阅读说明：本技术 一种具有特殊形貌的六棱氧化铟空心盒子的制备方法 (preparation method of hexagonal indium oxide hollow box with special appearance ) 是由 宋鹏 田哲宾 王�琦 孙静 于 2019-09-03 设计创作，主要内容包括：本发明提供了一种具有特殊形貌的六棱氧化铟空心盒子的制备方法。该制备方法具体包括：以N-N二甲基甲酰胺,对苯二甲酸和硝酸铟水合物为原料,经油浴反应、煅烧处理,得到六棱空心盒子结构的氧化铟。多孔结构具有较大的表面积,可以有效吸附更多的氧气和目标气体,空心结构可以有效提高材料的利用率,提高传感性能。因此兼备多孔及空心结构将有助于改善性能。本实验不使用昂贵的表面活性剂,成本比较低,对甲醛气体具有良好的气敏性能,因此在甲醛气体检测方面具有长远的应用前景。(The invention provides a preparation method of a hexagonal indium oxide hollow box with a special appearance. The preparation method specifically comprises the following steps: N-N dimethylformamide, terephthalic acid and indium nitrate hydrate are used as raw materials, and the indium oxide with the hexagonal hollow box structure is obtained through oil bath reaction and calcination treatment. The porous structure has a larger surface area, can effectively adsorb more oxygen and target gas, and the hollow structure can effectively improve the utilization rate of materials and improve the sensing performance. Thus, having both porous and hollow structures will help improve performance. The experiment does not use expensive surfactant, has lower cost and good gas-sensitive performance to formaldehyde gas, and thus has long-term application prospect in the aspect of formaldehyde gas detection.)

1. A preparation method of a hexagonal indium oxide hollow box with a special appearance comprises the following specific synthesis steps:

(1) Firstly, 160 mL of DMF is taken by a measuring cylinder and put into 1 clean and dry 250 mL beaker, and a clean magnetic rotor is put into the beaker, 0.05 to 0.08 g of terephthalic acid and 0.05 to 0.08 g of indium nitrate hydrate are accurately weighed by an electronic analytical balance and poured into the beaker filled with the DMF, and the beaker is put on a magnetic stirrer to be stirred;

(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 30-50 min after the temperature is raised to 120 ℃, taking out the beaker immediately after the heating is finished, standing, cooling, and washing the precipitate;

(3) and uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcination, wherein the temperature rise rate is controlled to be 1 minute and one degree till 400-500 ℃, the temperature is kept for 3 hours, the temperature drop rate is controlled to be 2 ~ 3 ℃ per minute, and the calcination is finished, so that a light yellow powdery sample can be obtained.

Technical Field

the invention relates to a preparation method of a hexagonal indium oxide hollow box with a special shape, and belongs to the technical field of advanced nano functional material preparation processes.

Background

in daily life, people are seriously damaged by industrial production waste gas, automobile exhaust, PM2.5 and other gases when going out, and are influenced by toxic gases such as formaldehyde, benzene and the like when going home. Therefore, it is very important to research and develop a high-performance gas sensor, whether the gas sensor is needed for detecting environmental pollution gas or for ensuring quality of life and industrial safety. With the increasing attention of people to the environmental protection problem and the strict monitoring of the emission of toxic and harmful gases, various gas inspection and early warning devices with different functions are developed, and further, the industrialization and the commercialization are achieved. The semiconductor gas sensor has the characteristics of high detection sensitivity, quick response recovery, simple circuit, simplicity in operation, small element size, low price and the like, and is widely applied to various gas detection fields.

in ₂ O ₃ has a large forbidden bandwidth, the energy band gap is close to GaN, the main factor influencing the performance of In ₂ O ₃ nanomaterial is its structural morphology, so at present, many researchers are dedicated to the research of controlling the formation of In ₂ O ₃ crystal morphology so as to improve its various performances In the light region, In recent years, developed countries In europe and the united states successively report the application of indium oxide nanomaterials In the field of photoelectric thin films, at present, researchers prepare one-dimensional, two-dimensional, three-dimensional In ₂ O ₃ nanomaterials by using a nanomaterial synthesis method of a gas phase method, a solid phase method, a liquid phase method, and the like, which are widely applied In the fields of optics, magnetics, electronics, medical care and the like, In order to improve recognition functions, besides selecting a good matrix material, modifying surface area by doping, compounding and surface modification, designing and preparing porous surface area and having high specific surface area and high active site density, and improving the surface area of the porous material by using a high-temperature-sensitive gas reduction technology, which is a more highly-sensitive material, and particularly, the research of the gas reduction of the gas produced nanomaterial has been greatly increased In the characteristics of the research of the gas reduction of the gas generated by using a gas ₂ O ₂, the gas-based on the research of the surface-based on the research of the surface-gas-sensitive material, the gas-sensitive material, the research of the gas-sensitive material, the gas-sensitive material, the gas-gas.

Disclosure of Invention

the invention aims to overcome the defects of the prior art and provide a preparation method of a hexagonal indium oxide hollow box with a special appearance. Has the characteristics of low cost, simple production process, high yield, no environmental pollution and easy industrialized large-scale production. The sensitivity of the obtained indium oxide gas-sensitive material with the porous structure is greatly improved, and the indium oxide gas-sensitive material can be used in the fields of gas sensors and the like. The technical scheme for realizing the purpose of the invention is as follows: a preparation method of a hexagonal indium oxide hollow box with a special appearance is characterized by comprising the following steps: N-N dimethylformamide, terephthalic acid and indium nitrate hydrate are used as raw materials, and the indium oxide box with the hollow structure is obtained through oil bath reaction and calcination treatment. The method has simple production process, does not use expensive surface active agent, has lower cost, and the obtained indium oxide can be used as a gas-sensitive material and has a hollow structure. Has good gas-sensitive performance to formaldehyde gas, thereby having long-term application prospect in the aspect of formaldehyde gas detection. The specific synthesis steps are as follows:

(1) Firstly, 160 mL of DMF is taken by a measuring cylinder and put into 1 clean and dry 250 mL beaker, and a clean magnetic rotor is put into the beaker, 0.05 to 0.08 g of terephthalic acid and 0.05 to 0.08 g of indium nitrate hydrate are accurately weighed by an electronic analytical balance and poured into the beaker filled with the DMF, and the beaker is put on a magnetic stirrer to be stirred;

(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 30-50 min after the temperature is raised to 120 ℃, taking out the beaker immediately after the heating is finished, standing, cooling, and washing the precipitate;

(3) uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcination, wherein the temperature rise rate is controlled to be 1 minute and one degree till 400-500 ℃, the temperature is kept for 3 hours, the temperature reduction system is controlled to be 2 ~ 3 ℃ per minute, and the calcination is finished, so that a light yellow powdery sample can be obtained.

Drawings

FIG. 1 is a low-magnification SEM image of a hexagonal indium oxide hollow box with a special morphology.

FIG. 2 is a high power SEM image of hexagonal indium oxide hollow boxes with special morphology.

FIG. 3 is a TEM image of a hexagonal indium oxide hollow box with a special morphology.

FIG. 4 is a graph of the XED of hexagonal indium oxide hollow boxes with a particular morphology.

FIG. 5 is a BET diagram of hexagonal indium oxide hollow boxes with a particular morphology.

Detailed Description

The following is a detailed description of the embodiments of the present invention, which is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.