CN103962159B - A kind of photocatalyst and its preparation method and application - Google Patents

A kind of photocatalyst and its preparation method and application Download PDF

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CN103962159B
CN103962159B CN201410204187.7A CN201410204187A CN103962159B CN 103962159 B CN103962159 B CN 103962159B CN 201410204187 A CN201410204187 A CN 201410204187A CN 103962159 B CN103962159 B CN 103962159B
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metal
photocatalyst
oxide
sulfide
metal sulfide
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CN103962159A (en
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王现英
刘洋洋
谢澍梵
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The open a kind of photocatalyst of the present invention and preparation method and application, described photocatalyst is that metal-oxide is calculated by mass percentage with metal sulfide, i.e. metal-oxide: metal sulfide be the ratio of 99.99% 98%:0.01% 2% carry out compound obtained by metal composite;Described metal-oxide is zinc oxide or titanium oxide;Described metal sulfide is molybdenum sulfide or tungsten sulfide.Its preparation method will metal-oxide and metal sulfide is the most agitated, mixing, ultrasonic, dry, obtain photocatalyst, this photocatalyst can realize the absorption to sunlight all band light can improve again its electricity conversion, the compound of carrier, comprehensive raising photocatalysis efficiency can also be suppressed simultaneously.This photocatalyst has higher catalytic efficiency and faster Catalysis Rate than other kinds of photocatalyst to analyte.More abundant, more comprehensively to the utilization rate of sunlight.The feature that additionally this catalyst also has inexpensively, is easy to get.

Description

A kind of photocatalyst and its preparation method and application
Technical field
The present invention relates to field of environment protection, particularly relate to a kind of photocatalyst and its preparation method and application.
Background technology
Problem of environmental pollution, as an one of difficult problem for the world today, is more and more paid attention to, efficiently, safety, low one-tenth This this problem of solution is it may be said that enjoy popular confidence.The mechanism of action of himself excellence of photocatalysis complies fully with above-mentioned requirements, only The requirement of one is exactly that we need to prepare the photocatalyst with efficient catalytic performance and the efficiency of light energy utilization.But it is the most domestic and international TiO is mainly had for light-catalysed material2The feature such as have benefited from that it is cheap, physico-chemical property good and bio-compatibility is good so that it is Become the photocatalyst material of a kind of natural excellence, but owing to the broad stopband of its 3.2eV makes it can only absorb ultraviolet band Light only account for the 5% of sunlight, greatly reduce the utilization to sunlight.The most commonly used another kind of urging to light But in change be zinc oxide its exist multiple nanostructured energy gap be 3.37eV exist and TiO2Outside same problem, oxygen Change zinc has again fast light corrosivity poor as photocatalyst, environmental pH requires the shortcomings such as harsh, mainly by adulterating it And surface modification is to adjust its band structure, to improve the conventional means that its performance is solution the problems referred to above.
The metal-oxide of nanostructured has big specific surface area, suitable energy gap, it is easy to the aspects such as preparation Excellent specific property and enjoy high praise, but there are again some drawbacks in self.The molybdenum bisuphide of two-dimensional structure is novel as one simultaneously The two-dimensional structure of class Graphene have excellent with Graphene many performances, its from the block structure of a band gap to having 2.83eV The straight band gap monoatomic layer structure of energy gap, is greatly enhanced it to the utilization especially visible wavelength of sunlight.And Owing to the energy gap of the molybdenum bisuphide of varying number layer slightly changes, so the molybdenum bisuphide of varying number layer is mixed and make Absorb, with making it have, the energy gap that all sunlight wave bands match, thus realize all band to solar energy and absorb, this Sample will improve the utilization to solar energy to a great extent thus improves light-catalysed efficiency.The perfect adaptation institute of these two kinds of materials The composite photo-catalyst of preparation will have the highest catalytic performance.
