CN103638915B - 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 PDF

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CN103638915B
CN103638915B CN201310686250.0A CN201310686250A CN103638915B CN 103638915 B CN103638915 B CN 103638915B CN 201310686250 A CN201310686250 A CN 201310686250A CN 103638915 B CN103638915 B CN 103638915B
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tio
porous material
sponge
tio2 nano
catalytic
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CN103638915A (en
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潘胜强
李梦琳
黄高山
梅永丰
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Fudan University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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

A kind of high catalytic property matter TiO2 nanometer powder/porous material and its preparation method and application
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 the fast development of industry; water resource limited on the earth is subject to serious pollution day by day; the potential danger side of body is brought to the Health and Living of the mankind; also the mankind are made to recognize the importance [Chen Lin of water conservation gradually; photocatalysis material of titanium dioxide and Research Advance in Modification Methods thereof, 2013].People are finding always and are attempting the way of administering water environment pollution for many years, such as adopt Physical, chemical method and biological treatment etc.Physical comprises sedimentation, filtration etc., these class methods are mainly through the pollutant in suspended state in physical action separation, recovery sewage and colloidal impurity, and for the dissolubility pollutant in water and metal ion, as lead ion widely used in industrial process stream, mercury ion, cadmium ion, arsenic ion etc., be all difficult to reach the object effectively removed; Be separated with effect of mass transmitting mainly through chemical reaction with the chemical method that stripping, stripping, ion-exchange etc. are representative, remove the pollutant in dissolved state in sewage, but this class methods processing cost is high, and inevitably bring secondary pollution; Bioanalysis mainly to make in sewage in dissolving by the metabolism of microorganism, the organic pollution of colloid and fine suspended state is converted into stable, harmless material.This class methods treatment cycle is longer and have higher requirement to content of organics in treatment temperature, time and water body etc.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 administering method, has that energy consumption is low, reaction condition is gentle, easy and simple to handle, non-secondary pollution, directly can utilize the advantages such as solar energy.Cleanliness without any pollution, inexhaustible solar energy are combined with protection with water pollution control, the research utilizing light-catalyzed reaction and reaction engineering equipment to carry out the pollutant removed in 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 be strong, non-toxic inexpensive, fast light burn into the selective little and mineralization degree comparatively high of organic pollution, its photocatalysis performance and chemical stability are better than ZnO, WO 3with other photochemical catalysts such as CdS.TiO is found from [Fujishima A, Honda K. Nature. 1972] such as Fujishim in 1972 2since can be used for decomposing aquatic products hydrogen as photochemical catalyst, about TiO 2research in organic matter degradation also gradually deeply, becomes the focus of environmental area research.
TiO 2there are brockite, rutile and anatase three kinds of crystal formations, wherein mainly contain two kinds of crystal formations for light-catalysed, i.e. Detitanium-ore-type and rutile-type.Due to TiO 2energy gap is comparatively large, and the Detitanium-ore-type bandwidth Eg of most photocatalytic activity is 3.2 ~ 3.5 ev, shows good reactivity and stability under the UV-irradiation condition being only less than 387 nm at wavelength.Ultraviolet light proportion in sunshine composition is only 3% ~ 5%, thus significantly limit TiO 2to the utilization rate of solar energy.In addition, the simple composite rate that optical excitation produces electronics and hole is higher, causes quantum utilization rate low, also governs 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 except 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 pattern and the technological means such as size, surface modification, for improving TiO 2the efficiency of catalysis material and performance, and then improve its photocatalytic activity and carried out various different trial.But up to the present from the angle of practical application, various result of study is at raising TiO 2photocatalysis performance aspect desirable all not enough.
Researcher is investigated TiO 2crystal structure is on the impact of 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 crystalline structure difference, rutile TiO 2micro-aobvious iris, band gap 3.0 eV, Detitanium-ore-type TiO 2distort in obvious iris, band gap 3.2 eV, and the higher energy gap of anatase makes its electron-hole have corrigendum or more negative current potential, thus has higher oxidability, anatase surface is to H 2o, O 2strong also compared with rutile of adsorption capacity, causes its photocatalytic activity higher.Therefore before correlative study person often visual cognitive ability at the TiO how suppressing anatase 2change to Rutile Type.
Recent study person [Li G H, Gray K A. Chemistry of Materials. 2007] finds when two kinds of crystal formations mix with certain proportion, and the photocatalysis effect obtained is better than single crystal form, and this is mainly owing to two kinds of crystal formation TiO 2fermi level different, between two-phase interface, form Schottky potential barrier (referring to the region with rectified action that metal-semiconductor border is formed), the transfer in electronics and hole can be promoted, be separated 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, and separation probability reduces, and recombination probability increases, and causes its photocatalytic activity not good, therefore control two kinds of TiO by strict 2the ratio of crystal formation, can realize the control to its photocatalysis effect.
The present invention have employed following preparation method in line with principle with low cost, simple to operate: on the sponge of porosity and looseness, prepared TiO by the method for ald 2after nano thin-film is used for increasing specific surface area, then film is annealed in the heat treatment temperature and suitable atmosphere of the best, reasonably improve TiO 2surface state and crystalline condition, at utmost to TiO 2intrinsic disadvantages improve, thus obtain a kind of material with more high light catalytic capability, compensate for 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 existing some problem existed in this field, improves TiO 2the photocatalysis performance of nanometer powder/porous material, expands the practical application of 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) Atomic layer deposition method is utilized to grow TiO on sponge 2nano thin-film:
In atomic layer deposition apparatus, using titanium source and water as presoma, it is 50 ~ 150 DEG C that titanium source temperature controls, it is 30 ~ 60 DEG C that coolant-temperature gage controls, reaction temperature and substrate temperature are set to 120 ~ 220 DEG C, the sponge of cleaning carries out the growth of several circulations, obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; Alumina crucible is put into tube furnace, gas (oxygen or nitrogen or ozone or hydrogen) is passed into the flow velocity of 0.2 ~ 1 liter/min, heat-treat, 200 ~ 700 DEG C are warming up to the programming rate of 5 ~ 20 DEG C/min, calcination, time is 1 ~ 5 hour, takes out, namely obtain the TiO with high catalytic performance after naturally cooling 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; Titanium source temperature preferably 100 ~ 110 DEG C, coolant-temperature gage is preferably 50 ~ 55 DEG C, and reaction temperature and substrate temperature are preferably 140 ~ 160 DEG C,
