CN107098388A - A kind of preparation method of open-type bismuth oxide hollow ball - Google Patents
A kind of preparation method of open-type bismuth oxide hollow ball Download PDFInfo
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- CN107098388A CN107098388A CN201710237516.1A CN201710237516A CN107098388A CN 107098388 A CN107098388 A CN 107098388A CN 201710237516 A CN201710237516 A CN 201710237516A CN 107098388 A CN107098388 A CN 107098388A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of preparation method of open-type bismuth oxide hollow ball.Ethanol and ethylene glycol are first configured to mixed solvent, bismuth salt is dissolved in the mixed solvent again and obtains the bismuth salt solution that molar concentration is 0.05 0.10mol/L, then bismuth salt solution is placed in and carries out the 6h of solvent thermal reaction 3 in 160 180 DEG C under confined conditions, be centrifuged, wash and drying process obtains bismuth oxide presoma；Bismuth oxide presoma is placed in Muffle furnace 250 300 DEG C of 2 3h of calcining are warming up to 23 DEG C/min heating rate, removed organic ligand and solvent obtains open-type bismuth oxide hollow ball.The present invention is with simple and easy to do, required equipment is few, preparation cost is low and is easily achieved industrialized feature, is a kind of environment-friendly green synthesis method not using strong acid and strong base and poisonous reaction raw materials.
Description
Technical field
The invention belongs to the synthesis technical field of nano material, and in particular to a kind of preparation of open-type bismuth oxide hollow ball
Method.
Background technology
Bismuth（Bi）It is unique heavy metal element for having the characteristics such as cheaper, low toxicity and low-activity concurrently in nature.By
In unique " green " property, many bismuth compounds are used widely in fields such as medicine, electronics, organic synthesis, catalysis.Bismuth
The valence band of oxide（VB）Be not only to be made up of O2p tracks, but formed by Bi6s and O2p orbital hybridizations, Bi6s tracks with
The strong interaction of O2p tracks reduces its symmetry, so as to produce the dipole of correlation, this makes it have higher oxidation and lived
Property and charge mobility, so that with higher photocatalytic activity.
Bismuth oxide（Bi2O3）Be a kind of band gap be 2.0-3.6eV p-type semiconductor, its specific bandwidth depend on phase structure,
Pattern and crystallite dimension.Research shows that crystal formation and pattern are to Bi2O3Photocatalytic activity have decisive influence.Bi2O3Mainly have
Monoclinic phase α-Bi2O3, Tetragonal β-Bi2O3, body Emission in Cubic γ-Bi2O3With face Emission in Cubic δ-Bi2O3Four kinds of crystalline phases, wherein, α and δ
It is respectively mutually low temperature and high-temperature stable phase, other two-phases are high temperature metastable phase.General β-Bi2O3Photocatalytic activity highest, but it
Belong to metastable type, easily change into α-Bi2O3, it is not easily-synthesized.
Nanometer material structure is to influence the key factor of its property, and catalytic activity is except the bandgap structure with material itself
It is relevant, it is also closely related with its pattern.The change of pattern can cause a series of changes of particle size, band-gap energy and specific surface area
Change, and extreme influence is to the utilization rate of incident light.Hollow structure material wall thickness is nanoscale, and internal cavities proportion is very big,
With density is low, specific surface area is high, thermal coefficient of expansion is low and the low characteristic of refractive index, catalysis, gas sensing, energy storage and
Had a good application prospect in terms of medicine controlled releasing.The controlledly synthesis of hollow ball is always the research heat of field of functional materials
Point, however, on nanometer Bi2O3The preparation of hollow ball and its rare report of the application in terms of catalysis and medicine controlled releasing.
The content of the invention
It is an object of the invention to provide a kind of simple and easy to do, raw material it is green, prepare with low cost and be easily achieved industry
The preparation method of the open-type bismuth oxide hollow ball of change.
It is of the invention to adopt the following technical scheme that to achieve the above object, a kind of preparation side of open-type bismuth oxide hollow ball
Method, it is characterised in that concretely comprise the following steps：
Step（1）, ethanol and ethylene glycol first are configured into mixed solvent, then bismuth salt is dissolved in into the mixed solvent obtain molar concentration
For 0.05-0.10mol/L bismuth salt solution, then bismuth salt solution is placed in and carries out solvent heat in 160-180 DEG C under confined conditions
3-6h is reacted, is centrifuged, washs and drying process obtains bismuth oxide presoma；
Step（2）, bismuth oxide presoma is placed in and is warming up to 250-300 DEG C with 2-3 DEG C/min heating rate in Muffle furnace and forges
2-3h is burnt, organic ligand is removed and solvent obtains open-type bismuth oxide hollow ball.
Further preferably, step（1）In the mixed solvent ethanol and ethylene glycol volume ratio be 1:1-2, wherein ethanol make
For solvent, ethylene glycol is used as complexant.
Further preferably, step（1）Bismuth salt be five water bismuth nitrates or bismuth chloride.
