CN103372424B - A kind of synthetic method of high activity N-F codope pucherite visible-light photocatalysis material - Google Patents
A kind of synthetic method of high activity N-F codope pucherite visible-light photocatalysis material Download PDFInfo
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Abstract
The invention discloses a kind of employing citric acid complex sol-gal process and prepare N F codope pucherite visible-light photocatalysis material and preparation technology thereof, the method is with Bi (NO3)3·5H2O(97%), NH4VO3(98.5%) being source material, citric acid (99.5%) is as chelating agen, NH4F is N and F source, ammonia regulation pH value, prepares navy blue colloidal sol, dries, and calcining obtains the pucherite catalysis material of N F codope.Compared with the pucherite of undoped, due to the synergism between nitrogen fluorine, make Lacking oxygen and the V in N F codope pucherite crystal with catalysis activity4+Increasing, and its band-gap energy becomes narrower, photocatalytic activity under visible light significantly improves.The inventive method technique is simple, mild condition and reproducible, can be widely used in the photocatalytic degradation of organic pollution, exist and be widely applied prospect in terms of environmental improvement.
Description
Technical field
The invention belongs to technical field of environment pollution control, relate to one and prepare N-F with citric acid complex sol-gel process
The method of codope pucherite catalysis material.
Background technology
Along with the development of modern industry, particularly organic chemical industry and dyeing industry so that the environmental pollution of human living is day by day
Increase the weight of.For some high concentrations, the organic wastewater of difficult degradation, traditional biochemistry and method of chemical treatment is used to be difficult to obtain preferable effect
Really.And photocatalytic oxidation is owing to having the various organic and universality of inorganic pollution of degraded, saving the energy and without secondary
The advantages such as pollution, make it in one of the most promising method for the treatment of of Organic Wastewater.Semiconductor light-catalyst technology, wherein
TiO2It is to study one of most commonly used photocatalyst, but due to TiO2Itself still have several drawbacks, such as semiconductor carriers
Recombination rate is high, and quantum efficiency is low, and light absorption wavelength is narrow, and the ratio utilizing sunlight is low, and is difficult to that treating capacity is big, pollutant levels
Big waste water.In order to improve the activity of photocatalyst and improve the utilization rate to solar energy, researcher passes through number of ways pair
TiO2It is modified research so that it is absorb red shift；The most then constantly look for developing the photocatalysis material of novel visible response
Material.
And BiVO4It it is exactly one of novel visible catalysis material of receiving much attention in recent years.BiVO4It is a kind of stable
Semi-conducting material, its energy gap is about 2.4 eV, and (2.6 eV, its ABSORPTION EDGE is permissible to be in close proximity to the center of solar spectrum
Extending to about 520nm, apparent colour is orange-yellow, is the novel visible responsible photocatalytic material of a kind of function admirable.Because of it
There is the advantages such as nontoxic, high stability, high sunlight utilization rate, clean at environment such as agricultural chemicals waste water, municipal sewage and trade effluents
Change field has shown good visible light photocatalytic degradation performance and wide industrial applications prospect.Research report
BiVO4Mainly there are 3 kinds of crystal structures, including tetragonal crystal system scheelite type (high-temperature-phase), tetragonal crystal system Zirconium orthosilicate. type and monoclinic crystal
System's deformation scheelite type (fergusonite type).The wherein monomer BiVO of monocrystalline scheelite-type structure4Photocatalytic activity relatively the highest.
But due to BiVO4Conduction band limit be positioned at 0V, its light induced electron be not easy by air oxygen capture and at catalyst surface area
Tired, add the recombination probability of electronics and hole, the ability causing degradation of organic substances under visible light is poor.Therefore in this feelings
Fast Acquisition photo-excited electron under condition, suppresses its compound, to improving this type of photocatalyst visible light catalytic fall with high energy holes
The efficiency solving pollutant is most important.To this end, scientific research scholar is to BiVO4Carry out research and probe, lived to improving its photocatalysis
Property.At present the method for document report mainly have Morphological control, transition metal ions and metal-oxide, the doping of rare earth element,
Compound and the load etc. of precious metal of quasiconductor.But these methods are limited to the raising of activity, and its preparation method is complicated, one-tenth
The defects such as the catalysis material photocatalytic activity of this height and preparation is unstable.
