CN106390992A - Preparation method and photocatalytic performance of Bi2WO6-x micro-nano material - Google Patents
Preparation method and photocatalytic performance of Bi2WO6-x micro-nano material Download PDFInfo
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- CN106390992A CN106390992A CN201610980022.8A CN201610980022A CN106390992A CN 106390992 A CN106390992 A CN 106390992A CN 201610980022 A CN201610980022 A CN 201610980022A CN 106390992 A CN106390992 A CN 106390992A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 124
- 238000005530 etching Methods 0.000 claims abstract description 68
- 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 claims abstract description 16
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 229910001868 water Inorganic materials 0.000 claims description 16
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 230000003628 erosive effect Effects 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 2
- 238000002474 experimental method Methods 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 17
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 7
- 238000001782 photodegradation Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 2
- 239000010937 tungsten Substances 0.000 abstract description 2
- 230000000873 masking effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 82
- 230000000694 effects Effects 0.000 description 21
- 230000007547 defect Effects 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 16
- 229910052760 oxygen Inorganic materials 0.000 description 16
- 239000001301 oxygen Substances 0.000 description 16
- 238000007146 photocatalysis Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 10
- 238000012216 screening Methods 0.000 description 9
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 230000008859 change Effects 0.000 description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 241000894007 species Species 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229940005561 1,4-benzoquinone Drugs 0.000 description 4
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000003321 amplification Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- -1 metals cation Chemical class 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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- 238000009396 hybridization Methods 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a preparation method of a Bi2WO6-x micro-nano material. A Bi2WO6 micro-nano material which is synthesized by a hydrothermal method under optimal conditions is used as a substrate, then NaOH is added for etching, after the concentration and the etching temperature of NaOH are optimized, and the degradation rate of prepared Bi2WO6-x to 10 mg/L of a solution of rhodamine B under visible light (a 200W tungsten lamp) reaches 98.84%, and Bi2WO6-x has good photocatalytic activity to the solution of the rhodamine B; and meanwhile, through discussion of a masking agent experiment, photogenerated holes are discovered to be main active species in the photodegradation process.
Description
Technical field
The present invention relates to the preparation method technical field of metal-oxide, more particularly, to a kind of Bi2WO6-xMicro Nano material
Preparation method and its photocatalysis performance.
Background technology
Since 20th century, environmental pollution increasingly increases, energy shortage become human survival have to faced by significant challenge,
Develop, obtained using solar energy solution global energy and environmental problem the attention of more and more national.Wherein, using solar energy
The Photocatalitic Technique of Semiconductor of degradable organic pollutant shows greater advantage, is increasingly becoming perpetual object.
Bi2WO6It is simplest Aurivillius type oxide, belongs to orthorhombic system, crystal structure is (Bi2O2)2+Layer
And WO6 6-The layer structure that layer is arranged alternately with each other.Bi2WO6It is typical N-shaped bandgap semiconductor material, energy gap is about
For 2.7eV.Its band structure is made up of the W5d track of conduction band and Bi6s, O2p orbital hybridization of valence band.Bi2WO6Dielectric, urge
The characteristics such as change are applied to a lot of aspects.Because of Bi2WO6Energy gap little and have absorption in visible region, many of degrading has
Organic pollutants, thus become study hotspot.
Study according to current, in photocatalyst, the low separation efficiency in photogenerated charge and hole pair is to lead to photocatalyst
One of not high essential reason of activity.For improving the migration rate of the separation efficiency that photogenerated charge is with hole and promotion electric charge,
Generally deposited by doping metals cation, noble metal surface and contain the technological means such as the surface hydridization of conjugatedπbond molecule Lai real
Existing, thus improving the activity of photocatalyst.It is worth noting that, there is researcher to propose, defect sturcture being capable of extreme influence photoproduction
The generation in electric charge and hole pair, separation, migration and light absorption process.Due to pure Bi2WO6The photo-generate electron-hole of material is to the life-span
Shorter, thus have impact on Bi2WO6Photocatalytic activity.In order to adapt to growing needs, to Bi2WO6Modification becomes inevitable.
Bi2WO6-xThe i.e. Bi of oxygen defect type2WO6, its preparation focuses primarily upon the introducing to Lacking oxygen, and introducing method can
By etching, vacuum deaeration, three kinds of modes of hydro-reduction.So-called Lacking oxygen is exactly from Bi by oxygen2WO6Lattice in deviate from, thus
Form defect sturcture.And Lacking oxygen both can serve as electronq donor it is also possible to improve the electron density of semiconductor light-catalyst.
