CN103420414B - Solvothermal preparation method of bismuth trioxide microspheres and application thereof - Google Patents
Solvothermal preparation method of bismuth trioxide microspheres and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of inorganic nanomaterials and environmental materials, and relates to a solvothermal preparation method of bismuth trioxide microspheres and application thereof. The solvothermal preparation method of the bismuth trioxide microspheres adopts the technical steps as follows: dissolving soluble bismuth salt into ethylene glycol and dissolving soluble indium salt and urea into ethanol respectively; performing ultrasonic agitation and uniformly mixing, and obtaining a precursor through solvothermal reaction; centrifugally washing and drying the precursor, and roasting the precursor at high temperature to prepare the bismuth trioxide microspheres. The bismuth oxide (Bi2O3) microspheres with relatively uniform morphology are prepared at a low temperature through the solvothermal reaction by a liquid-phase method, the morphology thereof is a microspherical structure, and the diameter thereof is about 1-2 microns. When the bismuth trioxide microspheres prepared according to the solvothermal preparation method method can be applied to optical degradation of tetracycline-containing wastewater, and have the advantages of high chemical stability and the like. The solvothermal preparation method is simple in process and high in repeatability; used raw materials meet environment-friendly requirements; and by the solvothermal preparation method, mass production can be facilitated.
Description
Technical field
The invention belongs to inorganic nano material and technical field of environmental material preparation, relate to the preparation method of bismuthous oxide bismuth trioxide micron ball, particularly relate to a kind of solvent-thermal method and prepare bismuthous oxide bismuth trioxide micron ball and application thereof.
Background technology
Current microbiotic is widely used in the control of the disease such as mankind's Perceived control infectious diseases and poultry, domestic animal, crop, but because antibiotic screening and the aspect such as production, strain improvement still exist technological difficulties, thus to there is in waste water the problems such as residual antibiotic content is high, great pollution is caused to environment.Therefore be the removal of the antibiotic substance of representative with tsiklomitsin, become a scientific research difficult problem urgently to be resolved hurrily.
Bismuthous oxide bismuth trioxide is the important p-type semiconductor material of a class, mainly contains α, β, γ and δ tetra-kinds of crystal formations, and crystal formation is different, and its application is also different.The band gap width of bismuthous oxide bismuth trioxide is 2.7 ~ 2.8eV, and absorbing wavelength is longer.Bismuthous oxide bismuth trioxide is widely used in mineral dye, optical material, electronic material, superconducting material and catalyzer etc., and its application and development prospect is very wide.
Summary of the invention
One object of the present invention is to adopt low temperature liquid polymerization process through solvent thermal reaction, discloses a kind of technique simple, bismuthous oxide bismuth trioxide (Bi of good performance
2o
3) preparation method of micron ball.
A kind of solvent-thermal method prepares bismuthous oxide bismuth trioxide micron ball, its technical scheme respectively soluble bismuth salt is dissolved in ethylene glycol, solubility indium salt and urea are dissolved in dehydrated alcohol, after ultrasonic agitation mixes, obtain precursor through solvent thermal reaction, precursor centrifuge washing is prepared from through high-temperature roasting after drying.
Solvent-thermal method disclosed in this invention prepares bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take soluble bismuth salt, ultrasonic agitation is dissolved in ethylene glycol, and form bismuth salt ethylene glycol solution, described soluble bismuth salt is 0.1 ~ 1.0 mmol:5 ~ 30 mL with the molecular volume ratio of ethylene glycol;
B, take solubility indium salt and urea respectively, magnetic agitation is dissolved in dehydrated alcohol, form the mixed ethanol solution of indium salt and urea, described solubility indium salt: urea: the molecular volume ratio of dehydrated alcohol is 0.1 ~ 1.0 mmol:5 ~ 30, mmol:0.1 ~ 1.0 mL;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to 100 ~ 180 DEG C of constant temperature 12 ~ 36 h, naturally cooling, obtains solvent thermal product;
E, the solvent thermal product deionized water of step D gained and dehydrated alcohol are washed three times respectively, at 60 ~ 80 DEG C of air drying 6 ~ 12h after centrifugation, obtain precursor;
F, by the precursor of step e gained roasting 60 ~ 180min under retort furnace 350 ~ 550 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
Soluble bismuth salt of the present invention is any one or several in Bismuth trinitrate, bismuth chloride, bismuth citrate and bismuth sulfate.
