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Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof

An indium oxide-based, gas-sensitive material technology, applied in the preparation and application of nanomaterials, can solve the problems of high raw material cost, complicated process, low formaldehyde sensitivity, etc., and achieve the effect of good sensitivity and short response recovery time

Active Publication Date: 2014-06-25
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The results of the gas sensitivity test show that the sensitivity of methanol at 50ppm is as high as 25, but the sensitivity of formaldehyde is low (about 4), and toluene has almost no response; Switzerland "Sensors and Actuators, Series B: Chemical Sensors" (Sensors and Actuators B 155 (2011) 752-758) reported the use of indium acetylacetonate (In(acac) 3 ), ethylene glycol, sodium lauryl sulfate (surfactant) as raw materials to synthesize the precursor by hydrothermal method, and calcined at 350°C for 3 hours to obtain porous nanosheets of indium oxide, which are used for gas sensing test and gas sensing structure display , the porous nanosheets have high sensitivity to methanol, propanol, n-butanol, formaldehyde and acetone, but the sensitivity to toluene at 50ppm is only about 3.5
The above method of preparation has high cost of raw materials and complicated process. Although it has good gas-sensing performance, it is not suitable for mass production.

Method used

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  • Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof
  • Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof
  • Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Take 0.3mol / L InCl 3 2ml of the solution and 17ml of glycerol were placed in a polytetrafluoroethylene liner of a 50ml reactor, and stirred to form a uniform mixed solution. Then, 0.9 ml of ethylenediamine was added dropwise during stirring, and after stirring for 5 minutes, 0.66 g of surfactant cetyltrimethylammonium bromide (CTAB) was added, and stirred evenly again. Then seal the liner and put it into a stainless steel reaction kettle, heat it in an oven to 180°C for 12 hours; after the reaction is completed, take out the reaction kettle and cool it to room temperature under the air, and move the product into a centrifuge tube.

[0027] (2) The product was washed with deionized water and ethanol for 3 to 5 times. After centrifugation, the precipitate was transferred to a petri dish and dried in an oven at 50°C for 30 minutes to obtain a white three-dimensional flower-like hollow multi-level structure. indium oxide precursor.

[0028] (3) Put the indium oxide pr...

Embodiment 2

[0031] This example mainly investigates the effects of indium ion concentration, reaction time, reaction temperature and the amount of ethylenediamine added on the morphology of the obtained indium oxide during the preparation process of the multi-level structure of indium oxide. The specific experimental process is the same as in Example 1, the main difference is to change the concentration of indium ions, the reaction time, the reaction temperature and the amount of ethylenediamine added dropwise. The specific experimental parameters are shown in Table 1. It can be seen from the experimental results that the indium ion concentration and the reaction temperature have little effect on the sample morphology, but the reaction time is long and the amount of ethylenediamine added is large, and the sample morphology tends to form a three-dimensional flower-like hollow multi-level structure.

Embodiment 3

[0033] This embodiment mainly investigates the influence of the calcination temperature and calcination time on the composition of the obtained indium oxide sample during the preparation process of the multi-level structure of indium oxide. The specific experimental process is the same as step (3) of Example 1. The main difference is that the sintering temperature and calcination time are different. The specific experimental parameters are shown in Table 1. From the experimental results, it can be seen that the obtained product can be completely transformed at 260 ° C and above, and the calcination time is longer than 30 minutes. It is indium oxide, so the calcination temperature should be higher than 260°C, and the calcination time should be longer than 30min.

[0034] The relevant parameters of the examples of other preparation materials are listed in Table 1, please forgive me for not repeating them.

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Abstract

The invention discloses a preparation method of an indium oxide-based gas-sensitive material with a three-dimensional hollow multi-stage structure and an application thereof. The material is prepared by taking an indium salt, deionized water and glycerol as solvents, taking ethylene diamine as an indium ion ligand and taking hexadecyl trimethyl ammonium bromide as a surfactant with a hydro-thermal synthesis method, has an indium oxide nanosheet self-assembly three-dimensional flower-shaped hollow multi-stage structure, and is 0.5-3 mum in diameter. The preparation method has a simple process and low cost, is environmentally-friendly, and is suitable for large-scale production. As proved by an experiment for manufacturing a gas-sensitive sensor by using the material prepared with the method, the material has very high sensitivity to acetone and toluene, the minimum detection limit can be up to grade ppb, and a device has very short response time and restoration time, high stability and high selectivity and can be applied to gas-sensitive sensors of acetone and toluene.

Description

technical field [0001] The invention belongs to the preparation and gas-sensing application of semiconductor oxide gas-sensitive materials, and relates to the field of preparation and application of nanometer materials. Background technique [0002] Indium oxide (In 2 o 3 ) is an important n-type semiconductor material with a large band gap (3.55-3.75eV) and unique electrical, chemical and optical properties. It can be used in solar cells, transparent conductors, flat panel displays, and ultraviolet-visible lasers , detectors and gas sensors, etc., have a wide range of applications. [0003] Due to its small resistivity and high catalytic activity, the conductivity of indium oxide is very sensitive to the external environment, so it is suitable as a high-sensitivity gas sensor. The principle of indium oxide as a gas sensor is the change in conductivity caused by the adsorption of the measured gas and the surface reaction process. By detecting the electrical signal, the ga...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00G01N27/04
Inventor 张龙柳洋董红星
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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