CN109133168A - The preparation method of octahedra pucherite crystal is truncated in a kind of monoclinic phase - Google Patents
The preparation method of octahedra pucherite crystal is truncated in a kind of monoclinic phase Download PDFInfo
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Abstract
The present invention relates to the preparation methods that octahedra pucherite crystal is truncated in a kind of monoclinic phase, comprising: obtains solution A by five water bismuth nitrates, nitric acid solution and fluoride solution water；Solution B is obtained by ammonium metavanadate and sodium hydroxide solution；Solution C is obtained by the solution B and the solution A；The solution C is subjected to microwave-hydrothermal method reaction, obtains crystal prototype；The crystal prototype is cleaned, is dried, the monoclinic phase is obtained and octahedra pucherite crystal is truncated.The present invention prepares pucherite crystal using microwave-hydrothermal method reaction, the parameters such as molar ratio, reaction temperature, reaction time by control fluorine ion and bismuth ion, preparation has synthesized monoclinic phase and octahedral pucherite crystal is truncated, and the crystal being prepared has purity is high, the good feature of photocatalysis performance.
Description
Technical field
The invention belongs to technical field of new energy material preparation, and in particular to a kind of octahedra pucherite of monoclinic phase truncation is brilliant
The preparation method of body.
Background technique
In past many years, researchers are dedicated to using noble metal loading, ion doping, dye sensitization, compound
The methods of semiconductor is to traditional photochemical catalyst TiO2It is modified.But simultaneously in its reaction process there is also light induced electron and
The extensive use for significantly limiting it such as low of the compound of hole, photocatalysis quantum efficiency.Researchers also develop many non-
TiO2The catalyst of type, such as the material that ZnO, silver orthophosphate, sulfide, several classes of bismuth based compound are representative.
Bi system catalysis material electronic structure is unique, and valence band is formed by Bi-6s and O-2p orbital hybridization.This unique knot
Structure makes it have more precipitous ABSORPTION EDGE in visible-range, the antibonding between zwitterion be more advantageous to the formation in hole with
Flowing, so that light-catalyzed reaction is easier to carry out, therefore some Bi system complex oxides with visible light catalytic ability, such as
Bi2O3、BiWO4、BiVO4It has obtained widely paying close attention to.Wherein, BiVO4It is a kind of nontoxic bright orange color substance, most starts mainly to make
For pigment and ferroelectric material.People have found BiVO during finding and designing novel semiconductor material4Crystal structure is main
There are 3 kinds: cubic zircon phase (z-t, Eg=2.9eV), monoclinic phase scheelite (s-m, Eg=2.4eV) and cubic scheelite phase (s-
T, Eg=2.4eV) three kinds of different crystal structures, and three-phase can mutually convert under certain condition, especially monoclinic phase is white
Tungsten ore has higher photocatalysis performance under visible light.
Currently, preparation BiVO4Method be to be developed on the basis of conventional crystal preparation method, such as solid phase reaction
Develop the solvent-thermal method come in method, coprecipitation, microemulsion method, sol-gel method, hydro-thermal method and hydrothermal basis and mixes
Bonding solvent thermal method.But prepared sample physical property is bad, purity is not high.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of monoclinic phases, and octahedra vanadic acid is truncated
The preparation method of bismuth crystal.The technical problem to be solved in the present invention is achieved through the following technical solutions:
The embodiment of the invention provides the preparation methods that octahedra pucherite crystal is truncated in a kind of monoclinic phase, comprising:
The fluoride solution of 0.5ml~4ml is added in nitric acid solution step 1, prepares solution D；Wherein, in the fluorine
In solion, the concentration of fluorine ion is 0.5mol/L；
Five water bismuth nitrate of 1mmol is dissolved in the solution D by step 2, prepares solution A；
The ammonium metavanadate of 0.75mmol~2mmol is dissolved in sodium hydroxide solution by step 3, prepares solution B；
Step 4 in solution A described in the solution B, will stir 10min~20min, preparation solution C；
Step 5 handles the solution C, obtains the monoclinic phase and octahedra pucherite crystal is truncated.
In one embodiment of the invention, before step 1, can also include:
Step 1X, 1ml~2ml concentrated nitric acid is mixed with 18ml~20ml deionized water, prepares the nitric acid solution.
In one embodiment of the invention, before step 3, can also include:
Step 3X, the standard caustic soda solution of 1ml~2ml is mixed with the deionized water of 20ml~25ml, prepares institute
State sodium hydroxide solution；Wherein, the standard caustic soda solution concentration is 1mol/L.
