CN102654474A - Making method of nano film of graphene doped zinc oxide - Google Patents
Making method of nano film of graphene doped zinc oxide Download PDFInfo
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- CN102654474A CN102654474A CN2011100500738A CN201110050073A CN102654474A CN 102654474 A CN102654474 A CN 102654474A CN 2011100500738 A CN2011100500738 A CN 2011100500738A CN 201110050073 A CN201110050073 A CN 201110050073A CN 102654474 A CN102654474 A CN 102654474A
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Abstract
The invention discloses a making method of a nano film of graphene doped zinc oxide. The making method comprises the steps of: preparing graphite oxide by using graphite, anhydrous sodium nitrate, concentrated sulfuric acid and potassium permanganate; preparing graphene by using the graphite oxide; dissolving the graphene and zinc oxide in an ethylene glycol solution, ultrasonically oscillating to obtain a mixture solution; and sucking the mixture solution by using a liquid-moving machine and dropping and coating on a sensitive film of a device, and vacuum-drying to obtain the nano file of the graphene doped zinc oxide. By using the excellent electronic conduction characteristic of the graphene, through change of conductivity, the change of the frequency is changed, and therefore, the purpose of detecting gas is achieved. Due to the adoption of the graphene doped with the zinc oxide, the sensitivity of the sensitive film can be greatly improved. The graphene is synthesized by adopting a chemical dispersal method; the making method has high controllability compared with that of the micro mechanical stripping method; and massive production of the nano film can be carried out.
Description
Technical field
The present invention relates to the gas sensor technical field; Be particularly related to a kind of method for making of nano thin-film of Graphene doping zinc-oxide; This method is to make the nano thin-film of Graphene doping zinc-oxide with chemical dispersion method synthesizing graphite alkene and doping zinc-oxide, is used at room temperature detecting the NO of low concentration
2Gas.
Background technology
NO
2Being a kind of intensive properties gas, also is thermal power generation, the main emission gases of chemical process.Owing to have extremely strong corrosivity and physiological stimulation effect, so to Architectural Equipment, production equipment and human health thereof cause very big harm.Therefore, to NO
2Gas carries out in time, detects exactly and measurement has crucial meaning.
Be used for NO at present
2The method of gas detection mainly contains galvanochemistry and semiconductor resistor formula sensor, yet the most of required instrument of these methods is expensive, and volume is big, and Analysis of Complex is consuming time of a specified duration, is not suitable for open-air monitoring in real time.
Summary of the invention
The technical matters that (one) will solve
In view of this, fundamental purpose of the present invention is to provide a kind of method for making of nano thin-film of Graphene doping zinc-oxide.
(2) technical scheme
For achieving the above object, the invention provides a kind of method for making of nano thin-film of Graphene doping zinc-oxide, comprising:
Utilize graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and potassium permanganate to prepare graphite oxide;
Utilize this graphite oxide to prepare Graphene;
This Graphene and zinc paste are dissolved in ethylene glycol solution, and sonic oscillation obtains mixed solution;
Draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device, vacuum drying obtains the nano thin-film of Graphene doping zinc-oxide.
In the such scheme, said graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and the potassium permanganate of utilizing prepares graphite oxide, specifically comprises:
In ice bath, graphite, anhydrous nitric acid sodium are evenly mixed with the concentrated sulphuric acid, add potassium permanganate in the stirring and obtain potpourri;
This potpourri was transferred to 40 degrees centigrade of water-baths 30 minutes, progressively adds deionized water, temperature is elevated to 98 degrees centigrade and continues reaction 40 minutes, thin up;
The adding massfraction is 30 percent hydrogen peroxide solution, the unreacted potassium permanganate that neutralizes, and centrifugal filtration and cyclic washing filter cake, vacuum drying just can obtain graphite oxide.
In the such scheme, said this graphite oxide that utilizes prepares Graphene, adopts chemical dispersion method; Specifically comprise: graphite oxide is ground configuration suspending liquid, ultrasonic, centrifugal removal impurity; Obtain stable graphene oxide suspending liquid, just obtain Graphene with hydrazine water redox graphene suspending liquid.
