CN109665558A - A kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film - Google Patents
A kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film Download PDFInfo
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- 230000001413 cellular effect Effects 0.000 title claims abstract description 23
- 239000002127 nanobelt Substances 0.000 title claims abstract description 23
- 239000013078 crystal Substances 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 239000011701 zinc Substances 0.000 claims abstract description 35
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 34
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000001699 photocatalysis Effects 0.000 claims abstract description 6
- 238000007146 photocatalysis Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 239000003054 catalyst Substances 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 230000001360 synchronised effect Effects 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000011017 operating method Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 abstract 2
- 239000011669 selenium Substances 0.000 abstract 1
- 229910052711 selenium Inorganic materials 0.000 abstract 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 239000002351 wastewater Substances 0.000 description 9
- 239000000975 dye Substances 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- -1 hydroxyl free radical Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010784 textile waste Substances 0.000 description 1
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/60—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation methods of cellular single crystal ZnO nanobelt photocatalyst film, belong to inorganic material, environmental protection, photocatalysis technology field.The problem of needing the operating procedure of a large amount of surfactant and complexity present invention aim to address the method for existing curing nano ZnO photocatalyst photochemical catalyst, the present invention is using metal zinc metal sheet as substrate and zinc source, ethylenediamine is solvent, selenium powder is selenium source, is synthesized on zinc metal sheet by solvent-thermal method presoma ZnSe (en)0.5Nanobelt film obtains cellular single crystal ZnO nanobelt photocatalyst film using roasting.The synthesis of cellular single crystal ZnO nanobelt photochemical catalyst is synchronous with load to be carried out, reduce the adverse effect factor in reaction process, so product will not introduce, impurity, purity is high are cheap with raw material, synthetic method is simple, the features such as easy to operate, in addition, gained cellular single crystal ZnO nanobelt film has preferable photocatalytic activity under ultraviolet light.
Description
Technical field
The invention belongs to inorganic material, environmental protection, photocatalysis technology fields, and in particular to prepare to metallic zinc on piece more
The preparation method of poroid single crystal ZnO nanobelt photocatalyst film.
Background technique
The industry such as weaving, printing and dyeing largely give off waste water from dyestuff daily.The big, organic contamination with water of these waste water from dyestuff
The features such as object content is high belongs to one of intractable industrial wastewater.China's textile waste is national discharged volume of industrial waste water
6th, wherein 80% belongs to dyeing waste water.These waste water from dyestuff have severely impacted ecological environment and the health of people.
One kind of more refractory reason in dyeing waste water category industrial wastewater.Due to technology, economy etc., the biology-of current most of uses
Physics administering method can only achieve basic emission request.Although being declined slightly in coloration, organic substance is only resolved into
Smaller substance is difficult control to these decomposition product properties and is also difficult to grasp, not can guarantee and do not generate harm to environment.In recent years
Come, it, can be by the harmful substance in organic wastewater under the irradiation of sunlight or ultraviolet source using Photocatalitic Technique of Semiconductor
It is converted to CO2, the innocuous substances such as water, to achieve the purpose that administer waste water.Therefore, waste water from dyestuff is administered by light-catalyzed reaction
With boundless application prospect.
Nano-ZnO is the Typical Representative of high efficiency semiconductor photochemical catalyst, forbidden bandwidth 3.37eV.Past tens
Nian Zhong, ZnO have been widely used for the research in terms of photo catalytically treating waste water.Under ultraviolet light, ZnO is excited to generate electricity
The water of son-hole pair, the hole energy decomposition catalyst adsorption of high activity generates hydroxyl free radical, and electronics can make around it
The Viability ion-oxygen of hydrogen reduction, and then the organic pollutant for being adsorbed on catalyst surface is resolved into product without secondary pollution
(such as CO2、H2O etc.), to reach decontamination purpose.
Currently, the nano ZnO photocatalyst for dye wastewater treatment is mainly powder-product.Powdered photochemical catalyst
Occur phenomena such as easy to reunite, easy loss in use, exists after use and be difficult to separate and be difficult to be recycled with solution
The problems such as, these disadvantages limit its practical application to a certain extent.Therefore, it is next real to generally select certain method by people
For existing ZnO in the immobilized of the surface of solids, the carrier generally selected is stainless steel, glass, quartz and tile etc..But the choosing of carrier
Select the activity that will affect catalyst, homogeneity and appendix amount；The structure of carrier also will affect transmitting of the light in system simultaneously
Process and substance (such as pollutant and O2Deng) it is transmitted to the mass transport process of catalyst surface, the selected method one for solidifying photochemical catalyst
As for infusion method, chemical vapor deposition (CVD) method, sol-gel method, pulsed laser deposition and spray heating decomposition etc..?
