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A kind of preparation method of highly sensitive optical ammonia-sensitive material

A sensitive and optical technology, applied in the field of ammonia-sensitive materials, can solve the problems of difficult industrialization, high production cost, complex process, etc., and achieve the effect of easy industrialization, fast response speed and simple process flow

Active Publication Date: 2019-01-25
ZHEJIANG TONGXING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A lot of research has been done on ammonia-sensitive materials at home and abroad, and many ammonia-sensitive materials with good selectivity and strong response intensity have been prepared. However, ammonia-sensitive materials with high sensitivity are usually accompanied by complicated processes and high production costs, making it difficult to realize industrialization.

Method used

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  • A kind of preparation method of highly sensitive optical ammonia-sensitive material
  • A kind of preparation method of highly sensitive optical ammonia-sensitive material
  • A kind of preparation method of highly sensitive optical ammonia-sensitive material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of nanoporous materials: use a solution mixed with hydrofluoric acid / ethanol / glycerol with a volume ratio of 3.5:1:0.005 as the electrolyte, and perform DC etching with an average etching current of 20mA / cm 2 , the etching time is 1200s, rinse with ethanol after etching, and dry with nitrogen to obtain nanoporous materials.

[0037] Preparation of the porous material carrier: the nanoporous material was oxidized at 550° C. for 1 hour to obtain the porous material carrier.

[0038]Preparation of ammonia-sensitive materials: Bromothymol blue is formulated into an ethanol solution with a mass percentage of 0.1% to form an ethanol solution of bromothymol blue, and then mixed with an aqueous solution of acetic acid with a mass percentage of 2% at a volume ratio of 10:0.5 for proton chemical treatment, and then loaded onto the surface of the porous material carrier by spin coating, and dried in a vacuum oven to obtain highly sensitive optical ammonia-sensitive mat...

Embodiment 2

[0041] Preparation of nanoporous materials: use a solution mixed with hydrofluoric acid / ethanol / glycerol with a volume ratio of 3.5:1:0.0005 as the electrolyte, and conduct DC etching with an average etching current of 100mA / cm 2 , the etching time is 200s, rinse with ethanol after etching, and blow dry with nitrogen to obtain nanoporous materials.

[0042] Preparation of the porous material carrier: the nanoporous material was oxidized at 450° C. for 3 hours to obtain the porous material carrier.

[0043] Preparation of ammonia-sensitive material: Bromocresol green is formulated into a 1% by mass ethanol solution to form an ethanol solution of bromcresol green, and then mixed with 2% by mass acetic acid solution at a volume ratio of 10:2 for proton chemical treatment, and then loaded onto the surface of the porous material carrier by dip-dyeing, and dried in a vacuum oven to obtain highly sensitive optical ammonia-sensitive materials.

[0044] The ammonia sensor made of this...

Embodiment 3

[0047] Preparation of nanoporous materials: use a solution mixed with hydrofluoric acid / ethanol / glycerol with a volume ratio of 3.5:1:0.0025 as the electrolyte, and conduct DC etching with an average etching current of 60mA / cm 2 , the etching time is 600s, rinse with ethanol after etching, and blow dry with nitrogen to obtain nanoporous materials.

[0048] Preparation of the porous material carrier: the nanoporous material was oxidized at 400° C. for 5 hours to obtain the porous material carrier.

[0049] Preparation of ammonia-sensitive materials: Bromophenol blue is made into 0.5% by mass ethanol solution to form an ethanol solution of bromophenol blue, and then mixed with 2% by mass acetic acid solution at a volume ratio of 10:1.5 for protonation treatment , and then loaded onto the surface of the porous material carrier by drop coating, and dried in a vacuum oven to obtain a high-sensitivity optical ammonia-sensitive material.

[0050] The ammonia sensor made of this ammo...

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Abstract

The invention discloses a method for preparing a high-sensitivity optical ammonia sensitive material. The method includes the following steps that 1, a P-shaped silicon slice is fixed into an electrolytic tank, a solution mixed by hydrofluoric acid, ethyl alcohol and glycerol serves as an electrolyte solution, electrochemistry direct-current etching is carried out, etching is carried out for 200 s to 1,200 s in the current of 20 mA / cm<2> to 100 mA / cm<2>, and then washing and drying are carried out; 2, oxidation is carried out for 1 hour to 5 hours at the temperature of 400 DEG to 550 DEG C; 3, acid-base sensitive dye and the ethyl alcohol are mixed, an acetic-acid water solution is added, a carrier of a nanometer porous material is loaded with an acid-base sensitive dye solution, drying is carried out, and the high-sensitivity optical ammonia sensitive material is obtained. According to the ammonia sensitive material, the porous material with the high specific surface area serves as the carrier, the loading capacity of an indicating agent is large, the sensitivity is high, and ammonia with the lowest value of 0.1 ppm can be detected; the response speed is high, the response time is in 10 s, and the method can be applied to online detection; the preparing technology is simple, and industrialization can be achieved.

Description

technical field [0001] The invention relates to the technical field of ammonia-sensitive materials, in particular to a preparation method of highly sensitive optical ammonia-sensitive materials. Background technique [0002] At present, there are many kinds of ammonia sensors used in the field of environmental protection. According to the detection principle used, there are mainly redox ammonia sensors, electrochemical ammonia sensors and photochemical ammonia sensors. [0003] Redox-type ammonia sensors mainly include metal oxide-based ammonia sensors and conductive polymer-based ammonia sensors. As a traditional ammonia sensor, the metal oxide ammonia sensor has the characteristics of low price and durability. However, this kind of sensor has high operating temperature, has potential safety hazards, and has poor gas selectivity and is easily disturbed. Although the conductive polymer ammonia sensor solves the problems of high temperature use and poor selectivity, it also ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31
CPCG01N21/31
Inventor 姚燕盛伟民李世雄徐晓军
Owner ZHEJIANG TONGXING TECH CO LTD
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