In one embodiment of the invention, step 6 includes:
Step 51 pours into the solution C in micro-wave diminishing pot, 100 DEG C~190 DEG C at a temperature of, pass through Microwave Water
Thermal method reacts 30min~4h, prepares sample solution；
Step 52, the filtering sample solution, obtain sediment, and the sediment is cleaned with dehydrated alcohol,
Obtain Sample crystals；
The Sample crystals are put into drying box by step 53,50 DEG C~80 DEG C at a temperature of, dry 10h-12h is obtained
Octahedra pucherite crystal is truncated to the monoclinic phase.
In one embodiment of the invention, the five water bismuth nitrate purity is to analyze pure AR, the ammonium metavanadate purity
To analyze pure AR.
In one embodiment of the invention, the solution A is clear solution.
In one embodiment of the invention, the solution B is clear solution.
In one embodiment of the invention, the solution C orange solution.
In one embodiment of the invention, cleaning way is ultrasonic cleaning；Wherein, wash number is 3 times.
In one embodiment of the invention, it is glassy yellow powder that octahedra pucherite crystal, which is truncated, in the monoclinic phase.
Compared with prior art, beneficial effects of the present invention:
The present invention prepares pucherite crystal using microwave-hydrothermal method, by the molar ratio of control fluorine ion and bismuth ion, instead
The parameters such as temperature, reaction time are answered, stablizes preparation and has synthesized the octahedral pucherite crystal of monoclinic phase truncation, the crystalline substance being prepared
Body has purity is high, the good feature of photocatalysis performance.
Detailed description of the invention
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 1, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
XRD diagram；
It is brilliant that octahedra pucherite is truncated in the monoclinic phase that Fig. 2 a-2b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
The SEM of body schemes；
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 3, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
Photocatalytic activity versus time curve；
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 4, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
XRD diagram；
It is brilliant that octahedra pucherite is truncated in the monoclinic phase that Fig. 5 a-5b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
The SEM of body schemes；
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 6, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
Photocatalytic activity versus time curve；
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 7, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
XRD diagram；
Octahedra pucherite is truncated in the monoclinic phase that Fig. 8 a-8b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
The SEM of crystal schemes；
Octahedra pucherite crystal is truncated in the monoclinic phase that Fig. 9, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
Photocatalytic activity versus time curve.
Specific embodiment
Further detailed description is done to the present invention combined with specific embodiments below, but embodiments of the present invention are not limited to
This.
Embodiment one
The preparation method of octahedra pucherite crystal is truncated in a kind of monoclinic phase, and steps are as follows:
The fluoride solution of 0.5ml~4ml is added in nitric acid solution step 1, prepares solution D；Wherein, in the fluorine
In solion, the concentration of fluorine ion is 0.5mol/L.
Specifically, the concentrated nitric acid of 1ml~2ml and the deionized water of 18ml~20ml are taken respectively；
Specifically, taking the deionized water by the concentrated nitric acid of 1ml~2ml and 18ml~20ml respectively.
The concentrated nitric acid of 1ml~2ml is slowly added in the deionized water of 18ml~20ml, the magnetic agitation when being added,
After cooling, nitric acid solution is obtained.
The fluoride solution for taking 0.5ml~4ml, is added into the nitric acid solution prepared, passes through magnetic agitation, preparation
Solution D.
Fluoride solution can be its of Fluorinse, potassium fluoride solution, ammonium fluoride solution or other fluoride solutions
Middle one kind, or be many of solution mixture, it is preferable that fluoride solution is Fluorinse.
Preferably, in above-mentioned fluoride solution, the concentration of fluorine ion is 0.5mol/L (mole every liter).
Five water bismuth nitrate of 1mmol (mM) is dissolved in the solution D of step 1 preparation by step 2, prepares solution A.
Specifically, weighing five water bismuth nitrates of 1mmol mass.
Five water bismuth nitrates of weighed 1mmol mass are added in the solution D that step 1 prepares, by magnetic agitation, are made
Five water bismuth nitrates are completely dissolved in solution D, obtain solution A.
Preferably, five above-mentioned water bismuth nitrate purity are to analyze pure AR.
Above-mentioned solution A is clear solution.
Preferably, the molar ratio of fluorine ion and bismuth ion is 1:4~2:1 in solution A.
The ammonium metavanadate of 0.75mmol~2mmol is dissolved in sodium hydroxide solution by step 3, prepares solution B.