In these methods, some need expensive instrument and equipment, accurate operating method, some are needed during realization is catalyst cured
The operating procedure of a large amount of surfactant and complexity is wanted, to solve the above-mentioned problems, urgent need is developed simple, economical, environmentally friendly
Method prepare efficient ZnO photocatalysis film.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides a kind of cellular single crystal ZnO nanobelt photocatalysis
The preparation method of agent film.Chemical reagent used in this method is few, and preparation process is simple, the equipment for not needing complex and expensive, closes
At mild condition；The synthesis of cellular single crystal ZnO nanobelt photochemical catalyst is synchronous with load to be carried out；The ZnO compound grown
Impurity, purity is high will not be introduced, it is easy to use, and be conducive to recycling and reuse.
The present invention provides a kind of preparation methods of cellular single crystal ZnO nanobelt photocatalyst film, and specific steps are such as
Under:
1) stand-by after zinc metal sheet being carried out surface clean with distilled water and dehydrated alcohol respectively；
2) sodium borohydride of the selenium powder of 0.1~0.3mmol and 0.2~0.8mmol is dissolved into 10mL ethylenediamine, by institute
Solution is stated to be transferred in 20mL reaction kettle；The zinc metal sheet handled well by step 1) is put into reaction kettle, and is immersed in the solution
In；
3) reaction kettle is kept the temperature to 18~30h at 160~200 DEG C；Zinc metal sheet is taken out after cooling, and respectively with deionized water and
Dehydrated alcohol washing；It dries at room temperature；
4) zinc metal sheet is calcined to 1~5h under 400~900 DEG C of air atmospheres, cellular single crystal ZnO nanobelt light is prepared
Catalyst film.
Wherein, the ZnO is the porous band-like structure of hexagonal phase nanometer monocrystalline, and width is 200~500nm, length
10~15 μm, average thickness is about 100nm.
The optimum condition of the method for the present invention is as follows:
Selenium powder described in step 2) is 0.2~0.3mmol；
Sodium borohydride described in step 2) is 0.3~0.7mmol.
Reaction kettle is in 170~190 DEG C of 20~28h of reaction in step 3)；
Zinc metal sheet calcination time under 500~800 DEG C of air atmospheres is 2~4h in step 4).
Beneficial effects of the present invention:
1, the present invention uses solvent-thermal method and postorder calcination method, prepares cellular monocrystalline by substrate and zinc source of metal zinc metal sheet
ZnO nano-band photocatalyst film, products therefrom are of uniform size.Simple production process of the invention, easy to operate, production cost
Lower, raw material is cheap and easy to get, easy to industrialized production.
2, zinc metal sheet is both the growth substrate of zinc source and ZnO nano-band, the synthesis and load of ZnO nano-band photochemical catalyst
It is synchronous to carry out；Reduce the adverse effect factor in reaction process, so product will not introduce impurity, purity is high.
3, present invention gained ZnO nano-band is cellular shape structure, can be come into full contact with dyestuff.Under ultraviolet light
Activity with higher, have many advantages, such as in photocatalytically degradating organic dye it is easy to use, be conducive to recycling, it is reusable,
Rhodamine B degradation rate can reach 98.5% or more within 60 minutes.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) spectrogram of 1~3 products therefrom of the embodiment of the present invention.
Fig. 2 is scanning electron microscope (SEM) figure of 1 products therefrom of the embodiment of the present invention.
Fig. 3 is scanning electron microscope (SEM) figure of 1 products therefrom of the embodiment of the present invention.
Fig. 4 is scanning electron microscope (SEM) figure of 1 products therefrom of the embodiment of the present invention.
Fig. 5 is that the saturating of 1 products therefrom of the embodiment of the present invention thanks to Electronic Speculum (TEM) figure.
Fig. 6 is selective electron diffraction (SAED) figure of 1 products therefrom of the embodiment of the present invention.
Fig. 7 is x-ray photoelectron spectroscopy (XPS) figure of 1 products therefrom of the embodiment of the present invention.
Fig. 8 is the degradation rate curve that 1~3 products therefrom of the embodiment of the present invention changes with the reaction time.