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 DEG C, calcination temperature preferably 500 ~ 600 DEG C, 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 prepared by the inventive method 2nanometer powder/porous material has high activity in the process of photocatalytic degradation of dye, can be used widely in light degradation organic pollution especially water pollutions process.
Utilize the method for ald on the sponge of cleaning, 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 the present invention has equipment simply, with low cost, with short production cycle, having the prospect of the good commercialization of production, is TiO 2be used widely in light degradation organic pollution especially water pollutions process and provide a practicable approach.
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 grown TiO for utilizing the method for ald 2the sponge of nano thin-film; 3 for eliminating 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 utilizing the method for ald to grow on the sponge of cleaning in embodiment 1 2the blocks photo in kind after annealing of nano thin-film.
Fig. 3 is the TiO in embodiment 1 prepared by scheme 2the XRD picture of nanometer powder/porous material, anneals 3 hours for 550 DEG C under oxygen atmosphere, the TiO obtained 2occurred the mixing crystal formation of 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 utilizing the method for ald to grow on the sponge of cleaning in the corresponding embodiment 1 of sample a 2nano thin-film, unannealed; TiO in the corresponding embodiment 1 of sample b prepared by scheme 2nanometer powder/porous material; Two groups of samples have all considered not containing the concentration offsets of the light degradation effect of blank methyl orange solution under ultraviolet lighting of sample.
Fig. 5 is the TiO in embodiment 1 prepared by scheme 2the electron scanning micrograph of nanometer powder/porous material, wherein a is macrograph, and b is high power photo.
Detailed description of the invention
Be intended to further illustrate the present invention below in conjunction with embodiment, but these embodiments only do not form limitation of the scope of the invention for illustration of the present invention.
Embodiment 1
(1) method of ald is utilized to grow TiO on the sponge of cleaning 2nano thin-film;
The method of described ald, using four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, its temperature is controlled as 105 DEG C and 55 DEG C.Reaction temperature and substrate temperature are set to 150 DEG C, and after the sponge of cleaning grows 1000 circulations, namely taking-up obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, pass into oxygen, heat-treat.Heat up with the programming rate of 18 DEG C/min, calcination temperature is 550 DEG C, and temperature retention time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; Take out after sample cools naturally, namely obtain the TiO with 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 leaves standstill and makes half an hour dyestuff and catalyst reach adsorption equilibrium.Ultraviolet source selects power to be the xenon lamp of 350 W, distance methyl orange (MO) liquid level 50 cm place vertical irradiation.Spectrophotometer is utilized to measure its solution concentration at methyl orange maximum absorption wavelength 464 nm place.This example annealing specimen degradation experiment result as shown in Figure 4.As can be seen from accompanying drawing 4, the TiO prepared by method provided by the invention 2nanometer powder/porous material possesses good photocatalysis performance.
Done XRD test (as accompanying drawing 3) to gained sample, XRD result shows, and the mixing crystal formation of anatase and rutile has appearred in gained sample, the reason of Here it is product has better photocatalysis performance: anatase and rutile two kinds of crystal formation TiO 2fermi level different, between two-phase interface, form Schottky potential barrier (referring to the region with rectified action that metal-semiconductor border is formed), the transfer in electronics and hole can be promoted, be separated 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.Thus restrained effectively the compound of electron-hole, thus improve the photocatalysis performance of prepared sample.
Embodiment 2
(1) method of ald is utilized to grow TiO on the sponge of cleaning 2nano thin-film;
The method of described ald, with titanium tetrachloride (TiCl 4) and water as presoma, its temperature is controlled as 115 DEG C and 60 DEG C.Reaction temperature and substrate temperature are set to 160 DEG C.After the sponge of cleaning grows 800 circulations, namely taking-up obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, pass into oxygen, heat-treat.Heat up with the programming rate of 16 DEG C/min, calcination temperature is 600 DEG C, and temperature retention time is 4 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; Take out after sample cools naturally, can TiO be obtained 2nanometer powder/porous material.
Embodiment 3
(1) method of ald is utilized to grow TiO on the sponge of cleaning 2nano thin-film;
The method of described ald, with butyl titanate (Ti (OBu) 4) and water as presoma, its temperature is controlled as 90 DEG C and 45 DEG C.Reaction temperature and substrate temperature are set to 180 DEG C.After the sponge of cleaning grows 500 circulations, namely taking-up obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, pass into oxygen, heat-treat.Heat up with the programming rate of 12 DEG C/min, calcination temperature is 300 DEG C, and the reaction time is 5 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; Take out after sample cools naturally, namely obtain the TiO with high catalytic performance 2nanometer powder/porous material.
Embodiment 4
(1) method of ald is utilized to grow TiO on the sponge of cleaning 2nano thin-film;
The method of described ald, using four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, its temperature is controlled as 105 DEG C and 55 DEG C.Reaction temperature and substrate temperature are set to 200 DEG C.After the sponge of cleaning grows 400 circulations, namely taking-up obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 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.Heat up with the programming rate of 18 DEG C/min, calcination temperature is 200 DEG C, and the reaction time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; Take out after sample cools naturally, namely obtain the TiO with high catalytic performance 2nanometer powder/porous material.
Embodiment 5
(1) method of ald is utilized to grow TiO on the sponge of cleaning 2nano thin-film;
The method of described ald, using four (dimethylamino) titanium Titanium tetrakis (dimethylamide) and water as presoma, its temperature is controlled as 105 DEG C and 55 DEG C.Reaction temperature and substrate temperature are set to 150 DEG C.After the sponge of cleaning grows 800 circulations, namely taking-up obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; And alumina crucible is put into tube furnace, pass into hydrogen, heat-treat.Annealing temperature is 700 DEG C, and temperature retention time is 3 hours, and passing into gas flow rate is 0.2 ~ 1 liter/min; Take out after sample cools naturally, namely obtain the TiO with high catalytic performance 2nanometer powder/porous material.