Specifically, taking the standard caustic soda solution and 20ml~25ml deionized water of 1ml~2ml respectively；Preferably, on
The concentration for stating standard caustic soda solution is 1mol/L.
The standard caustic soda solution of 1ml~2ml is slowly added in 20ml~25ml deionized water, the magnetic when being added
Power stirring, after cooling, obtains sodium hydroxide solution.
Weigh the ammonium metavanadate of 0.75mmol~2mmol mass；
The ammonium metavanadate of weighed 0.75mmol~2mmol mass is added in the sodium hydroxide solution prepared, is passed through
Magnetic agitation is completely dissolved in ammonium metavanadate in sodium hydroxide solution, obtains solution B.
Preferably, above-mentioned ammonium metavanadate purity is to analyze pure AR.
The above-mentioned solution B being prepared is clear solution.
Step 4 in solution A described in the solution B, will stir 10min (minute)~20min, preparation solution C.
Specifically, solution B prepared by step 3 is quickly added in solution A prepared by step 2, passes through magnetic agitation
10min~20min obtains solution C.
The solution C of above-mentioned preparation is orange-yellow liquid.
Step 5 handles the solution C, obtains the monoclinic phase and octahedra pucherite crystal is truncated.
Step 51, the solution C for preparing step 4 are poured into micro-wave diminishing pot, 100 DEG C~190 DEG C at a temperature of, pass through
Microwave-hydrothermal method reacts 30min~4h (hour), prepares sample solution.
The sample solution of above-mentioned preparation includes supernatant and sediment.
Step 52, the filtering sample solution, obtain sediment, and the sediment is cleaned with dehydrated alcohol,
Obtain Sample crystals.
Specifically, the supernatant for filtering out sample solution obtains the sediment of sample solution.
Sediment is cleaned by supersonic cleaning machine.
Specifically, cleaning agent is added in supersonic wave cleaning machine, and sediment obtained above is put into supersonic cleaning machine
Cleaning agent in, open super refreshing cleaning machine, sediment cleaned.Preferably, cleaning agent is dehydrated alcohol.
The sediment after cleaning is dried by centrifuge.
Sediment after cleaning is put into centrifuge, cleaning agent in sediment is removed by centrifuge.Preferably, centrifuge
Revolving speed be 6000 rpms (r/min)；
It repeats above-mentioned supersonic cleaning machine cleaning and centrifuge dries 2 times, obtain Sample crystals.
Obtained Sample crystals are put into drying box by step 53,50 DEG C~80 DEG C at a temperature of, dry 10h-12h,
It obtains the monoclinic phase and octahedra pucherite crystal is truncated.
It is glassy yellow powder that octahedra pucherite crystal, which is truncated, in obtained monoclinic phase.
Preferably, the present embodiment prepares pucherite crystal using microwave-hydrothermal method reaction, in control n (F-): n (Bi3+) rub
That ratio, and control reaction temperature and under conditions of the control reaction time, be prepared for monoclinic phase and octahedron pucherite crystal is truncated.
Wherein, in microwave-hydrothermal method reaction, the alternating electric field direction that microwave generates, deflecting per second is up to several hundred million times.This makes polarity
Dielectric molecule occurs dipole and turns to polarization, and lags because it is turned to due to polarization speed does not catch up with alternating electric field, causes in material
Portion's power dissipation.Meanwhile a part of microwave energy is thermal energy, makes substance heat temperature raising itself.
Microwave-hydrothermal method reaction is the hydro-thermal method using microwave as heating method, by microwave field and traditional hydrothermal synthesis method
Combine, a kind of method that heat source carries out hydrothermal synthesis is made with microwave field.When carrying out microwave-hydrothermal method reaction, in electromagnetic field
Substance cause whole heating because of dielectric loss itself, so as to realizing the stirring on molecular level, and different depth
Reactant can be penetrated by microwave, and the reactant of each depth can be heated simultaneously, homogeneous heating, woth no need to pass through temperature
Degree difference carries out heat transfer, and temperature gradient is small, and substance heating is rapidly, and energy utilization efficiency is very high, and the reaction time is obviously shortened.
The present invention prepares pucherite crystal using microwave-hydrothermal method reaction, by mole for controlling fluorine ion and bismuth ion
Than parameters such as, reaction temperature, reaction time, preparation has synthesized monoclinic phase and octahedral pucherite crystal is truncated, has been prepared
Crystal has purity is high, the good feature of photocatalysis performance.