Specific embodiment
Embodiment 1
It is that 1cm × 1cm metal zinc metal sheet uses distilled water and dehydrated alcohol respectively that commercially available purity, which is first greater than 99.9%, area,
It is stand-by after each ultrasonic cleaning 3 times.The selenium powder of 0.2mmol is dissolved into 10mL ethylenediamine, it is anti-that the solution is transferred to 20mL
It answers in kettle；Processed metal zinc metal sheet is put into autoclave again；Reaction kettle is kept the temperature for 24 hours at 180 DEG C；It is taken out after cooling
Zinc metal sheet, and washed respectively with deionized water and dehydrated alcohol, it dries at room temperature.Again by zinc metal sheet in 700 DEG C of air atmospheres
Cellular single crystal ZnO nanobelt photocatalyst film is prepared in lower calcining 2h.
Compliance test result: curve a is the X-ray diffractogram of products therefrom in Fig. 1, as shown in Fig. 1-a, products therefrom diffraction maximum
Other than the diffraction maximum of zinc-base piece (JCPDS No.87-0713), the peak position of remaining each diffraction maximum respectively with hexagonal phase ZnO
Diffraction peak on the standard card of (JCPDS No.36-1451) matches, and occurs without dephasign peak, illustrates that product is ZnO.
Fig. 2~Fig. 4 is that the SEM of the present embodiment products therefrom schemes.As shown in Fig. 2, the present embodiment products therefrom is banded structure, length
10~15 μm.As shown in Figure 3 and Figure 4, gained ZnO nano-band is porous structure, and width is 200~500nm, and average thickness is about
For 100nm.Fig. 5 is that the XPS of the present embodiment products therefrom schemes.As shown in figure 5, existed simultaneously in the present embodiment products therefrom Zn,
C, tri- kinds of elements of O.Wherein, C element comes from instrument itself, and O and Zn come from sample ZnO.Fig. 6 is the saturating of the present embodiment products therefrom
Penetrate electron microscope.It will be appreciated from fig. 6 that ZnO nano-band is made of the particle that average-size is 100nm.Fig. 7 is the present embodiment products therefrom
Selective electron diffraction figure.As shown in Figure 7, the present embodiment products therefrom is mono-crystalline structures.The present embodiment is with cellular single crystal ZnO
The degrade under ultraviolet light degradation rate of rhodamine B of nanobelt photocatalyst film assesses the activity of made catalyst.In Fig. 8
Curve 1 be the present embodiment products therefrom visible light catalytic rhodamine B degradation rate curve, as shown in figure 8, rhodamine B is molten
Liquid concentration: 5mg/L；Ultraviolet lamp dominant wavelength is 365nm, and power 300W, when the reaction time is 60min, degradation rate reaches
98.5%.
Embodiment 2
It is that 1cm × 1cm metal zinc metal sheet uses distilled water and dehydrated alcohol respectively that commercially available purity, which is first greater than 99.9%, area,
It is stand-by after each ultrasonic cleaning 3 times.The selenium powder of 0.1mmol is dissolved into 10mL ethylenediamine, it is anti-that the solution is transferred to 20mL
It answers in kettle；Processed metal zinc metal sheet is put into autoclave again；Reaction kettle is kept the temperature into 18h at 200 DEG C；It is taken out after cooling
Zinc metal sheet, and washed respectively with deionized water and dehydrated alcohol, it dries at room temperature.Again by zinc metal sheet in 400 DEG C of air atmospheres
Lower calcining 5h, is prepared ZnO nano-band photocatalyst film.
Compliance test result: curve b is the X-ray diffractogram of products therefrom in Fig. 1, as shown in Fig. 1-b, products therefrom diffraction maximum
Other than the diffraction maximum of zinc-base piece (JCPDS No.87-0713), the peak position of remaining each diffraction maximum respectively with hexagonal phase ZnO
Diffraction peak on the standard card of (JCPDS No.36-1451) matches, and occurs without dephasign peak, illustrates that product is ZnO.
Curve 2 in Fig. 8 is the visible light catalytic rhodamine B degradation rate curve of the present embodiment products therefrom, as shown in figure 8, Luo Dan
Bright-B solution concentration: 5mg/L；Ultraviolet lamp dominant wavelength is 365nm, power 300W, when the reaction time is 60min, degradation rate
Reach 94.3%.
Embodiment 3
It is that 1cm × 1cm metal zinc metal sheet uses distilled water and dehydrated alcohol respectively that commercially available purity, which is first greater than 99.9%, area,
It is stand-by after each ultrasonic cleaning 3 times.The selenium powder of 0.3mmol is dissolved into 10mL ethylenediamine, it is anti-that the solution is transferred to 20mL
It answers in kettle；Processed metal zinc metal sheet is put into autoclave again；Reaction kettle is kept the temperature into 30h at 160 DEG C；It is taken out after cooling
Zinc metal sheet, and washed respectively with deionized water and dehydrated alcohol, it dries at room temperature.Again by zinc metal sheet in 900 DEG C of air atmospheres
Lower calcining 1h, is prepared ZnO nano-band photocatalyst film.
Compliance test result: curve 3 is the X-ray diffractogram of products therefrom in Fig. 1, and as shown in Figure 1, products therefrom diffraction maximum is removed
Outside the diffraction maximum of zinc-base piece (JCPDS No.87-0713), the peak position of remaining each diffraction maximum respectively with hexagonal phase ZnO (JCPDS
No.36-1451 the diffraction peak on standard card) matches, and occurs without dephasign peak, illustrates that product is ZnO.In Fig. 8
Curve 3 is the visible light catalytic rhodamine B degradation rate curve of the present embodiment products therefrom, as shown in figure 8, rhodamine B solution
Concentration: 5mg/L；Ultraviolet lamp dominant wavelength is 365nm, and power 300W, when the reaction time is 60min, degradation rate reaches
90.7%.
Zinc metal sheet in embodiment is both the growth substrate of zinc source and ZnO nano-band, ZnO nano-band photochemical catalyst
Synthesize carry out synchronous with load；Reaction reagent is less, reduces production cost, while will not to introduce impurity, purity higher for product；
The high property of gained catalyst is higher, is conducive to recycling and reuses.
Claims (6)
1. a kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film, the specific steps are as follows:
1) stand-by after zinc metal sheet being carried out surface clean with distilled water and dehydrated alcohol respectively；
2) sodium borohydride of the selenium powder of 0.1~0.3mmol and 0.2~0.8mmol is dissolved into 10mL ethylenediamine, it will be described molten
Liquid is transferred in 20mL reaction kettle；The zinc metal sheet handled well by step 1) is put into reaction kettle, and is immersed in the solution；
3) reaction kettle is kept the temperature to 18~30h at 160~200 DEG C；Zinc metal sheet is taken out after cooling, and respectively with deionized water and anhydrous
Ethanol washing is dried at room temperature；
4) zinc metal sheet is calcined to 1~5h under 400~900 DEG C of air atmospheres, cellular single crystal ZnO nanobelt photocatalysis is prepared
Agent film；
The cellular single crystal ZnO nanobelt photocatalyst film, ZnO is monocrystalline, has cellular nanobelt shape structure,
Width be 200~500nm, 10~15 μm of length, average thickness 100nm.
2. the preparation method of cellular single crystal ZnO nanobelt photocatalyst film according to claim 1, feature exist
In the purity of metal zinc metal sheet described in step 1) is 99.9% or more, and area is 1cm × 1cm.
3. the preparation method of cellular single crystal ZnO nanobelt photocatalyst film according to claim 1, feature exist
In selenium powder described in step 2) is 0.2~0.3mmol.
4. the preparation method of cellular single crystal ZnO nanobelt photocatalyst film according to claim 1, feature exist
In sodium borohydride described in step 2) is 0.3~0.7mmol.
5. the preparation method of cellular single crystal ZnO nanobelt photocatalyst film according to claim 1, feature exist
In reaction kettle is in 170~190 DEG C of 20~28h of reaction in step 3).
6. the preparation method of cellular single crystal ZnO nanobelt photocatalyst film according to claim 1, feature exist
In zinc metal sheet calcination time under 500~800 DEG C of air atmospheres is 2~4h in step 4).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910000872.0A CN109665558A (en) | 2019-01-02 | 2019-01-02 | A kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film |
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| CN110204216A (en) * | 2019-06-26 | 2019-09-06 | 五邑大学 | A kind of ZnO nano-band and preparation method thereof |
| CN110550649A (en) * | 2019-08-23 | 2019-12-10 | 安徽大学 | Porous copper oxide nanobelt assembled film, electrode plate, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110204216A (en) * | 2019-06-26 | 2019-09-06 | 五邑大学 | A kind of ZnO nano-band and preparation method thereof |
| CN110550649A (en) * | 2019-08-23 | 2019-12-10 | 安徽大学 | Porous copper oxide nanobelt assembled film, electrode plate, preparation method and application thereof |
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