Preparation method of nanometer tin oxide fibre air-sensitive film

A nano-tin oxide and nano-fiber membrane technology, applied in the direction of material electrochemical variables, can solve problems such as difficult redissolving, difficult spinning solution configuration, and polyvinylpyrrolidone precipitation.

Inactive Publication Date: 2008-05-21
TIANJIN POLYTECHNIC UNIV
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Problems solved by technology

[0008] Patent CN 1858308 adopts electrospinning method to prepare low-density tin dioxide laser target material. In this patent, it is reported that polyvinylpyrrolidone / ethanol solution and tin chloride tetrahydrate / ethanol solution are blended at high speed to prepare spinning solution. The method has the disadvantage of difficult configuration of the spinning solution, and the blending of the two solutions can easily cause the precipitation of polyvinylpyrrolidone and it is difficult to redissolve

Method used

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  • Preparation method of nanometer tin oxide fibre air-sensitive film

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Comparison scheme
Effect test

Embodiment 1

[0025] Take 3 g of polyvinylpyrrolidone with a viscosity-average molecular weight of 600,000 and pour it into 57 mL of N,N-dimethylformamide solvent, stir at high speed until completely dissolved, and prepare a 5% polyvinylpyrrolidone / DMF solution. Weigh 1g of tin chloride tetrahydrate and dissolve it in 9mL of ethanol, then mix the two solutions and stir at high speed for 1 hour to obtain a sol-gel electrospinning solution; inject the prepared sol-gel spinning solution into the electrospinning device In the process, the aluminum chloride / polyvinylpyrrolidone nanofiber membrane was electrospun under the conditions of a voltage of 25kV, an extrusion speed of 10mL / min, and a receiving distance of 10cm; finally, the prepared tin chloride / polyvinylpyrrolidone nanofiber membrane Place in a muffle furnace, raise the temperature to 450°C at a rate of 50°C / h, and dry for 5h to obtain a dry tin chloride nanofiber gas-sensitive membrane.

Embodiment 2

[0027] Take 3g of polyvinylpyrrolidone with a viscosity-average molecular weight of 900,000 and pour it into 47mL N, N-dimethylformamide solvent, stir at a high speed until completely dissolved, and prepare a 6% polyvinylpyrrolidone ethanol / DMF solution. Weigh 2g of tin chloride tetrahydrate and dissolve it in 8mL of ethanol, then mix the two solutions and stir at high speed for 1 hour to obtain a sol-gel electrospinning solution; inject the prepared sol-gel spinning solution into the electrospinning device In the process, the aluminum chloride / polyvinylpyrrolidone nanofiber membrane was electrospun under the conditions of a voltage of 30kV, an extrusion speed of 5mL / min, and a receiving distance of 10cm; finally, the prepared tin chloride / polyvinylpyrrolidone nanofiber membrane Place it in a muffle furnace, raise the temperature to 450°C at a rate of 50°C / h, and calcinate for 5h to obtain a nano-tin oxide fiber gas-sensitive film.

Embodiment 3

[0029]Take 3g of polyvinylpyrrolidone with a viscosity-average molecular weight of 1.1 million and pour it into 40mL N, N-dimethylformamide solvent, stir at a high speed until completely dissolved, and prepare a 7% polyvinylpyrrolidone / DMF solution, weighing Dissolve 2 g of tin chloride tetrahydrate in 10 mL of ethanol, then mix the two solutions and stir at high speed for 1 hour to obtain a sol-gel electrospinning solution; inject the prepared sol-gel spinning solution into the electrospinning device , at a voltage of 30kV, an extrusion speed of 8mL / min, and a receiving distance of 15cm, electrospun into an aluminum chloride / polyvinylpyrrolidone nanofiber membrane; finally, the prepared tin chloride / polyvinylpyrrolidone nanofiber membrane was placed In a muffle furnace, the temperature was raised to 600° C. at a rate of 50° C. / h, and calcined for 5 hours to obtain a nano-tin oxide fiber gas-sensing membrane.

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Abstract

The present invention relates to a preparation technique for preparing nanometer tin anhydride fiber gas sensor film material by using an electrostatic spinning method. The present invention comprises: 1, collosol gel static filature liquid allocation: polyethylene ketopyrrolidine is poured into dissolvent containing N, N-dimethyfomamide (DMF); the dissolvent is mixed at high speed to be completely dissolved; the polyethylene ketopyrrolidine/DMF dissolvent with the concentration of 5 wt percent to 8 wt percent is produced; and then, the dissolvent is mixed with qua-water stannic chloride water solution with the concentration of 10 wt percent to 40 wt percent; wherein, the weight ratio of the polyethylene ketopyrrolidine and the stannic chloride is between 3 to 1 and 3 to 4; the product is made after being mixed for 3 hours. 2. electrostatic spinning: The prepared collosol gel static filature liquid is injected into a electrostatic spinning device and transformed into aluminum chloride/ polyethylene ketopyrrolidine nanometer fibrous coat on the conditions that the voltage is between 25 Kv and 35 Kv; the extrusion speed is between 1 ml/min and 10 ml/min and the receive distance is between 10 cm and 20 cm through the electrostatic spinning. 3. calcination: finally, the prepared aluminum chloride/ polyethylene ketopyrrolidine nanometer fibrous coat is placed in a muffle furnace; the temperature is raised to 450 DEG C to 600 DEG C at the speed of 50 DEG C per hour; nanometer tin anhydride fibrous coat is gained after being calcined for 5 hours. The nanometer tin anhydride fibrous coat produced by the present invention is gas sensing material with high specific area and high sensitivity; in addition, the material can be widely applied to the field of catalyst, laser target material and so on.

Description

technical field [0001] The invention relates to a preparation method of an inorganic nano-oxide fiber membrane, in particular to an electrostatic spinning preparation method of a nano-tin oxide fiber gas-sensitive membrane. Background technique [0002] The industrial revolution greatly increased labor productivity and enriched people's material and cultural life, but it also brought serious environmental problems. In recent years, acid rain, greenhouse effect, and ozone depletion have threatened the survival of human beings, which have attracted the attention of the whole society. For example: NOx, SOx and HCl in the air cause acid rain; CO 2 , CH 4 , NO 2 , O 3 and fluorocarbons (freon) produce a greenhouse effect; fluorocarbons and halocarbons cause ozone depletion; NH 3 , H 2 S produces a pungent odor. Therefore, the development of these gas sensors for environmental protection has become a hot topic that everyone cares about, especially the research on gas-sensit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/28
Inventor 康卫民程博闻庄旭品丁长坤朱杰吴薛亮
Owner TIANJIN POLYTECHNIC UNIV
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