For preparation method, chemical vapour deposition technique is to prepare one of nano structural material most common method, this side Method has degree of crystallinity and the feature such as taking property is good compared with additive method.Liquid phase stripping method prepares monolayer or which floor two sulfur of minority simultaneously Changing molybdenum to be more conducive to realize quantifying relative to additive method, the molybdenum bisuphide of its gained has various different layer, and prepared Cheng Feichang is simple, inexpensively.
It is contemplated that monoatomic layer prepared by the Zinc oxide nano sheet of high-quality CVD prepared and liquid phase stripping method Or which floor molybdenum bisuphide simple composite of minority, thus prepare efficient photocatalyst, it is achieved the efficient utilization to sunlight.
Chinese patent (CN 103464180) discloses the preparation method and applications of a kind of novel photocatalysis just material.Will Graphene is combined with P25, utilizes the excellent electronic conductivity of Graphene can promote that the photo-generated carrier of P25 migrates, reaches electricity Son and the high efficiency separation in hole, thus promote the ultraviolet catalytic performance of P25.Subsequently, the method utilizing surface chlorination will be compound Object depth enters modification, introduces chlorine radical, is that degradation property promotes further.
Chinese patent (CN1472007A) discloses sulphuric acid and titanium dioxide composite photocatalyst, has visible light activity, The activity of Ti4+ can be improve by the excited by visible light of wavelength 387-510 nanometer, i.e. capture the ability of light induced electron, and surface Hydroxyl or oxygen anion free radical capture photohole, thus reduce the recombination rate of photo-generate electron-hole pair, improve organic Pollute degradation effect.
Above two patents are the formula disclosing composite photo-catalyst, but this composite photo-catalyst utilizes ripple to light The little i.e. majority of long scope can only absorb the light of ultraviolet region, light induced electron and hole and easily be combined, needs noble metal as co-catalysis The shortcoming and defect of the aspects such as agent.
Summary of the invention
An object of the present invention is light to utilize wave-length coverage little i.e. the most in order to solve above-mentioned composite photo-catalyst Number can only absorb the light of ultraviolet region, light induced electron and hole be easily combined, need noble metal as the aspects such as promoter lack Point and not enough and provide one can utilize all band sunlight, postpones p-n junction that photo-generated carrier is quickly combined and not Need the photocatalyst that just can quickly realize organic degraded of any other promoter.
The two of the purpose of the present invention are to provide the preparation method of above-mentioned a kind of photocatalyst.
Technical scheme
A kind of photocatalyst, calculates with metal sulfide by mass percentage for metal-oxide, i.e. metal-oxide: gold Genus sulfide be the ratio of 99.99%-98%:0.01%-2%, preferably 99.99%-99%:0.01%-1% carry out compound obtained by gold Belong to complex;
Described metal-oxide is zinc oxide or titanium oxide;
Described metal sulfide is molybdenum sulfide or tungsten sulfide;
Described metal-oxide is random flaky nanometer structure, and the size of described flaky nanometer structure is 10- 900nm, thickness is 10-50nm;
Described metal sulfide is random flaky nanometer structure, and the size of described flaky nanometer structure is 10- 100nm, thickness is 0.6-5nm.
The preparation method of above-mentioned a kind of photocatalyst, specifically comprises the following steps that
Will metal-oxide and metal sulfide agitated 10-60min mixing after, control frequency be that 100-200W is carried out Ultrasonic 30-90min, then controls temperature 100-150 DEG C and is dried, obtain described photocatalyst;
Wherein metal-oxide can be by chemical vapour deposition technique, hydro-thermal method, pulsed laser deposition or molecular beam epitaxy Prepare etc. method, prioritizing selection chemical vapour deposition technique of the present invention;
Described chemical vapour deposition technique, i.e. with silicon chip or the Al of plating noble metal2O3For substrate, it is 99.99% by purity Metal oxide powder and carbon dust 1:10-10:1 in mass ratio that purity is 99.99% mixing, mix five oxidations of 2.5% 25% Two phosphorus (P2O5);
The control parameter of above-mentioned chemical vapour deposition technique process is as follows: growth temperature is 800-1000 DEG C, growth time Less than 10min, 40 DEG C/min of programming rate, argon (Ar) flow 10-120sccm, oxygen (O2) flow 10-80sccm.
