Silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material and preparation method thereof

A nitrogen dioxide, indium oxide technology, applied in the direction of analyzing materials, material analysis by electromagnetic means, measuring devices, etc., can solve problems such as reducing the working temperature of gas-sensitive materials, and achieve faster response recovery speed, enhanced sensitivity, and improved electronic The effect of the exchange reaction

Pending Publication Date: 2021-12-03
恩拓必(临沂)能源发展有限责任公司
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Abstract

The invention discloses a silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material and a preparation method thereof, and belongs to the technical field of sensing materials and preparation thereof. The preparation method of the nitrogen dioxide gas-sensitive material specifically comprises the following steps: dissolving 1, 4-terephthalic acid in N, N-dimethylformamide, adding indium salt, uniformly dispersing, performing thermal synthesis and calcining to obtain micron tubular indium oxide, dispersing the micron tubular indium oxide in a mixed solution of silver nitrate and sodium citrate, and dropwise adding a sodium borohydride solution to obtain the silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material. The silver-modified micron tubular indium oxide prepared by the invention has relatively high sensitivity to NO2 at room temperature, and is a high-performance gas sensitive material with potential application value.

Application Domain

Material analysis by electric/magnetic means

Technology Topic

Trisodium citrateIndium +8

Image

  • Silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material and preparation method thereof
  • Silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material and preparation method thereof
  • Silver-modified micron tubular indium oxide nitrogen dioxide gas-sensitive material and preparation method thereof

Examples

  • Experimental program(5)
  • Comparison scheme(2)
  • Effect test(1)

Example Embodiment

[0027] Example 1
[0028] A method of preparing a tubular indium oxide modified nitrogen dioxide sensitive material silver microns:
[0029] (1) 0.179g 1,4- terephthalic acid was dissolved in 60mL N, N- dimethylformamide (DMF) and stirred until the solution became clear, and then added 0.383g of indium nitrate hydrate (In (NO 3 ) 3 · 3h 2O) dispersion, ultrasonic until dissolved. The above solution was transferred to the autoclave, and the autoclave was placed in an oven at 100 deg.] C synthesis reaction heat 4h, centrifuged, washed and dried in the precursor 24h 80 deg.] C to obtain a tubular indium microns.
[0030] The tubular microns of indium oxide prepared in (2) in step (1) to give the precursor was heated to 450 deg.] C at a heating rate of 5 ℃ / min, and calcined 4h, to give a tubular indium microns.
[0031] (3) Weigh 80mg step (2) (0.288 mmol) of indium oxide prepared tubular microns dispersed in 100mL of silver nitrate (silver nitrate concentration of 0.5mmol / L) concentration of 1.5mL of sodium citrate (sodium citrate of 30mmol / L) mixed solution, stirred for 30min until fully dissolved to obtain a solution a, then solution a was added dropwise 6mL temperature of 0 ℃ sodium borohydride (concentration of sodium borohydride was 10mmol / L) was continuously stirred after 5min, the reaction was allowed to stand 2h, to give a dark brown suspension was then centrifuged and washed three times with deionized water and ethanol, and dried at 80 deg.] C 24h to give a silver indium oxide-modified tubular microns dioxide sensitive material. This XRD pattern of the tubular microns indium oxide modified nitrogen dioxide sensitive material silver obtained in Preparation Example See figure 1;From figure 1 As can be seen in the XRD patterns of the samples prepared using the present invention 2θ = 21.4 °, 30.6 °, 35.5 °, 37.8 °, 51.0 °, 60.5 ° and a diffraction peak corresponding to international standard diffraction data card (In 2 O 3 ) JPCDS No.06-0416 consistent, 2θ = 38.2 ° and 44.3 ° and a diffraction peak corresponding to international standard diffraction data card (Ag) JPCDS No.87-0597 match, and no other hetero peaks, indicating successful silver in the load 2 O 3 surface.
[0032] This SEM view of a tubular indium silver microns dioxide sensitive material obtained in Example MODIFIED see figure 2;From figure 2 As can be seen in samples prepared using the present invention, a length of 6 ~ 7μm hexagonal tubular stacked together.
[0033] The tubular micron silver indium oxide modified nitrogen dioxide gas-sensitive material obtained in Preparation Example of the present embodiment of the gas sensing different concentrations of nitrogen dioxide gas, see graph in response image 3 ,From image 3 As can be seen in NO 2 Concentration increases the sensitivity of the silver modified microns tubular indium oxide sensor gradually increases, and when concentrations as low as 0.5ppm, the sensitivity was 6.5, showing good NO 2 Gas sensing performance.
[0034] Preparation of silver modified embodiment of the present loading of the tubular indium microns nitrogen dioxide gas sensing material of silver was 6.3%.