Summary of the invention
It is an object of the invention to and existing modification technology low for pucherite catalysis material visible light catalytic efficiency not
Foot, and a kind of preparation process provided is simple, hold the preparation side of the low N-F codope pucherite of operation, cost and equipment requirements
Method, the photocatalyst that the method obtains has the highest visible light catalysis activity, the organic dirt in energy fast degradation waste water from dyestuff
Dye thing.
The technical scheme is that
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material, comprises the following steps that:
1) with Bi (NO that mass percent is 97%3)3·5H2O, the NH of 98.5%4VO3For source material, with mass percent
Be 99.5% citric acid as chelating agen, the ratio for 1:2 weighs 4.8580 g(0.01 mol in molar ratio) Bi
(NO3)3·5H2O and 4.2028 g(0.02 mol) citric acid monohydrate (C6H8O7·H2O), citric acid monohydrate is joined pre-
First with the 50mL Bi (NO of the dilute nitric acid dissolution that 10 mL concentration are 10%3)3·5H2In O solution, obtain A liquid；It is 1:2 in molar ratio
Ratio weigh 1.1698 g(0.01 mol) NH4VO3With 4.2028 g(0.02 mol) citric acid monohydrate (C6H8O7·
H2O), it is dissolved in the distilled water of 50mL boiling, obtains B liquid；By mixed in molar ratio A liquid and the B liquid of Bi:V=1:1, according still further to NH4F with
Bi3+Mol ratio be that 0-15% adds 0.0074g, 0.0148g, 0.0222g, 0.0370g or 0.0555g, NH4F enters to mix molten
Liquid, then be 6-7 with ammonia regulation pH value, continuously stirred at 80 DEG C, evaporation, finally obtain navy blue pucherite precursor molten
Glue.
2) the pucherite precursor colloidal sol containing different amounts of N-F source that will dry, under the conditions of air atmosphere, in Muffle
Stove is calcined at 350 DEG C-550 DEG C 5h, obtains the pucherite catalysis material of N-F codope.
The catalytic effect of prepared N-F codope pucherite visible-light photocatalysis material uses methyl orange solution to test
Card.
In order to check the photocatalysis performance of pucherite prepared by the present invention, it is carried out the reality of photo-catalytic degradation of methyl-orange
Test；In 250 mL beakers, add 0.01g BiVO4Photocatalyst, 50 mL concentration are the methyl orange solution of 10 mg/L, lucifuge
Magnetic agitation 20 min is to reach adsorption equilibrium；250 W metal halide lamps are light source, and lamp irradiates methyl orange solution away from 14 cm,
Change with the absorbance of the methyl orange solution of 721 type spectrophotometric determination difference light application times, evaluate photocatalyst activity.
The preparation method of the present invention is also the exploitation of other nonmetal doping pucherite catalysis material and on a large scale should
With providing significant reference.
The invention have the benefit that
1) one of advantages of the present invention is, compared with other preparation methoies, sol-gel process for preparing has following spy
Point: the powder body of synthesis is difficult to reunite, good dispersion；Low cost, easily operate, it is adaptable to large-scale commercial production.
2) present invention is to improve pucherite at the photocatalytic activity of visible-range, provide a kind of efficiently, economical and
Simple preparation method, selects ammonium fluoride to prepare N, F codope bismuth vanadate photocatalyst as doped source, it is possible to achieve N, F's
Codope, effective degradable organic pollutant.
3) UV-vis characterization result shows, N-F codope makes pucherite energy gap narrow, and its photoresponse scope extends, performance
Go out higher photocatalytic activity, be effectively increased and solar energy source is directly utilized.
