CN106345534A - Bi2WO6/Ag heterogeneous nano structure material as well as preparation method and application thereof - Google Patents
Bi2WO6/Ag heterogeneous nano structure material as well as preparation method and application thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 125000005842 heteroatom Chemical group 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 28
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 230000005693 optoelectronics Effects 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229960004756 ethanol Drugs 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 229940043267 rhodamine b Drugs 0.000 abstract description 5
- 239000002135 nanosheet Substances 0.000 abstract 4
- 238000000151 deposition Methods 0.000 abstract 2
- 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 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 241001198704 Aurivillius Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- 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
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- 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
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Abstract
The invention provides a Bi2WO6/Ag heterogeneous nano structure material as well as a preparation method and application thereof. Compared with the prior art, the Bi2WO6/Ag heterogeneous nano structure material is prepared by depositing Ag nanosheets on the surfaces of Bi2WO6 nanosheets through a simple low-temperature chemical liquid deposition method. The preparation process has the advantages of environmental friendliness, simplicity and low cost. The prepared Bi2WO6 nanosheet/Ag nanosheet material is used for photoelectric conversion, is high in photoelectric conversion efficiency, is used for organic dye rhodamine B visible light catalytic degradation, and has high activity and good stability.
Description
Technical field
The invention belongs to preparation method of nano material and Environmental Chemistry and Optical Electro-Chemistry cross-application field are and in particular to one
Plant bi2wo6/ ag hetero nano structure material, preparation method and applications.
Background technology
The water pollution that the development of today's society fast industrialization brings is a serious environmental problem it would be highly desirable to solve.Partly lead
Body base heterojunction structure photocatalysis are considered as a kind of green and the economic means of sewage disposal.
bi2wo6It is a kind of simplest aurivillius type compound, there is special layer structure and can respond visible
Light is to 460nm.Because excellent photocatalytic activity causes the extensively emerging of researcher in terms of water-splitting and organic pollutant degradation
Interest.But bi2wo6Limited visible light-responded region and being quickly combined of photo-generate electron-hole pair hinder its photocatalysis efficiency.For
Meet future source of energy and environmental applications needs improve its photocatalytic activity further.Building noble metal semiconductor heterostructure is
The available strategy solving the above problems.
Due to Schottky barrier, the electronic effect of noble metal can promote metal semiconductor interface photogenerated carriers to separate migration
Process.And, the unique surface plasma response of noble metal particularly ag will notable wideization visible absorption.
Content of the invention
It is an object of the invention to provide a kind of bi2wo6/ ag hetero nano structure material and preparation method thereof, in bi2wo6
Nanometer sheet surface deposits ag nanometer sheet, obtains bi2wo6Nanometer sheet/ag nanometer sheet hetero nano structure.Using cryochemistry liquid phase
Sedimentation, process is simple, low cost.
Present invention also offers a kind of bi2wo6The visible ray opto-electronic conversion application of/ag hetero nano structure material；Acceptable
For organic dyestuff visible light photocatalytic degradation.
A kind of bi that the present invention provides2wo6The preparation method of/ag hetero nano structure material, comprises the following steps:
(1) prepare bi2wo6；
(2) under condition of ice bath, by the bi of preparation2wo6It is placed in the acetum containing silver nitrate, add Vitamin C sour water
Solution, after reaction, is centrifuged, washs, is dried, obtain bi2wo6/ ag hetero nano structure material.
Preparation bi in step (1)2wo6Method be:
By bi (no3)3·5h2O is dissolved in hno3Form solution a, by na in solution2wo4·2h2O is dissolved in ethanol and deionization
Form solution b in the mixed solvent of water；Mixed solution a and b, after stirring reaction 5-10min, adds 1,6- hexamethylene diamine, carries out adding
Thermal response, centrifuge washing, drying, obtain bi2wo6Powder.
Further, hno3Solution concentration is 2m, bi (no3)3·5h2O is 1m in solution a concentration.
In solution b, the volume ratio of ethanol and deionized water is 4:3, na2wo4·2h2Concentration in solution b for the o is 0.07m；
Further, bi (no3)3·5h2O and na2wo4·2h2The mol ratio of o is 2:1.
The volume ratio of solution a, solution b and 1,6- hexamethylene diamine is 1:7:1.
Further, reacting by heating described in step (1), condition is: 160 DEG C of temperature, time 12h.
Washing described in step (1) is deionized water respectively and dehydrated alcohol is respectively washed 3-5 time.At described drying is 60 DEG C
Vacuum drying 6-10h.
Further, step (2) is particularly as follows: under condition of ice bath, take the bi that step (1) obtains2wo6Powder sample is ultrasonic
It is scattered in deionized water, add silver nitrate aqueous solution, add acetum, be eventually adding aqueous ascorbic acid, ice bath
Under the conditions of react, be collected by centrifugation, deionized water and dehydrated alcohol are respectively washed 3 times respectively, at 60 DEG C be vacuum dried 6h, obtain
bi2wo6/ ag powder sample.
Further, bi in step (2)2wo6Concentration is 0.025m to powder in deionized water；Described silver nitrate aqueous solution,
Concentration is 3-6mm；In acetum, glacial acetic acid and water volume ratio are 1.5:100；Aqueous ascorbic acid, concentration is 0.0115-
0.023mm；The volume ratio of deionized water, silver nitrate aqueous solution, acetum and aqueous ascorbic acid is 8:1:1:1.
Further, react under described condition of ice bath particularly as follows: reacting 15-25min under the conditions of 1-4 DEG C.
A kind of bi that the present invention provides2wo6/ ag hetero nano structure material, is prepared using above method, and form is
A diameter of 2.5-3 μm flower-shaped bi of nanometer sheet composition2wo6In structure, attachment average diameter is the ag nanometer sheet of 10nm.
A kind of bi that the present invention provides2wo6/ ag hetero nano structure material is applied as visible ray opto-electronic conversion.
Described visible ray opto-electronic conversion applies the bi particularly as follows: preparing the present invention2wo6/ ag hetero nano structure material
5mg ultrasonic disperse, in 1ml deionized water, takes 0.01ml dispersant liquid drop to be 0.28cm in area2Fto glass on.Afterwards,
This fto glass is put in drying baker, 30min is dried at 80 DEG C.Optical Electro-Chemistry test uses the three-electrode system of standard, to be loaded with
The fto glass of catalyst is working electrode, and platinum filament and ag/agcl electrode are respectively auxiliary electrode and reference electrode.With concentration it is
The na of 0.2m2so4Solution is electrolyte.Opto-electronic conversion is used 300w xenon lamp as light source, by electrochemical workstation
(chi660b) test, sweep fast 50mv s-1.
A kind of bi that the present invention provides2wo6/ ag hetero nano structure material is used for visible light photocatalytic degradation, specially organic
Dyestuff visible light photocatalytic degradation is applied；Visible light photocatalytic degradation especially to rhodamine b (rhb).
The described visible light photocatalytic degradation to rhodamine b (rhb) particularly as follows:
10mg bi prepared by the present invention2wo6It is 0.01mm that/ag hetero nano structure material is added to 100ml concentration
In rhb solution, and stir 0.5-1h in the dark, make catalyst surface reach the attached balance of absorption-desorption.Afterwards, using 300w
Xenon lamp is irradiated.Take 3ml sample every 5min centrifuge tube, after centrifugation (10000rpm, 2min), take supernatant, using purple
Outward-visible spectrophotometer measures the absorption spectrum of solution.Determine the concentration of rhb by the characteristic absorption peak at 554nm.
Compared with prior art, the present invention is by simple cryochemistry liquid phase deposition, in bi2wo6Nanometer sheet surface sinks
Long-pending ag nanometer sheet, obtains bi2wo6Nanometer sheet/ag nanometer sheet hetero nano structure.Due to bi (no3)3·5h2O facile hydrolysiss, this
In bright, first by bi (no3)3·5h2O is dissolved in salpeter solution prevents it from hydrolyzing before the reaction；And by na2wo4·2h2O is dissolved in
In the mixed solvent of ethanol and deionized water；The two before reactions fully dispersed in solvent, then after so that the two is mixed fully
Reaction.Using 1,6- hexamethylene diamine in bi2wo6Selective coordination in nanometer sheet particular crystal plane, suppresses bi2wo6Nanometer sheet longitudinally increases
Thickness, is conducive to nanometer sheet cross growth.Ascorbic acid is utilized to reduce ag further under condition of ice bath+, obtain ag nanometer seed,
And under the coordination of acetate ion, make ag nanometer seed oriented growth become ag nanometer sheet.Here condition of ice bath is conducive to
The slow oriented growth of ag nanometer seed becomes ag nanometer sheet, it is to avoid fast-growth forms the ag structure reunited.Preparation technology of the present invention
There is environmental friendliness and simple, low cost.The bi preparing2wo6Nanometer sheet/ag nanometer sheet material is used for photoelectricity
Conversion, has photoelectric transformation efficiency high；For organic dyestuff rhodamine b visible light photocatalytic degradation, active high, stability
Good.
Brief description
Fig. 1 is the bi of embodiment 1 preparation2wo6Scanning electron microscope (sem) figure of/ag hetero nano structure material；
Fig. 2 is the bi of embodiment 1 preparation2wo6Energy dispersive x-ray power spectrum (edx) figure of/ag hetero nano structure material；
Fig. 3 is embodiment 1bi2wo6X- ray powder diffraction (xrd) figure of/ag hetero nano structure material.