Further preferably, step（1）Precipitation after centrifugation is alternately washed using deionized water and absolute ethyl alcohol, is dried
Processing procedure is progress under 60-70 DEG C of vacuum condition.
Further preferably, step（2）The particle diameter of obtained open-type bismuth oxide hollow ball is 1-1.5 μm, and wall thickness is 10-
50nm, specific surface area is more than 16m2/g。
Further preferably, step（2）The crystalline phase of the obtained hollow bismuth oxide of open-type is Tetragonal β-Bi2O3。
The present invention has the advantages that compared with prior art：
1st, the present invention is prepared for β-Bi first2O3Nano-hollow ball, the hollow ball belongs to nano level hollow ball, size uniform,
Good dispersion, specific surface area is larger, highly stable, especially its internal cavities and bigger serface under normal temperature and in the aqueous solution,
Add the avtive spot of catalytic reaction, hollow-core construction can also improve refraction of the light in hollow ball, order of reflection, improve light
Utilization ratio, it is seen that optical absorption substantially, be a kind of new photocatalysis and photovoltaic material.Further, since the present invention
Hollow ball has larger specific surface area relative to traditional material, it may also be used for battery, gas sensing, bio-imaging, medicine are born
In terms of load；
2nd, the present invention proposes hot be combined with temperature programmed control calcination method of no templating solvent and prepares metal oxide nano hollow ball
New method.The method has that simple and easy to do, required equipment is few, it is with low cost to prepare and is easily achieved industrialized feature, does not have
Have using strong acid and strong base and poisonous reaction raw materials, be a kind of environment-friendly green synthesis method.
Brief description of the drawings
Fig. 1 is the SEM photograph of open-type bismuth oxide hollow ball made from the embodiment of the present invention 1；
Fig. 2 is the XRD spectrum of open-type bismuth oxide hollow ball made from the embodiment of the present invention 1；
Fig. 3 is the UV-Vis DRS collection of illustrative plates of open-type bismuth oxide hollow ball made from the embodiment of the present invention 1；
Fig. 4 is the N of open-type bismuth oxide hollow ball made from the embodiment of the present invention 12Adsorption-desorption curve.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
With 60mL ethanol-ethylene glycol mixed solution（Wherein the volume ratio of ethanol and ethylene glycol is 1:2）It is used as mixed solvent, room temperature
2.9100g Bi (NO are added after lower magnetic agitation 0.5h3)3•5H2O, stirring 1h makes bismuth nitrate be completely dissolved to form settled solution.
Then solution is moved into 100mL hydrothermal reaction kettles, is put into baking oven in 160 DEG C of isothermal reaction 4h, naturally cools to room temperature, from
The heart collects precipitation, and alternately washing for several times, Bi is obtained then at 60 DEG C of vacuum drying with deionized water and absolute ethyl alcohol2O3Presoma.
300 DEG C of calcining 2h are finally warming up to 2 DEG C/min heating rate in Muffle furnace and obtain yellow Bi2O3Hollow ball.
Fig. 1 is the stereoscan photograph of sample obtained by the present embodiment, as seen from Figure 1, and product is open-type hollow ball,
Uniform particle sizes, good dispersion, particle diameter is 1-1.5mm, and wall thickness is 10-50nm.
Fig. 2 is the XRD spectrum of sample obtained by the present embodiment, as can be seen from Figure 2, product diffraction maximum and standard card 27-0050
Fit like a glove, it was demonstrated that the prepared material of the present invention is pure Tetragonal β-Bi2O3。
Fig. 3 is the diffusing reflection collection of illustrative plates of sample obtained by the present embodiment, and the ABSORPTION EDGE of sample is estimated in 540nm by Tauc equations
Calculation band gap is 2.4eV, shows that product has preferable visible absorption.
Fig. 4 is the N of sample obtained by the present embodiment2Adsorption-desorption curve, as can be seen from Figure 4 product belong to mesoporous material, compare table
Area is more than 16m2/ g, its mesoporous and cavity structure can provide communication channel for molecule.
Embodiment 2
With 60mL ethanol-ethylene glycol mixed solution（Wherein the volume ratio of ethanol and ethylene glycol is 1:1）It is used as mixed solvent, room temperature
1.4550g Bi (NO are added after lower magnetic agitation 0.5h3)3•5H2O, stirring 1h makes bismuth nitrate be completely dissolved to form settled solution.
Then solution is moved into 100mL hydrothermal reaction kettles, is put into baking oven in 180 DEG C of isothermal reaction 3h, naturally cools to room temperature, centrifuged
Precipitation is collected, and alternately washing for several times, Bi is obtained then at 60 DEG C of vacuum drying 12h with deionized water and absolute ethyl alcohol2O3Forerunner
Body.250 DEG C of calcining 3h are finally warming up to 2 DEG C/min heating rate in Muffle furnace and obtain yellow Bi2O3Hollow ball.