4) XRD characterization result shows, the N of doping and F ion cause the change of pucherite crystal structure, result in lattice
The increase of defect, this is also one of the reason of increased activity.
5) XPS characterization result shows, adulterate N and F, makes oxygen defect in pucherite increase, active substance V4+Increase, thus increase
Strong pucherite visible light catalysis activity.
6) the inventive method is raw materials used cheap and easily-available, and utilizes the sol-gal process under normal temperature and pressure, in air atmosphere
The N-F codope pucherite that middle calcining obtains, degraded methyl orange solution shows good degradation effect under visible light.
Accompanying drawing explanation
Fig. 1 is the UV-vis spectrogram of the bismuth vanadate photocatalyst prepared by embodiment 1,2,3,4,5,6.
Fig. 2 is unadulterated sample XRD figure spectrum.
Fig. 3 is the sample XRD figure spectrum of 0.1%N-F codope.
Fig. 4 is the XRD figure of the bismuth vanadate photocatalyst prepared by embodiment 4,7,8,9,10.
Fig. 5 is the bismuth vanadate photocatalyst degraded methyl orange efficiency chart prepared by embodiment 1,2,3,4,5,6.
Fig. 6 is the bismuth vanadate photocatalyst degraded methyl orange efficiency chart prepared by embodiment 4,7,8,9,10.
Detailed description of the invention
Further illustrate how the present invention realizes below in conjunction with specific embodiment:
Embodiment 1
The preparation method of the pucherite of the present embodiment comprises the following steps:
1) with Bi (NO that mass percent is 97%3)3·5H2O, the NH of 98.5%4VO3For source material, with mass percent
Be 99.5% citric acid as chelating agen, the ratio for 1:2 weighs 4.8580 g(0.01 mol in molar ratio) Bi
(NO3)3·5H2O and 4.2028 g(0.02 mol) citric acid monohydrate (C6H8O7·H2O), citric acid monohydrate is joined pre-
First with the 50mL Bi (NO of suitable dilute nitric acid dissolution3)3·5H2In O solution, obtain A liquid.0.01 is weighed by the molar ratio of 1:2
Mol, the NH of 1.1698 g4VO3Citric acid monohydrate (C with 0.02 mol, 4.2028 g6H8O7·H2O), 50mL boiling it is dissolved in
B liquid in distilled water.By Bi:V=1:1 mixed in molar ratio A liquid and B liquid, it is 6-7 with ammonia regulation pH value, continues at 80 DEG C
Stirring, evaporation, finally obtain navy blue pucherite precursor colloidal sol.
2) the pucherite precursor colloidal sol of drying is put into and Muffle furnace is calcined at 500 DEG C 5h, obtain pure pucherite light
Catalysis material.
Fig. 1 (a) is the UV-vis collection of illustrative plates of product, the BiVO of this example synthesis4 Light absorb threshold value be 541nm, forbidden band width
Degree is 2.29 eV.Fig. 2 (a) is the XRD figure spectrum of product, the BiVO of this example synthesis418.7o、28.8o、30.5o、34.5o、
35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、63.6o、69.3oPosition occurs that diffraction maximum is monocline type vanadic acid
The characteristic peak of bismuth, crystalline phase purity is higher, and unit cell volume is 309.21 nm3。
In order to check the photocatalysis performance of pucherite prepared by this experiment, it is carried out the reality of photo-catalytic degradation of methyl-orange
Test.In 250 mL beakers, add 0.01 g BiVO4Photocatalyst, 50 mL concentration are the methyl orange solution of 10 mg/L, keep away
Light magnetic agitation 20 min is to reach adsorption equilibrium.250 W metal halide lamps are light source, and it is molten that lamp irradiates methyl orange away from 14 cm
Liquid, illumination 50min, the photocatalytic activity of methyl orange reaches 38.45%.
