CN110550652A - preparation method of hexagonal indium oxide hollow box with special appearance - Google Patents
preparation method of hexagonal indium oxide hollow box with special appearance Download PDFInfo
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- CN110550652A CN110550652A CN201910827046.3A CN201910827046A CN110550652A CN 110550652 A CN110550652 A CN 110550652A CN 201910827046 A CN201910827046 A CN 201910827046A CN 110550652 A CN110550652 A CN 110550652A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/40—Particle morphology extending in three dimensions prism-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
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.
Description
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.
Example 1:
(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, 0.07 g of terephthalic acid and 0.073 g of indium nitrate hydrate are accurately weighed by an electronic analytical balance and poured into the beaker filled with 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 min after the temperature is raised to 120 ℃, immediately taking out the beaker 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 calcining. Wherein the temperature rising rate is controlled to be 1 minute and one degree till 400 ℃, the temperature is preserved for 3 hours, the temperature reduction system is controlled to be 3 ℃ per minute, and the light yellow powdery sample can be obtained after the calcination is finished.
example 2:
(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, 0.08 g of terephthalic acid and 0.06 g of indium nitrate hydrate are accurately weighed by an electronic analytical balance and poured into the beaker filled with 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 40 min after the temperature is raised to 120 ℃, immediately taking out the beaker 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 calcining. Wherein the temperature rising rate is controlled to be 1 minute and one degree till 450 ℃, the temperature is preserved for 3 hours, the temperature reduction system is controlled to be 3 ℃ per minute, and the light yellow powdery sample can be obtained after the calcination is finished.
Example 3:
(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 g of terephthalic acid and 0.08 g of indium nitrate hydrate are accurately weighed by an electronic analytical balance and poured into the beaker filled with 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 50 min after the temperature is raised to 120 ℃, immediately taking out the beaker after heating, 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 calcining. Wherein the temperature rising rate is controlled to be 1 minute and one degree till 400 ℃, the temperature is preserved for 3 hours, the temperature reduction system is controlled to be 3 ℃ per minute, and the light yellow powdery sample can be obtained after the calcination is finished.
Example 4:
(1) taking 160 mL of DMF by using a measuring cylinder, putting the DMF into 1 clean and dry 250 mL beaker, putting the beaker into a clean magnetic rotor, accurately weighing 0.055 g of terephthalic acid and 0.06 g of indium nitrate hydrate by using an electronic analytical balance, pouring the terephthalic acid and the indium nitrate hydrate into the beaker filled with the DMF, and putting the beaker on a magnetic stirrer for stirring;
(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 min after the temperature is raised to 120 ℃, immediately taking out the beaker 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 calcining. Wherein the temperature rising rate is controlled to be 1 minute and one degree till 450 ℃, the temperature is preserved for 3 hours, the temperature reduction system is controlled to be 3 ℃ per minute, and the light yellow powdery sample can be obtained after the calcination is finished.
Claims (1)
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.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988460A (en) * | 2022-07-06 | 2022-09-02 | 重庆大学 | Indium oxide nano material and application thereof |
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| CN105668612A (en) * | 2016-03-15 | 2016-06-15 | 济南大学 | Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor |
| CN108663417A (en) * | 2018-06-22 | 2018-10-16 | 山东大学 | One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive |
| CN108821330A (en) * | 2018-08-01 | 2018-11-16 | 济南大学 | A kind of preparation method of the indium oxide hollow pipe with hierarchical structure |
| CN109019672A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of porous oxidation indium micro-pipe preparation method with unique morphology |
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- 2019-09-03 CN CN201910827046.3A patent/CN110550652A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668612A (en) * | 2016-03-15 | 2016-06-15 | 济南大学 | Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor |
| CN108663417A (en) * | 2018-06-22 | 2018-10-16 | 山东大学 | One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive |
| CN108821330A (en) * | 2018-08-01 | 2018-11-16 | 济南大学 | A kind of preparation method of the indium oxide hollow pipe with hierarchical structure |
| CN109019672A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of porous oxidation indium micro-pipe preparation method with unique morphology |
Non-Patent Citations (1)
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| YUNSHI LIU等: "Metal-organic-framework-derived In2O3 microcolumnar structures embedded with Pt nanoparticles for NO2 detection near room temperature", 《CERAMICS INTERNATIONAL》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988460A (en) * | 2022-07-06 | 2022-09-02 | 重庆大学 | Indium oxide nano material and application thereof |
| CN114988460B (en) * | 2022-07-06 | 2024-02-13 | 重庆大学 | Indium oxide nano material and application thereof |
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Application publication date: 20191210 |