Embodiment two
Referring to Figure 1, the monoclinic phase that Fig. 2 a-2b and Fig. 3, Fig. 1, which are the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
The XRD diagram of octahedra pucherite crystal is truncated；The monocline that Fig. 2 a-2b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
The SEM figure of octahedra pucherite crystal is mutually truncated；The monoclinic phase that Fig. 3, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:4
The photocatalytic activity versus time curve of octahedra pucherite crystal is truncated.
The preparation method of octahedra pucherite crystal is truncated in a kind of monoclinic phase, and steps are as follows:
Step 1: 1ml concentrated nitric acid is mixed with 19ml deionized water, nitric acid solution is prepared.
Specifically, the concentrated nitric acid of 1ml and the deionized water of 19ml are taken respectively；
The concentrated nitric acid of 1ml is slowly added in the deionized water of 19ml, when being added, magnetic agitation obtains after cooling
To nitric acid solution.
Step 2: the Fluorinse of 0.5ml is added in the nitric acid solution of step 1 preparation, solution D is prepared.
Specifically, the Fluorinse for taking 0.5ml is added into the nitric acid solution of step 1 preparation, is stirred by magnetic force
It mixes, prepares solution D.
Preferably, above-mentioned Fluorinse concentration is 0.5mol/L.
Step 3: five water bismuth nitrate of 1mmol is dissolved in the solution D of step 2 preparation, solution A is prepared.
Specifically, weighing five water bismuth nitrates of 1mmol mass；
Five water bismuth nitrates of weighed 1mmol mass are added in the solution D of step 2 preparation, by magnetic agitation, are made
Five water bismuth nitrates are completely dissolved in the solution D of step 2 preparation, obtain solution A.
Five above-mentioned water bismuth nitrate purity are to analyze pure AR, and solution A obtained above is clear solution.
Preferably, the molar ratio of fluorine ion and bismuth ion is 1:4 in solution A.
Step 4: the standard caustic soda solution of 1.5ml is mixed with the deionized water of 20ml, sodium hydroxide solution is prepared.
Specifically, taking the standard caustic soda solution and 20ml deionized water of 1.5ml respectively；
The standard caustic soda solution of 1.5ml is slowly added in 20ml deionized water, the magnetic agitation when being added, to
After cooling, sodium hydroxide solution is obtained.
The concentration of above-mentioned standard sodium hydroxide solution is 1mol/L.
Step 5: the ammonium metavanadate of 1mmol is dissolved in the sodium hydroxide solution of step 4 preparation, solution is prepared
B。
Specifically, the ammonium metavanadate of 1mmol mass is weighed；
The ammonium metavanadate of weighed 1mmol mass is added in the sodium hydroxide solution of step 4 preparation, is stirred by magnetic force
It mixes, is completely dissolved in ammonium metavanadate in the sodium hydroxide solution of step 4 preparation, obtains solution B.
Above-mentioned ammonium metavanadate purity is to analyze pure AR, and the above-mentioned solution B being prepared is clear solution.
Step 6: the solution B of step 5 preparation is added in the solution A of step 3 preparation, stirring 10min~
20min prepares solution C.
Specifically, solution B prepared by step 5 is quickly added in the solution A of step 3 preparation, is stirred by magnetic force
10min~20min is mixed, solution C is obtained.
The solution C of above-mentioned preparation is orange-yellow liquid.
Step 7: the solution C prepared by step 6 is poured into micro-wave diminishing pot, in 100 DEG C~190 DEG C of temperature
Under, 30min~4h is reacted by microwave-hydrothermal method, prepares sample solution.
The sample solution of above-mentioned preparation includes supernatant and sediment.
Step 8: the sample solution prepared by filtration step seven, obtains sediment, and by the anhydrous second of the sediment
Alcohol is cleaned, and Sample crystals are obtained；
Specifically, the supernatant for filtering out the sample solution of step 7 preparation, obtains the sediment of sample solution；
Dehydrated alcohol is added in supersonic wave cleaning machine；
Sediment obtained above is put into the dehydrated alcohol of super refreshing cleaning machine, super refreshing cleaning machine is opened, to sediment
It is cleaned；
Sediment after cleaning is put into centrifuge, impurity in sediment is removed by centrifuge, wherein centrifuge turns
Speed is 6000r/min；
Above-mentioned supersonic cleaning machine cleaning and centrifuge decontamination 2 times are repeated, Sample crystals are obtained.
Step 9: the Sample crystals that step 8 is obtained are put into drying box, 80 DEG C at a temperature of, dry 10h,
It obtains the monoclinic phase and octahedra pucherite crystal is truncated.