Embodiment 2
1) with Bi (NO that mass percent is 97%3)3·5H2O, the NH of 98.5%4VO3For source material, with mass percent
Be 99.5% citric acid as chelating agen, the ratio for 1:2 weighs 4.8580 g(0.01 mol in molar ratio) Bi
(NO3)3·5H2O and 4.2028 g(0.02 mol) citric acid monohydrate (C6H8O7·H2O), citric acid monohydrate is joined pre-
First with the 50mL Bi (NO of suitable dilute nitric acid dissolution3)3·5H2In O solution, obtain A liquid；Ratio for 1:2 weighs in molar ratio
0.01 mol, the NH of 1.1698 g4VO3Citric acid monohydrate (C with 0.02 mol, 4.2028 g6H8O7·H2O), it is dissolved in 50mL
In the distilled water of boiling, obtain B liquid；By Bi:V=1:1 mixed in molar ratio A liquid and B liquid, according to NH4F with Bi mol ratio is 2% to add
NH4F is in mixed solution, then is 6-7 with ammonia regulation pH value, continuously stirred at 80 DEG C, and evaporation finally obtains navy blue
Pucherite precursor colloidal sol.
2) the pucherite precursor colloidal sol of drying is put into and Muffle furnace is calcined at 500 DEG C 5h, obtain the N-F doping of 2%
Pucherite catalysis material.
Fig. 1 (b) is the UV-vis collection of illustrative plates of product, the BiVO of this example synthesis4 Light absorb threshold value be 546nm, forbidden band width
Degree is 2.27 eV.Fig. 2 (b) is the XRD figure spectrum of product, the BiVO of this example synthesis418.7o、28.8o、30.5o、34.5o、
35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、63.6o、69.3oPosition occurs that diffraction maximum is monocline type vanadic acid
The characteristic peak of bismuth, but characteristic peak significantly offsets to low-angle, and unit cell volume is 309.86 nm3。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 50min
Catalysis degradation modulus is 50.23%
Embodiment 3
According to the preparation method of the present invention of embodiment 2, different conditions is: NH4F Yu Bi mol ratio changes 4% into, is prepared into
The pucherite catalysis material of the N-F to 4%, the product UV-vis collection of illustrative plates obtained is shown in Fig. 1 (c), the BiVO of this example synthesis4 's
It is 556nm that light absorbs threshold value, and energy gap is 2.23 eV.Fig. 2 (c) is the XRD figure spectrum of product, the BiVO of this example synthesis4
18.7o、28.8o、30.5o、34.5o、35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、63.6o、69.3oPosition
Putting the characteristic peak occurring that diffraction maximum is monocline type pucherite, but characteristic peak significantly offsets to low-angle, unit cell volume is
310.33 nm3。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 50min
Catalysis degradation modulus is 63.78 %.
Embodiment 4
According to the preparation method of the present invention of embodiment 2, different reaction conditions is: NH4F Yu Bi mol ratio changes 6% into, system
The pucherite catalysis material of the standby N-F obtaining 4%.Fig. 1 (d) is shown in by the product UV-vis collection of illustrative plates obtained, the synthesis of this example
BiVO4 Light absorb threshold value be 564nm, energy gap is 2.20 eV.Fig. 2 (d) is the XRD figure spectrum of product, the synthesis of this example
BiVO418.7o、28.8o、30.5o、34.5o、35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、63.6o、
69.3oPosition occurs that diffraction maximum is the characteristic peak of monocline type pucherite, but characteristic peak significantly offsets to low-angle, unit cell volume
It is 310.96 nm3.As can be seen from Table 1, the pucherite of doping 6% lacks compared with oxygen in the pure pucherite crystal of preparation in example 1
Fall into and V4+Increase.
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 50min
Catalysis degradation modulus is 85.65 %.
