CN104591264A - Indium oxide nanosphere and preparation method thereof - Google Patents
Indium oxide nanosphere and preparation method thereof Download PDFInfo
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- CN104591264A CN104591264A CN201510063412.4A CN201510063412A CN104591264A CN 104591264 A CN104591264 A CN 104591264A CN 201510063412 A CN201510063412 A CN 201510063412A CN 104591264 A CN104591264 A CN 104591264A
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- indium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- 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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- 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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- 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
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/90—Other properties not specified above
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Abstract
The invention relates to the technical field of preparation of inorganic nanomaterials and particularly relates to an indium oxide nanosphere and a preparation method thereof. The invention aims at solving the problems of complex preparation process, high synthesis temperature and long reaction time of the existing preparation method of the indium oxide nanosphere and simultaneously providing a low-cost indium oxide nanosphere material. The preparation method of the indium oxide nanosphere comprises the following steps: firstly, preparing a mixed solution of indium nitrate and urea, adding ethanol and/or ethylene glycol, dissolving and magnetically stirring to obtain a homogeneous colorless transparent solution; secondly, reacting the colorless transparent solution by a solvothermal method and collecting a solvothermal product; thirdly, centrifuging and washing the solvothermal product to obtain an indium hydroxide precursor; and fourthly, carrying out high-temperature roasting to obtain the indium oxide nanosphere. The preparation method has the advantages of simple process, less reactants, low synthesis temperature, short reaction time and low obtained product cost, and can be widely applied.
Description
Technical field
The invention belongs to technical field of inorganic nano-material preparation, relate to Indium sesquioxide (In
2o
3) preparation, particularly relate to a kind of Indium sesquioxide nanometer ball and preparation method thereof.
Background technology
Nano indium oxide (In
2o
3) be the important special n N-type semiconductorN material of a class, its band gap width is 3.6 ~ 3.75eV, there is high conductivity and visible light transmissivity, and Indium sesquioxide has a wide range of applications in fields such as chemistry, bio-sensing, solar cell, photochemical catalysis, photoelectron and flat-panel monitors.The preparation method of Indium sesquioxide mainly contains vapor phase process, solid phase method and liquid phase method.The requirement of vapor phase process to device parameter is higher, and productive rate is lower, can not be used for industrial mass production; The nanoparticle granularity that solid phase method obtains is general not too homogeneous, and its application is also restricted.What current application was wider is liquid phase method, because liquid phase method is temperature required not high, is conducive to scale operation.
Liquid phase method mainly comprises the precipitator method and the hot method of hydrothermal/solvent in current bibliographical information, and current solvent-thermal method application is comparatively general, with " Solvothermal synthesis of N-doped
ceO 2 microspheres with visible light-driven photocatalytic activity " be example, in its document, synthetic nitrogen adulterates
ceO 2 micron ball adopts solvent-thermal method, prepared by this method
ceO 2 have and degrade under the visible ray of rhodamine 6G a tetrafluoro borate
;such as document " Solvothermal synthesis and photocatalytic performance of again
mn 4+ -doped anatase nanoplates with exposed 001} facets ", the document is also adopt solvent-thermal method preparation
mn 4+ the anatase octahedrite of doping.Current solvent-thermal method is apply very wide method preparing in nano material.
Now, nanomaterials and nanotechnology gradually for solving the energy and environment, and achieves good effect.The pollutent that nano semiconductor material is widely used in catalyzed degradation water because having good photocatalytic activity.The structure and morphology of nano material and size regulation and control attract the extensive concern of investigators always, and object makes material property more excellent.
Summary of the invention
One object of the present invention is, solves complicated process of preparation in current Indium sesquioxide nanometer ball preparation method, synthesis temperature is higher, the reaction times is longer problem.
Another object of the present invention is, the Indium sesquioxide nanometer ball material providing a kind of cost low.
In order to achieve the above object, technical scheme of the present invention is:
A preparation method for Indium sesquioxide nanometer ball, comprises the steps: successively
Step one: prepare analytically pure indium nitrate and urea mixing solutions, described 1 mmole indium nitrate mixes with the urea of 1 ~ 5 mmole, and add 35ml dissolution with solvents, described solvent is ethanol and/or ethylene glycol, makes uniform colorless clear solution after magnetic agitation;
Step 2: be transferred in hydro-thermal container by described colourless transparent solution, is warming up to 120 ~ 180 DEG C, and heating 1 ~ 12h, collects solvent thermal product after naturally cooling;
Step 3: solvent thermal product is obtained indium hydroxide precursor through washing, drying;
Step 4: described indium hydroxide precursor is obtained Indium sesquioxide nanometer ball through high-temperature roasting.
