CN106492845A - A kind of Ag loads the preparation method and applications of BiCuSeO wide spectrum photochemical catalysts - Google Patents
A kind of Ag loads the preparation method and applications of BiCuSeO wide spectrum photochemical catalysts Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 74
- 229910002903 BiCuSeO Inorganic materials 0.000 title claims abstract description 64
- 238000001228 spectrum Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 25
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 22
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 206010013786 Dry skin Diseases 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001073 sample cooling Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 description 17
- 230000015556 catabolic process Effects 0.000 description 16
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 15
- 230000003197 catalytic effect Effects 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000008859 change Effects 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- QAAXRTPGRLVPFH-UHFFFAOYSA-N [Bi].[Cu] Chemical compound [Bi].[Cu] QAAXRTPGRLVPFH-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- ZYDVNTYVDVZMKF-UHFFFAOYSA-N [Cl].[Ag] Chemical group [Cl].[Ag] ZYDVNTYVDVZMKF-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- -1 hydroxyl free radical Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000010010 raising Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- 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
- 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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of Ag loads BiCuSeO wide spectrum photochemical catalysts, preparation method is comprised the following steps：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix, vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C of roastings（700 DEG C of roasting 10h are warming up to after 5h, through grinding, ball milling after sample cooling；1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, stir 3h respectively under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain the BiCuSeO xAg composite catalysts of serial difference Ag load capacity.The preparation method and applications of the Ag load BiCuSeO wide spectrum photochemical catalysts of the present invention have that preparation method is simple, photocatalysis performance excellent characteristics.
Description
Technical field
The present invention relates to catalyst technical field, specially a kind of preparation of Ag loads BiCuSeO wide spectrum photochemical catalysts
Method and its application.
Background technology
Photocatalysis technology is increasingly received publicity in recent years, develop new, nontoxic, reusable, efficiently can inhale
The photochemical catalyst for receiving the photochemical catalyst sunshine of sunshine becomes the important topic of environment pollution control and sustainable development.But pass
The TiO of system2Photochemical catalyst forbidden band wider (Rutile Type 3.0eV, Anatase 3.2eV), can only be below absorbing wavelength 365nm
Ultraviolet light, only accounts for the 4～5% of sunshine, and the utilization to solar energy is substantially not enough.And TiO2Photo-generate electron-hole be combined
Probability is high, and photocatalytic oxidation efficiency is low, hinders which and further applies.Find and there is narrower energy gap, more can fill
Dividing becomes researcher's focus interested using the photochemical catalyst of sunshine.
In recent years, bismuth based semiconductor catalysis material is increasingly received significant attention.As the 6s electronics of Bi is in compound
Often become the part of energy band, be conducive to reducing band gap width, therefore most of bismuth based semiconductor material can absorb visible
Light, while its good delocalization also contributes to the activity for improving its photocatalysis degradation organic contaminant[4].Therefore more and more
Compound containing Bi be tried for as photochemical catalyst.For preferably utilizing sunshine, further widen semiconductor light and urge
Absorption region of the agent to light, researcher also begin to attempt by the use of near infrared light as light-catalysed light source.There are some researches show near
Infrared light can be absorbed by suitable inorganic material and trigger light-catalyzed reaction, and this is provided for the application of full spectrum light catalyst
May.
Content of the invention
It is an object of the invention to provide a kind of Ag loads the preparation method and applications of BiCuSeO wide spectrum photochemical catalysts,
Have that preparation method is simple, photocatalysis performance excellent characteristics.
The present invention can be achieved through the following technical solutions：
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.
Further, the silver nitrate solution is that concentration is 0.044χMol/L, wherein χ=0,0.1,0.2,0.5,1, institute
The addition for stating silver nitrate solution is 50ml.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst.
Further, the wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
A kind of Ag of the present invention loads the preparation method and applications of BiCuSeO wide spectrum photochemical catalysts, has with following
Beneficial effect：With the increase of Ag contents, BiCuSeO catalyst is lifted with the catalytic rate of near infrared light in visible ray, and deposition is described
Ag particles are effectively catalysis.Raisings of the photoelectric current description of test Ag to catalyst photoelectric properties simultaneously.The depositing of Ag is to sum up demonstrated
In the catalytic performance that can improve BiCuSeO catalyst in full spectral region.Photocatalysis and photoelectric current show, BiCuSeO energy
Excited by near infrared light, with degradation capability, it is seen that photodegradation rate reaches 41.5%, and near infrared light degradation rate reaches 47.1%.