In the such scheme, said this Graphene and zinc paste are dissolved in ethylene glycol solution, sonic oscillation obtains in the step of mixed solution, and sonic oscillation is half an hour at least.
In the such scheme, saidly draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device, vacuum drying obtains in the step of nano thin-film of Graphene doping zinc-oxide, and vacuum drying is 80 degrees centigrade vacuum drying chamber inner drying at least two hours.
(3) beneficial effect
The method for making of the nano thin-film of this Graphene doping zinc-oxide provided by the invention with chemical dispersion method synthesizing graphite alkene and doping zinc-oxide, is made the nano thin-film of Graphene doping zinc-oxide, is used at room temperature detecting the NO of low concentration
2Gas.The present invention utilizes the excellent electronic conduction characteristic of Graphene, changes the variation of frequency through the variation of conductivity, thereby reaches the purpose of detected gas.Used is the Graphene of doping zinc-oxide, can improve the sensitive membrane susceptibility greatly.Graphene is synthetic through chemical dispersion method, and phase ratio micro stripping means controllability is high, can produce on a large scale.
Description of drawings
Fig. 1-the 1st makes the synoptic diagram of the substrate that the nano thin-film of Graphene doping zinc-oxide adopts according to the embodiment of the invention.
Fig. 1-2 is that wherein circle is represented moisture according to the synoptic diagram of the nano thin-film that has moisture and organic Graphene doping zinc-oxide of embodiment of the invention making, and triangle is represented organism.
Fig. 1-the 3rd, the synoptic diagram of the removal moisture of making according to the embodiment of the invention and the nano thin-film of the Graphene doping zinc-oxide behind the organism.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
The invention provides a kind of method for making of nano thin-film of Graphene doping zinc-oxide, may further comprise the steps:
Step 1: utilize graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and potassium permanganate to prepare graphite oxide;
Step 2: utilize this graphite oxide to prepare Graphene;
Step 3: this Graphene and zinc paste are dissolved in ethylene glycol solution, and sonic oscillation obtains mixed solution;
Step 4: draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device, vacuum drying obtains the nano thin-film of Graphene doping zinc-oxide.
In the above-mentioned steps 1, said graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and the potassium permanganate of utilizing prepares graphite oxide, specifically comprises: in ice bath, graphite, anhydrous nitric acid sodium are evenly mixed with the concentrated sulphuric acid, add potassium permanganate in the stirring and obtain potpourri; This potpourri was transferred to 40 degrees centigrade of water-baths 30 minutes, progressively adds deionized water, temperature is elevated to 98 degrees centigrade and continues reaction 40 minutes, thin up; The adding massfraction is 30 percent hydrogen peroxide solution, the unreacted potassium permanganate that neutralizes, and centrifugal filtration and cyclic washing filter cake, vacuum drying just can obtain graphite oxide.
In the above-mentioned steps 2, said this graphite oxide that utilizes prepares Graphene, adopts chemical dispersion method; Specifically comprise: graphite oxide is ground configuration suspending liquid, ultrasonic, centrifugal removal impurity; Obtain stable graphene oxide suspending liquid, just obtain Graphene with hydrazine water redox graphene suspending liquid.
In the above-mentioned steps 3, said this Graphene and zinc paste are dissolved in ethylene glycol solution, sonic oscillation obtains in the step of mixed solution, and sonic oscillation is half an hour at least.
In the above-mentioned steps 4, saidly draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device, vacuum drying obtains in the step of nano thin-film of Graphene doping zinc-oxide, and vacuum drying is 80 degrees centigrade vacuum drying chamber inner drying at least two hours.