In described step 3, specifically will prepare the solvent thermal product centrifugation of gained in described step 2, after washing three times respectively with deionized water and dehydrated alcohol, at 60 ~ 80 DEG C of air drying 6 ~ 12 h.
High-temperature roasting in described step 4 refers to will prepare indium hydroxide precursor roasting 60 ~ 240 min under retort furnace 300 ~ 600 DEG C of air atmospheres of gained in described step 3.
The Indium sesquioxide nanometer ball that described preparation method obtains.
What the present invention adopted is solvent-thermal method, and its useful benefit is:
1, technique is simple: because reactant is indium nitrate, providing under alkaline condition namely under urea existent condition, can generate, without the need to other materials under etoh solvent and/or ethylene glycol existent condition;
2, synthesis temperature is lower, and the temperature of solvent-thermal process is no more than 180 degree; Reaction times is shorter, and can generate precursor within the shorter time (several hours), reaction conditions is not harsh;
3, cost is low, and therefore product of the present invention can be widely used in containing in the photodegradation of tetracycline wastewater.
Accompanying drawing explanation
X-ray diffraction analysis (XRD) collection of illustrative plates of Indium sesquioxide of Fig. 1 for preparing with the solvent-thermal method prepared by the present invention;
Fig. 2 is for testing the collection of illustrative plates of gained under the field emission scanning electron microscope (SEM) with the Indium sesquioxide prepared by the present invention;
Fig. 3 is the photocatalysis effect figure with the Indium sesquioxide prepared by the present invention.
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 Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2the urea of O) and 1 mmole, preparation indium nitrate and urea mixing solutions, be dissolved in 35mL ethanol, be configured to uniform colorless clear solution after magnetic agitation;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 1h at 120 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step 2 gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 60 DEG C of air drying 6 h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 60min under retort furnace 300 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer ball.
Indium sesquioxide (In
2o
3) nanometer ball is as follows to the degradation experiment step of tsiklomitsin under xenon source:
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), is that 20 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then adds this Indium sesquioxide (In
2o
3) nanometer ball photocatalyst 0.1 g, use magnetic stirring apparatus to react 1 hour 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: D
c=[(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.
Indium sesquioxide (In
2o
3) nanometer ball XRD figure spectrum see accompanying drawing 1, accompanying drawing 2 is shown in product morphology analysis, and degraded figure is shown in accompanying drawing 3.
In accompanying drawing 1 position of the diffraction peak of day part and relative intensity all with JCPDS(JCPDS) card (06-0416) matches, and do not have other diffraction to mix peak in XRD figure spectrum, and the In that the present invention prepares is described
2o
3thing is pure mutually.
In accompanying drawing 2, field emission scanning electron microscope (SEM) test shows, at room temperature, and the Indium sesquioxide (In prepared by solvent-thermal method
2o
3) diameter is about 400 ~ 800 nm.
In accompanying drawing 3, it is reach 50.72% to the degradation rate of tsiklomitsin under xenon source that photocatalysis effect figure demonstrates prepared Indium sesquioxide nanometer ball.
embodiment 2
A kind of Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2o) with the urea of 5 mmoles, be dissolved in 35mL ethylene glycol, after magnetic agitation, be configured to uniform colorless clear solution;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 12 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step 2 gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 80 DEG C of air drying 12 h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 240min under retort furnace 600 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer ball.
embodiment 3
A kind of Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2o) with the urea of 1 mmole, be dissolved in 20 mL ethanol and 15mL ethylene glycol, after magnetic agitation, be configured to uniform colorless clear solution;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 1 h at 120 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step B gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 80 DEG C of air drying 12 h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 240min under retort furnace 600 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer ball.
embodiment 4
A kind of Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2o) with the urea of 5 mmoles, be dissolved in 20 mL ethanol and 15mL ethylene glycol, after magnetic agitation, be configured to uniform colorless clear solution;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 10 h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step 2 gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 60 DEG C of air drying 6 h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 60min under retort furnace 300 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer ball.
