Summary of the invention
The present invention is in order to solve the standby precursor liquid of the hot legal system of hydrothermal/solvent long technical problem consuming time, discloses the method for the standby Indium sesquioxide cubic block of a kind of microwave-assisted hydro-thermal legal system.
The present invention adopts the Indium sesquioxide (In for preparing the relative homogeneous of pattern under low temperature through the microwave-assisted reaction
2O
3) cubic block, its technical scheme is the mixing solutions of preparation indium nitrate and urea, then reaction generates indium hydroxide (In (OH) through centrifuge washing again under microwave
3) precursor, finally by high-temperature roasting, make and form.
The method of the standby Indium sesquioxide cubic block of microwave-assisted hydro-thermal legal system disclosed in this invention, the mixing solutions of described preparation indium nitrate and urea is according to indium nitrate (In (NO
3)
34.5 H
2O) with the mol ratio of urea, be 1:1 ~ 10, preferably 1:0.5~2, do not comprise that 1:2 takes, and adds deionized water dissolving, after magnetic agitation 30 min, becomes even colourless transparent solution.
In preferred embodiment of the present invention, the mixing solutions of described preparation indium nitrate and urea is according to indium nitrate (In (NO
3)
34.5 H
2O) with the mol ratio of urea, be that 1:7 takes, add deionized water dissolving, after magnetic agitation 30 min, become even colourless transparent solution.
The method of the standby Indium sesquioxide cubic block of microwave-assisted hydro-thermal legal system disclosed in this invention, the described reaction under microwave is that the even colourless transparent solution of above-mentioned gained is transferred in quartz container, be placed in microwave reactor, be warming up to 80~100 ℃, power is that 600W~1000W heats 15~120min, naturally cooling, collect the microwave product.
The method of the standby Indium sesquioxide cubic block of microwave-assisted hydro-thermal legal system disclosed in this invention, described centrifuge washing is by the centrifugation of described microwave product, after with deionized water and dehydrated alcohol, washing respectively three times, at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor.
The method of the standby Indium sesquioxide cubic block of microwave-assisted hydro-thermal legal system disclosed in this invention, described high-temperature roasting is by the indium hydroxide of gained (In (OH)
3) precursor roasting 60~120min under 350~550 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
According to the Indium sesquioxide nano cubic block that the method for the standby Indium sesquioxide cubic block of microwave-assisted hydro-thermal legal system makes, length and width all are about 200~400 nm, and thickness is about 50~200 nm.
Microwave-assisted hydro-thermal method disclosed in this invention is compared with traditional hydrothermal method, can improve by a relatively large margin speed of reaction, and Reaction time shorten is saved the energy.Reaction times can even shorten to dozens of minutes in tens hours by several hours common hydro-thermal reaction time, and can reach pure phase within a short period of time.
The present invention regulated and controled the microwave reaction time, will be adjusted into 15min, 30min, 60min and 120min the reaction times, and while by experiment, finding microwave reaction 15min, the microwave product has reached pure phase.
Indium sesquioxide (In in the present invention
2O
3) structure by x-ray diffractometer, determined in x-ray diffraction pattern, there is no the peak of other materials, this collection of illustrative plates shows, by the microwave-assisted hydro-thermal method Indium sesquioxide (In of each prepared period
2O
3) be pure phase Indium sesquioxide (In
2O
3), itself and standard oxidation indium (In
2O
3) card (01-0929) matches.
Field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and by the prepared Indium sesquioxide (In of microwave-assisted hydro-thermal method
2O
3) length and width be about 200~400 nm, thickness is about 50~200 nm.
To Indium sesquioxide (In
2O
3) valence state of surface-element analyzes, 452.1 eV, these two strong peaks of 444.2 eV are correspondences and In respectively
2O
3In In 3d
3/2And In3d
5/2, 531.6 eV are corresponding to In
2O
3In O 1s, near and the not appearance of other small peak main peak, show that there is not oxidized phenomenon on the surface of product.Therefore Indium sesquioxide (the In prepared by this programme
2O
3) cubic block, more stable.
Indium nitrate (In (the NO that the present invention is used
3)
34.5 H
2O) and urea be all analytical pure, further purification is not done in experiment.
