Preparation method of silver-doped nano tin dioxide powder

Abstract

The invention belongs to the technical field of preparation of tin dioxide powder, and relates to a preparation method of silver-doped nano tin dioxide powder. The preparation method comprises the following steps of: firstly adding citric acid solution, a surface active agent and ammonia water sequentially into mixed solution of soluble tin salt and soluble silver salt, and adjusting the pH value of a reaction system to 2.5-11, and under the action of constant-temperature magnetic stirring, generating precursor sol; then, adding the precursor sol into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle in a drying oven, carrying out hydrothermal reaction, taking out the hydrothermal reaction kettle after hydrothermal reaction, cooling, and sampling; and finally, cleaning, drying and grinding to prepare a finished nano tin dioxide powder product. The tin dioxide powder prepared by the method has the advantages of fewer granularity, narrow distribution range and good dispersity; and a gas sensor based on the tin dioxide powder material has good detection performance for fault gas in transformer oil.

Description

technical field

[0001] The invention belongs to the technical field of tin dioxide powder preparation, in particular to a preparation method of silver-doped nano tin dioxide powder material. Background technique

[0002] On-line monitoring of dissolved gas in transformer oil is one of the key technologies for the implementation of condition-based maintenance of power transformers. Sensor gas detection technology is the core of on-line monitoring of dissolved gas in oil, which directly affects the correctness, stability and service life of the online monitoring system. Semiconductor metal oxide SnO 2 Base gas sensor is currently the most commonly used gas sensor for on-line monitoring of dissolved gas in oil. For the detection of trace hydrocarbon gas dissolved in oil, there are poor selectivity, serious cross-sensitivity, insufficient sensitivity, high working temperature, poor stability, and repeatability. Insufficient performance and other shortcomings, noble metal doping...

Examples

Embodiment 1

[0024] Weigh 3.506g of tin tetrachloride pentahydrate and 0.0085g of silver nitrate (so that the doping amount of silver is 0.5%), add deionized water to prepare 100ml of a mixed solution of 0.1mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.1mol / L ammonia solution, and slowly add the configured ammonia solution into the mixed solution with a basic burette to adjust the pH value of the reaction system To 8.5, react under constant temperature magnetic stirring at 80°C for 120min to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and react under the condition of 150°C for 10h, and take out the The hydrothermal reaction kettle was cooled to room temperature and sampled; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 80°C for 12 hours, and ground to make nano-tin dioxide powder Body finished product, the pa...

Embodiment 2

[0026] Weigh 2.256g of stannous chloride dihydrate and 0.017g of silver nitrate (so that the doping amount of silver is 1%), add deionized water to prepare 100ml of a mixed solution of 0.1mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.2mol / L ammonia solution, slowly add the configured ammonia solution into the mixed solution with a basic burette, and adjust the pH value of the reaction system To 9, react for 120 minutes under constant temperature magnetic stirring at 80°C to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and perform a hydrothermal reaction at 160°C for 12 hours, then take out the The hydrothermal reaction kettle was cooled to room temperature and sampled; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 90°C for 12 hours, and ground to make nano-tin dioxide powder finished product. Its...

Embodiment 3

[0028] Weigh 7.012g of tin tetrachloride pentahydrate and 0.068g of silver nitrate (so that the doping amount of silver is 2%), add deionized water to prepare 100ml of a mixed solution of 0.2mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.3mol / L ammonia solution, slowly add the configured ammonia solution into the mixed solution with a basic burette, and adjust the pH value of the reaction system To 9.5, react under constant temperature magnetic stirring at 80°C for 120min to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and conduct a hydrothermal reaction at 170°C for 14h, then take out the Hydrothermal reaction kettle, cooled to room temperature, sampling; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 100°C for 12 hours, and ground to make nano-tin dioxide powder Body finished product, the particle...

technical field

[0001] The invention belongs to the technical field of tin dioxide powder preparation, in particular to a preparation method of silver-doped nano tin dioxide powder material. Background technique

[0002] On-line monitoring of dissolved gas in transformer oil is one of the key technologies for the implementation of condition-based maintenance of power transformers. Sensor gas detection technology is the core of on-line monitoring of dissolved gas in oil, which directly affects the correctness, stability and service life of the online monitoring system. Semiconductor metal oxide SnO 2 Base gas sensor is currently the most commonly used gas sensor for on-line monitoring of dissolved gas in oil. For the detection of trace hydrocarbon gas dissolved in oil, there are poor selectivity, serious cross-sensitivity, insufficient sensitivity, high working temperature, poor stability, and repeatability. Insufficient performance and other shortcomings, noble metal doping...

Examples

Embodiment 1

[0024] Weigh 3.506g of tin tetrachloride pentahydrate and 0.0085g of silver nitrate (so that the doping amount of silver is 0.5%), add deionized water to prepare 100ml of a mixed solution of 0.1mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.1mol / L ammonia solution, and slowly add the configured ammonia solution into the mixed solution with a basic burette to adjust the pH value of the reaction system To 8.5, react under constant temperature magnetic stirring at 80°C for 120min to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and react under the condition of 150°C for 10h, and take out the The hydrothermal reaction kettle was cooled to room temperature and sampled; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 80°C for 12 hours, and ground to make nano-tin dioxide powder Body finished product, the pa...

Embodiment 2

[0026] Weigh 2.256g of stannous chloride dihydrate and 0.017g of silver nitrate (so that the doping amount of silver is 1%), add deionized water to prepare 100ml of a mixed solution of 0.1mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.2mol / L ammonia solution, slowly add the configured ammonia solution into the mixed solution with a basic burette, and adjust the pH value of the reaction system To 9, react for 120 minutes under constant temperature magnetic stirring at 80°C to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and perform a hydrothermal reaction at 160°C for 12 hours, then take out the The hydrothermal reaction kettle was cooled to room temperature and sampled; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 90°C for 12 hours, and ground to make nano-tin dioxide powder finished product. Its...

Embodiment 3

[0028] Weigh 7.012g of tin tetrachloride pentahydrate and 0.068g of silver nitrate (so that the doping amount of silver is 2%), add deionized water to prepare 100ml of a mixed solution of 0.2mol / L, add 10ml of 0.1 mol / L citric acid solution and 2 g polyethylene glycol 4000, configure 500ml 0.3mol / L ammonia solution, slowly add the configured ammonia solution into the mixed solution with a basic burette, and adjust the pH value of the reaction system To 9.5, react under constant temperature magnetic stirring at 80°C for 120min to generate a precursor sol; put the precursor sol into a hydrothermal reaction kettle, place it in an oven, and conduct a hydrothermal reaction at 170°C for 14h, then take out the Hydrothermal reaction kettle, cooled to room temperature, sampling; the sample was ultrasonically washed 10 times with deionized water and 10 times with absolute ethanol, dried at 100°C for 12 hours, and ground to make nano-tin dioxide powder Body finished product, the particle...

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