Increased electronic energy can form donor level in turn, reduces energy gap, extends the absorption region to light, thus improving light
Catalysis activity.
Content of the invention
The present invention is with Bi (NO3)3·5H2O、Na2WO4·2H2O and NaOH is raw material, first uses hydro-thermal method in optimal conditions
Under synthesize Bi2WO6Micro Nano material, then be prepared into Bi through NaOH solution etching processing2WO6-x.The present invention has also inquired into not
With the consumption of NaOH, different etching time and etching temperature to preparation Bi2WO6-xImpact.Meanwhile, X-ray has been carried out to sample
Diffraction (XRD), Energy disperaive quantitative analysis (EDS), UV-Vis DRS spectrum (UV-Vis DRS), x-ray photoelectron power spectrum
(XPS), scanning electron microscope (SEM), the relevant characterization of fluorescence spectrum (PL) are to analyze Bi2WO6-xThing phase, pattern, and with
Rhodamine B is target degradation product, thus investigating Bi2WO6-xPhotocatalysis performance.
A kind of Bi2WO6-xThe preparation method of micro Nano material, comprises the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add Bi (NO3)3·5H2O, distilled water and concentrated nitric acid, in magnetic force
On agitator, agitating solution is to being completely dissolved；Simultaneously by Na2WO4·2H2O and distilled water stir to being completely dissolved in beaker B；
By Na2WO4Solution dropwise enter in A beaker by Deca, time-consuming 20-30min；After completion of dropping, use HNO3Adjust forerunner with NaOH solution
Liquid pH value is 0.9-1.1, is stirred for 12-18min；Above-mentioned solution is transferred in hydrothermal reaction kettle, meets compactedness≤75%,
It is placed in baking oven, 120 DEG C of reaction 18-24h of constant temperature；After the completion of reaction, sample centrifugation repeatedly washes with water respectively, that alcohol is washed is heavy
Form sediment, then 70 DEG C of constant temperature is dried 18-21h, grinding can obtain Bi2WO6；
Step 2, etching reaction：Take highly basic to be dissolved in deionized water, add Bi2WO6, regulation magnetic stirring apparatuss to 20-90
DEG C, etch 0.5-6 hour；After completion of the reaction, by sample centrifugation, repeatedly being washed to solution with 60-70 DEG C of hot water is in neutrality；
Again solid is placed in baking oven, 70 DEG C of constant temperature is dried 5-8h, that is, obtain product Bi2WO6-x.
Below by way of specific experiment, the condition of etching reaction is carried out preferably, specific experimental technique is：To control
Unitary variant is principle, by substantial amounts of experiment, is provided with different alkali, the NaOH of variable concentrations, etch period, etching temperature
The variable of four big groups, is prepared for altogether 23 samples.
Table 1 etching method prepares Bi2WO6-xExperiment condition one
By Experimental comparison, using control variate method, under same etch period, etching temperature, only change etching institute
Bases is prepared for Bi2WO6-xSample.Tested by photocatalytic degradation, filtered out the alkali species being suitable for.
Fig. 1 is Bi after NaOH and KOH etching processing under the same terms2WO6-xThe SEM of sample schemes, and amplification is
10000 times.Wherein, the Bi that a crosses for NaOH etching processing2WO6-xSample, the Bi that b crosses for KOH etching processing2WO6-xSample.From figure
In as can be seen that a still keep spherical laminated structure；And b spherical structure slightly destroys, in flocculent structure, agglomeration is serious, from
And lead to its photocatalytic activity to reduce.
Table 2 etching method prepares Bi2WO6-xExperiment condition two
By Experimental comparison, using control variate method, under different NaOH concentration, it is prepared for Bi2WO6-xSample.Finally lead to
Cross photocatalytic degradation experiment, filter out the NaOH concentration being suitable for.
Fig. 2 is under the same terms, the Bi of preparation under different NaOH concentration2WO6-xThe SEM of sample schemes, and amplification is
10000 times.Wherein, a adds 0.2gNaOH concentration is 0.1mol/L, and it is 0.2mol/L that b adds 0.4gNaOH concentration.Can from figure
To find out, a still keeps spherical laminated structure；In b, spherical structure is destroyed, and laminated structure projects, and also agglomeration, leads to
Photocatalytic activity reduces.