Solubility indium salt of the present invention is any one or several in indium nitrate, indium chloride and indium sulfate.
In reaction process of the present invention, solubility indium salt plays pattern inducing action in the forming process of bismuth oxide, and urea has gas to produce in heat-processed, so can be formed spherical; Have impurity in solvent thermal product to produce, by deionized water and washing with alcohol, the inorganic and organic impurity be dissolved in wherein can be washed away, finally by x-ray diffraction pattern determination final product whether pure phase.
Bismuthous oxide bismuth trioxide (Bi in the present invention
2o
3) structure of micron ball determined do not have the peak of other materials in x-ray diffraction pattern by x-ray diffractometer, this collection of illustrative plates shows, the bismuthous oxide bismuth trioxide (Bi prepared by solvent-thermal method
2o
3) be pure phase bismuthous oxide bismuth trioxide (Bi
2o
3), itself and standard bismuthous oxide bismuth trioxide (Bi
2o
3) card (27-0050) matches.
Field emission scanning electron microscope (SEM) test shows, at room temperature, and the bismuthous oxide bismuth trioxide (Bi prepared by solvent-thermal method
2o
3) micron ball diameter is about 1 ~ 2 μm.
Another object of the present invention is by preparation-obtained bismuthous oxide bismuth trioxide (Bi according to the method described above
2o
3) micron ball is applied to photodegradation containing tetracycline wastewater.
Photocatalytic activity evaluation:
Carry out in GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), be that 20 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then add the bismuthous oxide bismuth trioxide (Bi obtained by the embodiment of the present invention 1
2o
3) micron ball 0.1 g, magnetic stirring apparatus reaction 30min is used in darkroom, sampling is started after reaching reactive adsorption balance, then open aerating apparatus and open xenon source, it is keep catalyzer to be in suspension or afloat that aeration passes into air object, at interval of 10 min samplings in Xenon light shining process, get supernatant liquid after centrifugation at tsiklomitsin maximum absorption wavelength λ
max=357 nm places, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A
0] × 100% calculates photodegradation rate, wherein A
0the absorbancy of tetracycline during for reaching adsorption equilibrium, A
ifor the absorbancy of the tetracycline that timing sampling measures.
Bismuthous oxide bismuth trioxide (Bi prepared by the embodiment of the present invention 1
2o
3) micron ball when visible ray illumination 1h to the degradation rate of tsiklomitsin up to 91.07%.
The present invention's reagent used is analytical pure, does not purify further in reaction process.
beneficial effect
Utilize the bismuthous oxide bismuth trioxide (Bi prepared by simple solvent thermal reaction
2o
3), pattern is spherical micrometer structure, and this material has good chemical stability.Present invention process is simple, favorable reproducibility, and cheap and easy to get, cost is low, meets environmental friendliness requirement, is convenient to batch production.Bismuthous oxide bismuth trioxide (the Bi that the present invention is obtained
2o
3) micron ball photocatalyst, degradation efficiency is higher, during visible ray illumination 1h to the degradation rate of tsiklomitsin up to 91.07%.
Accompanying drawing explanation
Fig. 1 embodiment 1 obtains bismuthous oxide bismuth trioxide (Bi
2o
3) the X-ray diffraction analysis figure (XRD) of micron ball.
Fig. 2 embodiment 1 obtains bismuthous oxide bismuth trioxide (Bi
2o
3) scanning electron microscope (SEM) photograph (SEM) of micron ball.
