CN104437516A - CuCrO2/TiO2 composite photocatalyst and preparation method thereof - Google Patents

CuCrO2/TiO2 composite photocatalyst and preparation method thereof Download PDF

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CN104437516A
CN104437516A CN201410653514.7A CN201410653514A CN104437516A CN 104437516 A CN104437516 A CN 104437516A CN 201410653514 A CN201410653514 A CN 201410653514A CN 104437516 A CN104437516 A CN 104437516A
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cucro
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CN104437516B (en
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赵修建
常海梅
熊德华
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Wuhan University of Technology WUT
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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
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Abstract

The invention relates to a CuCrO2/TiO2 composite photocatalyst. The CuCrO2/TiO2 composite photocatalyst is prepared by the following steps of depositing CuCrO2 nanocrystals on a TiO2 nanorod array film by using a spinning method or a dipping method so as to obtain a CuCrO2/TiO2 composite film, and then carrying out thermal treatment on the CuCrO2/TiO2 composite film so as to obtain the CuCrO2/TiO2 composite photocatalyst. The photocatalyst prepared by the method provided by the invention can solve the problems of catalyst curing, recycling difficulty and the like, meanwhile can develop the advantages of the p-n junction; the recombination of a current carrier can be inhibited effectively under the effect of establishing an electric field in the p-n junction; the separation of a photon-generated current carrier can be improved; the quantum efficiency can be improved, and further the photocatalysis efficiency is improved.