Table 3 etching method prepares Bi2WO6-xExperiment condition three
By Experimental comparison, using control variate method, under suitable NaOH concentration, by changing etch period preparation
Bi2WO6-xSample.Finally by photocatalytic degradation experiment, filter out suitable etch period.
Fig. 3 is the Bi of preparation under the different etching time2WO6-xThe SEM figure of sample, amplification is 10000 times, wherein：
(a)0h(b)1h(c)2h(d)3h.Etching 0h is pure Bi2WO6, process without NaOH solution, be shaped as spherical laminated structure.With
The prolongation of etch period, a, b, c, d sample remains in that spherical structure, shows in etching process, Bi2WO6Sample is in NaOH
There is certain inertia, etching occurs between laminated structure in solution.
Table 4 etching method prepares Bi2WO6-xExperiment condition four
By Experimental comparison, using control variate method, under suitable NaOH concentration, etch period, change etching temperature
It is prepared for Bi2WO6-xSample.Finally by photocatalytic degradation experiment, filter out suitable etching temperature.
Fig. 4 is in the case that other conditions are constant, changes the Bi of etching temperature preparation2WO6-xSample SEM spectrogram, amplifies
Multiple is 10000 times.As seen from the figure, when etching temperature is 25 DEG C, most of sample is in spherical laminated structure.Work as etching temperature
When gradually rising, laminated structure starts to highlight, but when temperature is increased to 80 DEG C, Bi2WO6-xSample has agglomeration, occurs
It may be possible to temperature is too high, degree of crystallinity is too high to be led to for conglomeration.
Fig. 5 is under control variable, changes the Bi that etching temperature prepares2WO6-xThe XRD spectra of sample.By this sample
Figure is understood with standard card (PDF#39-0256) relative analyses, find sample the angle of diffraction 2 θ be 28.299 °, 32.790 °,
Obvious diffraction maximum can be seen, they are belonging respectively to Bi at 47.138 ° and 55.820 °2WO6(131) in oblique crystallographic system,
(200), all miscellaneous peak in (202), the diffraction maximum of (331) each crystal face, and this shows that sample is pure phase Bi2WO6.By to difference
At a temperature of Bi after etching processing2WO6-xSample, each peak shape is no clearly distinguished from thus it is speculated that being located at because of oxygen defect structure
Bi2WO6Caused by surface, and the oxygen defect structure that surface occurs can strengthen photocatalysis performance.
Preferably, in described etching reaction, highly basic is sodium hydroxide.
Preferably, NaOH and Bi in described etching reaction2WO6Mass ratio be 1:1.
Preferably, in described etching reaction, etch period is 3 hours.
Preferably, in described etching reaction, etching temperature is 60 DEG C.
The Bi that the present invention provides2WO6-xThe preparation method of micro Nano material, is first synthesized under optimum conditions with hydro-thermal method
Obtain Bi2WO6Micro Nano material be substrate, add NaOH and perform etching, the concentration and etching temperature of NaOH is optimized
Afterwards, the Bi of preparation2WO6-xUnder visible ray (200W tungsten lamp), the rhodamine B solution degradation rate of 10mg/L is reached with 98.84%, right
Rhodamine B solution has preferable photocatalytic activity；Meanwhile, the discussion tested by screening agent, finds that photohole is this light fall
The chief active species of solution preocess.
Brief description：
Fig. 1：The Bi that alkaline etching is processed2WO6-xThe SEM figure of sample, (a) NaOH (b) KOH.
Fig. 2：The Bi of different NaOH concentration etchings2WO6-xThe SEM figure of sample, (a) 0.1mol/L, (b) 0.2mol/L.
Fig. 3：The Bi of different etching time preparation2WO6-xThe SEM figure of sample, (a) 0h (b) 1h (c) 2h (d) 3h.
Fig. 4：The Bi of different etching temperature preparation2WO6-xThe SEM figure of sample, 40 DEG C of 60 DEG C of 80 DEG C of (a) (b) (c) (d) 25
℃.
Fig. 5：Bi at a temperature of different etching2WO6-xThe XRD spectra of sample.
Fig. 6：Pure phase Bi2WO6And Bi2WO6-xThe XRD spectra of sample.