Fig. 1-1 is a process chart of making the nano thin-film of Graphene doping zinc-oxide according to the embodiment of the invention to 1-3, this method by synthetic, sonic oscillation, centrifugal, drip to be coated with and realize that its step is following with step such as vacuum drying:
Step 10, in ice bath, graphite and anhydrous nitric acid sodium are evenly mixed with the concentrated sulphuric acid, slowly add potassium permanganate in the stirring;
Step 20, it was transferred to 40 degrees centigrade of water-baths 30 minutes, progressively adds deionized water, temperature is elevated to 98 degrees centigrade and continues reaction 40 minutes, thin up;
Step 30, handle with about 30 percent the hydrogen peroxide solution of massfraction, the unreacted potassium permanganate that neutralizes, centrifugal filtration and cyclic washing filter cake, vacuum drying just can obtain graphite oxide;
Step 40, graphite oxide is ground configuration suspending liquid, ultrasonic, centrifugal removal small amount of impurities obtains stable graphene oxide suspending liquid, just obtains Graphene with a certain amount of hydrazine water redox graphene suspending liquid;
Step 50, Graphene and an amount of zinc paste are dissolved in ethylene glycol solution, sonic oscillation half an hour;
Step 60, draw the part mixed solution with pipettor and drip on the sensitive membrane that is coated in device;
Step 70, device is put into vacuum drying chamber, removed moisture and organism in two hours, obtain the nano thin-film of Graphene doping zinc-oxide 80 degrees centigrade of dryings.
Wherein, substrate is a quartz substrate, and its purpose is to reduce the device temperature influence; Phase ratio micro stripping means, described Graphene is synthetic through chemical dispersion method, and controllability is high, can produce on a large scale.What described Graphene mixed is zinc paste, can improve the electronic conduction characteristic of sensitive membrane greatly.The Graphene sensitive membrane of described doping zinc-oxide is to detect NO at normal temperatures
2Gas.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the method for making of the nano thin-film of a Graphene doping zinc-oxide is characterized in that, comprising:
Utilize graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and potassium permanganate to prepare graphite oxide;
Utilize this graphite oxide to prepare Graphene;
This Graphene and zinc paste are dissolved in ethylene glycol solution, and sonic oscillation obtains mixed solution;
Draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device, vacuum drying obtains the nano thin-film of Graphene doping zinc-oxide.
2. the method for making of the nano thin-film of Graphene doping zinc-oxide according to claim 1 is characterized in that, said graphite, anhydrous nitric acid sodium, the concentrated sulphuric acid and the potassium permanganate of utilizing prepares graphite oxide, specifically comprises:
In ice bath, graphite, anhydrous nitric acid sodium are evenly mixed with the concentrated sulphuric acid, add potassium permanganate in the stirring and obtain potpourri;
This potpourri was transferred to 40 degrees centigrade of water-baths 30 minutes, progressively adds deionized water, temperature is elevated to 98 degrees centigrade and continues reaction 40 minutes, thin up;
The adding massfraction is 30 percent hydrogen peroxide solution, the unreacted potassium permanganate that neutralizes, and centrifugal filtration and cyclic washing filter cake, vacuum drying just can obtain graphite oxide.
3. the method for making of the nano thin-film of Graphene doping zinc-oxide according to claim 1 is characterized in that, said this graphite oxide that utilizes prepares Graphene, adopts chemical dispersion method, specifically comprises:
Graphite oxide is ground configuration suspending liquid, and ultrasonic, centrifugal removal impurity obtains stable graphene oxide suspending liquid, just obtains Graphene with hydrazine water redox graphene suspending liquid.
4. the method for making of the nano thin-film of Graphene doping zinc-oxide according to claim 1 is characterized in that, said this Graphene and zinc paste is dissolved in ethylene glycol solution, and sonic oscillation obtains in the step of mixed solution, and sonic oscillation is half an hour at least.
