CN110540233B - Indium oxide nanorod with uniform size and preparation method and application thereof - Google Patents
Indium oxide nanorod with uniform size and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of nano indium oxide, and particularly relates to an indium oxide nanorod with uniform size, and a preparation method and application thereof. The method comprises the steps of firstly preparing indium hydroxide precursor powder from indium trichloride tetrahydrate, polyvinylpyrrolidone (PVP), polyethylene glycol (PEG-600), deionized water and KOH, then carrying out gradient centrifugation on the redispersed indium hydroxide precursor powder, and finally carrying out high-temperature calcination to obtain the indium oxide nanorod with uniform size. The indium oxide nanorod has the diameter of 30-50 nm, the length of 1-5 mu m and the length-diameter ratio of 20-170. The nano-rods exist in a single-dispersed form, and are beneficial to the application of the nano-rods in photoelectric devices, gas sensitivity, sensing and other aspects. The method has simple and feasible process and mild reaction conditions, and is convenient for large-scale production.
Description
Technical Field
The invention belongs to the technical field of preparation of nano indium oxide, and particularly relates to an indium oxide nanorod with uniform size, and a preparation method and application thereof.
Background
Since the morphology of nanomaterials is a key factor affecting their chemical, physical properties and function, the controllable design and preparation of the nanomaterial's size and morphology is crucial. One-dimensional nanostructures such as nanowires, nanorods, nanotubes, etc. have been a research focus in recent years due to their unique structural properties and physical/chemical characteristics, and have potential application prospects in the fields of next-generation nanoelectronics, optoelectronics, sensing devices, etc.
Indium oxide is a representative n-type semiconductor material, has a direct band gap of 3.55-3.75eV and an indirect energy gap of 2.62eV, has the characteristics of high electron mobility, high visible light transmittance, stable chemical properties, easiness in doping, easiness in preparation and the like, and is particularly suitable for application in the fields of FETs, photoelectrochemical detection, gas sensors, photocatalysts and the like. The indium oxide nanorods are mostly synthesized by a hydrothermal synthesis method or a solvothermal synthesis method, mostly exist in the form of nanorod bundles, and few cases are reported to exist in the form of single nanorods. Therefore, it is necessary to find a simple synthesis method capable of preparing single dispersed indium oxide nanorods having a uniform size.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide a preparation method of indium oxide nanorods with uniform size, which has simple process and low cost and can prepare indium oxide nanorods with high yield and uniform size and single indium oxide nanorods with dispersion.
The invention also aims to provide the indium oxide nanorod obtained by the preparation method.
The invention also aims to provide an application of the indium oxide nanorod.
In order to realize the technical scheme, the technical scheme adopted by the invention is as follows:
a preparation method of indium oxide nanorods with uniform size comprises the following steps:
(1) preparation of indium hydroxide precursor powder
By adopting a solvothermal synthesis method, mixing indium trichloride tetrahydrate, polyvinylpyrrolidone (PVP), polyethylene glycol (PEG-600), deionized water and KOH serving as raw materials, uniformly stirring to obtain a reactant, heating for reaction, cooling to room temperature after reaction, washing and centrifugally separating a product, and finally drying to obtain milky indium hydroxide precursor powder;
(2) preparing indium hydroxide precursor powder with uniform size
Ultrasonically dispersing the indium hydroxide precursor powder obtained in the step (1) in deionized water, performing gradient centrifugation to obtain an indium hydroxide suspension with uniform size, and then sequentially performing centrifugation, washing and drying to obtain milky indium hydroxide precursor powder with uniform size;
(3) preparation of indium oxide nanorod powder
And (3) calcining the milky white uniform-size indium hydroxide precursor powder obtained in the step (2) at high temperature to obtain the indium oxide nanorod, wherein the indium oxide nanorod is yellow.
Preferably, the molecular weight of the polyvinylpyrrolidone in the step (1) is 1300000.
Preferably, in the reactant in the step (1), the concentration of the indium trichloride tetrahydrate is 15.25 mg/mL.