Fig. 7：Bi2WO6And Bi2WO6-xThe UV-Vis DRS spectrogram of sample.
Fig. 8：Bi2WO6-xThe XPS spectrum figure of sample.
Fig. 9：Pure phase Bi2WO6With Bi2WO6-xThe PL spectrogram of sample.
Figure 10：The Bi that alkaline etching is processed2WO6-xThe photocatalytic activity figure of sample.
Figure 11:The Bi of different NaOH concentration etchings2WO6-xThe photocatalytic activity figure of sample.
Figure 12：The Bi of different etching time preparation2WO6-xThe photocatalytic activity figure of sample.
Figure 13：The Bi of different etching temperature preparation2WO6-xThe photocatalytic activity figure of sample.
Figure 14：Bi2WO6-xUv-visible absorption spectrum figure for RhB during catalyst.
Figure 15：The impact figure of the photocatalytic activity to sample for the different screening agents.
Specific embodiment
Embodiment 1：
A kind of Bi2WO6-xThe preparation method of micro Nano material, comprises the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add 1.2118g Bi (NO3)3·5H2O, 1mL distilled water and
0.5mL concentrated nitric acid, on magnetic stirring apparatuss, agitating solution is to being completely dissolved；Simultaneously by 0.4123g Na2WO4·2H2O and 30mL
Distilled water stirs to being completely dissolved in beaker B；By Na2WO4Solution dropwise enter in A beaker by Deca, and time for adding is 25min；Drip
Add after finishing, use HNO3Adjusting precursor liquid pH value with NaOH solution is 1, is stirred for 15min；Above-mentioned solution is transferred into hydro-thermal anti-
Answer in kettle, meet compactedness≤75%, be placed in baking oven, 120 DEG C of reaction 20h of constant temperature；After the completion of reaction, by sample centrifugation,
Repeatedly wash with water respectively, precipitation washed by alcohol, then 70 DEG C of constant temperature is dried 20h, grinding can obtain Bi2WO6；
Step 2, etching reaction：Take 0.2gNaOH to be dissolved in 50mL deionized water, add 0.2g Bi2WO6, adjust magnetic force
Agitator, to 60 DEG C, etches 3h；After completion of the reaction, by sample centrifugation, in repeatedly being washed with 60-70 DEG C of hot water and to solution being in
Property；Again solid is placed in baking oven, 70 DEG C of constant temperature is dried 6h, that is, obtain product Bi2WO6-x.
Embodiment 2：
A kind of Bi2WO6-xThe preparation method of micro Nano material, comprises the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add 1.2118g Bi (NO3)3·5H2O, 1mL distilled water and
0.5mL concentrated nitric acid, on magnetic stirring apparatuss, agitating solution is to being completely dissolved；Simultaneously by 0.4123g Na2WO4·2H2O and 30mL
Distilled water stirs to being completely dissolved in beaker B；By Na2WO4Solution dropwise enter in A beaker by Deca, and time for adding is 22min；Drip
Add after finishing, use HNO3Adjusting precursor liquid pH value with NaOH solution is 1, is stirred for 17min；Above-mentioned solution is transferred into hydro-thermal anti-
Answer in kettle, meet compactedness≤75%, be placed in baking oven, 120 DEG C of reaction 21h of constant temperature；After the completion of reaction, by sample centrifugation,
Repeatedly wash with water respectively, precipitation washed by alcohol, then 70 DEG C of constant temperature is dried 18h, grinding can obtain Bi2WO6；
Step 2, etching reaction：Take 0.2gNaOH to be dissolved in 50mL deionized water, add 0.1g Bi2WO6, adjust magnetic force
Agitator, to 50 DEG C, etches 4h；After completion of the reaction, by sample centrifugation, in repeatedly being washed with 60-70 DEG C of hot water and to solution being in
Property；Again solid is placed in baking oven, 70 DEG C of constant temperature is dried 5h, that is, obtain product Bi2WO6-x.