Metal sulfide therein can be inserted stripping method, liquid phase stripping method, change by mechanical stripping method, electrochemical lithium ion The method such as vapour deposition process or hydro-thermal method is produced, prioritizing selection liquid chromatography ultrasound stripping method of the present invention.
Which floor the preparation of metal sulfide of monoatomic layer or minority:
Use the metal sulfide needed for the method preparation of liquid chromatography ultrasound stripping, first choose and lamina block metal is vulcanized Thing has the solution such as N-Methyl pyrrolidone (NMP) of fine suspension effect, NVP (NVP), hydrogen peroxide Isopropylbenzene (CHP) or water etc. are used as liquid phase carrier to prepare which floor metal sulfide of monoatomic layer or minority;
Being placed in liquid phase carrier by the metallic sulfide powder that purity is 99.99%, wherein the concentration of metal sulfide is 0.01-1g/mL, then carries out ultrasonic stripping, and after ultrasonic stripping, controlling centrifugal speed is that 1500-12000r/min is centrifuged 30-60min, obtains photocatalyst, the metal composite that i.e. metal-oxide and metal sulfide are composited.
Above-mentioned ultrasonic stripping process controls parameter: ultrasonic time 30-800min, supersonic frequency 80-500W.
Above-mentioned a kind of photocatalyst is for the photocatalytic degradation of Organic substance methylene blue, and its consumption presses photocatalyst with sub- The mass ratio of methyl blue is that the ratio of 1:100 calculates.
The Advantageous Effects of the present invention
The photocatalyst of the present invention due to selected two kinds be well suited for for photocatalyst material i.e. metal-oxide and Metal sulfide and its compound after have and be adapted for light-catalysed energy gap, therefore both compound after can realize too The absorption of sunlight all band light can improve again its electricity conversion, can also delay the compound of carrier, comprehensive raising simultaneously Photocatalysis efficiency.
Further, the photocatalyst of the present invention, compared to other kinds of photocatalyst, methylene blue is had higher Catalytic efficiency and faster Catalysis Rate.Secondly this kind of catalyst is more abundant, more comprehensively to the utilization rate of sunlight.
Further, the photocatalyst of the present invention, it is metal-oxide due to selected material and metal sulfide is all Common and widely used metallic compound therefore raw material is easy to get, and production cost is low.
Further, the photocatalyst of the present invention, its preparation technology is simple, all has good catalysis under Uv and visible light Effect, can effectively adapt to large-scale industrial production and can apply in large-scale water treatment technology.
Further, the photocatalyst of the present invention, owing to metal-oxide and metal sulfide are all almost in the knot of two dimension Therefore structure has a huge specific surface area, and adding less and catalytic effect is high, and stable chemical nature, can effectively compatibility arrive In any one advanced treatment process that existing water processes, and described two kinds of compositions of photocatalyst of the present invention all do not dissolve in Water, the response rate is high, has huge environment protection significance and value.
In sum, the photocatalyst of the present invention, than other kinds of photocatalyst, analyte had higher catalysis Efficiency and faster Catalysis Rate.More abundant, more comprehensively to the utilization rate of sunlight.Additionally this photocatalyst also have inexpensively, The feature being easy to get.