Preferably, in the reactant in the step (1), the concentration of the polyvinylpyrrolidone is 0-26 mg/mL.
Preferably, in the reactant in the step (1), the concentration of KOH is 60 mg/mL.
In the concentration of the above reactants, the total volume of the reactants is calculated by the volume of PEG-600.
Preferably, the volume ratio of the PEG-600 to the deionized water in the step (1) is 5: 0-5: 0.069.
Preferably, the stirring time in the step (1) is 1-30 minutes.
Preferably, the heating reaction condition in the step (1) is that the reaction is carried out for 36-72 hours at 180-210 ℃.
Preferably, the reaction described in step (1) is carried out in a polytetrafluoroethylene liner.
Preferably, the temperature for drying in step (1) is 60 ℃.
Preferably, the centrifugal speed of the gradient centrifugation in the step (2) is 500-2000 rpm.
More preferably, the centrifugation speeds of the gradient centrifugation in the step (2) are 500rpm, 1000rpm, 1500rpm and 2000rpm in sequence.
Preferably, the temperature of the high-temperature calcination in the step (3) is 500-650 ℃, and the duration is 2-4 hours.
The invention further provides the indium oxide nanorod with uniform size, which is obtained by the preparation method, and the indium oxide nanorod has the diameter of 30-50 nm, the length of 1-5 mu m and the length-diameter ratio of 20-170.
The invention further provides the application of the indium oxide nanorod in photoelectric, gas-sensitive and sensing devices.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the process for preparing the indium oxide nanorod is simple and feasible, the reaction conditions are mild, and the large-scale production is facilitated;
(2) the preparation method can simply prepare the indium oxide nano-rods with uniform size, and the nano-rods exist in a single-dispersed form, thereby being beneficial to the application of the nano-rods in the aspects of photoelectric devices, gas sensitivity, sensing and the like.
Drawings
FIG. 1 is a scanning electron micrograph of the indium oxide nanorods prepared in example 4;
FIG. 2 is an X-ray diffraction pattern of the indium oxide nanorods prepared in example 4.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
The embodiment provides an indium oxide powder without deionized water and PVP and without gradient centrifugation and a preparation method thereof.
The preparation method comprises the following steps: 152.5mg of InCl were weighed out3·4H2O, 0.6g KOH, 10mL PEG-600, magnetically stirred at ambient temperature for 30 minutes, then transferred to a 50mL Teflon linerAnd then the mixture is put into a hydrothermal reaction kettle and is reacted for 36 hours at the temperature of 180 ℃. And after cooling, obtaining a black brown viscous solution and a precipitate, washing the precipitate with deionized water, centrifuging the product, respectively centrifuging and washing the product for 3 times with deionized water and ethanol, repeating the washing for two times, washing for three times, and drying the obtained product in an oven to obtain the milky indium hydroxide precursor. And calcining the dried indium hydroxide precursor at 500 ℃ for 2 hours to prepare light yellow indium oxide powder. The nano-particle is obtained by testing a scanning electron microscope, and the product prepared under the condition is a nano-particle with the size of 100-200 nm. Therefore, the indium oxide nanorods cannot be obtained without adding deionized water and PVP and without gradient centrifugation.
Example 2
The present embodiment provides an indium oxide powder without PVP and without gradient centrifugation, and a method for preparing the same.
The preparation method comprises the following steps: 152.5mg of InCl were weighed out3·4H2O, 0.6g KOH, 10mL PEG-600 and 0.138mL deionized water, magnetically stirred at ambient temperature for 30 minutes, then transferred to a 50mL Teflon liner, charged to a hydrothermal reaction kettle, and then allowed to react at a temperature of 210 ℃ for 72 hours. And after cooling, obtaining a black brown viscous solution and a precipitate, washing the precipitate with deionized water, centrifuging the product, respectively centrifuging and washing the product for 3 times with deionized water and ethanol, repeating the washing for two times, washing for three times, and drying the obtained product in an oven to obtain the milky indium hydroxide precursor. And calcining the dried indium hydroxide precursor at 650 ℃ for 4 hours to prepare light yellow indium oxide powder. The product is obtained by testing through a scanning electron microscope, and the product prepared under the condition is square nanoparticles with the size of 100-500 nm. Therefore, the indium oxide nanorods cannot be obtained without adding PVP and without gradient centrifugation.
