CN105217615A - A kind of preparation method of Graphene - Google Patents
A kind of preparation method of Graphene Download PDFInfo
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- CN105217615A CN105217615A CN201510677219.XA CN201510677219A CN105217615A CN 105217615 A CN105217615 A CN 105217615A CN 201510677219 A CN201510677219 A CN 201510677219A CN 105217615 A CN105217615 A CN 105217615A
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Abstract
The invention discloses a kind of preparation method of Graphene, comprise the steps: 1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 3 ~ 4 hours in Vltrasonic device, obtain graphene oxide suspension; 2) be the hydroxylamine hydrochloride solution of 28 ~ 50g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide; 3) filtered by the above-mentioned mixing solutions that obtains, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process, all in inert gas environment, obtains final finished.The present invention in terms of existing technologies, has the following advantages: this preparation method preparation efficiency is high, and gained Graphene purity is high, and not easily reunites, and dispersing property is better, and lamella integrity is good.
Description
Technical field
The present invention relates to field of new material preparation, be specifically related to a kind of Graphene and preparation method thereof.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separated from graphite material, and the thickness of this two-dimentional graphite crystal film only has a carbon atom thick, and intensity is but 100 times of steel.It is the material that current room temperature conduction is fastest, mechanical strength is maximum, the capacity of heat transmission is the strongest.Thickness is called Graphene at the Nano graphite crystal of 1-10 layer, according to the number of the carbon atom number of plies, or the thickness of Graphene, be divided into single-layer graphene (Single-layergraphene), bilayer graphene (Double-layergraphene) and multi-layer graphene (Few-layergraphene), when thickness more than 10 layers, its performance and the conventional basic indifference of graphite material.The theoretical specific surface area of single-layer graphene is 2650m2/g, and thermal conductivity is up to 5300W/mK, and under room temperature, electronic mobility is up to 15000cm2/VS.A series of special propertys of Graphene, in fields such as matrix material, opto-electronic conversion, battery electrode material, catalytic material, touch-screen material, chip material, transistor equivalent material, hydrogen storage materials, have huge potential investigation and application and are worth.The special property of Graphene has attracted the Study on Preparation Technology of large quantities of scientist to Graphene, and current method mainly contains: micromechanics stripping method, graphite oxide reduction method, chemical vapour deposition (CVD) etc.Wherein expensive high orientation pyrolytic graphite adhesive tape bonds, peels off by micromechanics stripping method repeatedly, then transfers on substrate material surface, and this method efficiency is extremely low, is only limitted to laboratory study; Chemical Vapor deposition process and epitaxial growth method are suitable for the Graphene monolithic manufacturing larger area, but efficiency is also extremely low; By contrast, the comparatively front two method output of graphite oxide reduction method output are comparatively large, but complex manufacturing, produce more spent acid, bring pollution to environment, simultaneously when redox graphene, comparatively large to the structure deteriorate of Graphene, and the Graphene prepared easily is reunited, and greatly have impact on performance.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of graphene preparation method.
Technical scheme: for achieving the above object, the preparation method of a kind of Graphene provided by the invention, comprises the steps:
1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 3 ~ 4 hours in Vltrasonic device, obtain graphene oxide suspension;
2) be the hydroxylamine hydrochloride solution of 28 ~ 50g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide;
3) filtered by the above-mentioned mixing solutions that obtains, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process, all in inert gas environment, obtains final finished.
Further, the weight part percentage of hydroxylamine hydrochloride solution, pyridine or tetrahydrofuran (THF) is 3:1:1.
Further, described graphene oxide suspension concentration is 300 ~ 450g/L.
Further, described step 3) in microwave power be 900 ~ 1000W, heat-up time is 6 minutes.
Further, described rare gas element comprises one in neon, argon or two kinds.
