CN104045107A - Preparation method for three-dimensional laminar six-pointed star indium oxide - Google Patents
Preparation method for three-dimensional laminar six-pointed star indium oxide Download PDFInfo
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- CN104045107A CN104045107A CN201410251243.2A CN201410251243A CN104045107A CN 104045107 A CN104045107 A CN 104045107A CN 201410251243 A CN201410251243 A CN 201410251243A CN 104045107 A CN104045107 A CN 104045107A
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- indium sesquioxide
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Abstract
The invention relates to nano indium oxide, particularly relates to a preparation method for three-dimensional laminar six-pointed star indium oxide, and belongs to the technical field of nano material synthesis. According to the preparation method, with distilled water as a solvent, nano indium oxide six-pointed star with uniform morphology is prepared by adopting a hydrothermal synthesis method, wherein the six-pointed star consists of two-dimensional nano sheets. According to the technical scheme, the preparation method comprises the following steps: firstly, mixing In(NO3)3.4.5H2O, urea and glucose (C6H12O6.H2O) in distilled water, and preparing indium oxide nano six-pointed star precursor liquor by the hydrothermal method after uniformly stirring; and roasting the precursor liquor at a high temperature to obtain the indium oxide nano six-pointed star. The preparation method disclosed by the invention is simple in process, and good in repeatability; moreover, the used raw materials are inorganic compounds, cheap and easy to obtain and low in cost, satisfy environment-friendly requirements, and are shorter in reaction time, so that energy consumption and reaction cost are reduced, and therefore, large-scale production is facilitated; meanwhile, a rhombus indium oxide light catalyst has stronger photocatalytic degradation ability, the three-dimensional laminar six-pointed star indium oxide prepared by the preparation method has higher practical application ability.
Description
Technical field
The present invention relates to nano indium oxide, refer in particular to a kind of preparation method of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide, belong to nano material synthesis technical field; Especially utilize Hydrothermal Synthesis to prepare pattern good, the preparation method of the Indium sesquioxide nanometer double triangles six rayed star being formed by two-dimensional nano, this semiconductor material can be used for Visible Light Induced Photocatalytic field of antibiotics.
Background technology
Photocatalyst reaction is mainly to occur in light-catalysed surface, and one have good pattern and undersized inorganic nano material has represented better photocatalytic activity than large invisible nano material; Pattern is as a much-talked-about topic in recent years, and how many investigators control pattern and size in research, and Indium sesquioxide is the good semiconductor material of 3.77 eV as energy gap.Indium sesquioxide contains two kinds of crystal formation: rh-In
2o
3(rhombus Indium sesquioxide) and bcc-In
2o
3(body-centered Indium sesquioxide), till now, body-centered Indium sesquioxide is synthesized out various patterns, as nanometer blocks, nanoparticle, nano wire, nanometer sheet etc., little about the report of rhombus Indium sesquioxide; The common synthesis method of rhombus Indium sesquioxide is to form by the method for High Temperature High Pressure, it has more excellent photochemical properties with respect to the Indium sesquioxide of body-centered, a large amount of research shows that the nano indium oxide of three-dimensional structure has higher specific surface, high light capture ability, and, it by widely in optoelectronic device, catalyzer, sensor, and solar cell; Seldom having document is that report hydrothermal method is produced 3 D rhombic fins Indium sesquioxide.In general method, be the method by solvent thermal, or use the method for High Temperature High Pressure synthetic, so find environmental protection in the synthetic method of three-dimensional structure, succinct method is very necessary.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, the hydrothermal method of environmental protection is prepared a kind of method of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide.
The present invention uses distilled water for solvent, adopts hydrothermal synthesis method to prepare the Indium sesquioxide (rh-In of pattern homogeneous
2o
3) nanometer double triangles six rayed star, this double triangles six rayed star is made up of two-dimensional nano sheet, and its technical scheme is first to use In (NO
3)
34.5H
2o(indium nitrate), urea, glucose (C
6h
12o
6h
2o) after being mixed in and stirring in distilled water, hydro-thermal makes Indium sesquioxide nanometer double triangles six rayed star precursor liquid; Again precursor liquid is obtained to Indium sesquioxide nanometer double triangles six rayed star through high-temperature calcination.
Concrete, one forms rhombus Indium sesquioxide (rh-In by two-dimensional nano sheet
2o
3) preparation method of nanometer double triangles six rayed star, carry out according to following step:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the mol ratio of urea and glucose is 1:7.0-7.1:9.1-9.2, and is dissolved in distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 160 DEG C of-200 DEG C of constant temperature 12-36h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 450 DEG C-600 DEG C, and the time is 2h.
In the present invention, add urea as OH
-supplier, and adding of glucose is to have formed one deck carbon film, the advantage of the method is to utilize urea and grape to make environment for alkalescence forms indium hydroxide, can not form by product, the Indium sesquioxide obtaining does not like this have other impurity.