Accompanying drawing explanation
Fig. 1, ZnO-MoS2The SEM figure of the scanning electron microscope of composite photo-catalyst;
Fig. 2, ZnO-MoS2The TEM figure of composite photo-catalyst transmission electron microscope under 790000X multiplying power;
Fig. 3, ZnO-MoS2TEM diffraction pattern under composite photo-catalyst transmission electron microscope under 200X multiplying power;
Fig. 4, ZnO-MoS2The XPS figure of the x-ray photoelectron power spectrum of composite photo-catalyst;
Fig. 5, ZnO-MoS2Composite photo-catalyst, the absorption curve of pure ZnO, P25 pressed powder;
Fig. 6, Zn-MoS2Composite photo-catalyst, the photocurrent curve of pure ZnO, P25 pressed powder;
Fig. 7, ZnO-MoS2The absorption curve of composite photocatalyst for degrading methylene blue;
Fig. 8, ZnO-MoS2The degradation curve of the degradation of methylene blue of composite photo-catalyst and pure ZnO and P25 pressed powder;
Fig. 9, ZnO-MoS2The reaction power of the degradation of methylene blue of composite photo-catalyst and pure ZnO and P25 pressed powder Learn calculated curve;
Figure 10, ZnO-MoS2The bar graph of the degradation of methylene blue of composite photo-catalyst and pure ZnO and P25 pressed powder;
Figure 11, ZnO-MoS2The organic schematic diagram of composite photocatalyst for degrading.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, but it is not limiting as the present invention.
Embodiment 1
A kind of photocatalyst, calculates with metal sulfide by mass percentage for metal-oxide, i.e. metal-oxide: gold Belong to sulfide be the ratio of 99%:1% carry out compound obtained by metal composite;
Described metal-oxide is zinc oxide;
Described metal sulfide is molybdenum bisuphide;
Described zinc oxide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-900nm, thickness For 10-50nm;
Described molybdenum bisuphide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-100nm, thick Degree is 0.6-5nm.
The preparation method of above-mentioned photocatalyst, specifically includes following steps:
1, traditional chemical vapour deposition technique is used to prepare Zinc oxide nano sheet
(1), by etc. the Zinc oxide powder of mass ratio and graphite powder be fully ground, add 5% phosphorus pentoxide, then fill Enter in quartz boat;
(2), the Al of Au thin film will be coated with2O3Substrate is placed on quartz boat powder, is placed in quartz glass by quartz boat;
(3), quartz boat glass tubing is put in tube furnace, and make quartz boat be directed at stove centre;
(4), being warming up to 1000 DEG C, heating rate is 40 DEG C/min;
(5) argon (Ar) flow 10 Sccm, oxygen (O, it are passed through2) flow 30Sccm, growth time 5min;
(6), it is always maintained at aeration status, until naturally cooling to room temperature;
(7), on substrate, whiteness is Zinc oxide nano sheet;
2, liquid phase stripping method is used to prepare monoatomic layer molybdenum bisuphide
(1), by molybdenum disulfide powder adding NVP (NVP), its concentration is 0.05g/ml, and will mixing Thing is placed in brown vial;
(2), by brown vial being placed in ultrasound wave and carry out ultrasonic, frequency is 400W, ultrasonic time 400min, and protects Hold ultrasonic temperature below 15 DEG C;
(3), by ultrasonic complete mixed liquor being placed in centrifuge tube and be centrifuged, centrifugal speed is 11000r/min, centrifugal Time 60min;
(4), the supernatant of centrifuge tube top 1ml is taken out;
(5), by the supernatant of taking-up it is placed in beaker after repeatedly diluting with deionized water, clean and dries again, until by N- Vinyl pyrrolidone (NVP) is removed completely, so that it may obtain high-quality monoatomic layer molybdenum bisuphide;
Wherein in centrifuged supernatant, the amount of monoatomic layer molybdenum bisuphide can be passed through thermogravimetric analysis (TGA) and carries out quantitatively;
3, the preparation of composite photo-catalyst
After step 1 metal-oxide and step 2 metal sulfide are stirred 30min mixing, controlling frequency is that 200W is carried out Ultrasonic 30min, then controls 100 DEG C of dry 24h of temperature, obtains photocatalyst, i.e. ZnO-MoS2Composite photo-catalyst.