Embodiment 3
By 0.9460g BiCl3It is added to 60mL ethanol-ethylene glycol mixed solution（Wherein the volume ratio of ethanol and ethylene glycol is 1:
1）In, stirring at room temperature makes to be completely dissolved to form settled solution.Then solution is moved into 100mL hydrothermal reaction kettles, is put into baking
Case naturally cools to room temperature in 180 DEG C of isothermal reaction 6h, precipitation is collected by centrifugation, and alternately washed with deionized water and absolute ethyl alcohol
Wash for several times, Bi is obtained then at 60 DEG C of vacuum drying 12h2O3Presoma.Finally with 3 DEG C/min heating rate liter in Muffle furnace
Temperature calcines 3h to 250 DEG C and obtains yellow Bi2O3Hollow ball.
Embodiment 4
By 1.8920g BiCl3It is added to 60mL ethanol-ethylene glycol mixed solution（Wherein the volume ratio of ethanol and ethylene glycol is 1:
2）In, stirring at room temperature makes to be completely dissolved to form settled solution.Then solution is moved into 100mL hydrothermal reaction kettles, is put into baking
Case naturally cools to room temperature in 160 DEG C of isothermal reaction 4h, precipitation is collected by centrifugation, and alternately washed with deionized water and absolute ethyl alcohol
Wash for several times, Bi is obtained then at 70 DEG C of vacuum drying2O3Presoma.Finally it is warming up in Muffle furnace with 2 DEG C/min heating rate
300 DEG C of calcining 2h obtain yellow Bi2O3Hollow ball.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (6)
1. a kind of preparation method of open-type bismuth oxide hollow ball, it is characterised in that concretely comprise the following steps：
Step（1）, ethanol and ethylene glycol first are configured into mixed solvent, then bismuth salt is dissolved in into the mixed solvent obtain molar concentration
For 0.05-0.10mol/L bismuth salt solution, then bismuth salt solution is placed in and carries out solvent heat in 160-180 DEG C under confined conditions
3-6h is reacted, is centrifuged, washs and drying process obtains bismuth oxide presoma；
Step（2）, bismuth oxide presoma is placed in and is warming up to 250-300 DEG C with 2-3 DEG C/min heating rate in Muffle furnace and forges
2-3h is burnt, organic ligand is removed and solvent obtains open-type bismuth oxide hollow ball.
2. the preparation method of open-type bismuth oxide hollow ball according to claim 1, it is characterised in that：Step（1）It is mixed
The volume ratio of ethanol and ethylene glycol is 1 in bonding solvent:1-2, wherein ethanol are used as complexant as solvent, ethylene glycol.
3. the preparation method of open-type bismuth oxide hollow ball according to claim 1, it is characterised in that：Step（1）Middle bismuth
Salt is five water bismuth nitrates or bismuth chloride.
4. the preparation method of open-type bismuth oxide hollow ball according to claim 1, it is characterised in that：Step（1）Centrifugation
Precipitation after separation is alternately washed using deionized water and absolute ethyl alcohol, and drying process process is to enter under 60-70 DEG C of vacuum condition
OK.
5. the preparation method of open-type bismuth oxide hollow ball according to claim 1, it is characterised in that：Step（2）Obtain
The particle diameter of open-type bismuth oxide hollow ball be 1-1.5 μm, wall thickness is 10-50nm, and specific surface area is more than 16m2/g。
6. the preparation method of open-type bismuth oxide hollow ball according to claim 1, it is characterised in that：Step（2）Obtain
The hollow bismuth oxide of open-type crystalline phase be Tetragonal β-Bi2O3。
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| CN201710237516.1A CN107098388A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of open-type bismuth oxide hollow ball |
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| CN201710237516.1A CN107098388A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of open-type bismuth oxide hollow ball |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888206A (en) * | 2019-01-23 | 2019-06-14 | 江苏理工学院 | A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754837A (en) * | 2013-12-17 | 2014-04-30 | 武汉工程大学 | Method for preparation of bismuth-containing nano-hollow ball by using porous bismuth oxide as template |
-
2017
- 2017-04-12 CN CN201710237516.1A patent/CN107098388A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754837A (en) * | 2013-12-17 | 2014-04-30 | 武汉工程大学 | Method for preparation of bismuth-containing nano-hollow ball by using porous bismuth oxide as template |
Non-Patent Citations (2)
| Title |
|---|
| YUNHUI YAN等: "A controlled anion exchange strategy to synthesize core-shell b-bismuth oxide/bismuth sulfide hollow heterostructures with enhanced visible-light photocatalytic activity", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| YUNHUI YAN等: "Template-free fabrication of a- and b-Bi2O3 hollow spheres and their visible light photocatalytic activity for water purification", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888206A (en) * | 2019-01-23 | 2019-06-14 | 江苏理工学院 | A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application |
| CN109888206B (en) * | 2019-01-23 | 2021-09-28 | 江苏理工学院 | Lithium ion battery cathode material Bi/Bi2O3C, preparation and application thereof |
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