Another object of the present invention, is to provide the visible light catalyst degraded application of prepared rhombus Indium sesquioxide double triangles six rayed star to tsiklomitsin.
Rhombus Indium sesquioxide nanometer double triangles six rayed star degradation experiment step to tsiklomitsin under radiation of visible light is as follows:
In GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carrying out, is that 10 mg/L tsiklomitsin 100 mL add in photochemical catalysis instrument reactor by concentration, then adds the rhombus Indium sesquioxide (rh-In of Hydrothermal Synthesis
2o
3) photocatalyst 0.1 g, use magnetic stirring apparatus reaction 30 minutes in darkroom, after reaching reaction adsorption equilibrium, start sampling, then open aerating apparatus and open the 150W xenon source of loading onto spectral filter, it is to keep catalyzer in suspending or afloat that aeration passes into air object, in Xenon light shining process, sample at interval of 30 min, after centrifugation, get supernatant liquid at tsiklomitsin maximum absorption wavelength λ max=357nm place, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A0] × 100% calculate photodegradation rate, wherein A
0the absorbancy of tetracycline when reaching adsorption equilibrium, A
ithe absorbancy of tetracycline of measuring for timing sampling.
The three-dimensional manometer double triangles six rayed star rh-In that the present invention is prepared
2o
3in the time of radiation of visible light, the degradation rate of tsiklomitsin is reached to 82% when the 240min.
Urea used in the present invention, glucose and indium nitrate are analytical pure.
The present invention utilizes simple hydrothermal synthesis method to synthesize rhombus Indium sesquioxide photocatalyst, and its pattern is three-dimensional manometer double triangles six rayed star, as a kind of novel photocatalysis material, and the advantage such as this material has chemical stability, nontoxic.
Technique of the present invention is simple, favorable reproducibility, and raw materials is mineral compound, and cheap and easy to get, cost is low, meets environmental friendliness requirement, and the reaction times is shorter, thereby has reduced energy consumption and reaction cost, is convenient to batch production; Because rhombus Indium sesquioxide photocatalyst has stronger photocatalytic degradation ability, there is very high actual application ability simultaneously.
Brief description of the drawings
Fig. 1 is three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide X-ray diffraction analysis figure (XRD).
Fig. 2 is three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide scanning electron microscope (SEM) photograph (SEM).
Fig. 3 is three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide XPS collection of illustrative plates at room temperature.
Fig. 4 is indium XPS collection of illustrative plates at room temperature.
Fig. 5 is oxygen XPS collection of illustrative plates at room temperature.
Fig. 6 is the photodegradation figure of three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, so that those skilled in the art better understand the present invention, but the present invention is not limited to following examples.
embodiment 1:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Embodiment 2:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.3838g, 0.4254g and 1.818g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Embodiment 3:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 160 DEG C of constant temperature 36h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Embodiment 4:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 200 DEG C of constant temperature 12h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Embodiment 5:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 450 DEG C, and the time is 2h.
Embodiment 6:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 600 DEG C, and the time is 2h.
Embodiment 7:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively than 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Embodiment 8:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively than 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) ultrasonic agitation evenly obtains settled solution.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 180 DEG C of constant temperature 24h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, obtains the product of pure phase.
(7) getting the calcining temperature of choosing in step 6 is 500 DEG C, and the time is 2h.
Embodiment 9:
(1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the quality of urea and glucose is respectively than 0.7676g, 0.8507g and 3.636g, and be dissolved in 30ml distilled water.
(2) by extremely clarification of solution ultrasonic agitation in step 1.
(3) solution step 2 being obtained is transferred in teflon-lined reactor, at 160 DEG C of constant temperature 36h, then, after naturally cooling, obtains hydrothermal product.
(4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal.
(5) will in step 4, obtain precipitation vacuum-drying, drying temperature is 60 DEG C, and the time is 12h.
(6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
(7) in setting steps 6, calcining temperature is 500 DEG C, and the time is 2h.
Three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide degradation experiment step to tsiklomitsin under radiation of visible light is as follows:
In GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carrying out, is that 10 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then adds the rhombus Indium sesquioxide (rh-In of Hydrothermal Synthesis
2o
3) photocatalyst 0.1 g, use magnetic stirring apparatus reaction 30 minutes in darkroom, after reaching reaction adsorption equilibrium, start sampling, then open aerating apparatus and open the 150W xenon source of loading onto spectral filter, it is to keep catalyzer in suspending or afloat that aeration passes into air object, in Xenon light shining process, sample at interval of 30 min, after centrifugation, get supernatant liquid at tsiklomitsin maximum absorption wavelength λ max=357nm place, 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 when reaching adsorption equilibrium, A
ithe absorbancy of tetracycline of measuring for timing sampling.
The rh-In that the present invention is prepared
2o
3nano flower reaches 82% to the degradation rate of tsiklomitsin when the 240min in the time of radiation of visible light.