Embodiment 3：
A kind of Bi2WO6-xThe preparation method of micro Nano material, comprises the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add 1.2118g Bi (NO3)3·5H2O, 1mL distilled water and
0.5mL concentrated nitric acid, on magnetic stirring apparatuss, agitating solution is to being completely dissolved；Simultaneously by 0.4123g Na2WO4·2H2O and 30mL
Distilled water stirs to being completely dissolved in beaker B；By Na2WO4Solution dropwise enter in A beaker by Deca, and time for adding is 25min；Drip
Add after finishing, use HNO3Adjusting precursor liquid pH value with NaOH solution is 1, is stirred for 15min；Above-mentioned solution is transferred into hydro-thermal anti-
Answer in kettle, meet compactedness≤75%, be placed in baking oven, 120 DEG C of reaction 20h of constant temperature；After the completion of reaction, by sample centrifugation,
Repeatedly wash with water respectively, precipitation washed by alcohol, then 70 DEG C of constant temperature is dried 20h, grinding can obtain Bi2WO6；
Step 2, etching reaction：Take 0.2gNaOH to be dissolved in 50mL deionized water, add 0.2g Bi2WO6, adjust magnetic force
Agitator, to 40 DEG C, etches 3h；After completion of the reaction, by sample centrifugation, in repeatedly being washed with 60-70 DEG C of hot water and to solution being in
Property；Again solid is placed in baking oven, 70 DEG C of constant temperature is dried 6h, that is, obtain product Bi2WO6-x.
Hereinafter the sample of embodiment 1 is carried out multinomial detecting and making a concrete analysis of.
Test one：X-ray diffraction (XRD)
This experiment employs Dutch PANalytical Panalytical company XPert Powder type X-ray powder diffraction instrument
Levy the phase structure of sample.Cu target K α radiation as incident light source, X-ray wavelength λ K α=1.5406, the condition of scanning is：Step-length
0.026,5 ° -75 ° of scanning angle, often walk time of staying 20.4s, material phase analysis are carried out to sample.
Fig. 6 is pure phase Bi2WO6And Bi2WO6-xThe XRD spectra of sample.It can be seen that both diffraction peak width and peak
Height does not almost have difference, and peak shape all compares sharply, diffraction peak intensity.With respect to pure phase Bi2WO6, Bi2WO6-xXRD spectra there is no phase
State change and impurity structural generation, therefore speculate, through over etching, the formation of a number of Lacking oxygen occurs in Bi2WO6Surface.
Test two：Scanning electron microscope (SEM)
This experiment adopts the S-3400N scanning electron microscope (SEM) of HIT to observe pattern and the chi of sample
Very little, accelerating potential is 20-30KV.Specific spectrogram is referring to Fig. 1-Fig. 4.
Test three：UV-Vis DRS spectrum (DRS)
UV-Vis DRS spectrum is carried out on Shimadzu UV-2450 type spectrophotometer, and test wavelength is 200-
800nm, with high-purity BaSO4For standard reagent.The light abstraction width of analysis of catalyst and optical absorption intensity are determining catalyst
Light absorbs sideband and energy gap etc..
Fig. 7 is the pure Bi synthesizing at optimum conditions2WO6And Bi2WO6-xThe UV-Vis DRS spectrum of sample.By scheming
As can be seen that Bi2WO6-xThe obvious red shift of spectral line of sample.(λ g is to absorb pole to calculate energy gap Eg=1240/ λ g according to formula
Limit, is estimated by the tangent line of ABSORPTION EDGE and the intersection point of transverse axis), such as Fig. 7 obtains Bi2WO6And Bi2WO6-xEnergy gap respectively
2.81eV, 2.69eV, Bi2WO6-xEnergy gap less, show that sample increases to the absorption region of visible ray after etching processing,
Utilization rate also increases.This is likely due to the Bi after NaOH solution is processed2WO6Sample defines more oxygen defect structure, increases
The strong capture ability to electronics, thus improve the utilization rate to visible ray.
Test four：X-ray photoelectron power spectrum (XPS)
The XPS analysis of this experiment are to carry out on Thermo escalab 250Xi photoelectron spectrograph.All of XPS surveys
Examination is all with the C1s peak 284.6eV of surface adsorption carbon compound as reference.
Fig. 8 is Bi2WO6-xThe XPS analysis spectrogram of sample.