It is glassy yellow powder that octahedra pucherite crystal, which is truncated, in monoclinic phase.
Preferably, the monoclinic phase truncation eight prepared when as shown in Figure 1, being 1:4 by the molar ratio of fluorine ion and bismuth ion
X-ray diffraction (X-ray diffraction, referred to as: XRD) figure of face body pucherite crystal, it can be deduced that, the crystal it is main
Diffraction maximum respectively (number, wherein cell parameter with NO.14-0688 by monoclinic phase pucherite crystal standard PDF card) diffraction maximum is corresponding, it is brilliant that (040) crystal face intensity is higher than main peak (121)
Face determines that the crystal is that the octahedra pucherite crystal (BiVO of monocline scheelite knot phase structure is truncated in monoclinic phase4Crystal).
Preferably, as shown in Figure 2 a and 2 b, SEM figure is scanning electron microscope (SEM) figure.The list of the present embodiment synthesis
It is in that truncation is octahedronlike that octahedra pucherite crystal morphology, which is truncated, in monoclinic phase, and size is uneven, and big crystal grain diameter is about 5 μm, thickness
About 2 μm, lesser diameter is about 2.5 μm, with a thickness of 1 μm.
Preferably, it is the organic pollutant being degraded with methylene blue (MB) solution, the filter of 420nm is added with the xenon lamp of 500W
Mating plate carrys out simulated visible light to BiVO manufactured in the present embodiment4Sample carries out photocatalysis performance test, it is preferable that the model of xenon lamp
Are as follows: XQ350-500.Specific experimental implementation is as follows:
(1) methylene blue solution is configured.By 1mg methylene blue powder, it is dissolved in the deionized water of 100mL, stirs to get
Concentration is the MB aqueous solution of 10mg/L.
(2) sample is handled, adsorption desorption balance is reached.Weigh the BiVO of 5mg4Sample, the MB for being dissolved in 100mL are water-soluble
In liquid, ultrasonic vibration 20min stirs 10h under the conditions of being strictly protected from light, so that BiVO4Powder reaches adsorption-desorption in the solution
Balance.
(3) photocatalysis efficiency is tested.The solution example handled well is placed on illumination degrading MB solution under xenon lamp.During Illumination
In at interval of 20min take a sample, take 10 samples under normal circumstances, and carry out centrifuging and taking supernatant liquor and be put into cuvette,
Use spectrophotometer test sample absorbance, wherein spectrophotometer can be chosen with UV-vis spectrophotometer.
(4) degradation rate is calculated.According to absorbance data, BiVO is calculated4The efficiency of degradation of methylene blue solution.
Preferably, as shown in figure 3, BiVO manufactured in the present embodiment4, the photocatalytic degradation time in 200min, to Asia
Methyl blue solution reaches 84% degradation rate.
Embodiment three
Refer to Fig. 4, Fig. 5 a-5b and Fig. 6, the monoclinic phase that Fig. 4, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
The XRD diagram of octahedra pucherite crystal is truncated；The monocline that Fig. 5 a-5b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
The SEM figure of octahedra pucherite crystal is mutually truncated；The monoclinic phase that Fig. 6, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1:1
The photocatalytic activity versus time curve of octahedra pucherite crystal is truncated.
The present embodiment provides the preparation method that octahedra pucherite crystal is truncated in another monoclinic phase, the present embodiment and implementation
It is in place of the difference of example two:
The 0.5ml Fluorinse of step 2 in embodiment two is substituted for 2ml by the present embodiment；
Corresponding the present embodiment is by the molar ratio of fluorine ion and bismuth ion is 1:4 in the solution A of step 3 in embodiment two
Replacing with the molar ratio of fluorine ion and bismuth ion in solution A is 1:1
In the present embodiment Step 1: step 4 to step 9 with implement two corresponding step just as details are not described herein again.
Preferably, as shown in figure 4, octahedra pucherite crystal (040) crystal face of monoclinic phase manufactured in the present embodiment truncation is strong
Degree is about the 42% of main peak (121) crystal face.
Preferably, as shown in figure 5 a and 5b, octahedra pucherite crystal morphology is truncated in the monoclinic phase of the present embodiment synthesis
Octahedronlike in being truncated, size distribution is more uniform, and crystal grain diameter is about 2 μm, with a thickness of 2 μm.
Preferably, as shown in fig. 6, the BiVO of this implementation preparation4, the photocatalytic degradation time in 200min, to methylene
Base indigo plant solution reaches degradation rate up to 78% degradation rate.