Beneficial effect
The present invention uses microwave-assisted hydro-thermal legal system to get Indium sesquioxide (In
2O
3), method is simple, and the reaction times can even shorten to dozens of minutes in tens hours by several hours common hydro-thermal reaction time, and can reach pure phase within a short period of time, and the reactant crystal formation is better.Utilize simple microwave-assisted reaction to prepare the Indium sesquioxide (In of the relative homogeneous of pattern
2O
3), pattern is a cube block nanostructure, this material has good chemical stability.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 the environmental friendliness requirement, is convenient to suitability for industrialized production.
Embodiment
The present invention is described in detail below in conjunction with embodiment, so that 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 cubic block, be to carry out according to following step:
A, to take mol ratio be 1:0.5 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 80 ℃, after power was 600W heating 15min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 60min under 350 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Indium sesquioxide (In
2O
3) the XRD figure spectrum of nano cubic block is shown in accompanying drawing 1, the product morphology analysis is shown in accompanying drawing 2, X-ray photoelectron spectroscopic analysis 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 (01-0929) matches, and in the XRD figure spectrum, there is no other diffraction peak of mixing, and the In that the present invention prepares is described
2O
3Phase is pure.
In accompanying drawing 2, field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and by the prepared Indium sesquioxide (In of microwave-assisted hydro-thermal method
2O
3) length and width all be about 200~400 nm, thickness is about 50~200 nm.
In accompanying drawing 3, by the Indium sesquioxide (In of the standby relative homogeneous of pattern of microwave-assisted hydro-thermal legal system
2O
3), the valence state of the element on its product surface is analyzed, in accompanying drawing 3a, 452.1 eV, these two strong peaks of 444.2 eV are correspondences and In respectively
2O
3In In 3d
3/2And In3d
5/2, in accompanying drawing 3b, 531.6 eV are corresponding to In
2O
3In O 1s, near and the not appearance of other small peak main peak, show that there is not oxidized phenomenon on the surface of product.Therefore by a process for preparing next Indium sesquioxide (In
2O
3) cubic block, more stable.
Embodiment 2
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, to take mol ratio be 1:7 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 100 ℃, after power was 1000W heating 120min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 120min under 550 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 3
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, to take mol ratio be 1:0.9 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 90 ℃, after power was 800W heating 90min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 90min under 400 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 4
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, to take mol ratio be 1:7 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 100 ℃, after power was 600W heating 120min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 120min under 550 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 5
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, to take mol ratio be 1:0.5 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 80 ℃, after power was 600W heating 120min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 120min under 550 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 6
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, to take mol ratio be 1:4 indium nitrate (In (NO
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the quartz container that capacity is 250mL, is placed in microwave reactor, be warming up to 100 ℃, after power was 800W heating 120min, naturally cooling, collected the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain indium hydroxide (In (OH)
3) precursor;
E, by the indium hydroxide of step D gained (In (OH)
3) precursor calcines 100min under 400 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 7
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, take the indium nitrate (In (NO that mol ratio is 1:1
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the container of quartz that capacity is 250mL, is placed in microwave reactor, be warming up to 80 ℃, power is that 600W heats after 60min, and naturally cooling, collect the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain the indium hydroxide precursor liquid;
E, the indium hydroxide precursor liquid of step D gained is calcined to 60min under 350 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
Embodiment 8
A kind of Indium sesquioxide (In
2O
3) preparation method of cubic block, be to carry out according to following step:
A, take the indium nitrate (In (NO that mol ratio is 1:10
3)
34.5 H
2O) and urea, be dissolved in 100 mL deionized waters, be configured to even colourless transparent solution after magnetic agitation 30 min;
B, the solution of steps A gained is transferred in the container of quartz that capacity is 250mL, is placed in microwave reactor, be warming up to 100 ℃, power is that 1000W heats after 240min, and naturally cooling, collect the microwave product;
C, by the microwave product centrifugation of step B gained, with deionized water and dehydrated alcohol, wash respectively three times;
D, by the product after the centrifugation of step C gained at 60 ℃ of air drying 6 h, obtain the indium hydroxide precursor liquid;
E, the indium hydroxide precursor liquid of step D gained is calcined to 240min under 550 ℃ of air atmospheres of retort furnace, can obtain flaxen Indium sesquioxide (In
2O
3) cubic block.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or equivalent flow process conversion that utilizes specification sheets of the present invention to do, or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.