Fig. 3 embodiment 1 obtains bismuthous oxide bismuth trioxide (Bi
2o
3) the photodegradation figure of micron ball.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 0.5 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.1 mmoL In (NO respectively
3)
34.5H
2o and 0.1mmoL urea, magnetic agitation makes it be dissolved in 5 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 350 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
Bismuthous oxide bismuth trioxide (Bi
2o
3) micron ball visible light source irradiate under as follows to the degradation experiment step of tsiklomitsin:
Photocatalytic activity evaluation: carry out in GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), be that 20 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then add the bismuthous oxide bismuth trioxide (Bi of this solvent thermal reaction
2o
3) photocatalyst 0.1 g, magnetic stirring apparatus reaction 30min is used in darkroom, sampling is started after reaching reactive adsorption balance, then open aerating apparatus and open xenon source, it is keep catalyzer to be in suspension or afloat that aeration passes into air object, at interval of 10 min samplings in Xenon light shining process, supernatant liquid is got at tsiklomitsin maximum absorption wavelength λ max=357 nm place after centrifugation, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A
0] × 100% calculates photodegradation rate, wherein A
0the absorbancy of tetracycline during for reaching adsorption equilibrium, A
ifor the absorbancy of the tetracycline that timing sampling measures.
Bismuthous oxide bismuth trioxide (Bi
2o
3) micron ball XRD figure spectrum see accompanying drawing 1, accompanying drawing 2 is shown in product morphology analysis, and photocatalysis effect is shown in accompanying drawing 3.
In accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (27-0050) matches, and do not have other diffraction to mix peak in XRD figure spectrum, the bismuthous oxide bismuth trioxide (Bi prepared under solvent thermal condition that the present invention proposes is described
2o
3) thing of micron ball is pure mutually.
In accompanying drawing 2, field emission scanning electron microscope (SEM) test shows, at room temperature, and the bismuthous oxide bismuth trioxide (Bi prepared by solvent-thermal method
2o
3) micron ball diameter is about 1 ~ 2 μm.
In accompanying drawing 3, photocatalysis effect figure demonstrates prepared bismuthous oxide bismuth trioxide (Bi
2o
3) micron ball reaches 91.07% to the degradation rate of tsiklomitsin under visible light source.
embodiment 2
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 5.0 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 30 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 1.0 mmoL In (NO respectively
3)
34.5H
2o and 1.0mmoL urea, magnetic agitation makes it be dissolved in 30 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 100 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 550 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 3
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 0.5 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.1 mmoL In (NO respectively
3)
34.5H
2o and 1.0mmoL urea, magnetic agitation makes it be dissolved in 30 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 120 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 550 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 4
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 5.0 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 30 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 1.0 mmoL In (NO respectively
3)
34.5H
2o and 0.1mmoL urea, magnetic agitation makes it be dissolved in 5 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 140 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 180min under retort furnace 350 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 5
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 1.0 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 10 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.5 mmoL In (NO respectively
3)
34.5H
2o and 0.8mmoL urea, magnetic agitation makes it be dissolved in 25 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 160 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 400 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 6
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 3.0 mmoL
3)
35H
2o, ultrasonic agitation is dissolved in 25mL ethylene glycol solution, forms bismuth nitrate solution;
B, take 0.2 mmoL In (NO respectively
3)
34.5H
2o and 0.5mmoL urea, magnetic agitation makes it be dissolved in 10 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 180min under retort furnace 400 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 7
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the BiCl of 1.0 mmoL
3, ultrasonic agitation is dissolved in 15mL ethylene glycol solution, forms bismuth chloride solution;
B, take 0.2 mmoL InCl respectively
34H
2o and 0.8 mmoL urea, magnetic agitation makes it be dissolved in 25 mL second anhydrous alcohol solutions, forms the mixing solutions of indium chloride and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 12 h at 160 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 80 DEG C of air drying 12h, obtains precursor;
F, by the precursor of step e gained roasting 180min under retort furnace 450 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 8