embodiment 5
A kind of Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2o) with the urea of 4 mmoles, be dissolved in 25 mL ethanol and 10mL ethylene glycol, after magnetic agitation, be configured to uniform colorless clear solution;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 3 h at 160 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step 2 gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 70 DEG C of air drying 8 h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 120min under retort furnace 400 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer ball.
embodiment 6
A kind of Indium sesquioxide (In
2o
3) preparation method of nanometer ball, be carry out according to following step:
Step one: the indium nitrate (In (NO taking 1 mmole
3)
34.5 H
2o) with the urea of 4 mmoles, be dissolved in 15 mL ethanol and 25mL ethylene glycol, after magnetic agitation, be configured to uniform colorless clear solution;
Step 2: the mixed system of step one gained is transferred in teflon-lined reactor, be warmed up to constant temperature 5h at 180 DEG C of temperature, naturally cooling, obtains solvent thermal product;
Step 3: by the solvent thermal product centrifugation of step 2 gained, wash three times respectively with deionized water and dehydrated alcohol; Product after centrifugation, at 60 DEG C of air drying 8h, obtains precursor indium hydroxide (In (OH)
3);
Step 4: by the indium hydroxide (In (OH) of step 3 gained
3) precursor calcines 240 min under retort furnace 500 DEG C of air atmospheres, can obtain Indium sesquioxide (In
2o
3) nanometer 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 (4)
1. a preparation method for Indium sesquioxide nanometer ball, is characterized in that: comprise the steps: successively
Step one: prepare analytically pure indium nitrate and urea mixing solutions, described 1 mmole indium nitrate mixes with the urea of 1 ~ 5 mmole, and add 35ml dissolution with solvents, described solvent is ethanol and/or ethylene glycol, makes uniform colorless clear solution after magnetic agitation;
Step 2: be transferred in hydro-thermal container by described colourless transparent solution, is warming up to 120 ~ 180 DEG C, and heating 1 ~ 12h, collects solvent thermal product after naturally cooling;
Step 3: solvent thermal product is obtained indium hydroxide precursor through washing, drying;
Step 4: described indium hydroxide precursor is obtained Indium sesquioxide nanometer ball through high-temperature roasting.
2. the preparation method of Indium sesquioxide nanometer ball according to claim 1, is characterized in that:
In described step 3, specifically will prepare the solvent thermal product centrifugation of gained in described step 2, after washing three times respectively with deionized water and dehydrated alcohol, at 60 ~ 80 DEG C of air drying 6 ~ 12 h.
3. the preparation method of Indium sesquioxide nanometer ball according to claim 1 and 2, is characterized in that:
High-temperature roasting in described step 4 refers to will prepare indium hydroxide precursor roasting 60 ~ 240 min under retort furnace 300 ~ 600 DEG C of air atmospheres of gained in described step 3.
4. the Indium sesquioxide nanometer ball that obtains of preparation method according to claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN109999780A (en) * | 2019-05-05 | 2019-07-12 | 江苏师范大学 | In with double-shell structure2O3The synthetic method of micro-and nanorods |
| CN113277549A (en) * | 2021-06-15 | 2021-08-20 | 先导薄膜材料有限公司 | Indium tin oxide powder and preparation method thereof |
| CN115784297A (en) * | 2022-11-21 | 2023-03-14 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
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| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
| CN103420414A (en) * | 2013-08-12 | 2013-12-04 | 江苏大学 | Solvothermal preparation method of bismuth trioxide microspheres and application thereof |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
| CN103420414A (en) * | 2013-08-12 | 2013-12-04 | 江苏大学 | Solvothermal preparation method of bismuth trioxide microspheres and application thereof |
Non-Patent Citations (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN109999780A (en) * | 2019-05-05 | 2019-07-12 | 江苏师范大学 | In with double-shell structure2O3The synthetic method of micro-and nanorods |
| CN109999780B (en) * | 2019-05-05 | 2021-02-12 | 江苏师范大学 | In having a double-layer shell structure2O3Synthesis method of micro-nano rod |
| CN113277549A (en) * | 2021-06-15 | 2021-08-20 | 先导薄膜材料有限公司 | Indium tin oxide powder and preparation method thereof |
| CN115784297A (en) * | 2022-11-21 | 2023-03-14 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
| CN115784297B (en) * | 2022-11-21 | 2024-03-29 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
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