Example IV
Refer to Fig. 7, Fig. 8 a-8b and Fig. 9, the monocline that Fig. 7, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
The XRD diagram of octahedra pucherite crystal is mutually truncated；Fig. 8 a-8b, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
The SEM figure of octahedra pucherite crystal is truncated in monoclinic phase；Fig. 9, which is the molar ratio of fluorine ion and bismuth ion, to be prepared when being 1.5:1
The photocatalytic activity versus time curve of octahedra pucherite crystal is truncated in monoclinic phase.
The present embodiment provides the preparation method that octahedra pucherite crystal is truncated in another monoclinic phase, the present embodiment and implementation
It is in place of the difference of example two:
The 0.5ml Fluorinse of step 2 in embodiment two is substituted for 3ml by the present embodiment；
Corresponding the present embodiment is by the molar ratio of fluorine ion and bismuth ion is 1:4 in the solution A of step 3 in embodiment two
Replacing with the molar ratio of fluorine ion and bismuth ion in solution A is 1.5:1
In the present embodiment Step 1: step 4 to step 9 with implement two corresponding step just as details are not described herein again.
Preferably, as shown in fig. 7, octahedra pucherite crystal (040) crystal face of monoclinic phase manufactured in the present embodiment truncation is strong
Degree is the 43.9% of main peak (121) crystal face.
Preferably, as figures 8 a and 8 b show, octahedra pucherite crystal morphology is truncated in the monoclinic phase of the present embodiment synthesis
Octahedronlike in being truncated, size is unevenly distributed, and big crystal grain diameter is about 8 μm, and it is about 3 compared with little crystal grain diameter that thickness, which is about 5 μm,
μm, with a thickness of 2 μm.
Preferably, as shown in figure 9, BiVO manufactured in the present embodiment4, the photocatalytic degradation time in 200min, to Asia
Methyl blue solution reaches degradation rate up to 74% degradation rate.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (10)
1. the preparation method that octahedra pucherite crystal is truncated in a kind of monoclinic phase characterized by comprising
The fluoride solution of 0.5ml~4ml is added in nitric acid solution step 1, prepares solution D；Wherein, in the fluorine ion
In solution, the concentration of fluorine ion is 0.5mol/L；
Five water bismuth nitrate of 1mmol is dissolved in the solution D by step 2, prepares solution A；
The ammonium metavanadate of 0.75mmol~2mmol is dissolved in sodium hydroxide solution by step 3, prepares solution B；
Step 4 in solution A described in the solution B, will stir 10min~20min, preparation solution C；
Step 5 handles the solution C, obtains the monoclinic phase and octahedra pucherite crystal is truncated.
2. preparation method according to claim 1, which is characterized in that before step 1, further includes:
Step 1X, 1ml~2ml concentrated nitric acid is mixed with 18ml~20ml deionized water, prepares the nitric acid solution.
3. preparation method according to claim 1, which is characterized in that before step 3, further includes:
Step 3X, the standard caustic soda solution of 1ml~2ml is mixed with the deionized water of 20ml~25ml, prepares the hydrogen
Sodium hydroxide solution；Wherein, the standard caustic soda solution concentration is 1mol/L.
4. preparation method according to claim 1, which is characterized in that step 5 includes:
Step 51 pours into the solution C in micro-wave diminishing pot, 100 DEG C~190 DEG C at a temperature of, pass through microwave-hydrothermal method
30min~4h is reacted, sample solution is prepared；
Step 52, the filtering sample solution, obtain sediment, and the sediment is cleaned with dehydrated alcohol, obtain
Sample crystals；
The Sample crystals are put into drying box by step 53,50 DEG C~80 DEG C at a temperature of, dry 10h-12h obtains institute
It states monoclinic phase and octahedra pucherite crystal is truncated.
5. preparation method according to claim 1, which is characterized in that the five water bismuth nitrate purity is to analyze pure AR, institute
Ammonium metavanadate purity is stated to analyze pure AR.
6. preparation method according to claim 1, which is characterized in that the solution A is clear solution.
7. preparation method according to claim 1, which is characterized in that the solution B is clear solution.
8. preparation method according to claim 1, which is characterized in that the solution C orange solution.
9. preparation method according to claim 1, which is characterized in that cleaning way is ultrasonic cleaning；Wherein, wash number
It is 3 times.
10. preparation method according to claim 1, which is characterized in that octahedra pucherite crystal is truncated in the monoclinic phase
For glassy yellow powder.
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