In order to further appreciate that Bi2WO6-xEach element valence state information in sample, is analyzed to sample by XPS.From
It can be seen that containing tetra- kinds of elements of Bi, W, O, C in sample in Fig. 8 a, wherein C element is derived from external carbon source.Figure b, c, d give respectively
Go out the region high-resolution XPS spectrum figure of Bi4f, W4f, O1s.Peak at electron binding energy 159.2eV and 164.5eV in figure b is respectively
Corresponding to Bi4f7/2And Bi4f5/2, illustrate that Bi element is with+trivalent state presence.Figure c in electron binding energy be 35.0eV and
Peak at 37.2eV corresponds to W4f respectively7/2And W4f5/2, illustrate that W element is that exist with+6 valence states.In figure d, O1s electronics combines
Hydroxyl oxygen and absorption oxygen can be corresponded respectively to for the peak at 531.9eV and 530.2eV.After etching processing forms Lacking oxygen,
Bi2WO6-xIn sample, the valence state of each element does not change, but Bi2WO6-xThe peak of the Bi4f of sample, W4f and O1s there occurs a little shifting
Dynamic, this can be owing to Bi3+And W6+Fermi level and the change of electron density.
Test five：Fluorescence spectrum (PL)
This experiment scans, using Japanese SHIMADZU company RF-5301PC spectrofluorophotometer, the fluorescence that sample is sent
Spectrum.
Fig. 9 is pure Bi2WO6With Bi2WO6-xThe PL spectrogram of sample.
Photoluminescence spectra can probe into carrier in conductor photocatalysis material effectively, and (light induced electron and photoproduction are empty
Cave) separation efficiency.PL peak intensity means greatly the recombination probability height of light induced electron and photohole, and peak intensity is little, can say
The recombination probability of bright light induced electron and photohole is low, and then the separation efficiency height of light induced electron and photohole can be described, from
And have preferable photocatalytic activity.Under excitation wavelength is for 332nm, pure Bi2WO6And Bi2WO6-xThe PL spectrum of sample is shown in Fig. 9, by
Figure can be seen that Bi2WO6Peak intensity be higher than Bi2WO6-x, because peak intensity is higher, light induced electron is higher with hole combination rate,
And catalytic efficiency is lower, thus provable Bi2WO6-xCatalysis activity be higher than Bi2WO6's.
Below to Bi2WO6-xThe photocatalysis performance of sample is detected
The impact of Different Alkali
Figure 10 is constant in other conditions, etches the photocatalytic activity figure of sample using KOH or NaOH.When being carved using KOH
When erosion processes sample, its photocatalytic degradation efficiency 80.00%；And the degradation efficiency of NaOH etching processing sample is 86.04%.Two
Person compares, stronger than NaOH because of KOH alkalescence, causes that Surface Oxygen defects count is less and body phase defect is more, hole and electricity
Sub- recombination rate is high, thus leading to activity weaker.
The impact of different NaOH consumptions
Figure 11 is the Bi preparing under adding different amounts of NaOH2WO6-xThe photocatalytic activity figure of sample.Wherein, 1
Number do not add NaOH, No. 2 addition 0.2g NaOH, No. 3 addition 0.4g NaOH.In the case of other condition identicals, survey respectively
The catalysis activity of each sample fixed.Wherein, No. 1 sample activity is 70%, and No. 2 sample activity reach 86.01%, and No. 3 samples are lived
Property be 81.81%.Therefore, the addition of NaOH is set to 0.2g.
The impact of different etching time
Figure 12 is in the case of other conditions identical only change etch period, the Bi preparing2WO6-xThe light of sample
Catalysis activity figure.It can be seen that the sample pair under different etching time 0h, 0.5h, 1h, 2h, 3h, 4h, 5h, 6h process
The degradation rate of rhodamine B is respectively 70%, 72%, 78%, 93%, 99%, 92%, 92%, 90%.Therefrom it is recognised that dropping
Solution rate is in the trend fallen after rising substantially, and with the increase of etch period, oxygen defect quantity increases, and great majority lack for surface
Fall into, have facilitation to photocatalysis, activity increases to maximum always.When etch period is for 3h, degradation rate highest, to Luo Dan
Bright B photocatalysis effect is best.After etch period extends further, oxygen defect goes to body phase by surface, leads to photohole
Reduce with the capture ability of electric charge, suppression hole is separated with electric charge, reduces photocatalysis performance, activity starts to weaken.