Table 1 analysis of O 1s and V 2pof pure BiVO4 (a) and 6% N-F codoped
BiVO4(b)
Embodiment 5
According to the preparation method of the present invention of embodiment 2, simply by the NH in embodiment 24F Yu Bi mol ratio changes 10% into, system
The pucherite catalysis material of the standby N-F obtaining 4%.Fig. 1 (e) is shown in by the product UV-vis collection of illustrative plates obtained, the synthesis of this example
BiVO4 Light absorb threshold value be 554 nm, energy gap is 2.24 eV.Fig. 2 (e) is the XRD figure spectrum of product, and this example synthesizes
BiVO418.7o、28.8o、30.5o、34.5o、35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、
63.6o、69.3oPosition occurs that diffraction maximum is the characteristic peak of monocline type pucherite, but characteristic peak starts gradually to offset to wide-angle,
Unit cell volume is 309.94 nm3。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 50min
Catalysis degradation modulus is 64.28 %.
Embodiment 6
According to the preparation method of the present invention of embodiment 2, simply by the NH in embodiment 24F Yu Bi mol ratio changes 15 % into,
Prepare the pucherite catalysis material of the N-F of 4%.Fig. 1 (f) is shown in by the product UV-vis collection of illustrative plates obtained, the synthesis of this example
BiVO4 Light absorb threshold value be 554 nm, energy gap is 2.24 eV.Fig. 2 (f) is the XRD figure spectrum of product, and this example synthesizes
BiVO418.7o、28.8o、30.5o、34.5o、35.1o、37.8o、39.8o、42.4o、47.2o、53.2o、59.8o、
63.6o、69.3oPosition occurs that diffraction maximum is the characteristic peak of monocline type pucherite, but characteristic peak starts gradually to offset to wide-angle,
Unit cell volume is 309.88 nm3。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 50min
Catalysis degradation modulus is 55.88 %.
Embodiment 7
According to the preparation method of the present invention of embodiment 4, simply change into the calcining heat in embodiment 4 calcining at 350 DEG C
5h, prepares 6%N-F doping pucherite catalysis material.Fig. 3 (a) is gained sample XRD figure, the BiVO of this example synthesis4
In addition to having the characteristic peak of monocline type pucherite, Bi2O3 impurity peaks also occur, and its degree of crystallinity is relatively low, crystal particle diameter is 40.61
nm。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 10min
Catalysis degradation modulus is 59.17 %.
Embodiment 8
According to the preparation method of the present invention of embodiment 4, simply change into the calcining heat in embodiment 4 calcining at 400 DEG C
5h, prepares 6%N-F doping pucherite catalysis material.Fig. 3 (b) is gained sample XRD figure, the BiVO of this example synthesis4
In addition to having the characteristic peak of monocline type pucherite, Bi also occurs2O3Impurity peaks, and its degree of crystallinity is relatively low, crystal particle diameter is 42.74
nm。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 10min
Catalysis degradation modulus is 61.45 %.
Embodiment 9
According to the preparation method of the present invention of embodiment 4, simply change into the calcining heat in embodiment 4 calcining at 450 DEG C
5h, prepares 6%N-F doping pucherite catalysis material.Fig. 3 (c) is gained sample XRD figure, the BiVO of this example synthesis4
In addition to having the characteristic peak of monocline type pucherite, Bi also occurs2O3Impurity peaks, and its degree of crystallinity is relatively low, crystal particle diameter is 50.76
nm。
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 10min
Catalysis degradation modulus is 74.59 %.
Embodiment 10
According to the preparation method of the present invention of embodiment 4, simply change into the calcining heat in embodiment 4 calcining at 550 DEG C
5h, prepares 6%N-F doping pucherite catalysis material.Fig. 3 (e) is gained sample XRD figure, the BiVO of this example synthesis4
Only have the characteristic peak of monocline type pucherite, there is no Bi2O3Impurity peaks occurs, degree of crystallinity is high, and crystal particle diameter is 50.44 nm.
According to the photocatalysis performance of the pucherite synthesized by the method detection described in embodiment 1, the light of methyl orange during 10min
Catalysis degradation modulus is 70.45 %.