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take 2.0 mmoL C
6h
5biO
7, ultrasonic agitation is dissolved in 10mL ethylene glycol solution, forms bismuth citrate solution;
B, take 0.2 mmoL In respectively
2(SO
4)
34H
2o and 0.8 mmoL urea, magnetic agitation makes it be dissolved in 20 mL ethanol solutions, forms the mixing solutions of indium nitrate and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 120 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 70 DEG C of air drying 10h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 450 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 9
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi of 1.5 mmoL
2(SO
4)
3, ultrasonic agitation is dissolved in 25mL ethylene glycol solution, forms bismuth sulfate solution;
B, take 0.2 mmoLInCl respectively
34H
2o and 1.0 mmoL urea, magnetic agitation makes it be dissolved in 10 mL ethanol solutions, forms the mixing solutions of indium chloride and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 160 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 10h, obtains precursor;
F, by the precursor of step e gained roasting 180min under retort furnace 400 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 10
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the Bi (NO of 0.25 mmoL respectively
3)
35H
2o, and the BiCl of 0.25mmol
3, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms soluble bismuth salts solution;
B, take 0.05 mmoL In (NO respectively
3)
34.5H
2o, 0.05mmolIn
2(SO
4)
34H
2o and 0.1mmoL urea, magnetic agitation makes it be dissolved in 5 mL ethanol solutions, forms the mixing solutions of solubility indium salt and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 350 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
embodiment 11
A kind of bismuthous oxide bismuth trioxide (Bi
2o
3) preparation method of micron ball, be carry out according to following step:
A, take the BiCl of 0.25mmol
3with 0.25mmol C
6h
5biO
7, ultrasonic agitation is dissolved in 10 mL ethylene glycol solutions, forms soluble bismuth salts solution;
B, take 0.25 mmoL In respectively
2(SO
4)
34H
2o, 0.25mmolInCl
34H
2o and 0.8mmoL urea, magnetic agitation makes it be dissolved in 25 mL ethanol solutions, forms the mixing solutions of solubility indium salt and urea;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to constant temperature 24 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, wash three times respectively with deionized water and dehydrated alcohol, the product after centrifugation, at 60 DEG C of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under retort furnace 400 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide (Bi that pattern is homogeneous can be obtained
2o
3) micron ball.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (3)
1. solvent-thermal method prepares bismuthous oxide bismuth trioxide micron ball, respectively soluble bismuth salt is dissolved in ethylene glycol, solubility indium salt and urea are dissolved in dehydrated alcohol, after ultrasonic agitation mixes, precursor is obtained through solvent thermal reaction, precursor centrifuge washing is prepared from through high-temperature roasting after drying, and it is characterized in that, carries out according to following step:
A, take soluble bismuth salt, ultrasonic agitation is dissolved in ethylene glycol, and form bismuth salt ethylene glycol solution, described soluble bismuth salt is 0.1 ~ 1.0 mmol:5 ~ 30 mL with the molecular volume ratio of ethylene glycol;
B, take solubility indium salt and urea respectively, magnetic agitation is dissolved in dehydrated alcohol, form the mixed ethanol solution of indium salt and urea, described solubility indium salt: urea: the molecular volume ratio of dehydrated alcohol is 0.1 ~ 1.0 mmol:5 ~ 30, mmol:0.1 ~ 1.0 mL;
C, the solution described in step B is added in the solution of steps A, then magnetic agitation 30 min;
D, be transferred in teflon-lined reactor by the mixed system of step C gained, be warmed up to 100 ~ 180 DEG C of constant temperature 12 ~ 36 h, naturally cooling, obtains solvent thermal product;
E, the solvent thermal product deionized water of step D gained and dehydrated alcohol are washed three times respectively, at 60 ~ 80 DEG C of air drying 6 ~ 12h after centrifugation, obtain precursor;
F, by the precursor of step e gained roasting 60 ~ 180min under retort furnace 350 ~ 550 DEG C of air atmospheres, the bismuthous oxide bismuth trioxide micron ball that pattern is homogeneous can be obtained.
2. solvent-thermal method according to claim 1 prepares bismuthous oxide bismuth trioxide micron ball, it is characterized in that, described soluble bismuth salt is any one or several in Bismuth trinitrate, bismuth chloride, bismuth citrate and bismuth sulfate.
3. solvent-thermal method according to claim 1 prepares bismuthous oxide bismuth trioxide micron ball, it is characterized in that, described solubility indium salt is any one or several in indium nitrate, indium chloride and indium sulfate.
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| CN114944288B (en) * | 2022-06-20 | 2023-04-25 | 江西科技师范大学 | Flower-like bismuth trioxide, preparation method and application thereof, and prepared electrode |
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