CN103995088A - Preparation method and application of graphene/tin oxide nano composite material - Google Patents
Preparation method and application of graphene/tin oxide nano composite material Download PDFInfo
- Publication number
- CN103995088A CN103995088A CN201410221595.3A CN201410221595A CN103995088A CN 103995088 A CN103995088 A CN 103995088A CN 201410221595 A CN201410221595 A CN 201410221595A CN 103995088 A CN103995088 A CN 103995088A
- Authority
- CN
- China
- Prior art keywords
- graphene
- composite material
- nano composite
- tin
- tin oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention relates to the field of preparation and application of a nano composite material and particularly relates to a preparation method and an application of a graphene/tin oxide nano composite material. The preparation method comprises the following steps: (1) dissolving 2-2.5 parts of tin tetrachloride or tin dichloride into methanol and carrying out ultrasonic assistance to sufficiently dissolve; then adding 0.0005-0.001 part of graphene oxide; carrying out ultrasonic treatment for 30-45 minutes and adding 0.05-0.06 part of cetyl trimethyl ammonium bromide to be mixed sufficiently; adjusting the pH (Potential of Hydrogen) of a solution to 9 by using ammonia water; continuing to carry out the ultrasonic treatment for 30-45 minutes, wherein the mass/volume ratio of the tin tetrachloride or the tin dichloride to the methanol is 5% (w/v); (2) putting a mixed solution obtained by the step (1) into a reaction kettle and carrying out a constant-temperature reaction at 140-150 DEG C for 18-20 hours; after cooling the reaction kettle to room temperature, taking out reactants; centrifuging, washing and drying to obtain the graphene/tin oxide nano composite material.
Description
Technical field
The present invention relates to preparation and the application thereof of nano composite material, specifically a kind of preparation method of Graphene/tin oxide nano composite material and application thereof.
Background technology
The method of preparing at present the compound substance of Graphene-metal oxide mainly contains: (1) spraying thermal decomposed deposition method, the people such as Zhang adopt spraying thermal decomposed deposition method to synthesize the compound of Graphene/tin oxide, this method requires stricter to instrument, production cost is higher; (2) microwave irradiation/method of radiating, the people such as Yan adopt the method for microwave to prepare the compound of Graphene/cobaltosic oxide, this legal system is for fairly simple, but operation is more dangerous, and in the compound of preparation, nano particle can not be dispersed in the surface of Graphene uniformly; (3) Ink Jet Printing method, the people such as manga adopt Ink Jet Printing legal system for the photoconduction conductive film compound of Graphene/titania, and this method is strict to equipment requirement, operates more loaded down with trivial details; (4) molecule engrafting method, the people such as tang have prepared the photoconduction conductive film of Graphene/titania by molecule engrafting method, and this method is strict to the control of experiment condition, experiment poor reproducibility, operating difficulties; (5) hydro-thermal method, the method is simple, and security is good, is to develop at present the reasonable method of preparing Graphene and metal oxide compounds.
Summary of the invention
The present invention aims to provide a kind of preparation method and application thereof of Graphene/tin oxide nano composite material.
The present invention is achieved by the following technical solutions: the preparation method of Graphene/tin oxide nano composite material, the steps include:
(1) 2～2.5 parts of butters of tin or stannous chloride are dissolved in methyl alcohol, ultrasonicly auxiliary add 0.0005～0.001 part of graphene oxide after it is fully dissolved; After ultrasonic 30～45min, add the cetyl trimethyl ammonium bromide of 0.05～0.06 part, fully mix; Ammoniacal liquor regulator solution to pH be 9, continue ultrasonic 30～45min; The mass volume ratio of butter of tin or stannous chloride and methyl alcohol is 5%(w/v);
(2) mixed solution step (1) being obtained is put into reactor, in 140～150 ℃ of isothermal reaction 18～20h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/tin oxide nano composite material.
In the present invention, take butter of tin or stannous chloride as raw material, and raw material is cheaply easy to get, and can effectively be compounded to form nano composite material with graphene oxide, and this compound substance can effectively detect triethylamine.Cetyl trimethyl ammonium bromide has been controlled nucleation and the growth rate of butter of tin or stannous chloride in compound substance building-up process, plays the effect of spreading agent.
