CN104007236A - Preparation method and application of graphene/zinc oxide nano composite material - Google Patents
Preparation method and application of graphene/zinc oxide nano composite material Download PDFInfo
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- CN104007236A CN104007236A CN201410221606.8A CN201410221606A CN104007236A CN 104007236 A CN104007236 A CN 104007236A CN 201410221606 A CN201410221606 A CN 201410221606A CN 104007236 A CN104007236 A CN 104007236A
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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/zinc oxide nano composite material. The preparation method comprises the following steps: (1) dissolving 2.5-3 parts of zinc nitrate into water; carrying out ultrasonic wave assistance to sufficiently dissolve the zinc nitrate; then adding 0.0005-0.001 part of graphene oxide; carrying out ultrasound treatment for 30-45 minutes; adding 0.05-0.06 part of cetyl trimethyl ammonium bromide and sufficiently mixing; finally, adding hydrazine hydrate into the solution and continuing to carry out the ultrasound treatment for 30-45 minutes, wherein the mass/volume ratio of the zinc nitrate to the water is 3.8% (w/v) and the mass/volume ratio of the zinc nitrate to the hydrazine hydrate is 50% (w/v); (2) putting a mixed solution obtained by the step (1) into a reaction kettle and carrying out a constant-temperature reaction at 150-160 DEG C for 12-14 hours; cooling the reaction kettle to room temperature and taking out reactants; carrying out centrifuging, washing and drying treatment to obtain the graphene/zinc 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/zinc oxide nanometer 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/zinc paste, 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/zinc oxide nanometer composite material.
The present invention is achieved by the following technical solutions: the preparation method of Graphene/zinc oxide nanometer composite material, the steps include:
(1) 2.5～3 parts of zinc nitrates are soluble in water, ultrasonicly auxiliary after fully being dissolved, it adds 0.0005～0.001 part of graphene oxide; After ultrasonic 30～45min, add the cetyl trimethyl ammonium bromide of 0.05～0.06 part, fully mix; Finally in above-mentioned solution, add hydrazine hydrate, continue ultrasonic 30～45min; The mass volume ratio of zinc nitrate and water is 3.8%(w/v), the mass volume ratio of zinc nitrate and hydrazine hydrate is 50%(w/v);
(2) mixed solution step (1) being obtained is put into reactor, in 150～160 ℃ of isothermal reaction 12～14h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/zinc oxide nanometer composite material.
In the present invention, take zinc nitrate as raw material, be cheaply easy to get, can effectively be compounded to form Graphene/zinc oxide nanometer composite material with Graphene, can effectively detect monoethanolamine.Cetyl trimethyl ammonium bromide plays the effect of structure directing agent, controls nucleation and the growth rate of zinc paste in building-up process.Hydrazine hydrate both provided formation zinc paste needed alkaline environment, was also that Graphene is at the reductive agent of recombination process situ reduction simultaneously.
In the present invention, when zinc nitrate obtains mass parts and is 2.5～3, if the mass parts of graphene oxide is greater than 0.001, easy capping oxidation zinc surface, affects 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 zinc paste and Graphene; If be less than 0.05, can not effectively play the effect of adjuvant.
Further, the application of the gas sensor that prepared by described Graphene/zinc oxide nanometer composite material in detecting monoethanolamine.
As seen from Figure 3, the gas sensor that prepared by compound substance of the present invention has higher selectivity to 80ppm monoethanolamine.
As seen from Figure 4, gas sensor prepared by compound substance of the present invention has higher sensitivity to low-concentration ethanol amine, and can respond fast and recover, and lowest detection limit reaches 1ppm, and be 10s release time.
The preparation method of Graphene/zinc oxide nanometer composite material of the present invention, preparation process is simple, easy to operate, and technological parameter is easy to control.When nano zine oxide is synthetic, graphene oxide is reduced, and a step obtains Graphene/zinc oxide nanometer composite material.Take its gas sensor of preparing as gas sensitive has very high sensitivity and response fast, recovers aminated compounds, and detection limit can reach 1ppm, is a kind of new gas sensing property material that detects volatility monoethanolamine.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of Graphene/zinc oxide nanometer composite material of the present invention.
Fig. 2 is the ultimate analysis figure of Graphene/zinc oxide nanometer composite material of the present invention.
Fig. 3 is the sensitive selectivity of the gas sensor prepared of Graphene/zinc oxide nanometer composite material of the present invention to the different volatile matter of 80ppm.
Fig. 4 is that the sensitivity of the gas sensor prepared of Graphene/zinc oxide nanometer composite material of the present invention is with the curve map of monoethanolamine concentration change.
Embodiment
every part of embodiment 1(is 1g)
The preparation method of Graphene/zinc oxide nanometer composite material, the steps include:
(1) 2.5g zinc nitrate is dissolved in 66mL water, ultrasonicly auxiliary adds 0.0007g graphene oxide after it is fully dissolved; After ultrasonic 45min, add the cetyl trimethyl ammonium bromide of 0.055g, fully mix; Finally in above-mentioned solution, add 5mL hydrazine hydrate, continue ultrasonic 30min;
(2) mixed solution step (1) being obtained is put into reactor, in 155 ℃ of isothermal reaction 14h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/zinc oxide nanometer composite material.