Beneficial effect: the present invention in terms of existing technologies, has the following advantages: this preparation method preparation efficiency is high, gained Graphene purity is high, and not easily reunites, and dispersing property is better, and lamella integrity is good.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1:
A preparation method for Graphene, comprises the steps:
1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 4 hours in Vltrasonic device, obtain graphene oxide suspension;
2) be the hydroxylamine hydrochloride solution of 50g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide; The weight percent ratio of hydroxylamine hydrochloride solution, pyridine or tetrahydrofuran (THF) is 3:1:1;
3) the above-mentioned mixing solutions that obtains is filtered, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process is all in inert gas environment, and microwave power is 1000W, heat-up time is 6 minutes, obtains final finished.
Embodiment 2:
A preparation method for Graphene, comprises the steps:
1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 4 hours in Vltrasonic device, obtain graphene oxide suspension;
2) be the hydroxylamine hydrochloride solution of 28g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide; The ratio of hydroxylamine hydrochloride solution, pyridine or tetrahydrofuran (THF) is 3:1:1;
3) the above-mentioned mixing solutions that obtains is filtered, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process is all in inert gas environment, and microwave power is 900W, heat-up time is 6 minutes, obtains final finished.
Embodiment 3:
A preparation method for Graphene, comprises the steps:
1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 4 hours in Vltrasonic device, obtain graphene oxide suspension;
2) be the hydroxylamine hydrochloride solution of 40g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide; The ratio of hydroxylamine hydrochloride solution, pyridine or tetrahydrofuran (THF) is 3:1:1;
3) the above-mentioned mixing solutions that obtains is filtered, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process is all in inert gas environment, and microwave power is 1000W, heat-up time is 6 minutes, obtains final finished.
The performance test of embodiment 1 ~ 3 is as following table:
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
1) graphite oxide is joined in ethanol and water mixed liquid and vibrate 3 ~ 4 hours in Vltrasonic device, obtain graphene oxide suspension;
2) be the hydroxylamine hydrochloride solution of 28 ~ 50g/L by concentration, pyridine or tetrahydrofuran (THF) mixed solution join in described graphene oxide suspension, stirs, obtain the mixing solutions of graphene oxide;
3) filtered by the above-mentioned mixing solutions that obtains, and screening is carried out microwave heating activation process, after cooling, through pickling, washing, filtration, centrifugal and dry, whole process, all in inert gas environment, obtains final finished.
2. the preparation method of Graphene according to claim 1, is characterized in that, the ratio of described hydroxylamine hydrochloride solution, pyridine or tetrahydrofuran (THF) is 3:1:1.
3. the preparation method of Graphene according to claim 1, is characterized in that, described graphene oxide suspension concentration is 300 ~ 450g/L.
4. the preparation method of Graphene according to claim 1, is characterized in that, described step 3) in microwave power be 900 ~ 1000W, heat-up time is 6 minutes.
5. the preparation method of Graphene according to claim 1, is characterized in that, described rare gas element comprises one in neon, argon or two kinds.
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| CN201510677219.XA CN105217615A (en) | 2015-10-19 | 2015-10-19 | A kind of preparation method of Graphene |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502612A (en) * | 2011-11-21 | 2012-06-20 | 南京工业大学 | Method for preparing grapheme through oxidation reduction |
| CN102765716A (en) * | 2012-07-17 | 2012-11-07 | 上海大学 | Preparation method of graphene |
| CN103787317A (en) * | 2014-01-02 | 2014-05-14 | 上海应用技术学院 | Preparation method of graphene oxide dispersion liquid |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502612A (en) * | 2011-11-21 | 2012-06-20 | 南京工业大学 | Method for preparing grapheme through oxidation reduction |
| CN102765716A (en) * | 2012-07-17 | 2012-11-07 | 上海大学 | Preparation method of graphene |
| CN103787317A (en) * | 2014-01-02 | 2014-05-14 | 上海应用技术学院 | Preparation method of graphene oxide dispersion liquid |
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