Claims (9)
1. the synthetic method of a high activity N-F codope pucherite visible-light photocatalysis material, it is characterised in that include following
Processing step:
1) with Bi (NO that mass percent is 97%3)3·5H2O, the NH of 98.5%4VO3For source material, with mass percent it is
The citric acid of 99.5% is as chelating agen, and the ratio for 1:2 weighs the Bi (NO of 4.8580g (0.01mol) in molar ratio3)3·
5H2Citric acid monohydrate (the C of O and 4.2028g (0.02mol)6H8O7·H2O), citric acid monohydrate is joined dense with 10mL in advance
Degree is the 50mLBi (NO of the dilute nitric acid dissolution of 10%3)3·5H2In O solution, obtain A liquid；Ratio for 1:2 weighs in molar ratio
The NH of 1.1698g (0.01mol)4VO3Citric acid monohydrate (C with 4.2028g (0.02mol)6H8O7·H2O), 50mL boiling it is dissolved in
In the distilled water risen, obtain B liquid；By mixed in molar ratio A liquid and the B liquid of Bi:V=1:1, according still further to NH4F and Bi3+Mol ratio be
0-15% adds the NH of 0.0074g, 0.0148g, 0.0222g, 0.0370g or 0.0555g4F enters mixed solution, then adjusts with ammonia
Joint pH value is 6-7, continuously stirred at 80 DEG C, evaporation, finally obtains navy blue pucherite precursor colloidal sol；
2) the pucherite precursor colloidal sol containing different amounts of N-F source that will dry, under the conditions of air atmosphere, in Muffle furnace
At 350 DEG C-550 DEG C, calcine 5h, obtain the pucherite catalysis material of N-F codope.
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 1,
It is characterized in that:
1) with Bi (NO that mass percent is 97%3)3·5H2O, the NH of 98.5%4VO3For source material, with mass percent it is
The citric acid of 99.5% is as chelating agen, and the ratio for 1:2 weighs the Bi (NO of 4.8580g (0.01mol) in molar ratio3)3·
5H2Citric acid monohydrate (the C of O and 4.2028g (0.02mol)6H8O7·H2O), citric acid monohydrate is joined use dust technology in advance
50mL Bi (the NO dissolved3)3·5H2In O solution, obtain A liquid；Ratio for 1:2 weighs 0.01mol in molar ratio, 1.1698g's
NH4VO3And the citric acid monohydrate (C of 0.02mol, 4.2028g6H8O7·H2O), it is dissolved in the distilled water of 50mL boiling, obtains B liquid；
By Bi:V=1:1 mixed in molar ratio A liquid and B liquid, according to NH4F Yu Bi mol ratio is 2% to add NH4F is in mixed solution, then uses
Ammonia regulation pH value is 6-7, continuously stirred at 80 DEG C, and evaporation finally obtains navy blue pucherite precursor colloidal sol；
2) the pucherite precursor colloidal sol of drying is put into and Muffle furnace is calcined at 500 DEG C 5h, obtain the N-F doping vanadium of 2%
Acid bismuth catalysis material；
The BiVO of above-mentioned synthesis4Light absorb threshold value be 546nm, energy gap is 2.27eV, the BiVO of synthesis418.7 °,
28.8 °, 30.5 °, 34.5 °, 35.1 °, 37.8 °, 39.8 °, 42.4 °, 47.2 °, 53.2 °, 59.8 °, 63.6 °, 69.3 ° of positions go out
Existing diffraction maximum is the characteristic peak of monocline type pucherite, but characteristic peak significantly offsets to low-angle, and unit cell volume is
309.86nm3。
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 2,
It is characterized in that:
Different conditions is: NH4F Yu Bi mol ratio changes 4% into, prepares the pucherite catalysis material of the N-F of 4%, synthesis
BiVO4Light absorb threshold value be 556nm, energy gap is 2.23eV；The BiVO of synthesis418.7 °, 28.8 °, 30.5 °,
34.5 °, 35.1 °, 37.8 °, 39.8 °, 42.4 °, 47.2 °, 53.2 °, 59.8 °, 63.6 °, 69.3 ° of positions occur that diffraction maximum is single
The tiltedly characteristic peak of type pucherite, but characteristic peak significantly offsets to low-angle, and unit cell volume is 310.33nm3。