Three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide (rh-In
2o
3) XRD figure spectrum see appendix 1, product morphology analysis is shown in accompanying drawing 2, accompanying drawing 3,4,5 is shown in the analysis of surface-element valence state, photocatalysis effect is shown in accompanying drawing 6.
In accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (22-3306) matches, and in XRD figure spectrum, there is no other diffraction peak of mix, the rhombus Indium sesquioxide (rh-In preparing under the hydrothermal condition of the present invention's proposition is described
2o
3) thing of nano flower is pure mutually.
In accompanying drawing 2, field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and the rhombus Indium sesquioxide (rh-In being prepared by hydrothermal method
2o
3) nano flower diameter is 1～1.2 μ m, thickness is 124 nm.
In accompanying drawing 3,4,5, rhombus Indium sesquioxide (rh-In
2o
3) nanometer double triangles six rayed star XPS collection of illustrative plates at room temperature, can find out that from accompanying drawing 3 at 443.6 eV and 451.3 eV are the In 3 corresponding Indium sesquioxide
d5, In3
d3/2, and O in the corresponding Indium sesquioxide of 530.6ev
1S, there are not in the drawings other peaks, show that product Indium sesquioxide surface does not have other impurity, the three-dimensional manometer double triangles six rayed star rhombus Indium sesquioxide therefore preparing by this programme is more stable.
In accompanying drawing 6, photocatalysis effect figure shows the three-dimensional manometer double triangles six rayed star rh-In that the present invention is prepared
2o
3in the time of radiation of visible light, the degradation rate of tsiklomitsin is reached to 82% when the 240min.
Claims (7)
1. a preparation method for three-layer laminated nanometer double triangles six rayed star Indium sesquioxide, is characterized in that: after first mixing and be dissolved in and stir in distilled water with indium nitrate, urea, glucose, hydro-thermal makes indium hydroxide nano double triangles six rayed star presoma; Again presoma is obtained to three-layer laminated nanometer double triangles six rayed star rhombus Indium sesquioxide through high-temperature calcination.
2. the preparation method of a kind of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide as claimed in claim 1, is characterized in that: described nanometer double triangles six rayed star Indium sesquioxide is made up of two-dimensional nano sheet, and diameter is 1～1.2 μ m, and thickness is 124 nm.
3. the preparation method of a kind of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide as claimed in claim 1, is characterized in that carrying out according to following step:
1) take indium nitrate, urea and glucose are dissolved in distilled water, described indium nitrate, and the mol ratio of urea and glucose is 1:7.0-7.1:9.1-9.2, and is dissolved in distilled water;
2) by extremely clarification of solution ultrasonic agitation in step 1;
3) solution step 2 being obtained is transferred in teflon-lined reactor, at 160 DEG C of-200 DEG C of constant temperature 12-36h, then, after naturally cooling, obtains hydrothermal product;
4) precipitation step 3 being obtained is by water and alternately washing of ethanol, centrifugal;
5) precipitation vacuum-drying will be obtained in step 4;
6) the dry thing obtaining of getting in step 5 carries out high-temperature calcination, to remove Glucose Carbon compound, thereby obtains pure phase product.
4. the preparation method of a kind of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide as claimed in claim 3, is characterized in that: in described step (5), vacuum drying drying temperature is 60 DEG C, and the time is 12h.
5. the preparation method of a kind of three-layer laminated nanometer double triangles six rayed star Indium sesquioxide as claimed in claim 3, is characterized in that: in described step (6), calcining temperature is 450 DEG C-600 DEG C, and the time is 2h.
6. the three-layer laminated nanometer double triangles six rayed star Indium sesquioxide that prepared by the method for claim 1 is as the purposes of the photocatalyst of degraded tsiklomitsin.
7. the three-layer laminated nanometer double triangles six rayed star Indium sesquioxide that prepared by method as claimed in claim 6 is as the purposes of the photocatalyst of degraded tsiklomitsin, it is characterized in that: for the 10 mg/L tsiklomitsin aqueous solution of every 100ml, the three-layer laminated nanometer double triangles six rayed star of 0.1g rhombus Indium sesquioxide can reach 82% to the degradation rate of tsiklomitsin when the 4h under radiation of visible light.
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| CN109647373A (en) * | 2018-11-28 | 2019-04-19 | 天津大学 | Black oxidation indium ultrathin nanometer piece and preparation method thereof and photo-thermal catalytic applications |
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| CN103183374A (en) * | 2013-03-13 | 2013-07-03 | 济南大学 | Method for preparing monodisperse indium oxide nanometer porous microsphere |
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| CN105540643A (en) * | 2016-02-22 | 2016-05-04 | 武汉工程大学 | Multipod-like indium oxide compound sensitive material and preparation and application thereof |
| CN109647373A (en) * | 2018-11-28 | 2019-04-19 | 天津大学 | Black oxidation indium ultrathin nanometer piece and preparation method thereof and photo-thermal catalytic applications |
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Application publication date: 20140917 |