Claims (4)

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) Atomic layer deposition method is utilized to grow TiO on sponge 2nano thin-film:
In atomic layer deposition apparatus, using titanium source and water as presoma, controlling titanium source temperature is 50 ~ 150 DEG C, coolant-temperature gage 30 ~ 60 DEG C, and reaction temperature and substrate temperature are set to 120 ~ 220 DEG C, the sponge of cleaning carries out the growth of several circulations, obtains having TiO 2the sponge of nano thin-film;
(2) TiO will be had 2the sponge of nano thin-film is placed in alumina crucible; Alumina crucible is put into tube furnace, passes into gas with the flow velocity of 0.2 ~ 1 liter/min, be warming up to 200 ~ 700 DEG C, calcination with the programming rate of 5 ~ 20 DEG C/min, the time is 1 ~ 5 hour; Take out after naturally cooling, namely obtain the TiO with high catalytic property matter 2nanometer powder/porous material;
Described gas is O 2, N 2, O 3or H 2pure gas.
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. the TiO prepared by the described preparation method of one of claim 1 ~ 2 2nanometer powder/porous material.
4. a TiO as claimed in claim 1 2the application of nanometer powder/porous material in photocatalysis.
CN201310686250.0A 2013-12-16 2013-12-16 High-catalytic-property TiO2 nano powder/porous material as well as preparation method and application of high-catalytic-property TiO2 nano powder/porous material Expired - Fee Related CN103638915B (en)

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