The impact of different etching temperature
Figure 13 is constant in other conditions, only changes the photocatalytic activity figure of sample after etching temperature.Can from figure
Go out, after illumination 3h, 40 DEG C of different temperatures, the sample of 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C process are to rhodamine B degradation rate
It is respectively：76.76%th, 77.52%, 98.84%, 83.24%, 63.05%, 53.79%.Generally speaking, raise Temperature Treatment
Properties of sample afterwards is changed, and in first raising the trend reducing afterwards, when 60 DEG C, performance reaches maximum.Speculate that reason can
Can be when temperature is low, oxygen defect concentration is low, and is mostly surface defect, raise and defect sturcture increase with temperature；When
After temperature rises to a certain extent, defects count reaches maximum, and activity is also maximum；After temperature is further up, defect sturcture
Transfer to body phase from surface, and the reduced capability in body phase defect capture photogenerated charge and hole, thus suppressing photocatalytic activity.
Bi2WO6-xThe photolytic activity analysis of sample
It is prepared that degradation process using rhodamine B to evaluate (0.2gNaOH etches 3h, 25 DEG C of etching temperature)
Bi2WO6-xThe visible light photocatalysis active of sample.Figure 14 is the photocatalytic degradation curve of rhodamine B.As seen from the figure, in rhodamine
At B maximum absorption wavelength 554nm, with the lengthening of light application time, absorbance declines always it was demonstrated that Bi2WO6-xSample is to Luo Dan
Bright B has Degradation.Rhodamine B solution colour gradually becomes shallower as, and illustrates that rhodamine B molecular structure is destroyed degraded and generates other thing
Matter.
Bi2WO6-xThe active specy of catalytic degradation rhodamine B solution shelters experiment
For further appreciating that the chief active species of light-catalyzed reaction, to Bi after adding different screening agents2WO6-xCarry out
Photocatalysis experiments.Experiment employs following screening agent：AgNO3(e-Screening agent), 1,4-benzoquinone (O2 -Screening agent), the tert-butyl alcohol (
OH screening agent), EDTA-2Na (h+Screening agent).
Figure 15 is the Bi to optimum condition preparation2WO6-xIt is separately added into the active specy that different screening agents carry out in sample to cover
Cover experiment.Wherein, 1 is 0.01mol/L AgNO3, 2 is 0.001mol/L 1,4-benzoquinone, and 3 is the 0.01mol/L tert-butyl alcohol, and 4 are
0.01mol/L EDTA-2Na.After illumination 3h, 1,2,3,4 last degradation rate is 66.21%, 53.67%, 86.22%,
32.49%.To analyze from result, the t-BuOH of addition is little to the Photo-degradation of rhodamine, this explanation hydroxyl radical free radical is not
It is the chief active species of reaction.AgNO3Reaction is had a certain impact, but EDTA-2Na and 1,4-benzoquinone all significantly inhibit
Bi2WO6-xPhotocatalytic activity, wherein add 1,4-benzoquinone system activity than add EDTA-2Na system activity good.Thus
It can be seen that, photohole h+It is chief active species, O2 -It is secondary active specy.Infer that correlated response equation may be as follows：
Bi2WO6-x+hv→e-+h+(1)
Major:h++H2O→·OH+H+(2)
·OH+RhB→CO2+H2O (3)
h++RhB→CO2+H2O (4)
Minor:O2+e-→·O2 -(5)
·O2 -+RhB→CO2+H2O (6)
Drawn by above analysis to draw a conclusion：
(1) when NaOH consumption is 0.2g, etching effect is best；
(2) when etch period be 3h, etching temperature be 60 DEG C when, the Bi preparing2WO6-xSample photocatalytic activity is
Good.Under visible light, 98.84% is reached to 10mg/L rhodamine B degradation rate, than the Bi not processed2WO6High by about 29%；
(3) Bi in etch period, temperature respectively 3h, 60 DEG C, after addition 0.2gKOH etching processing2WO6-xSample
Product catalysis activity is 83.99%, the Bi crossing less than NaOH etching processing under similarity condition2WO6-xSample；
(4) active specy is sheltered experiment and is shown, Bi2WO6-xIn play major catalytic effect be photohole h+, O2 -For secondary
Want active specy.
In a word, by introducing defect sturcture, especially Surface Oxygen defect sturcture, so that Bi2WO6Band gap narrows, photoproduction electricity
The recombination rate in son and hole all substantially reduces, and improves photocatalytic activity.This paper will be for improving Bi2WO6Photocatalytic activity provides
Experimental basis, provide new thinking for the organic pollution in effective control, degraded dyeing waste water simultaneously.
