阅读说明：本技术 一种尺寸均匀的氧化铟纳米棒及其制备方法与应用 (Indium oxide nanorod with uniform size and preparation method and application thereof ) 是由 刘岚 彭泽飞 李林桦 郑荣敏 邓智富 邢舒婷 李俊云 伍垚屹 于 2019-09-20 设计创作，主要内容包括：本发明属于纳米氧化铟的制备技术领域,具体涉及一种尺寸均匀的氧化铟纳米棒及其制备方法与应用。该方法首先用四水合三氯化铟、聚乙烯吡咯烷酮(PVP)、聚乙二醇(PEG-600)、去离子水和KOH制备氢氧化铟前驱体粉体,然后将重新分散的氢氧化铟前驱体粉体进行梯度离心,最后经过高温煅烧即得到尺寸均匀的的氧化铟纳米棒。该的氧化铟纳米棒直径为30～50nm,长度为1～5μm,长径比的范围为20～170。纳米棒呈单根分散的形式存在,有利于其在光电器件、气敏、传感等方面的应用。其工艺简单可行,反应条件较为温和,便于大规模生产。(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.)

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 for reaction, cooling to room temperature after the 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 indium hydroxide precursor powder with uniform size obtained in the step (2) at high temperature to obtain the indium oxide nanorod.

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 0-26 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 claim 2, characterized in that: the volume ratio of the PEG-600 to the deionized water in the step (1) is 5: 0-5: 0.069.

5. The method for preparing indium oxide nanorods with uniform size according to claim 3, characterized in that:

The heating reaction condition in the step (1) is that the reaction is carried out for 36-72 hours at 180-210 ℃;

The high-temperature calcination in the step (3) is carried out at the temperature of 500-650 ℃ for 2-4 hours.

6. the method for preparing indium oxide nanorods with uniform size according to any one of claims 1 to 5, 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 ℃.

7. the method for preparing indium oxide nanorods with uniform size according to any one of claims 1 to 5, characterized in that: the centrifugal rotating speed of the gradient centrifugation in the step (2) is 500-2000 rpm.

8. the method for preparing indium oxide nanorods with uniform size according to claim 7, wherein: the centrifugal rotating speeds of the gradient centrifugation in the step (2) are 500rpm, 1000rpm, 1500rpm and 2000rpm in sequence.

9. An indium oxide nanorod with uniform size is characterized in that: the preparation method of any one of claims 1 to 8, wherein the indium oxide nanorods have a diameter of 30 to 50nm, a length of 1 to 5 μm, and an aspect ratio of 20 to 170.

10. The use of the uniform-sized indium oxide nanorods according to claim 9, characterized in that: the indium oxide nanorod is used in the fields of photoelectricity, gas sensitivity and sensing device materials.

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.