Gas sensor prepared by the described Graphene/zinc oxide nanometer composite material application in detecting monoethanolamine.
every part of embodiment 2(is 1g)
The preparation method of Graphene/zinc oxide nanometer composite material, the steps include:
(1) 2.8g zinc nitrate is dissolved in 74mL water, ultrasonicly auxiliary adds 0.001g graphene oxide after it is fully dissolved; After ultrasonic 40min, add the cetyl trimethyl ammonium bromide of 0.05g, fully mix; Finally in above-mentioned solution, add 5.6mL hydrazine hydrate, continue ultrasonic 40min;
(2) mixed solution step (1) being obtained is put into reactor, in 160 ℃ of isothermal reaction 14h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/zinc oxide nanometer composite material.
every part of embodiment 3(is 1g)
The preparation method of Graphene/zinc oxide nanometer composite material, the steps include:
(1) 3g zinc nitrate is dissolved in 79mL water, ultrasonicly auxiliary adds 0.0005g graphene oxide after it is fully dissolved; After ultrasonic 30min, add the cetyl trimethyl ammonium bromide of 0.06g, fully mix; Finally in above-mentioned solution, add 6mL hydrazine hydrate, continue ultrasonic 45min;
(2) mixed solution step (1) being obtained is put into reactor, in 150 ℃ of isothermal reaction 13h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/zinc oxide nanometer composite material.
Claims (2)
1. the preparation method of Graphene/zinc oxide nanometer composite material, is characterized in that, the steps include:
(1) 2.5～3 parts of zinc nitrates are soluble in water, ultrasonicly auxiliary after fully being dissolved, it adds 0.0005～0.001 part of graphene oxide; After ultrasonic 30～45min, add the cetyl trimethyl ammonium bromide of 0.05～0.06 part, fully mix; Finally in above-mentioned solution, add hydrazine hydrate, continue ultrasonic 30～45min; The mass volume ratio of zinc nitrate and water is 3.8%(w/v), the mass volume ratio of zinc nitrate and hydrazine hydrate is 50%(w/v);
(2) mixed solution step (1) being obtained is put into reactor, in 150～160 ℃ of isothermal reaction 12～14h; Reactor is cooled to after room temperature, takes out reactant, after centrifugal, washing and dry processing, obtains Graphene/zinc oxide nanometer composite material.
2. the application of the gas sensor that prepared by Graphene/zinc oxide nanometer composite material as claimed in claim 1 in detecting monoethanolamine.
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| CN105181896A (en) * | 2015-09-01 | 2015-12-23 | 上海理工大学 | Acetone gas detection gas-sensitive material, acetone gas detection gas-sensitive element, and preparation methods of acetone gas detection gas-sensitive material and acetone gas detection gas-sensitive element |
| CN106057481A (en) * | 2016-08-11 | 2016-10-26 | 安徽省宁国天成电工有限公司 | Preparation method of graphene/zinc oxide nanocomposite and purpose thereof |
| CN106700660A (en) * | 2017-01-06 | 2017-05-24 | 上海烯古能源科技有限公司 | Graphene-coated oxide heat conduction filler and preparation method thereof |
| CN107285370A (en) * | 2017-07-11 | 2017-10-24 | 济南大学 | A kind of preparation method of sheet rGO/ZnO nano composite material one-step synthesis |
| CN107629242A (en) * | 2017-09-17 | 2018-01-26 | 赵兵 | Nano zine oxide/graphene macroscopic view self-assembled compound material using sponge as template |
| CN108949102A (en) * | 2018-07-20 | 2018-12-07 | 青岛大学 | A kind of nano zine oxide/graphene composite material and preparation method thereof |
| CN109752411A (en) * | 2017-11-07 | 2019-05-14 | 国家纳米科学中心 | A kind of composite air-sensitive material and its preparation method and application |
| CN111484705A (en) * | 2020-04-17 | 2020-08-04 | 中国人民解放军陆军工程大学 | Zinc oxide coated graphene/epoxy resin nonlinear conductive composite material and preparation method thereof |
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| CN105181896A (en) * | 2015-09-01 | 2015-12-23 | 上海理工大学 | Acetone gas detection gas-sensitive material, acetone gas detection gas-sensitive element, and preparation methods of acetone gas detection gas-sensitive material and acetone gas detection gas-sensitive element |
| CN105181896B (en) * | 2015-09-01 | 2017-06-23 | 上海理工大学 | A kind of gas sensitive and its element and preparation method for detecting acetone gas |
| CN106057481A (en) * | 2016-08-11 | 2016-10-26 | 安徽省宁国天成电工有限公司 | Preparation method of graphene/zinc oxide nanocomposite and purpose thereof |
| CN106700660A (en) * | 2017-01-06 | 2017-05-24 | 上海烯古能源科技有限公司 | Graphene-coated oxide heat conduction filler and preparation method thereof |
| CN107285370A (en) * | 2017-07-11 | 2017-10-24 | 济南大学 | A kind of preparation method of sheet rGO/ZnO nano composite material one-step synthesis |
| CN107629242A (en) * | 2017-09-17 | 2018-01-26 | 赵兵 | Nano zine oxide/graphene macroscopic view self-assembled compound material using sponge as template |
| CN109752411A (en) * | 2017-11-07 | 2019-05-14 | 国家纳米科学中心 | A kind of composite air-sensitive material and its preparation method and application |
| CN109752411B (en) * | 2017-11-07 | 2021-09-17 | 国家纳米科学中心 | Composite gas-sensitive material and preparation method and application thereof |
| CN108949102A (en) * | 2018-07-20 | 2018-12-07 | 青岛大学 | A kind of nano zine oxide/graphene composite material and preparation method thereof |
| CN111484705A (en) * | 2020-04-17 | 2020-08-04 | 中国人民解放军陆军工程大学 | Zinc oxide coated graphene/epoxy resin nonlinear conductive composite material and preparation method thereof |
| CN111484705B (en) * | 2020-04-17 | 2023-01-10 | 中国人民解放军陆军工程大学 | Zinc oxide coated graphene/epoxy resin nonlinear conductive composite material and preparation method thereof |
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