Ability near infrared region catalytic degradation is had based on BiCuSeO, the composite catalyst of BiCuSeO have full spectrum (ultraviolet, can
See, near-infrared) absorbability.Therefore the material has good prospect.BiCuSeO/Ag (x) has good catalysis activity,
Photocatalysis result shows that BiCuSeO/Ag (0.1) shows highest degradation rate under the visible catalysis with near-infrared, in 180min
Degradation rate respectively reaches 78% and 76%.
Description of the drawings
Accompanying drawing 1 is the XRD spectrum that Ag of the present invention loads BiCuSeO wide spectrum photochemical catalysts；
Accompanying drawing 2 is BiCuSeO and BiCuSeO- under the near-infrared of Ag of the present invention load BiCuSeO wide spectrum photochemical catalysts
10Ag (embodiment 5) photocurrent response；
Accompanying drawing 3 is BiCuSeO and BiCuSeO- under the visible ray of Ag of the present invention load BiCuSeO wide spectrum photochemical catalysts
10Ag (embodiment 5) photocurrent response.
Specific embodiment
In order that those skilled in the art more fully understand technical scheme, with reference to embodiment and to this
Invention product is described in further detail.
Embodiment 1
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.In this step, the silver nitrate solution is that concentration is 0.044χMol/L, its
Middle χ=0, the addition of the silver nitrate solution is 50ml, and the load capacity for finally giving Ag in catalyst is 0%.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst；The wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
Embodiment 2
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.In this step, the silver nitrate solution is that concentration is 0.044χMol/L, its
Middle χ=0.1, the addition of the silver nitrate solution is 50ml, and the load capacity for finally giving Ag in catalyst is 1%.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst；The wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
Embodiment 3
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.In this step, the silver nitrate solution is that concentration is 0.044χMol/L, its
Middle χ=0.2, the addition of the silver nitrate solution is 50ml, and the load capacity for finally giving Ag in catalyst is 2%.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst；The wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
Embodiment 4
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.In this step, the silver nitrate solution is that concentration is 0.044 χ mol/L, its
Middle χ=0.5, the addition of the silver nitrate solution is 50ml, and the load capacity for finally giving Ag in catalyst is 5%.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst；The wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
Embodiment 5
The invention discloses a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix,
Vacuum ball milling 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C
Roasting (is warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling after 5h；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, point
3h is not stirred under visible light source irradiation, precipitation is washed with deionized water repeatedly, 75 DEG C of drying 12h obtain serial difference Ag
The BiCuSeO-xAg composite catalysts of load capacity.In this step, the silver nitrate solution is that concentration is 0.044 χ mol/L, its
Middle χ=1, the addition of the silver nitrate solution is 50ml, and the load capacity for finally giving Ag in catalyst is 10%.
Ag loads the application of BiCuSeO wide spectrum photochemical catalysts, and the catalyst is under visible ray and near infrared light
Use as photochemical catalyst；The wave-length coverage of the visible ray be 420nm≤λ≤780nm, the wave-length coverage of the near infrared light
For 800nm≤λ≤1100nm.
The performance of BiCuSeO wide spectrum photochemical catalysts is loaded to effectively assess Ag of the present invention, respectively to embodiment
1-5 carries out the test of XRD structural characterizations, catalytic performance test and photoelectric properties.
1st, XRD structural characterizations
The XRD of the BiCuSeO of different silver load capacities is as shown in Figure 1.As a result show, the diffraction maximum of all samples with
BiCuSeO standards JCPDS (PDF#45-0296) card is identical, and only a small amount of Bi2O3 is present, and shows with vacuum sealing tube heat
The method of reason has obtained purer BiCuSeO powder.Although the load capacity of experimental design Ag be 1%～10%, XRD results simultaneously
The diffraction maximum of Ag is not found, shows that Ag is not present in sample with simple substance form in a large number.
2nd, catalytic performance test
Method of testing：The Congo red solution 80mL of 100mg/L are taken, 0.2g catalyst samples, ultrasonic disperse under dark is added
After 10min, 30min is stirred in dark surrounds, be that dyestuff reaches adsorption equilibrium with catalyst.Sample is placed in visible ray or infrared
Under radiant, in low temperature environment, stirring carries out degradation reaction.A sample is taken every 30min, 3000r/s is centrifuged, and uses UV, visible light
Light spectrophotometric determination clarified solution at λ max=495nm (Congo red maximum absorption wavelength) absorbance (At), pass throughTo calculate relatively Congo red change in concentration.
Test result：Found with the change in concentration of the Congo red solution of spectrophotometry, under visible light illumination bismuth copper
, to Congo red with obvious degradation effect, concrete outcome is as shown in table 1 for selenolite：As can be seen from Table 1,3 hours visible rays shine
After penetrating, Congo red concentration is reduced to original 59.5%.Its degradation rate is calculated with the time with the characteristic absorption at Congo red 495nm
Change, it can be found that with the increase of Ag load capacity, bismuth copper selenolite has strengthened to Congo red catalytic degradation effect, theoretical negative
Carrying capacity makes Congo red concentration be reduced to original 22.7% for 3 hours for the BiCuSeO of 10%Ag under visible light illumination.Experiment is not only
Demonstrating BiCuSeO powder can be used as visible-light photocatalyst, and it was found that its catalytic performance can pass through carried noble metal
Further get a promotion.
Under 1 radiation of visible light of table, difference Ag load capacity BiCuSeO is to Congo red degradation effect
| Degradation rate | BiCuSeO | BiCuSeO-1Ag | BiCuSeO-2Ag | BiCuSeO-5Ag | BiCuSeO-10Ag |
| 0min | 1 | 1 | 1 | 1 | 1 |
| 30min | 0.887 | 0.860 | 0.840 | 0.793 | 0.754 |
| 60min | 0.789 | 0.752 | 0.712 | 0.654 | 0.639 |
| 90min | 0.739 | 0.662 | 0.674 | 0.547 | 0.521 |
| 120min | 0.665 | 0.629 | 0.541 | 0.510 | 0.352 |
| 150min | 0.621 | 0.603 | 0.476 | 0.461 | 0.282 |
| 180min | 0.595 | 0.574 | 0.430 | 0.346 | 0.227 |
By near infrared light, according under, (800nm≤λ≤1100nm) carries out catalytic degradation, concrete outcome such as table to Congo red
Shown in 2, there is obvious degradation effect as can be found from Table 2, Congo red concentration is reduced to originally after near infrared light is lower 3 hours
52,9%.Compare pure bismuth copper selenolite and the 2%, catalytic effect of 10%Ag theoretical negative carrying capacity simultaneously, find load silver near
Infrared can equally improve catalytic capability, under near infrared light, BiCuSeO-10Ag can make Congo red concentration in 3 hours
It is reduced to original 24.7%.The Congo red experiment of radiation of visible light and near infrared light catalytic degradation is it is also shown that the load of Ag
Amount has significantly impact for catalysis activity.The bismuth copper selenolite of load 10%Ag has best catalytic effect.
Under 2 near infrared light of subordinate list, difference Ag load capacity BiCuSeO is to Congo red degradation effect
| Degradation rate | BiCuSeO | BiCuSeO-2Ag | BiCuSeO-10Ag |
| 0min | 1 | 1 | 1 |
| 30min | 0.85863 | 0.879045997 | 0.637518142 |
| 60min | 0.72327 | 0.724020443 | 0.431059507 |
| 90min | 0.61194 | 0.604770017 | 0.337445573 |
| 120min | 0.58186 | 0.507666099 | 0.253991292 |
| 150min | 0.5519 | 0.494037479 | 0.250362845 |
| 180min | 0.52941 | 0.490630324 | 0.246734398 |
Catalytic mechanism：BiCuSeO just has stronger light absorbs under near infrared light, and under the conditions of irradiation, photon energy is big
Electronics in semiconductor absorber threshold value, BiCuSeO valence band is excited by light quantum, and valence-band electrons band-to-band transition is moved to
On the conduction band of BiCuSeO, while blank valence band hole is formed,.But due to BiCuSeO catalyst structural factor itself, catalysis
Even if there is electronics remover (e with hole in the electronics of agent surface capture-), recombination probability is still higher.But when with the addition of Ag, can catch
Electronics is obtained, is conducive to electron-hole to separate, electronics forms superoxide anion, the hole with oxidisability on surface with dissolved oxygen
Then stay in valence band, by absorption surface hydroxyl and aquation be hydroxyl free radical.
3rd, photoelectric properties test
Method of testing：BiCuSeO is dispersed in ethylene glycol, blade coating to FTO electro-conductive glass is simultaneously dried at 250 DEG C, electricity consumption
Chemical work stands in test light current-responsive in three-electrode system, and (working electrode is FTO-BiCuSeO, and reference electrode is silver-chlorine
Change silver electrode, be that 0.5M sodium sulphate is electrolyte to electrode with platinum electrode).
Test result：Photoelectric properties test can reflect semi-conducting material for absorption and the conversion capability of light, often by
It is considered as the embodiment of catalysis material performance.Using standard three electrode system in 0.5MNa2SO4 solution to BiCuSeO and
The photocurrent response of BiCuSeO-10Ag working electrodes compares test.As shown in figure (Fig. 2 and Fig. 3), pure BiCuSeO
Good response is all shown in visible ray and near infrared light, and shows the photoelectric respone feature of p-type semiconductor.And loaded Ag
BiCuSeO photoelectric properties further enhanced, in visible ray and near infrared light according under the conditions of photoelectric current be all higher than pure
The photoelectric current of BiCuSeO working electrodes.This is consistent with the result of photocatalytic degradation.Illustrate light deposition Ag loaded favourables in entering
One step improves activity of the BiCuSeO in whole spectral region.
The above, only presently preferred embodiments of the present invention not makees any pro forma restriction to the present invention；All
The those of ordinary skill of the industry can shown in by specification and the above and swimmingly implement the present invention；But, all familiar
Professional and technical personnel is made using disclosed above technology contents in the range of without departing from technical solution of the present invention
A little change, modification with develop equivalent variations, be the present invention Equivalent embodiments；Meanwhile, all realities according to the present invention
The change of any equivalent variations that matter technology is made to above example, modification and differentiation etc., still fall within the technology of the present invention
Within the protection domain of scheme.
Claims (4)
1. a kind of Ag loads the preparation method of BiCuSeO wide spectrum photochemical catalysts, it is characterised in that comprise the following steps：
The first step, high temperature process heat BiSeCuO powder：Press Bi2O3：Bi：Cu:Se=1:1:3:3 molar ratios mix, vacuum sphere
Mill 8h post-dryings；The piece that raw material powder is pressed into diameter 20mm, and by its Vacuum Package in quartz glass tube, 350 DEG C of roastings（5h
After be warming up to 700 DEG C of roasting 10h, through grinding, ball milling after sample cooling；
Second step, the synthesis of BiCuSeO/Ag catalyst：1.5gBiCuSeO powder is weighed, silver nitrate solution is added dropwise respectively, is existed respectively
The lower stirring 3h of visible light source irradiation, precipitation are washed with deionized water repeatedly, and 75 DEG C of drying 12h obtain serial difference Ag loads
The BiCuSeO-xAg composite catalysts of amount.
2. Ag according to claim 1 loads BiCuSeO wide spectrum photochemical catalyst preparation methods, it is characterised in that：Described
It is 0.044 that silver nitrate solution is concentrationMol/L, wherein=0,0.1,0.2,0.5,1, the addition of the silver nitrate solution
For 50ml.
3. the Ag described in a kind of claim 1 loads the application of BiCuSeO wide spectrum photochemical catalysts, it is characterised in that：Described urge
Agent is used as photochemical catalyst under visible ray and near infrared light.
4. Ag according to claim 3 loads the application of BiCuSeO wide spectrum photochemical catalysts, it is characterised in that：Described can
The wave-length coverage for seeing light is 420nm≤λ≤780nm, and the wave-length coverage of the near infrared light is 800nm≤λ≤1100nm.
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