described ald, with butyl titanate (Ti (OBu)
4) and water as presoma, it is 90 ℃ and 45 ℃ that its temperature is controlled respectively.Reaction temperature is that substrate temperature is made as 180 ℃.500 the rear taking-ups of circulation of growing on clean sponge obtain having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, and pass into oxygen, heat-treat.With the programming rates of 12 ℃/min, heat up, calcination temperature is 300 ℃, and the reaction time is 5 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; After sample is naturally cooling, take out, obtain having the TiO of high catalytic performance
2nanometer powder/porous material.
(1) utilize the method for the ald TiO that grows on clean sponge
2nano thin-film;
The method of described ald, usings four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, and it is 105 ℃ and 55 ℃ that its temperature is controlled respectively.Reaction temperature is that substrate temperature is made as 200 ℃.400 the rear taking-ups of circulation of growing on clean sponge obtain having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, pass into N
2, heat-treat.With the programming rates of 18 ℃/min, heat up, calcination temperature is 200 ℃, and the reaction time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; After sample is naturally cooling, take out, obtain having the TiO of high catalytic performance
2nanometer powder/porous material.
Embodiment 5
(1) utilize the method for the ald TiO that grows on clean sponge
2nano thin-film;
The method of described ald, usings four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, and it is 105 ℃ and 55 ℃ that its temperature is controlled respectively.Reaction temperature is that substrate temperature is made as 150 ℃.800 the rear taking-ups of circulation of growing on clean sponge obtain having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, and pass into hydrogen, heat-treat.Annealing temperature is 700 ℃, and temperature retention time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; After sample is naturally cooling, take out, obtain having the TiO of high catalytic performance
2nanometer powder/porous material.
Claims (5)
1. a high catalytic property matter TiO
2the preparation method of nanometer powder/porous material, is characterized in that concrete steps are as follows:
(1) utilize the Atomic layer deposition method TiO that grows on sponge
2nano thin-film:
In atomic layer deposition apparatus, using titanium source and water as presoma, controlling titanium source temperature is 50 ~ 150 ℃, 30 ~ 60 ℃ of coolant-temperature gages, reaction temperature is that substrate temperature is made as 120 ~ 220 ℃, carries out the growth of several circulations on clean sponge, obtains having TiO
2the sponge of nano thin-film;
(2) will there is TiO
2the sponge of nano thin-film is placed in alumina crucible; Alumina crucible is put into tube furnace, with the flow velocity of 0.2 ~ 1 liter/min, pass into gas, with the programming rates of 5 ~ 20 ℃/min, be warming up to 200 ~ 700 ℃, calcination, the time is 1 ~ 5 hour; After naturally cooling, take out, obtain having the TiO of high catalytic performance
2nanometer powder/porous material.
2. high catalytic property matter TiO as claimed in claim 1
2the preparation method of nanometer powder/porous material, is characterized in that described titanium source is selected from: four (dimethylamino) titanium, titanium tetrachloride or butyl titanate.
3. high catalytic property matter TiO as claimed in claim 1
2the preparation method of nanometer powder/porous material, is characterized in that described gas is O
2, N
2, O
3or H
2pure gas.
4. the TiO being prepared by the described preparation method of one of claim 1 ~ 3
2nanometer powder/porous material.
5. a TiO as claimed in claim 1
2the application of nanometer powder/porous material in photocatalysis.
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