Example 3
The embodiment provides an indium oxide nanorod with a small amount of PVP and without gradient centrifugation and a preparation method thereof.
The preparation method comprises the following steps: 152.5mg of InCl were weighed out3·4H2O, 0.6g KOH, 10mL PEG-600, 75mg PVP and 0.138mL deionized water, magnetically stirred at ambient temperature for 1 minute, transferred to a 50mL Teflon liner, charged to a hydrothermal reaction kettle and allowed to react at 210 ℃ for 72 hours. And after cooling, obtaining a black brown viscous solution and a precipitate, washing the precipitate with deionized water, centrifuging the product, respectively centrifuging and washing the product for 3 times with deionized water and ethanol, repeating the washing for two times, washing for three times, and drying the obtained product in an oven to obtain the milky indium hydroxide precursor. And calcining the dried indium hydroxide precursor at 650 ℃ for 4 hours to prepare light yellow indium oxide powder. The nano-particles are obtained by testing through a scanning electron microscope, the product prepared under the condition is a mixture of a large amount of nano-particle clusters and a small amount of large nano-rods, the diameter of each nano-rod is about 150 nanometers, and the diameter of each nano-rod is about 5 micrometers. It can be seen that the diameter of the obtained indium oxide nanorod is larger under the condition of adding a small amount of PVP and not carrying out gradient centrifugation.
Example 4
The embodiment provides an indium oxide nanorod without gradient centrifugation and a preparation method thereof.
The preparation method comprises the following steps: 152.5mg of InCl were weighed out3·4H2O, 0.6g KOH, 10mL PEG-600, 260mg PVP and 0.138mL deionized water, magnetically stirred at ambient temperature for 3 minutes, transferred to a 50mL Teflon liner, charged to a hydrothermal reaction kettle and allowed to react at 210 ℃ for 72 hours. And after cooling, obtaining a black brown viscous solution and a precipitate, washing the precipitate with deionized water, centrifuging the product, respectively centrifuging and washing the product for 3 times with deionized water and ethanol, repeating the washing for two times, washing for three times, and drying the obtained product in an oven to obtain the milky indium hydroxide precursor. And calcining the dried indium hydroxide precursor at 650 ℃ for 4 hours to prepare light yellow indium oxide powder. The product prepared under the condition is a large amount of nano particles by the test of a scanning electron microscopeThe particle cluster and a small amount of nano rods are mixed, the diameter of each nano rod is about 50-150 nanometers, and the diameter of each nano rod is about 1-5 micrometers. It can be seen that the diameter of the obtained indium oxide nanorod is still large without gradient centrifugation.
Example 5
The embodiment provides an indium oxide nanorod with uniform size and a preparation method thereof.