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 2,
It is characterized in that:
Different reaction conditions is: NH4F Yu Bi mol ratio changes 6% into, prepares the pucherite catalysis material of the N-F of 6%,
The BiVO of synthesis4Light absorb threshold value be 564nm, energy gap is 2.20eV, the BiVO of synthesis418.7 °, 28.8 °,
30.5 °, 34.5 °, 35.1 °, 37.8 °, 39.8 °, 42.4 °, 47.2 °, 53.2 °, 59.8 °, 63.6 °, 69.3 ° of positions diffraction occurs
Peak is the characteristic peak of monocline type pucherite, but characteristic peak significantly offsets to low-angle, and unit cell volume is 310.96nm3。
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 2,
It is characterized in that:
Different reaction conditions is: NH4F Yu Bi mol ratio changes 10% into, prepares the pucherite photocatalysis material of the N-F of 10%
Material, the BiVO of synthesis4Light absorb threshold value be 554nm, energy gap is 2.24eV, the BiVO of synthesis418.7 °, 28.8 °,
30.5 °, 34.5 °, 35.1 °, 37.8 °, 39.8 °, 42.4 °, 47.2 °, 53.2 °, 59.8 °, 63.6 °, 69.3 ° of positions diffraction occurs
Peak is the characteristic peak of monocline type pucherite, but characteristic peak starts gradually to offset to wide-angle, and unit cell volume is 309.94nm3。
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 2,
It is characterized in that:
Different reaction conditions is: NH4F Yu Bi mol ratio changes 15% into, prepares the pucherite photocatalysis material of the N-F of 15%
Material, the BiVO of synthesis4Light absorb threshold value be 554nm, energy gap is 2.24eV, the BiVO of synthesis418.7 °, 28.8 °,
30.5 °, 34.5 °, 35.1 °, 37.8 °, 39.8 °, 42.4 °, 47.2 °, 53.2 °, 59.8 °, 63.6 °, 69.3 ° of positions diffraction occurs
Peak is the characteristic peak of monocline type pucherite, but characteristic peak starts gradually to offset to wide-angle, and unit cell volume is 309.88nm3。
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 4,
It is characterized in that:
Different reaction conditions is: calcining heat changes calcining at 350 DEG C 5h into, prepares 6%N-F doping pucherite photocatalysis
Material, the BiVO of synthesis4In addition to having the characteristic peak of monocline type pucherite, Bi also occurs2O3Impurity peaks, and its degree of crystallinity is relatively low,
Crystal particle diameter is 40.61nm.
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 4,
It is characterized in that:
Different reaction conditions is: calcining heat changes calcining at 400 DEG C 5h into, prepares 6%N-F doping pucherite photocatalysis
Material, the BiVO of synthesis4In addition to having the characteristic peak of monocline type pucherite, Bi also occurs2O3Impurity peaks, and its degree of crystallinity is relatively low,
Crystal particle diameter is 42.74nm.
The synthetic method of a kind of high activity N-F codope pucherite visible-light photocatalysis material the most according to claim 4,
It is characterized in that:
Different reaction conditions is: calcining heat changes calcining at 450 DEG C 5h into, prepares 6%N-F doping pucherite photocatalysis
Material, the BiVO of synthesis4In addition to having the characteristic peak of monocline type pucherite, Bi also occurs2O3Impurity peaks, and its degree of crystallinity is relatively low,
Crystal particle diameter is 50.76nm.
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| CN110339843B (en) * | 2019-08-08 | 2021-06-29 | 重庆大学 | Preparation method of magnetic bismuth oxide/bismuth vanadate composite photocatalyst |
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