Fig. 4 is the bi of embodiment 1 preparation2wo6Transmission electron microscope (tem) figure of/ag hetero nano structure material；
Fig. 5 is the bi of embodiment 1 preparation2wo6The high resolution transmission electron microscopy of/ag hetero nano structure material
(hrtem) figure；
Fig. 6 is the bi of embodiment 1 preparation2wo6/ ag hetero nano structure material solid ultraviolet overflows emission spectrum, is given simultaneously
bi2wo6The experimental result of nanometer sheet is in order to compare；
Fig. 7 is embodiment 2bi2wo6Under/ag hetero nano structure material visible-light during initial potential 0.2v, transient current is close
Degree over time, provides bi simultaneously2wo6The result of nanometer sheet material is in order to compare.
Fig. 8 is embodiment 3bi2wo6The ultraviolet-ray visible absorbing of/ag hetero nano structure material visible-light catalytic degradation rhb
Spectrum；
Fig. 9 is embodiment 3bi2wo6The concentration changes with time of/ag hetero nano structure material visible-light catalytic degradation rhb
Curve, provides bi simultaneously2wo6Nanometer sheet, plus catalyst blank experiment result in order to compare；
Figure 10 embodiment 3bi2wo6The 5 of/ag hetero nano structure material visible-light catalytic degradation rhb concentration changes with time
Secondary circulation figure；
Specific embodiment
Embodiment 1
A kind of bi2wo6The preparation method of/ag hetero nano structure material, comprises the following steps:
(1) by 5mmol bi (no3)3·5h2O is dissolved in the hno of 5ml 2m3Form solution a in solution, then by 2.5mmol
na2wo4·2h2O is dissolved in formation solution b, mixed solution a and b in 20ml ethanol and the mixed solvent of 15ml deionized water, stirring
Add 5ml 1,6- hexamethylene diamine in mixed solution after reaction 5-10min, liquid is transferred to 160 DEG C of reacting by heating in reactor
12h, naturally cools to room temperature afterwards, is collected by centrifugation, and deionized water and dehydrated alcohol respectively wash 3 times respectively.Then true at 60 DEG C
Sky is dried 6h, obtains bi2wo6Powder sample.
(2) under condition of ice bath, take the bi that step (1) obtains2wo6Powder sample 1mmol ultrasonic disperse is in 40ml deionization
In water, add 6mm silver nitrate aqueous solution 5ml, being subsequently adding glacial acetic acid with water volume ratio is the acetum 5ml of 1.5:100,
Add 0.023m aqueous ascorbic acid 5ml afterwards, ice bath reacts 15-25min.It is collected by centrifugation, respectively deionized water and anhydrous
Ethanol is respectively washed 3 times, is vacuum dried 6h, obtains bi at 60 DEG C2wo6/ ag powder sample.
The structure of product and morphology characterization:
With scanning electron microscope, morphology analysis are carried out to embodiment 1 products therefrom, result is as shown in Figure 1.Show made
The flower-like structure of about 2.5-3 μm of the diameter that standby sample forms for nanometer sheet.With energy dispersive x-ray power spectrum, product component is carried out
Analysis, result is as shown in Figure 2.Show that ag element is successfully coupled to bi2wo6It is upper that (cu element is derived from substrate copper used by test sample
Piece).With x-ray powder diffractometer, the thing phase of product is analyzed, result is as shown in Figure 3.Diffraction maximum can distinguish index
Bi for orthorhombic phase2wo6Ag (jcpds standard card number: the 04- of (jcpds standard card number: 39-0256) and Emission in Cubic
0783).Further morphology analysis are carried out to embodiment 1 products therefrom with transmission electron microscope, result is as shown in Figure 4.Table
Bright prepared sample is bi2wo6In nanometer sheet, uniformly attachment average diameter is the ag nanometer sheet of 10nm.Use high-resolution transmitted electron
Microscope is analyzed to embodiment 1 products therefrom further, and result is as shown in Figure 5.The wherein interplanar distance of 0.31nm can
With index for orthorhombic phase bi2wo6(131) crystal face, the interplanar distance of 0.23nm can with index (111) crystal face for Emission in Cubic ag,
Further demonstrate that sample is bi2wo6With ag hetero nano structure.With solid uv drses further to embodiment 1 products therefrom
Analyzed, result is as shown in Figure 6.Result shows bi2wo6/ ag hetero nano structure material absorbs in visible region and substantially increases
Plus.
Embodiment 2
A kind of bi2wo6/ ag hetero nano structure visible ray opto-electronic conversion is applied.