Example Embodiment

[0035] Example 2
[0036] (1) terephthalic acid was dissolved 0.45g 1,4- 80mL N, N- dimethylformamide (DMF) and stirred until the solution became clear, then adding 0.96g of indium nitrate hydrate (In (NO 3 ) 3 · 3h 2 O) dispersion, ultrasonic until dissolved. The above solution was transferred to the autoclave, and the autoclave was placed in an oven at 100 deg.] C synthesis reaction heat 14H, centrifuged, washed and dried in the precursor 24h 80 deg.] C to obtain a tubular indium microns.
[0037] (2) Preparation of step (1) obtained indium oxide precursor tubular microns at a ramp rate 2 ℃ / min heating to 475 ℃, calcined 5h, to obtain a tubular indium microns.
[0038] (3) Weigh 80mg step (2) of indium oxide prepared tubular microns dispersed in 90mL of silver nitrate (silver nitrate concentration of 0.5mmol / L) 2mL with sodium citrate (sodium citrate concentration of 30mmol / L) the mixed solution was stirred for 30min until fully dissolved to obtain a solution a, then solution a was added dropwise 5.7mL temperature of 0 ℃ sodium borohydride (concentration of sodium borohydride was 10mmol / L) was continuously stirred 5min, static the reaction set 2h, to give a dark brown suspension was then centrifuged and washed three times with deionized water and ethanol, and dried at 80 deg.] C 24h to give a silver indium oxide modified nitrogen dioxide microns tubular gas-sensitive material, silver loading is 5.7%.

Example Embodiment

[0039] Example 3
[0040] (1) terephthalic acid was dissolved 0.21g 1,4- 70mL N, N- dimethylformamide (DMF) and stirred until the solution became clear, then adding 0.45g of indium nitrate hydrate (In (NO 3 ) 3 · 3h 2 O) dispersion, ultrasonic until dissolved. The above solution was transferred to the autoclave, and the autoclave was placed in an oven at 90 deg.] C synthesis reaction heat 24h, centrifuged, washed and dried in the precursor 24h 80 deg.] C to obtain a tubular indium microns.
[0041] (2) Preparation of step (1) obtained in the tubular indium oxide precursor was heated to 500 microns deg.] C at a heating rate of 4 ℃ / min, and calcined 4h, to give a tubular indium microns.
[0042] (3) Weigh 80mg step (2) obtained in Preparation microns tubular indium oxide dispersed in 70mL of silver nitrate (silver nitrate concentration of 0.5mmol / L) and 1.5mL of sodium citrate (sodium citrate concentration of 30mmol / L ) of the mixed solution was stirred for 30min until fully dissolved to obtain a solution a, then solution a was added dropwise 4.7mL temperature sodium borohydride (sodium borohydride concentration is 10mmol / L) was continuously stirred 0 ℃ after 5min, the reaction was allowed to stand 2h, to give a dark brown suspension was then centrifuged and washed three times with deionized water and ethanol, and dried at 80 deg.] C 24h to give a silver indium oxide modified nitrogen dioxide microns tubular gas-sensitive material, the silver loading 4.5%.

PUM

PropertyMeasurementUnit
Diameter600.0 ~ 800.0nm
Length5.0 ~ 7.0µm

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