The preparation method comprises the following steps: 152.5mg of InCl were weighed out3·4H2O, 0.6g KOH, 10mL PEG-600, 260mg PVP and 0.138mL deionized water, magnetically stirred at ambient temperature for 3 minutes, transferred to a 50mL Teflon liner, charged to a hydrothermal reaction kettle and allowed to react at 210 ℃ for 72 hours. And after cooling, obtaining a black brown viscous solution and a precipitate, washing the precipitate with deionized water, centrifuging the product, respectively centrifuging and washing the product for 3 times with deionized water and ethanol, repeating the washing for two times, washing for three times, and drying the obtained product in an oven to obtain the milky indium hydroxide precursor. And re-dispersing the indium hydroxide precursor in deionized water, and then centrifuging at 500rpm, 1000rpm, 1500rpm and 2000rpm in sequence, and separating to obtain the indium hydroxide precursor with uniform size. And calcining the dried indium hydroxide precursor at 650 ℃ for 4 hours to prepare light yellow indium oxide powder. The nano-indium oxide nano-rods are obtained by scanning electron microscope tests, as shown in figure 1, the products prepared under the condition are a large number of indium oxide nano-rods, the diameters of the nano-rods are about 30-50 nanometers, and the diameters of the nano-rods are about 1-5 micrometers. FIG. 2 is an X-ray diffraction pattern of the indium oxide nanorods obtained in the example, and the comparison with a standard card (JCPDS No.71-2194) shows that the product is indeed indium oxide nanorods.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of indium oxide nanorods with uniform size is characterized by comprising the following steps:
(1) preparation of indium hydroxide precursor powder
By adopting a solvothermal synthesis method, taking indium trichloride tetrahydrate, polyvinylpyrrolidone, PEG-600, deionized water and KOH as raw materials, mixing and uniformly stirring to obtain a reactant, then heating to react for 36-72 hours at 180-210 ℃, cooling to room temperature after the reaction, washing and centrifugally separating a product, and finally drying to obtain milky indium hydroxide precursor powder;
the volume ratio of the PEG-600 to the deionized water is 5: 0.069;
(2) preparing indium hydroxide precursor powder with uniform size
Ultrasonically dispersing the indium hydroxide precursor powder obtained in the step (1) in deionized water, performing gradient centrifugation to obtain an indium hydroxide suspension with uniform size, and then sequentially performing centrifugation, washing and drying to obtain milky indium hydroxide precursor powder with uniform size;
(3) preparation of indium oxide nanorod powder
Calcining the milky-white indium hydroxide precursor powder with uniform size obtained in the step (2) at the high temperature of 500-650 ℃ for 2-4 hours to obtain the indium oxide nanorod;
the diameter of the indium oxide nanorod is 30-50 nm, the length of the indium oxide nanorod is 1-5 mm, and the length-diameter ratio of the indium oxide nanorod ranges from 20-170.
2. The method of preparing indium oxide nanorods with uniform size according to claim 1, characterized in that: the molecular weight of the polyvinylpyrrolidone in the step (1) is 1300000.
3. The method of preparing indium oxide nanorods with uniform size according to claim 1, characterized in that:
in the reactant in the step (1), the concentration of the indium trichloride tetrahydrate is 15.25 mg/mL;
in the reactant in the step (1), the concentration of polyvinylpyrrolidone is 7.5-26 mg/mL;
in the reactant in the step (1), the concentration of KOH is 60 mg/mL.
4. The method for preparing indium oxide nanorods with uniform size according to any one of claims 1 to 3, characterized in that:
the stirring time in the step (1) is 1-30 minutes;
the reaction in the step (1) is carried out in a polytetrafluoroethylene lining;
the drying temperature in the step (1) is 60 ℃.
5. The method for preparing indium oxide nanorods with uniform size according to any one of claims 1 to 3, characterized in that: the centrifugal rotating speed of the gradient centrifugation in the step (2) is 500-2000 rpm.
6. The method for preparing indium oxide nanorods with uniform size according to claim 5, wherein: the centrifugal rotating speeds of the gradient centrifugation in the step (2) are 500rpm, 1000rpm, 1500rpm and 2000rpm in sequence.
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| CN108423642A (en) * | 2018-04-04 | 2018-08-21 | 南京邮电大学 | A kind of preparation method of small size Transition-metal dichalcogenide two-dimensional nano piece |
| CN108455659A (en) * | 2018-04-28 | 2018-08-28 | 电子科技大学 | A kind of preparation method of nano bar-shape indium oxide gas sensitive |
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| CN108423642A (en) * | 2018-04-04 | 2018-08-21 | 南京邮电大学 | A kind of preparation method of small size Transition-metal dichalcogenide two-dimensional nano piece |
| CN108455659A (en) * | 2018-04-28 | 2018-08-28 | 电子科技大学 | A kind of preparation method of nano bar-shape indium oxide gas sensitive |
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| "Effect of polyvinylpyrrolidone on morphology and structure of In2O3 nanorods by hydrothermal synthesis";Tzu-Tsung Tseng et al.;《Ceramics International》;20090415;第2837页摘要部分，第2838页第3段 * |
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