This detection data is just for above-mentioned detection sample.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (8)
1. a kind of Bi2WO6-xThe preparation method of micro Nano material is it is characterised in that comprise the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add Bi (NO3)3·5H2O, distilled water and concentrated nitric acid, in magnetic agitation
On device, agitating solution is to being completely dissolved；Simultaneously by Na2WO4·2H2O and distilled water stir to being completely dissolved in beaker B；Will
Na2WO4Solution dropwise enter in A beaker by Deca, time-consuming 20-30min；After completion of dropping, use HNO3Adjust precursor liquid with NaOH solution
PH value is 0.9-1.1, is stirred for 12-18min；Above-mentioned solution is transferred in hydrothermal reaction kettle, meets compactedness≤75%, put
In baking oven, 120 DEG C of reaction 18-24h of constant temperature；After the completion of reaction, sample centrifugation repeatedly washes with water respectively, precipitation washed by alcohol,
70 DEG C of constant temperature is dried 18-21h again, and grinding can obtain Bi2WO6；
Step 2, etching reaction：Take highly basic to be dissolved in deionized water, add Bi2WO6, adjust magnetic stirring apparatuss to 20-90 DEG C, carve
Erosion 0.5-6 hour；After completion of the reaction, by sample centrifugation, repeatedly being washed to solution with 60-70 DEG C of hot water is in neutrality；Again will
Solid is placed in baking oven, and 70 DEG C of constant temperature is dried 5-8h, that is, obtain product Bi2WO6-x.
2. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that in described etching reaction
Highly basic is sodium hydroxide.
3. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that in described etching reaction
NaOH and Bi2WO6Mass ratio be 1:1.
4. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that in described etching reaction
Etch period is 3 hours.
5. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that in described etching reaction
Etching temperature is 60 DEG C.
6. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that comprise the following steps：
Step one, Bi2WO6Preparation：In beaker A, first add 1.2118gBi (NO3)3·5H2O, 1mL distilled water and 0.5mL are dense
Nitric acid, on magnetic stirring apparatuss, agitating solution is to being completely dissolved；Simultaneously by 0.4123g Na2WO4·2H2O and 30mL distilled water exists
Stir in beaker B to being completely dissolved；By Na2WO4Solution dropwise enter in A beaker by Deca, and time for adding is 25min；Completion of dropping
Afterwards, use HNO3Adjusting precursor liquid pH value with NaOH solution is 1, is stirred for 15min；Above-mentioned solution is transferred into hydrothermal reaction kettle
In, meet compactedness≤75%, be placed in baking oven, 120 DEG C of reaction 20h of constant temperature；After the completion of reaction, by sample centrifugation, difference
Repeatedly wash with water, precipitation washed by alcohol, then 70 DEG C of constant temperature is dried 20h, grinding can obtain Bi2WO6；
Step 2, etching reaction：Take 0.2gNaOH to be dissolved in 50mL deionized water, add 0.2g Bi2WO6, adjust magnetic agitation
Device, to 60 DEG C, etches 3 hours；After completion of the reaction, by sample centrifugation, in repeatedly being washed with 60-70 DEG C of hot water and to solution being in
Property；Again solid is placed in baking oven, 70 DEG C of constant temperature is dried 6h, that is, obtain product Bi2WO6-x.
7. Bi as claimed in claim 12WO6-xThe preparation method of micro Nano material is it is characterised in that described Bi2WO6-xMicro-
Nano material possesses photocatalytic activity.
8. Bi as claimed in claim 72WO6-xThe preparation method of micro Nano material is it is characterised in that described Bi2WO6-xMicro-
Nano material has preferable photocatalytic activity to rhodamine B solution.
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| CN110465286A (en) * | 2019-06-21 | 2019-11-19 | 广东工业大学 | A kind of bismuth tungstate photocatalyst and its preparation method and application of Surface Oxygen vacancy defect modification |
| CN110947387A (en) * | 2019-11-25 | 2020-04-03 | 中国工程物理研究院材料研究所 | Preparation method and application of nickel-iron double metal hydroxide nano film material |
| CN110947387B (en) * | 2019-11-25 | 2022-07-01 | 中国工程物理研究院材料研究所 | Preparation method and application of nickel-iron double metal hydroxide nano film material |
| CN110921709A (en) * | 2019-12-12 | 2020-03-27 | 中国矿业大学 | Method for determining impurities and purifying bismuth tungstate synthesized by hydrothermal method |
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