The ZnO-MoS of above-mentioned gained2The pattern of composite photo-catalyst use scanning electron microscope (manufacturer: FEI, Model: Quanta FEG) be scanned, the SEM of gained figure as it is shown in figure 1, from Fig. 1 it is observed that sheet irregularly and very Thin Zinc oxide nano sheet, trickles down the molybdenum bisuphide of some nearly transparent monoatomic layers, such as Fig. 1 on Zinc oxide nano sheet The part of middle black circles, it is observed that Zinc oxide nano sheet has big area and the thinnest from Fig. 1, and is scattered in it On nearly transparent molybdenum sulfide very uniform, there is big specific surface area.
The ZnO-MoS of above-mentioned gained2The appearance structure of composite photo-catalyst use transmission electron microscope (manufacturer: TESEQ, model: D-TEM) it is scanned, the TEM of gained schemes as shown in Figure 2 and Figure 3, from the TEM figure of Fig. 2 and Fig. 3 further Being confirmed, can will be apparent from understanding sees zinc oxide and the existence of molybdenum bisuphide and is all monocrystalline, and crystallization effect is very Good.
The ZnO-MoS of above-mentioned gained2The element of composite photo-catalyst uses x-ray photoelectron power spectrum (manufacturer: Britain Kratos company, model: XSAM 800) it is analyzed, the XPS of gained schemes as shown in Figure 4, demonstrates again that from the XPS figure of Fig. 4 The existence of the molybdenum bisuphide in the photocatalyst of gained of the present invention.
Embodiment 2
A kind of photocatalyst, calculates with metal sulfide by mass percentage for metal-oxide, i.e. metal-oxide: gold Belong to sulfide be the ratio of 99.9%:0.1% carry out compound obtained by metal composite;
For the composite construction of metal-oxide Yu metal sulfide, a kind of photocatalyst, for metal-oxide and metal sulfur The composite construction of compound, is mixed by metal-oxide and metal sulfuration in mass ratio 99.9%, stirs 30 minutes, ultrasonic 30 minutes, Power is 200W, baking temperature 100 DEG C, time 24h described photocatalyst;
Described metal-oxide is zinc oxide;
Described metal sulfide is molybdenum bisuphide;
Described zinc oxide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-900nm, thickness For 10-50nm;
Described molybdenum bisuphide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-100nm, thick Degree is 0.6-5nm.
The preparation method of above-mentioned a kind of photocatalyst, with embodiment 1.
Embodiment 3
A kind of photocatalyst, calculates with metal sulfide by mass percentage for metal-oxide, i.e. metal-oxide: gold Belong to sulfide be 99.99%:0.01% carry out compound obtained by metal composite;
Described metal-oxide is zinc oxide;
Described metal sulfide is molybdenum bisuphide;
Described zinc oxide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-900nm, thickness For 10-50nm;
Described molybdenum bisuphide is random flaky nanometer structure, and the size of its flaky nanometer structure is 10-100nm, thick Degree is 0.6-5nm.
The preparation method of above-mentioned a kind of photocatalyst, with embodiment 1.
The ZnO-MoS of above-described embodiment 1-3 gained2Composite photo-catalyst and pure ZnO and P25 pressed powder are at room temperature bar The absorption to light measured by ultraviolet-visual spectrometer (manufacturer: Shimadzu Corporation, model: Shimadzu UV-2600) is utilized under part Curve is as it is shown in figure 5, the most relatively pure ZnO and P25, the ZnO-MoS of this experiment gained2Composite photo-catalyst Absorption to light is greatly reinforced, and this not only shows and visible region is also manifested by the light to UV light region, is indicated above Composite photo-catalyst described in is remarkably productive in terms of improving sunlight all band light absorption, and this is to its photocatalysis efficiency During raising very favorable.