5. the method for making of the nano thin-film of Graphene doping zinc-oxide according to claim 1; It is characterized in that; Saidly draw this mixed solution with pipettor and drip on the sensitive membrane that is coated in device; Vacuum drying obtains in the step of nano thin-film of Graphene doping zinc-oxide, and vacuum drying is 80 degrees centigrade vacuum drying chamber inner drying at least two hours.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866178A (en) * | 2012-09-07 | 2013-01-09 | 清华大学 | Gas sensor and forming method thereof |
| CN103252228A (en) * | 2013-06-08 | 2013-08-21 | 江苏悦达墨特瑞新材料科技有限公司 | Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet |
| CN103400632A (en) * | 2013-07-17 | 2013-11-20 | 常州二维碳素科技有限公司 | Graphene doping material, and preparation method and application of graphene doping material |
| CN103435033A (en) * | 2013-08-12 | 2013-12-11 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN103884423A (en) * | 2012-12-20 | 2014-06-25 | 国家纳米科学中心 | Zinc oxide/ reduced graphene oxide composite nanomaterial and preparation method thereof and ultraviolet light detector |
| CN104597082A (en) * | 2015-01-23 | 2015-05-06 | 清华大学 | Preparation method of hybridized hierarchical structure sensitive thin-film sensing device based on two-dimensional material |
| CN105129778A (en) * | 2015-07-22 | 2015-12-09 | 上海工程技术大学 | Preparation method of nano ZnO/graphene composite material |
| CN105692680A (en) * | 2016-02-26 | 2016-06-22 | 武汉理工大学 | Zinc oxide @ graphene nanocomposite of layered structure and preparation method thereof |
| CN106044845A (en) * | 2016-05-26 | 2016-10-26 | 中国科学院合肥物质科学研究院 | Graphene oxide modified orderly porous zinc oxide composite film and preparation method thereof |
| CN106706710A (en) * | 2015-11-11 | 2017-05-24 | 中国科学院上海微***与信息技术研究所 | Nitrogen oxide gas sensor based on sulphur-doped graphene, and preparation method thereof |
| CN107261558A (en) * | 2017-06-07 | 2017-10-20 | 电子科技大学 | A kind of chromatographic column and its preparation method of stationary phase based on graphite alkenes Yu zinc oxide duplicature stationary phase |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866178A (en) * | 2012-09-07 | 2013-01-09 | 清华大学 | Gas sensor and forming method thereof |
| CN103884423B (en) * | 2012-12-20 | 2016-01-20 | 国家纳米科学中心 | Zinc paste/redox graphene composite nano materials and preparation method thereof and ultraviolet light detector |
| CN103884423A (en) * | 2012-12-20 | 2014-06-25 | 国家纳米科学中心 | Zinc oxide/ reduced graphene oxide composite nanomaterial and preparation method thereof and ultraviolet light detector |
| CN103252228A (en) * | 2013-06-08 | 2013-08-21 | 江苏悦达墨特瑞新材料科技有限公司 | Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet |
| CN103400632A (en) * | 2013-07-17 | 2013-11-20 | 常州二维碳素科技有限公司 | Graphene doping material, and preparation method and application of graphene doping material |
| CN103400632B (en) * | 2013-07-17 | 2016-05-11 | 常州二维碳素科技股份有限公司 | A kind of Graphene dopant material and application thereof |
| CN103435033A (en) * | 2013-08-12 | 2013-12-11 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN103435033B (en) * | 2013-08-12 | 2014-11-26 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN104597082A (en) * | 2015-01-23 | 2015-05-06 | 清华大学 | Preparation method of hybridized hierarchical structure sensitive thin-film sensing device based on two-dimensional material |
| CN104597082B (en) * | 2015-01-23 | 2017-02-22 | 清华大学 | Preparation method of hybridized hierarchical structure sensitive thin-film sensing device based on two-dimensional material |
| CN105129778A (en) * | 2015-07-22 | 2015-12-09 | 上海工程技术大学 | Preparation method of nano ZnO/graphene composite material |
| CN106706710A (en) * | 2015-11-11 | 2017-05-24 | 中国科学院上海微***与信息技术研究所 | Nitrogen oxide gas sensor based on sulphur-doped graphene, and preparation method thereof |
| CN105692680A (en) * | 2016-02-26 | 2016-06-22 | 武汉理工大学 | Zinc oxide @ graphene nanocomposite of layered structure and preparation method thereof |
| CN106044845A (en) * | 2016-05-26 | 2016-10-26 | 中国科学院合肥物质科学研究院 | Graphene oxide modified orderly porous zinc oxide composite film and preparation method thereof |
| CN107261558A (en) * | 2017-06-07 | 2017-10-20 | 电子科技大学 | A kind of chromatographic column and its preparation method of stationary phase based on graphite alkenes Yu zinc oxide duplicature stationary phase |
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Application publication date: 20120905 |