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Few-layer graphene modified oxygen vacancy stannic oxide material and preparation method thereof

A few-layer graphene, tin dioxide technology, applied in the field of gas sensors and electrochemical energy storage, can solve the problems of limited technical level, poor conductivity of tin dioxide powder, large specific surface area, etc., to achieve high sensitivity and cycle stability good dispersion, high-volume manufacturing, and improved performance

Inactive Publication Date: 2021-02-12
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the prior art discloses a variety of preparation technologies related to tin dioxide and its application in the field of gas sensing or electrochemical energy storage, for example, the authorized patent CN109342523B uses graphene as a substrate and uses a wet heat method to modify tin dioxide on its surface , to achieve NO 2 Rapid detection of gas; patent application CN110436515A discloses a method of chemical vapor deposition combined with heat treatment process for the preparation of black mesoporous SnO rich in oxygen vacancies 2 Nanosheets; the patent application CN109835945A discloses a preparation method of an oxygen-deficient tin dioxide gas-sensitive material using Zn powder as a reducing agent and a stabilizer; the authorized patent CN105600818B uses a vacuum sintering process to heat-treat the tin dioxide precursor powder to obtain rich Tin dioxide nanopowder containing oxygen vacancies, etc., but there are obvious technical defects and insufficient performance, which can be summarized as follows: 1. The existing synthesis technology cannot ensure that the microstructure of tin dioxide powder is uniformly dispersed and has a large ratio Surface area; 2. The existing oxygen vacancy introduction technology level is limited and lacks the necessary characterization technology to confirm; 3. The problem of poor electrical conductivity of tin dioxide powder has not been solved, resulting in its multifunctionality cannot be realized, especially for electrode materials When the specific capacitance value and cycle life are seriously reduced
In order to overcome the current technical defects and performance deficiencies in the controllable preparation and multifunctional application of tin dioxide, it is necessary to develop a tin dioxide-based composite with simple process, large-scale production, multifunctionality and excellent performance. Material

Method used

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  • Few-layer graphene modified oxygen vacancy stannic oxide material and preparation method thereof
  • Few-layer graphene modified oxygen vacancy stannic oxide material and preparation method thereof
  • Few-layer graphene modified oxygen vacancy stannic oxide material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0035] Example 1 Oxygen vacancy SnO 2 Preparation of @rGO composites

[0036] 1) Pure SnO 2 preparation of

[0037] After measuring 5mL of deionized water and 50mL of absolute ethanol and mixing them thoroughly, add 0.190g of SnCl4 Fully dissolve in the mixed solution, then add 0.5mL of concentrated hydrochloric acid.

[0038] The mixed solution was ultrasonically oscillated for 30 minutes, transferred to a reaction kettle, and heated at 200 °C for 24 hours.

[0039] The white precipitate generated by the reaction was poured out, and washed three times by centrifugation with deionized water and absolute ethanol, respectively.

[0040] The washed sample was dried at 60°C for 12 hours, put into a muffle furnace from room temperature to 400°C at a rate of 10°C / min, and calcined for 2 hours.

[0041] After the calcination, the sample was freely cooled to room temperature, and the SnO obtained from the calcined sample was collected. 2 .

[0042] 2) Preparation of few-layer gr...

Embodiment 2

[0063] Embodiment 2 electrochemical performance test

[0064] Electrode sheet preparation process:

[0065] ①Cut a piece with a size of 1×1.5cm 2 Nickel foam, weigh and record its initial weight m 1 .

[0066] ② Measure 7mg of SnO 2 @rGO, 2mg of acetylene black and 1mg of PVDF.

[0067] ③The weighed SnO 2 Pour @rGO, acetylene black and vinylidene fluoride into a mortar, add a few drops of N-methylpyrrolidone, and grind with a pestle for 5-6 minutes to make the various materials uniformly mixed in a gel-like state.

[0068] ④Apply the ground mixture evenly on one end of nickel foam 1×1cm 2 On the surface, just apply a thin layer of the mixture on the surface. Do not apply too much, otherwise it will affect the test performance. °C for 12 hours.

[0069] ⑤ After drying, take out the nickel foam and weigh its final mass m 2 , minus the initial mass m 1 After that, the quality of the coated mixture can be known, and the active material SnO can be obtained by multiplying ...

Embodiment 3

[0086] Example 3 Gas Sensitive Performance Test

[0087] Preparation process of gas sensor components:

[0088] The alumina ceramic tube is used as the substrate, and the two sides of the ceramic tube are composed of ring substances made of gold electrodes, and are connected to the gold electrodes through four platinum wires. Ni-Cr is inserted into the alumina ceramic tube as a heater to control the temperature.

[0089] Weigh an appropriate amount of prepared SnO 2 and SnO 2 @rGO powders were dispersed in flasks filled with distilled water, and placed in an ultrasonic machine for thorough ultrasonic vibration to disperse them evenly in the solution.

[0090] In order to enhance the mechanical adhesion of the powder on the surface of the substrate, a small amount of sodium carboxymethylcellulose was added as an organic binder to the mixed powder, and finally the obtained paste was coated on the surface of the substrate.

[0091] The organic binder is removed from the substr...

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Abstract

The invention discloses a few-layer graphene modified oxygen vacancy stannic oxide material and a preparation method thereof. The preparation method comprises the steps that stannic oxide hollow nanosphere powder uniform in size and good in dispersion and graphene oxide with few-layer characteristics and high uniformity are prepared, and the surface of the stannic oxide is coated with the grapheneoxide; by means of surface graphene, sodium borohydride and subsequent vacuum heat treatment, a large number of oxygen vacancies are successfully manufactured in the stannic oxide hollow nanospheres,and the oxygen vacancy SnO2@rGO composite material is obtained. The method disclosed by the invention is simple to operate and can be put into production on a large scale, and the obtained compositematerial has very high sensitivity and cycling stability to reducing gas and can be used as a positive electrode material of a supercapacitor.

Description

technical field [0001] The invention belongs to the technical field of gas sensors and electrochemical energy storage, and in particular relates to a few-layer graphene-modified oxygen-vacancy tin dioxide material and a preparation method thereof. Background technique [0002] With the continuous progress and development of society, materials with a single function cannot meet people's needs, and multifunctional composite materials have become the object of research and development by scientists. The introduction of oxygen vacancies into semiconductor materials, especially metal oxide semiconductors, can have an important impact on their physical and chemical properties, including the electronic structure of the system, surface adsorption and electron transfer, thus greatly expanding their performance such as gas sensing, energy storage, catalysis and so on. Therefore, it is of great significance for the development of multifunctional composite materials to select suitable ...

Claims

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Application Information

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IPC IPC(8): C01G19/02C01B32/19B82Y15/00B82Y30/00B82Y40/00
CPCB82Y15/00B82Y30/00B82Y40/00C01G19/02C01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/64C01P2004/80C01P2006/12C01P2006/16C01B32/19
Inventor 陈素素林栎阳胡宁
Owner CHONGQING UNIV
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