The ZnO-MoS of above-described embodiment 1-3 gained2Composite photo-catalyst and pure ZnO and P25 pressed powder are at room temperature bar Photocurrent curve such as Fig. 6 that probe station (manufacturer: U.S. Cascade Microtch, model: M150) records is utilized under part Shown in, as can be seen from Figure 6 relative to pure ZnO and P25, the ZnO-MoS of this experiment gained2Composite photo-catalyst is in illumination Lower photocurrent values significantly increases, and is 3-4 times of P25, is indicated above described composite photo-catalyst and improves to a certain extent Its electricity conversion.
Application ExampleThe photocatalysis experiment of photocatalyst
The ZnO-MoS of gained in Example 1-32Composite photo-catalyst is respectively used to the photocatalysis of Organic substance methylene blue Degraded, specifically comprises the following steps that
(1) ZnO-MoS of 40mg above-described embodiment 1-3 gained, is taken respectively2Pure ZnO and 40mg of composite photo-catalyst, 40mg P25 pressed powder is placed in beaker, and being separately added into 40ml concentration is in 10mg/L aqueous solution of methylene blue;
(2), above-mentioned beaker being first placed in darkroom 10min, take 5ml and be placed in centrifuge tube, dislocation is under sunlight the most again (light rate density is 1800uV/cm2), magnetic agitation, sample every 2min;
(3), being centrifuged by centrifuge tube, centrifugal speed is 8000r/min, centrifugal 15min;
(4) centrifugal complete supernatant is placed in ultraviolet-visual spectrometer, owing to the characteristic absorption peak of methylene blue exists At 664nm, therefore observe the change of its light absorption value herein.
The ZnO-MoS of above-described embodiment 2 gained2Absorption curve after composite photocatalyst for degrading methylene blue such as Fig. 7 institute Showing as can be seen from Figure 7 have the methylene blue of 90% to be degraded under sunlight after 2min, after 4 minutes, methylene blue is complete Degradable, has been indicated above composite catalyst and has had good catalytic effect.
The ZnO-MoS of above-described embodiment 1-3 gained2Composite photo-catalyst and pure ZnO and P25 pressed powder degraded methylene Degradation curve after basket as shown in Figure 8, as can be seen from Figure 8 adds MoS2ZnO degradation of methylene blue is produced certain later Impact, along with MoS2The degradation rate increasing methylene blue of amount is by gradually accelerating, but works as MoS2Amount reach certain value after Restricting its reduction of speed rate on the contrary, this is mainly because of because of too much MoS2The composite catalyst absorption to light can be hindered, thus reduce Catalytic efficiency, has been indicated above the MoS that addition is appropriate2The photocatalysis efficiency of ZnO had significant reinforced effects.
The ZnO-MoS of above-described embodiment 1-3 gained2Composite photo-catalyst, pure ZnO, P25 pressed powder degradation of methylene blue After kinetics calculated curve and bar graph respectively such as Fig. 9 and as shown in Figure 10, further demonstrate appropriate MoS2 Raising to ZnO photocatalysis efficiency.
In sum, the Zinc oxide nano sheet of gained and the compound photocatalyst of monoatomic layer molybdenum bisuphide are relative to pure ZnO and P25 pressed powder has outstanding absorbing ability, the ability of photo-generated carrier and good photocatalytic degradation Organic substance Ability.
The photocatalyst of the present invention is only combined the light of gained with metal oxide zinc and metal sulfide molybdenum bisuphide Illustrate as a example by catalyst, but be not limiting as other metal-oxides and the composite photo-catalyst of metal sulfide gained.