When the mass parts of butter of tin or stannous chloride is 2～2.5, if the mass parts of graphene oxide is greater than 0.001, easily cover the surface of butter of tin or stannous chloride, affect the air-sensitive performance of compound substance; If be less than 0.0005, affect the composite effect of Graphene, can not effectively bring into play the effect of Graphene in compound substance.If the mass parts of cetyl trimethyl ammonium bromide is greater than 0.06, affect the compound of the growth of butter of tin or stannous chloride and Graphene; If be less than 0.05, do not have the effect of dispersion.
Further, the application of the gas sensor that prepared by described Graphene/tin oxide nano composite material in detecting triethylamine.
As seen from Figure 3, gas sensor PARA FORMALDEHYDE PRILLS(91,95), acetaldehyde and triethylamine etc. prepared by compound substance of the present invention all have higher sensitivity, especially triethylamine are had to higher selectivity.。
As seen from Figure 4, gas sensor prepared by compound substance of the present invention has higher sensitivity to triethylamine, and can respond fast and recover, and lowest detection limit reaches 5ppm.
The preparation method of Graphene/tin oxide nano composite material of the present invention, preparation process is simple, easy to operate, and technological parameter is easy to control.When nano tin dioxide is synthetic, graphene oxide is reduced, and a step obtains Graphene/tin oxide nano composite material.Take its gas sensor of preparing as gas sensitive has very high sensitivity and response fast, recovers different volatile matter, and detection limit can reach 5ppm, for detecting volatility triethylamine, has increased a kind of new gas sensitive.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of Graphene/tin oxide nano composite material of the present invention.
Fig. 2 is the ultimate analysis figure of Graphene/tin oxide nano composite material of the present invention.
Fig. 3 is the sensitive selectivity of the gas sensor prepared of Graphene/tin oxide nano composite material of the present invention to the different volatile matter of 50ppm.
Fig. 4 is the curve map that the sensitivity of the gas sensor prepared of Graphene/tin oxide nano composite material of the present invention changes with triethylamine concentration.
Embodiment
every part of embodiment 1(is 1g)
The preparation method of Graphene/tin oxide nano composite material, the steps include:
(1) 2.5g butter of tin is dissolved in 50mL methyl alcohol, ultrasonicly auxiliary adds 0.001g graphene oxide after it is fully dissolved; After ultrasonic 30min, add the cetyl trimethyl ammonium bromide of 0.055g, fully mix; Ammoniacal liquor regulator solution to pH be 9, continue ultrasonic 45min;
(2) mixed solution step (1) being obtained is put into reactor, in 145 ℃ of isothermal reaction 18h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/tin oxide nano composite material.
Gas sensor prepared by the described Graphene/tin oxide nano composite material application in detecting triethylamine.
every part of embodiment 2(is 1g)
The preparation method of Graphene/tin oxide nano composite material, the steps include:
(1) 2g stannous chloride is dissolved in 40mL methyl alcohol, ultrasonicly auxiliary adds 0.0007g graphene oxide after it is fully dissolved; After ultrasonic 40min, add the cetyl trimethyl ammonium bromide of 0.06g, fully mix; Ammoniacal liquor regulator solution to pH be 9, continue ultrasonic 40min;
(2) mixed solution step (1) being obtained is put into reactor, in 140 ℃ of isothermal reaction 19h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/tin oxide nano composite material.
every part of embodiment 3(is 1g)
The preparation method of Graphene/tin oxide nano composite material, the steps include:
(1) 2.2g butter of tin is dissolved in 44mL methyl alcohol, ultrasonicly auxiliary adds 0.0005g graphene oxide after it is fully dissolved; After ultrasonic 45min, add the cetyl trimethyl ammonium bromide of 0.05g, fully mix; Ammoniacal liquor regulator solution to pH be 9, continue ultrasonic 30min;
(2) mixed solution step (1) being obtained is put into reactor, in 150 ℃ of isothermal reaction 20h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/tin oxide nano composite material.
Claims (2)
1. the preparation method of Graphene/tin oxide nano composite material, is characterized in that, the steps include:
(1) 2～2.5 parts of butters of tin or stannous chloride are dissolved in methyl alcohol, ultrasonicly auxiliary add 0.0005～0.001 part of graphene oxide after it is fully dissolved; After ultrasonic 30～45min, add the cetyl trimethyl ammonium bromide of 0.05～0.06 part, fully mix; Ammoniacal liquor regulator solution to pH be 9, continue ultrasonic 30～45min; The mass volume ratio of butter of tin or stannous chloride and methyl alcohol is 5%(w/v);
(2) mixed solution step (1) being obtained is put into reactor, in 140～150 ℃ of isothermal reaction 18～20h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/tin oxide nano composite material.