Description

A kind of CuCrO 2/ TiO 2composite photo-catalyst and preparation method thereof
Technical field
The invention belongs to photocatalysis technology field, be specifically related to a kind of CuCrO 2/ TiO 2composite photo-catalyst and preparation method thereof.
Background technology
Reported first TiO is taught from Fujishima in 1972 2after photocatalytic water phenomenon, experience the development of more than 40 year, TiO 2, Cu 2o, CuO, ZnO, WO 3in the photocatalysis removal of water and the organic and inorganic pollutant of gas phase, greater advance is achieved Deng catalyst.TiO 2be considered to the photochemical catalyst of most DEVELOPMENT PROSPECT and application potential because of advantages such as it is nontoxic, cheap and easy to get, photocatalytic activity is high, good stabilities, be widely applied in field of environmental improvement such as sewage disposal, purification of air, antibiotic and sterilizings.But TiO 2also there is the limitation of himself as photochemical catalyst, if its energy gap is 3.2eV, absorbing wavelength can only be less than the ultraviolet light of 387nm; Because the compound of electron hole in transmitting procedure causes quantum efficiency too low, constrain the further raising of its photocatalysis efficiency.
For improving TiO 2photocatalysis efficiency, people are devoted to reduce the compound of carrier always and improve solar energy utilization ratio two aspect research.Conventional method has supported precious metal nano-particle, doping metals, nonmetallic ion, adds sacrifice agent and preparation p-n heterojunction type composite catalyst etc.Wherein, p-n heterojunction type catalyst both can have the advantage of both p, n semiconductors concurrently, the unique property that the two combines can be played again, the p-n junction region formed after the two contact can effectively separate electronic and hole, suppress the compound of carrier, improve quantum efficiency, improve photocatalysis efficiency further.
Delafossite structure oxide CuAlO 2film was had p-type electric-conducting characteristic in 1997 by reported first, to cause in world wide researchers to ABO 2(A=Cu or Ag; B=Al, Ga, In, Y, Cr etc.) concern of series semiconductor material.Wherein CuAlO 2, CuCrO 2, CuGaO 2due to features such as its optical transparence are better, electrical conductivity is higher, valence band location is lower, be used widely as electrode material.
At present, the application study both at home and abroad about p-n heterojunction composite photocatalyst has been reported, as Cu 2o-TiO 2, AgO 2-TiO 2, NiO-TiO 2, NiO-ZnO, Cu 2o-BiVO 4deng.But, about p-type delafossite structure ABO 2materials application is little in the report of p-n heterojunction photocatalyst, only has one section about p-type AgAlO 2-N-shaped TiO 2the patent report (CN 103480372A) of heterogeneous photochemical catalyst.The many preparation of this catalyst is complicated and be powder pattern, is unfavorable for solidification and recovery.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, provides composite photo-catalyst of a kind of film morphology and preparation method thereof, and its photocatalysis efficiency is higher, and can solve catalyst fix and reclaim difficulty problem.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of CuCrO is provided 2/ TiO 2composite photo-catalyst, it is by CuCrO 2nanocrystallinely be deposited on TiO by spin-coating method or infusion process 2on nano-stick array thin film, obtain CuCrO 2/ TiO 2laminated film, then to CuCrO 2/ TiO 2laminated film is heat-treated and is obtained.
Preferably, described CuCrO 2nanocrystalline particle diameter is 10-20nm; Described TiO 2nano-stick array thin film thickness is 2-6 μm.
Above-mentioned TiO 2nano-stick array thin film is according to the report method preparation of document [J.Am.Chem.Soc, 2009,131,3985-3990.] institute; Described CuCrO 2nanocrystalline according to document [J.Mater.Chem., 2012,22,24760-24768.; ChemSusChem, 2013,6,1432-1437.] institute's report method preparation.
Present invention also offers above-mentioned CuCrO 2/ TiO 2the preparation method of composite photo-catalyst, its step is as follows:
1) CuCrO 2/ TiO 2the preparation of laminated film: by CuCrO 2nanocrystalline ultrasonic disperse, in absolute ethyl alcohol, obtains the dispersion liquid that concentration is 0.1-10g/L, then dispersion liquid is spun on TiO 2on nano-stick array thin film, then dry; Or by TiO 2nano-stick array thin film impregnated in dispersion liquid, dries and obtains CuCrO 2/ TiO 2laminated film;
2) CuCrO 2/ TiO 2the preparation of composite photo-catalyst: by step 1) gained CuCrO 2/ TiO 2laminated film is placed in Muffle furnace, under air or inert protective atmosphere, to CuCrO 2/ TiO 2laminated film is heat-treated, and obtains CuCrO 2/ TiO 2composite photo-catalyst.
By such scheme, step 1) described spin coating proceeding be rotating speed is 1000-6000 rev/min, spin coating 20 seconds, spin coating number of times is 3-15 time.
By such scheme, step 1) described impregnation technology be temperature is 20-50 DEG C, dip time is 2-32h.
By such scheme, step 2) described Technology for Heating Processing is be warming up to 300-500 DEG C with the heating rate of 5 DEG C/min under room temperature, insulation 1-5h, cools with stove subsequently.
Beneficial effect of the present invention is: 1, the present invention is with monodimension nanometer material (N-shaped TiO 2nanometer rods) and zero dimensional nanometer materials (p-type CuCrO 2nanocrystalline) be raw material, utilize spin-coating method or infusion process by CuCrO 2nanocrystallinely be deposited on TiO 2on film, then obtain CuCrO through heat treatment 2/ TiO 2composite photo-catalyst, this preparation method's technique is simple, controlled flexibly.2, due to CuCrO 2the energy gap of nanocrystalline material is about 3.25eV, and top of valence band level of energy about-5.44eV, with TiO 2level of energy coupling is good, is conducive to forming electron-hole pair, can improves quantum yield.So, use p-type CuCrO 2-N-shaped TiO 2composite photo-catalyst, the advantage of p-n hetero-junctions can have been given play to, the compound of carrier is effectively suppressed under the effect of p-n junction built in field, promote the separation of photo-generated carrier, increase the life-span of carrier, make it more effectively transfer to catalyst surface, be beneficial to light-catalyzed reaction and carry out, can further improve TiO 2photocatalysis efficiency.3, compared with prior art, according to the CuCrO that the inventive method is prepared 2/ TiO 2composite photo-catalyst can also solve the problems such as catalyst cured, recovery is difficult.
Accompanying drawing explanation
The CuCrO of Fig. 1 prepared by embodiment 2 2/ TiO 2composite photo-catalyst and blank sample (TiO 2nano-stick array thin film) degradation of methylene blue efficiency comparative figure;
The CuCrO of Fig. 2 prepared by embodiment 3 2/ TiO 2the field emission scanning electron microscope figure of composite photo-catalyst;
The CuCrO of Fig. 3 prepared by embodiment 5 2/ TiO 2composite photo-catalyst and blank sample (TiO 2nano-stick array thin film) XRD figure, wherein a, b, c, d, e are respectively CuCrO 2/ TiO 2composite photo-catalyst, blank sample test collection of illustrative plates and CuCrO 2, TiO 2, SnO 2standard diagram;
The CuCrO of Fig. 4 prepared by embodiment 6 2/ TiO 2the transmission electron microscope picture of composite photo-catalyst.
Detailed description of the invention
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 0.10g/L, with TiO 2nano-stick array thin film (6 μm), as substrate, adopts spin-coating method to prepare composite photo-catalyst: use pipettor to get the CuCrO of 0.15mL 2homogeneous dispersion drips and is coated in film substrate, and under 1000 revs/min of rotating speeds, spin coating 20 seconds, carries out spin coating next time after sample natural drying, till full 15 times of spin coating.Then sample is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 500 DEG C of heat treatment 5 hours under Ar atmosphere protection, then with stove cooling, namely obtains CuCrO 2/ TiO 2composite photo-catalyst.
Carry out photocatalysis performance test to photochemical catalyst prepared by the present embodiment, detailed process is: select methylene blue (MB) aqueous solution (5 μMs/L) as the simulating pollution thing of photocatalytic degradation, by CuCrO after heat treatment 2/ TiO 2sample is cut into 0.8 × 4cm 2size, is placed in the quartz colorimetric utensil filling 3mL methylene blue solution.Before illumination, leave standstill 1 hour to reach adsorption equilibrium in dark place, then carry out illumination with 30W uviol lamp, intensity of illumination is 1.2mW/cm 2.At interval of 1 hour, ultraviolet-visible absorption spectroscopy (UV-1601 spectrometer) test is carried out to the solution in quartz colorimetric utensil afterwards.Because of in low strength range, absorbance is directly proportional to concentration, and aqueous solution of methylene blue has maximum absorption band at 664nm place, therefore indirect calculation can go out the photocatalysis efficiency of composite catalyst by contrasting 664nm place absorption peak.After tested, this CuCrO 2/ TiO 2composite photo-catalyst 8h degradation rate is 81.0% (single TiO 2nano-stick array thin film 8h degradation rate is 74.6%).
Embodiment 2
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 0.50g/L, with TiO 2nano-stick array thin film (2 μm), as substrate, adopts spin-coating method to prepare composite catalyst: use pipettor to get the CuCrO of 0.15mL 2homogeneous dispersion drips and is coated in film substrate, and under 5000 revs/min of rotating speeds, spin coating 20 seconds, carries out spin coating next time after sample natural drying, till full 5 times of spin coating.Then sample is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 500 DEG C of heat treatment 1 hour under Ar atmosphere protection, then with stove cooling, namely obtains CuCrO 2/ TiO 2composite photo-catalyst.
Be illustrated in figure 1 the CuCrO prepared by the present embodiment 2/ TiO 2composite photo-catalyst and blank sample (TiO 2nano-stick array thin film) degradation of methylene blue efficiency comparative figure, CuCrO prepared as seen from the figure 2/ TiO 2the more blank sample of photocatalysis efficiency of composite photo-catalyst has and more significantly improves, and 8h degradation rate brings up to 82.3% by 74.6%.
Embodiment 3
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 1.0g/L, with TiO 2nano-stick array thin film (2 μm), as substrate, adopts spin-coating method to prepare composite catalyst: use pipettor to get the CuCrO of 0.15mL 2homogeneous dispersion drips and is coated in film substrate, and under 5000 revs/min of rotating speeds, spin coating 20 seconds, carries out spin coating next time after sample natural drying, till full 5 times of spin coating.Then the sample that spin coating is good is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 300 DEG C of heat treatments 1 hour, then with stove cooling, namely obtains CuCrO 2/ TiO 2composite photo-catalyst.Carried out Characterization of Its Photocatalytic Activity, its 8h degradation rate is 81.1%.Be illustrated in figure 2 CuCrO prepared by the present embodiment 2/ TiO 2the field emission scanning electron microscope figure of composite photo-catalyst, as seen from the figure, CuCrO 2nanocrystalline size is 10-20nm, TiO 2nanometer rods average side length is 90nm, and average length is 2 μm, CuCrO 2nanocrystallinely to be deposited in nanorod surfaces.
Embodiment 4
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 2.0g/L, with TiO 2nano-stick array thin film (2 μm), as substrate, adopts infusion process to prepare composite catalyst.It is impregnated at 50 DEG C the CuCrO of 2.0g/L 2in dispersion liquid, after 2 hours, take out sample, dry under being placed in natural environment.Then sample is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 300 DEG C of heat treatments 1 hour, then with stove cooling, namely obtains CuCrO by infusion process 2/ TiO 2composite photo-catalyst.Carried out Characterization of Its Photocatalytic Activity, its 8h degradation rate is 78.8%.
Embodiment 5
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 10g/L, with TiO 2nano-stick array thin film (2 μm), as substrate, adopts infusion process to prepare composite catalyst.It is impregnated at 20 DEG C the CuCrO of 10g/L 2in dispersion liquid, completely take out sample after 32 hours, dry under being placed in natural environment.Then sample is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 300 DEG C of heat treatments 1 hour, then with stove cooling, namely obtains CuCrO by infusion process 2/ TiO 2composite photo-catalyst.Carried out Characterization of Its Photocatalytic Activity, its 8h degradation rate is 75.6%.The CuCrO of Fig. 3 prepared by the present embodiment 2/ TiO 2composite photo-catalyst and blank sample (TiO 2nano-stick array thin film) XRD figure, wherein a, b, c, d, e are respectively CuCrO 2/ TiO 2composite photo-catalyst, blank sample test collection of illustrative plates and CuCrO 2, TiO 2, SnO 2standard diagram, wherein SnO 2diffraction maximum comes from TiO 2nano-stick array thin film substrate FTO glass.TiO as seen from the figure 2for rutile structure (JCPDS No.21-1276), CuCrO 2for delafossite structure (JCPDS No.39-0247), in curve (a), the diffraction maximum of 31.4 ° of place's appearance belongs to CuCrO 2, confirm CuCrO in composite photo-catalyst 2existence.
Embodiment 6
Adopt the method for ultrasonic disperse by CuCrO 2nanocrystalline (10-20nm) is dispersed in absolute ethyl alcohol, is configured to the dispersion liquid that concentration is 0.50g/L, with TiO 2nano-stick array thin film (2 μm), as substrate, adopts infusion process to prepare composite catalyst.It is impregnated at 20 DEG C the CuCrO of 0.50g/L 2in dispersion liquid, completely take out sample after 32 hours, dry under being placed in natural environment.Then sample is placed in Muffle furnace, with the heating rate of 5 DEG C/min, 300 DEG C of heat treatments 1 hour, then with stove cooling, namely obtains CuCrO by infusion process 2/ TiO 2composite photo-catalyst.Carried out Characterization of Its Photocatalytic Activity, its 8h degradation rate is 82.2%.Be illustrated in figure 4 the CuCrO prepared by the present embodiment 2/ TiO 2the transmission electron microscope picture of composite photo-catalyst, as seen from the figure TiO 2nanometer rods and CuCrO 2nanocrystalline size is basic consistent with scanning electron microscope (SEM) photograph, CuCrO 2nanocrystallinely be deposited on TiO 2nanometer rods top and surrounding.

Claims (6)

1. a CuCrO 2/ TiO 2composite photo-catalyst, is characterized in that: it is by CuCrO 2nanocrystallinely be deposited on TiO by spin-coating method or infusion process 2on nano-stick array thin film, obtain CuCrO 2/ TiO 2laminated film, then to CuCrO 2/ TiO 2laminated film is heat-treated and is obtained.
2. CuCrO according to claim 1 2/ TiO 2composite photo-catalyst, is characterized in that: described CuCrO 2nanocrystalline particle diameter is 10-20nm; Described TiO 2nano-stick array thin film thickness is 2-6 μm.
3. a CuCrO 2/ TiO 2the preparation method of composite photo-catalyst, is characterized in that step is as follows:
1) CuCrO 2/ TiO 2the preparation of laminated film: by CuCrO 2nanocrystalline ultrasonic disperse, in absolute ethyl alcohol, obtains the dispersion liquid that concentration is 0.1-10g/L, then dispersion liquid is spun on TiO 2on nano-stick array thin film, then dry; Or by TiO 2nano-stick array thin film impregnated in dispersion liquid, makes CuCrO 2nanocrystallinely be deposited on TiO 2on nano-stick array thin film, dry and obtain CuCrO 2/ TiO 2laminated film;
2) CuCrO 2/ TiO 2the preparation of composite photo-catalyst: by step 1) gained CuCrO 2/ TiO 2laminated film is placed in Muffle furnace, under air or inert protective atmosphere, to CuCrO 2/ TiO 2laminated film is heat-treated, and obtains CuCrO 2/ TiO 2composite photo-catalyst.
4. CuCrO according to claim 3 2/ TiO 2the preparation method of composite photo-catalyst, is characterized in that step 1) described spin coating proceeding is rotating speed 1000-6000 rev/min, spin coating 20 seconds, spin coating number of times is 3-15 time.
5. CuCrO according to claim 3 2/ TiO 2the preparation method of composite photo-catalyst, is characterized in that step 1) described impregnation technology is dipping temperature 20-50 DEG C, dip time is 2-32h.
6. CuCrO according to claim 3 2/ TiO 2the preparation method of composite photo-catalyst, is characterized in that step 2) described Technology for Heating Processing is be warming up to 300-500 DEG C with the heating rate of 5 DEG C/min under room temperature, insulation 1-5h, cools with stove subsequently.
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CN108295868A (en) * 2018-03-06 2018-07-20 湖北文理学院 AgCrO2-CuCr2O4Composite material, preparation method and application
CN113952954A (en) * 2021-11-25 2022-01-21 白银新大孚科技化工有限公司 Composite material and preparation method thereof
CN114534684A (en) * 2022-02-16 2022-05-27 武汉工程大学 Preparation method of magnetic recyclable composite material for removing chromium

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN108295868A (en) * 2018-03-06 2018-07-20 湖北文理学院 AgCrO2-CuCr2O4Composite material, preparation method and application
CN108295868B (en) * 2018-03-06 2020-11-06 湖北文理学院 AgCrO2-CuCr2O4Composite material, preparation method and application thereof
CN113952954A (en) * 2021-11-25 2022-01-21 白银新大孚科技化工有限公司 Composite material and preparation method thereof
CN114534684A (en) * 2022-02-16 2022-05-27 武汉工程大学 Preparation method of magnetic recyclable composite material for removing chromium

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