Further, the schematic diagram reacted by the photocatalyst in Figure 11 is it can be seen that work as photon energy higher than quasiconductor When absorbing the light irradiation quasiconductor of codomain, the valence-band electrons generation band-to-band transition of quasiconductor.I.e. transit to conduction band from valence band, thus Produce electronics (e-) and hole (h+), now adsorb the dissolved oxygen trapped electron at nano grain surface and form superoxide anion, and Absorption is oxidized to hydroxyl free radical at hydroxide ion and the water of catalyst surface by hole.And superoxide anion and hydrogen-oxygen are freely Base has the strongest oxidisability, can be by most of oxidation operation to end product CO2And H2O, even to some inorganic matters Also can thoroughly decompose, thus further confirm employing ZnO and MoS2Compound gained photocatalyst uses this principle to organic Thing decomposes.
Summary is described, and the photocatalyst of the present invention can realize the absorption to sunlight all band light can improve again its photoelectricity Transformation efficiency, can also delay the compound of carrier, comprehensive raising photocatalysis efficiency simultaneously.
Above said content is only the basic explanation under present inventive concept, and according to appointing that technical scheme is made What equivalent transformation, all should belong to protection scope of the present invention.

Claims (4)

1. a preparation method for photocatalyst, described photocatalyst is metal-oxide with metal sulfide by percent mass Than calculating, i.e. metal-oxide: metal sulfide be the ratio of 99.99%-98%:0.01%-2% carry out compound obtained by metal multiple Compound;Described metal-oxide is zinc oxide or titanium oxide;Described metal sulfide is molybdenum sulfide or tungsten sulfide;
Described metal-oxide is random flaky nanometer structure, and the size of described flaky nanometer structure is 10-900nm, thick Degree is 10-50nm;Described metal sulfide is random flaky nanometer structure, and the size of described flaky nanometer structure is 10- 100nm, thickness is 0.6-5nm;
It is characterized in that the method specifically comprises the following steps that
After being mixed by agitated to metal-oxide and metal sulfide 10-60min, controlling frequency, to be that 100-200W is carried out ultrasonic 30-90min, then controls temperature 100-150 DEG C and is dried, obtain described photocatalyst;
Wherein prepared by metal-oxide chemical vapour deposition technique, hydro-thermal method, pulsed laser deposition or molecular beam epitaxy method;
Metal sulfide therein uses mechanical stripping method, electrochemical lithium ion to insert stripping method, liquid chromatography ultrasound stripping method, chemistry Prepared by vapour deposition process or hydro-thermal method.
The preparation method of a kind of photocatalyst the most as claimed in claim 1, it is characterised in that described chemical vapour deposition technique Prepare metal-oxide, i.e. with silicon chip or the Al of plating noble metal2O3For substrate, it is the metal oxide powder of 99.99% by purity Mixing with the carbon dust that purity is 99.99% 1:10-10:1 in mass ratio, the phosphorus pentoxide mixing 2.5%-25% carries out chemistry gas Deposit mutually;
The control parameter of above-mentioned chemical vapour deposition technique process is as follows: growth temperature is 800-1000 DEG C, and growth time is less than 10min, 40 DEG C/min of programming rate, argon flow amount 10-120sccm, oxygen flow 10-80sccm.
The preparation method of a kind of photocatalyst the most as claimed in claim 1, it is characterised in that described liquid chromatography ultrasound stripping method Prepare metal sulfide, first choose N-Methyl pyrrolidone, NVP, cumyl hydroperoxide or water and make For liquid phase carrier;
Then being placed in liquid phase carrier by the metallic sulfide powder that purity is 99.99%, wherein the concentration of metal sulfide is 0.01-1g/mL, then carries out ultrasonic stripping, and after ultrasonic stripping, controlling centrifugal speed is that 1500-12000r/min is centrifuged 30-60min, obtains metal sulfide;
Above-mentioned ultrasonic stripping process controls parameter: ultrasonic time 30-800min, supersonic frequency 80-500W.
4. an application for the catalyst prepared by the preparation method of photocatalyst described in claim 1, for Organic substance methylene The photocatalytic degradation that base is blue, its consumption is calculated in the ratio that mass ratio is 1:100 of photocatalyst with methylene blue.
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