2. the application of the gas sensor that prepared by Graphene/tin oxide nano composite material as claimed in claim 1 in detecting triethylamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410221595.3A CN103995088B (en) | 2014-05-26 | 2014-05-26 | The preparation method of Graphene/tin oxide nano composite material and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410221595.3A CN103995088B (en) | 2014-05-26 | 2014-05-26 | The preparation method of Graphene/tin oxide nano composite material and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103995088A true CN103995088A (en) | 2014-08-20 |
| CN103995088B CN103995088B (en) | 2015-12-02 |
Family
ID=51309309
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410221595.3A Active CN103995088B (en) | 2014-05-26 | 2014-05-26 | The preparation method of Graphene/tin oxide nano composite material and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103995088B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198540A (en) * | 2014-09-18 | 2014-12-10 | 安徽工业大学 | Gas sensitive material for detecting low-concentration acetaldehyde |
| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| CN104528701A (en) * | 2014-12-23 | 2015-04-22 | 哈尔滨工业大学 | Preparation method of graphene-loaded high-dispersibility stannic oxide nanoparticle composite material |
| CN104556209A (en) * | 2015-01-09 | 2015-04-29 | 太原理工大学 | Preparation method for spherical tin dioxide self-assembled from nano-fragments |
| CN106501449A (en) * | 2016-10-17 | 2017-03-15 | 上海理工大学 | A kind of gas sensitive and element and preparation method for detecting formaldehyde gas |
| CN109142627A (en) * | 2018-08-01 | 2019-01-04 | 济南大学 | A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material |
| CN110498405A (en) * | 2019-08-21 | 2019-11-26 | 南京倍格电子科技有限公司 | A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778478A (en) * | 2012-05-15 | 2012-11-14 | 中国科学技术大学 | Graphene-modified doped tin oxide composite material and preparation method thereof |
| CN103007935A (en) * | 2012-12-13 | 2013-04-03 | 北京化工大学常州先进材料研究院 | Preparation method of Pt/antimony-doped tin oxide-graphene catalyst |
| CN103035916A (en) * | 2012-11-28 | 2013-04-10 | 华中科技大学 | Preparation method of nano tin dioxide-graphene composite material and product thereof |
| CN103112846A (en) * | 2013-02-06 | 2013-05-22 | 华中科技大学 | Preparation method of graphene-carbon nanotube-nano tin dioxide three-dimensional composite material and product thereof |
-
2014
- 2014-05-26 CN CN201410221595.3A patent/CN103995088B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778478A (en) * | 2012-05-15 | 2012-11-14 | 中国科学技术大学 | Graphene-modified doped tin oxide composite material and preparation method thereof |
| CN103035916A (en) * | 2012-11-28 | 2013-04-10 | 华中科技大学 | Preparation method of nano tin dioxide-graphene composite material and product thereof |
| CN103007935A (en) * | 2012-12-13 | 2013-04-03 | 北京化工大学常州先进材料研究院 | Preparation method of Pt/antimony-doped tin oxide-graphene catalyst |
| CN103112846A (en) * | 2013-02-06 | 2013-05-22 | 华中科技大学 | Preparation method of graphene-carbon nanotube-nano tin dioxide three-dimensional composite material and product thereof |
Non-Patent Citations (4)
| Title |
|---|
| PEICHAO LIAN: "High reversible capacity of SnO", 《ELECTROCHIMICA ACTA》, vol. 56, 31 December 2011 (2011-12-31), pages 4532 - 4539, XP028195621, DOI: 10.1016/j.electacta.2011.01.126 * |
| XIAODAN HUANG: "A Facile One-Step Solvothermal Synthesis of SnO2-Graphene Nanocomposite and Its Application as an Anode Material for Lithium-Ion Batteries", 《CHEMPHYSCHEM》, 31 December 2011 (2011-12-31), pages 278 - 281 * |
| 初璇: "二氧化锡杂化材料的制备及气敏性能研究", 《中国优秀硕士学位论文数据库》, 15 September 2013 (2013-09-15) * |
| 王彩红: "Cd2SnO4水热制备及其气敏性能研究", 《化工新材料》, vol. 40, no. 6, 30 June 2012 (2012-06-30), pages 108 - 110 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| CN104198540A (en) * | 2014-09-18 | 2014-12-10 | 安徽工业大学 | Gas sensitive material for detecting low-concentration acetaldehyde |
