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Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S

An iron molybdate, micro-nano technology, applied in the field of preparation of H2S gas sensor materials, can solve the problems of insufficient sensor stability and complex preparation process, and achieve the effects of short response-recovery time, good selectivity and high sensitivity

Inactive Publication Date: 2015-07-22
三亚哈尔滨工程大学南海创新发展基地
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past ten years, domestic and foreign in H 2 Great progress has been made in the research, development and application of S gas-sensing materials, but there are still some problems to be solved, such as gas-sensing materials with high sensitivity (especially for low concentration H 2 S), fast response-recovery and other aspects cannot be satisfied at the same time; the stability of the sensor is not enough; the preparation process is complicated

Method used

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  • Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S
  • Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S
  • Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of raw materials: Calcining ammonium molybdate powder in air at 500°C for 4 hours to prepare MoO 3 powder; 35mg of MoO 3 Powder, 0.6g of urea and 35mg of thioacetamide are dissolved in 15ml of deionized water and 25ml of ethanol mixed solution, placed in an autoclave, heated in an oven at 200°C for 24 hours, cleaned and dried after cooling, to obtain flower clusters MoS 2 raw materials.

[0021] (2) Add 1g MoS 2 The powder was annealed in air at 500°C for 4 hours.

[0022] (3) Dissolve 0.075g of the annealed product in 300mL of 0.014mol / L Fe(NO 3 ) 3 In the solution, stir in a water bath at 50°C for 2 hours, and filter with suction.

[0023] (4) Add all the products from the previous step to 300mL of 0.014mol / L Fe(NO 3 ) 3 The solution was stirred in a 50°C water bath for 2 hours.

[0024] (5) The obtained product was vacuum-dried at 40°C.

[0025] (6) The obtained product was heated at 500° C. for 4 hours at a heating rate of 5° C. / min.

Embodiment 2

[0027] (1) Preparation of raw materials: Calcining ammonium molybdate powder in air at 500°C for 4 hours to prepare MoO 3 powder; 35mg of MoO 3 Powder, 0.6g of urea and 35mg of thioacetamide are dissolved in 15ml of deionized water and 25ml of ethanol mixed solution, placed in an autoclave, heated in an oven at 200°C for 24 hours, cleaned and dried after cooling, to obtain flower clusters MoS 2 raw materials.

[0028] (2) Add 1g MoS 2 The powder was annealed in air at 500°C for 4 hours.

[0029] (3) Dissolve 0.01g of the annealed product in 300mL of 0.02mol / L Fe(NO 3 ) 3 In the solution, stir in a water bath at 50°C for 2 hours, and filter with suction.

[0030] (4) Add all the products from the previous step to 300mL of 0.02mol / L Fe(NO 3 ) 3 The solution was stirred in a 50°C water bath for 2 hours.

[0031] (5) The obtained product was vacuum-dried at 40°C.

[0032] (6) The obtained product was heated at 500° C. for 4 hours at a heating rate of 5° C. / min.

Embodiment 3

[0034] (1) Preparation of raw materials: Calcining ammonium molybdate powder in air at 500°C for 4 hours to prepare MoO 3 powder; 35mg of MoO 3 Powder, 0.6g of urea and 35mg of thioacetamide are dissolved in 15ml of deionized water and 25ml of ethanol mixed solution, placed in an autoclave, heated in an oven at 200°C for 24 hours, cleaned and dried after cooling, to obtain flower clusters MoS 2 raw materials.

[0035] (2) Add 1g MoS 2 The powder was annealed in air at 500°C for 4 hours.

[0036] (3) Dissolve 0.01g of the annealed product in 300mL of 0.02mol / L Fe(NO 3 ) 3 In the solution, stir in a water bath at 60°C for 2 hours, and filter with suction.

[0037] (4) Add all the products from the previous step to 300mL of 0.02mol / L Fe(NO 3 ) 3 The solution was stirred in a 60°C water bath for 2 hours.

[0038] (5) The obtained product was vacuum-dried at 40°C.

[0039] (6) The obtained product is heated at 500°C for 3 hours at a heating rate of 5°C / min.

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Abstract

The invention provides a method for preparing iron molybdate micro-nano materials with the sensitive feature for low-concentration H2S. The method comprises the steps of calcinating ammonium molybdate powder for four hours at the temperature of 500 DEG C, dissolving 30-35mg of MoO3 powder, 0.5-0.6g of urea and 30-35mg of thioacetamide in a mixed solution containing 15ml of deionized water and 25ml of ethyl alcohol, conducting heating for 24 hours at the temperature of 200 DEG C to obtain flower-shaped MoS2 powder, calcinating the MoS2 powder in the air for 2-5 hours at the temperature of 400-600 DEG C, dissolving the obtained product in a Fe(NO3)3 solution, conducting stirring for 1-3 hours in a 50-60 DEG C water bath, conducting suction filtration, adding the product obtained in the last step in the Fe(NO3)3 solution, then conducting stirring for 1-3 hours in the 50-60 DEG C water bath, conducting vacuum drying, conducting calcination for 3-5 hours in the air at the 5 DEG C / min heating rate at the temperature of 400-600 DEG C, conducting natural cooling, and obtaining the iron molybdate micro-nano materials with the sensitive feature for the low-concentration H2S. The method for preparing the iron molybdate micro-nano materials is simple, the obtained iron molybdate micro-nano materials are high in sensitivity for the low-concentration H2S, good in selection performance and short in response-recovery time, and at the temperature of 270 DEG C, the 0.5ppm H2S gas can be detected.

Description

technical field [0001] The invention relates to a method for preparing a nanostructure semiconductor oxide gas sensor material, specifically a H 2 The preparation method of the S gas-sensitive material can be. Background technique [0002] Hydrogen sulfide is an acute and highly toxic gas. Human inhalation of a small amount of high-concentration hydrogen sulfide can be fatal in a short time. Low concentrations of hydrogen sulfide have effects on the eyes, respiratory system and central nervous system. At the same time, H 2 S is also a flammable gas, which can form an explosive mixture when mixed with air, and can cause combustion and explosion when exposed to open flame and high heat. It reacts violently with concentrated nitric acid, oleum or other strong oxidizing agents, resulting in an explosion. h 2 S gas is heavier than air and can spread to a relatively long distance at a lower place, and it will cause back-burning when it encounters an open flame. [0003] In t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/00B82Y30/00
Inventor 陈玉金刘照虹吴红雨徐铮朱春玲
Owner 三亚哈尔滨工程大学南海创新发展基地