Bi prepared by the present invention2wo6/ ag hetero nano structure material 5mg ultrasonic disperse, in 1ml deionized water, takes
0.01ml dispersant liquid drop is 0.28cm in area2Fto glass on.Afterwards, this fto glass is put in drying baker, at 80 DEG C
30min is dried.Optical Electro-Chemistry test using standard three-electrode system, be loaded with catalyst fto glass as working electrode, platinum
Silk and ag/agcl electrode are respectively auxiliary and reference electrode.Na with concentration as 0.2m2so4Solution is electrolyte.Opto-electronic conversion
It is used 300w xenon lamp as light source, tested by electrochemical workstation (chi660b), sweep fast 50mv s-1.Initial potential 0.2v
When it is seen that under light transient current density over time, result (provides bi as shown in Figure 7 simultaneously2wo6The result of nanometer sheet with
Make comparisons).bi2wo6The electrode pair visible light exposure of/ag hetero nano structure material preparation presents enhanced instantaneous photoelectric current
Response.
Embodiment 3
A kind of bi2wo6The application of/ag hetero nano structure material visible-light catalytic degradation organic dyestuff.
Take the bi of the above-mentioned preparation of 10mg2wo6It is 0.01mm rhb solution that/ag hetero nano structure material adds 100ml concentration
In and in the dark stir 1h, make catalyst surface reach the attached balance of absorption-desorption.Afterwards, it is irradiated using 300w xenon lamp.
Take 3ml sample every 5min centrifuge tube, after centrifugation (10000rpm, 2min), take supernatant, using UV-vis spectroscopy light
Degree meter (shimadzu uv-2550) measures the absorption spectrum of solution.Determine that by the characteristic absorption peak at 554nm rhb's is dense
Degree.The uv absorption spectrogram of photocatalytic degradation rhb result is as shown in Figure 8.Degradation process concentration versus time curve such as Fig. 9
Shown (provide bi simultaneously2wo6The photocatalysis result of nanometer sheet and blank experiment is to compare).After visible ray shines 30min, solution
In rhodamine b degradation rate reach 85.5%, total removal rate reaches 99.0%.Cyclical stability result such as Figure 10 institute of catalyst
Show.Still there is 96.0% total removal rate after 5th circulation, show that catalyst has good circulating effect.Obviously, ag nano junction
Between the component that the electronic effect of structure is brought, cooperative effect and plasma-induced heat effect significantly enhance visible ray photoelectricity and turn
Change efficiency and photocatalytic activity, stability.
Claims (10)
1. a kind of bi2wo6The preparation method of/ag hetero nano structure material it is characterised in that described preparation method include following
Step:
(1) prepare bi2wo6；
(2) under condition of ice bath, by the bi of preparation2wo6It is placed in the acetum containing silver nitrate, add aqueous ascorbic acid,
After reaction, it is centrifuged, washs, is dried, obtain bi2wo6/ ag hetero nano structure material.
2. preparation method according to claim 1 is it is characterised in that prepare bi in step (1)2wo6Method be: by bi
(no3)3·5h2O is dissolved in hno3Form solution a, by na in solution2wo4·2h2O is dissolved in the mixed solvent of ethanol and deionized water
Middle formation solution b；Mixed solution a and b, after stirring reaction 5-10min, adds 1,6- hexamethylene diamine, carries out reacting by heating, centrifugation is washed
Wash, be dried, obtain bi2wo6Powder.
3. it is characterised in that reacting by heating described in step (1), condition is preparation method according to claim 2: temperature
Spend for 160 DEG C, time 12h.
4. preparation method according to claim 2 is it is characterised in that bi (no3)3·5h2O is 1m in solution a concentration,
na2wo4·2h2Concentration in solution b for the o is 0.07m, bi (no3)3·5h2O and na2wo4·2h2The mol ratio of o is 2:1.
5. preparation method according to claim 2 is it is characterised in that solution a, solution b and 1,6- hexamethylene diamine in step (1)
Volume ratio be 1:7:1.
6. preparation method according to claim 1 and 2 is it is characterised in that step (2) is particularly as follows: under condition of ice bath, take
The bi that step (1) obtains2wo6Powder sample ultrasonic disperse, in deionized water, adds silver nitrate aqueous solution, adds acetic acid molten
Liquid, is eventually adding aqueous ascorbic acid, reacts, be collected by centrifugation under condition of ice bath, and deionized water and dehydrated alcohol are each respectively
Wash 3 times, be vacuum dried 6h at 60 DEG C, obtain bi2wo6/ ag powder sample.
7. preparation method according to claim 6 is it is characterised in that react concrete under condition of ice bath described in step (2)
For: react 15-25min under the conditions of 1-4 DEG C.
8. a kind of bi2wo6/ ag hetero nano structure material, is prepared using claim 1-7 any one methods described.
9. a kind of bi2wo6/ ag hetero nano structure material is applied as visible ray opto-electronic conversion.
10. a kind of bi2wo6/ ag hetero nano structure material is used for the application of visible light photocatalytic degradation.
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