| CN104528701A (en) * | 2014-12-23 | 2015-04-22 | 哈尔滨工业大学 | Preparation method of graphene-loaded high-dispersibility stannic oxide nanoparticle composite material |
| CN104556209A (en) * | 2015-01-09 | 2015-04-29 | 太原理工大学 | Preparation method for spherical tin dioxide self-assembled from nano-fragments |
| CN104556209B (en) * | 2015-01-09 | 2016-03-23 | 太原理工大学 | By the preparation method of the spherical tindioxide of nanometer fragment self-assembly |
| CN106501449A (en) * | 2016-10-17 | 2017-03-15 | 上海理工大学 | A kind of gas sensitive and element and preparation method for detecting formaldehyde gas |
| CN106501449B (en) * | 2016-10-17 | 2019-05-24 | 上海理工大学 | A kind of gas sensitive and element and preparation method for detecting formaldehyde gas |
| CN109142627A (en) * | 2018-08-01 | 2019-01-04 | 济南大学 | A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material |
| CN110498405A (en) * | 2019-08-21 | 2019-11-26 | 南京倍格电子科技有限公司 | A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103995088B (en) | 2015-12-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103995088A (en) | Preparation method and application of graphene/tin oxide nano composite material | |
| CN104007236A (en) | Preparation method and application of graphene/zinc oxide nano composite material | |
| Bersani et al. | Combined EXAFS, XRD, DRIFTS, and DFT study of nano copper-based catalysts for CO2 hydrogenation | |
| JP5331305B2 (en) | Method for producing hydrogenation accelerator, hydrogenation catalyst and alkene compound | |
| CN104174421A (en) | Heterogeneous catalyst for selective hydrogenation reaction of aryl nitro-compound and application of heterogeneous catalyst | |
| Vargeese et al. | Anatase–brookite mixed phase nano TiO2 catalyzed homolytic decomposition of ammonium nitrate | |
| CN106732731B (en) | A kind of ZnO/g-C3N4The preparation method and application of ozone composite catalyst | |
| Wang et al. | Unveiling single atom nucleation for isolating ultrafine fcc Ru nanoclusters with outstanding dehydrogenation activity | |
| CN107311194B (en) | A kind of preparation method and application of Ti-MWW molecular sieve | |
| CN105502373B (en) | A kind of environment-friendly preparation method thereof of graphene | |
| CN104307515A (en) | Au-Pd/graphene catalyst and preparation method and application thereof | |
| CN107570149A (en) | A kind of monatomic method for preparing catalyst using mesoporous TiO 2 as carrier | |
| CN111804346B (en) | Method for rapidly preparing metal organic layer material and application thereof | |
| Pozdnyakov et al. | A Polymer Nanocomposite with CuNP Stabilized by 1-Vinyl-1, 2, 4-triazole and Acrylonitrile Copolymer | |
| Dong et al. | Anchoring Pt particles onto mesoporousized ZnO holey cubes for triethylamine detection with multifaceted superiorities | |
| Reiber et al. | The tetra alkyl methylene immonium salts | |
| CN103143390A (en) | Modification method of microsphere titanium silicon molecular sieve catalyst | |
| CN103933973A (en) | Preparation method of supported nano palladium/carbon catalyst | |
| CN104525265B (en) | 2,4-dihydroxy-5-Chlorobenzaldehyde contracting aminoacid copper complex catalyst, preparation method and application | |
| CN103224445B (en) | Technology for preparing resorcinol by direct oxidation of benzene | |
| CN102505125A (en) | Method for preparing 2,4-dimethylanisole | |
| CN103157508B (en) | Modification method for catalytic oxime synthesis catalyst | |
| CN105435846B (en) | Platinum complex catalyst and preparation method thereof, purposes | |
| CN106040123B (en) | Microreactor applied to ethanol steam reforming reaction and preparation method thereof | |
| CN104672275A (en) | Synthetic method and application of asymmetric cage-shaped polyhedral low oligomeric silsesquioxane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |