CN102897757A - Preparation method for single-layered graphene oxide - Google Patents
Preparation method for single-layered graphene oxide Download PDFInfo
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- CN102897757A CN102897757A CN2012103928395A CN201210392839A CN102897757A CN 102897757 A CN102897757 A CN 102897757A CN 2012103928395 A CN2012103928395 A CN 2012103928395A CN 201210392839 A CN201210392839 A CN 201210392839A CN 102897757 A CN102897757 A CN 102897757A
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Abstract
A preparation method for single-layered graphene oxide includes the following steps: expanded graphite and concentrated sulfuric acid or concentrated sulfuric acid mixture are mixed in ice-water bath, added with potassium permanganate as strong oxidant and agitated in ice-water bath for 10 minutes to 1 hour, the mixture is heated to 30 DEG C to 50 DEG C and continues to be agitated for 0.5 hours to 2 hours, deionized water is then added for hydrolyzation, hydrogen peroxide is added after reaction becomes stable, the obtained product is repetitively washed with 5 percent of diluted hydrochloric acid and deionized water, and after centrifugal separation, the single-layered graphene oxide is obtained. The preparation process is simple, the consumed time is short, the single-layered graphene oxide can be obtained by the oxidation step, and the stripping step is dispensed with.
Description
Technical field
The present invention relates to technical field of nano material, particularly a kind of preparation method of mono-layer graphite oxide alkene.
Background technology
The A.K.Geim group of Univ Manchester UK in 2004 has prepared Graphene with the method for mechanically peel graphite first, and has further characterized the various essential propertys of grapheme material.The research work of Geim in 2010 and Novoselov is awarded Nobel Prize in physics.Single-layer graphene is that thickness only is
Two dimensional crystal.When Graphene is still undiscovered, community of physicists generally believes that the one dimension of long-range order or two dimensional crystal material are non-existent, transmission electron microscope observation finds that there is intrinsic waviness wrinkle in the single-layer graphene surface, and this is to make Graphene keep thermodynamically stable possible cause.Graphene be the thinnest in the world be the hardest nano material also, have many peculiar physicalies, its thermal conductivity is up to 5300W/mK, its electronic mobility surpasses 15000cm under the normal temperature
2/ Vs, and resistivity only has an appointment 10
-6Ω cm.Graphene has boundless application prospect, such as field emission source and vacuum electron device, thermally conductive material/heat interfacial material, transparency conductive electrode and solar cell etc.
In the existing graphene preparation method, the graphite oxide method is the method that is hopeful to realize the grapheme material production in enormous quantities.The standby Graphene of graphite oxide legal system is broadly divided into oxidation, peeled off, reduces three steps, and wherein the step of most critical is the preparation graphene oxide.Ultimate principle is: graphite can form low order GIC under the effect of one or more mixed strong acids such as sulfuric acid, nitric acid, phosphoric acid and oxygenant, low order GIC can be continued oxidation, and subsequently hydrolysis obtains the very high graphite product of a kind of oxygen-containing functional group content and namely is called graphite oxide.Graphite oxide is because the existence of interlayer oxygen-containing functional group, interlamellar spacing is about 0.7 ~ 1.1nm, interlamellar spacing 0.335nm much larger than graphite, can adopt suitable stripping means to process graphite oxide, with its graphene oxide of peeling off into which floor or even individual layer, stripping means commonly used has ultrasonic peeling off with thermal expansion to peel off etc.Ultrasonic to peel off local energy very high, can in stripping process graphene oxide be smashed, and long-time ultrasonicly also may change the graphene oxide surface property, makes it that polymerization occur again.And the functional group on the rare surface of graphite oxide meeting decomposes in the thermal expansion stripping process finally obtains the lower Graphene of oxygen level, and performance is fully different with graphene oxide.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method who does not need the mono-layer graphite oxide alkene of stripping technology, this preparation method is simple to operate, and preparation time is short, the graphene oxide thickness homogeneous that obtains.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of preparation method of mono-layer graphite oxide alkene, comprise following process: expanded graphite is mixed in ice-water bath with acid, add strong oxidizer, ice-water bath mix and blend 10min ~ 1h is warming up to 30 ~ 50 ℃ and the lasting 0.5 ~ 2h of stirring with mixture, adds subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, and centrifugation obtains mono-layer graphite oxide alkene, it is dissolved in deionized water is prepared into the preservation of graphene oxide liquid.
In the above-mentioned reaction process, acid is 20-40ml:1g with the expanded graphite ratio, and strong oxidizer and expanded graphite ratio are 2-5g:1g, and deionized water and expanded graphite ratio are 40-150ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5-10ml:1g.
In the aforesaid method, the acid that mixes with expanded graphite is the vitriol oil, phosphoric acid, nitric acid or their mixing acid; Strong oxidizer is potassium permanganate, NaNO
3, KNO
3, perchloric acid, high chromic acid content or their arbitrary proportions mixture.
The granularity of described expanded graphite is 2-500 μ m.
The present invention has the following advantages: preparation process is simple, and is consuming time few, can obtain the graphene oxide of individual layer by one step of oxidation, save strip step, can see resulting graphene oxide thickness homogeneous by measuring, be 0.8 ~ 1.2nm, meet the yardstick of mono-layer graphite oxide alkene.The two dimension width is that submicron is to micron order.
Description of drawings
Accompanying drawing is the TEM picture of the graphene oxide that makes of example 1 of the present invention.
Embodiment:
Embodiment one
A kind of preparation method of mono-layer graphite oxide alkene, comprise following process: be that the expanded graphite micro mist of 2 μ m mixes in ice-water bath with the vitriol oil with granularity, add strong oxidizer potassium permanganate, ice-water bath mix and blend 1h, mixture is warming up to 30 ℃ and the lasting 1h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, in the above-mentioned reaction process, acid is 25ml:1g with the expanded graphite ratio, potassium permanganate and expanded graphite ratio are 3g:1g, and deionized water and expanded graphite ratio are 50ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 10ml:1g.
Graphene oxide TEM photo is with reference to accompanying drawing, and as can be seen from the figure the carbon film of graphene oxide contrast and little grid is suitable, and has more fold.
Embodiment two
A kind of preparation method of mono-layer graphite oxide alkene, comprise following process: be that the expanded graphite micro mist of 10 μ m mixes in ice-water bath with the vitriol oil with granularity, add strong oxidizer potassium permanganate, ice-water bath mix and blend 10min, mixture is warming up to 40 ℃ and the lasting 2h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, in the above-mentioned reaction process, acid is 30ml:1g with the expanded graphite ratio, potassium permanganate and expanded graphite ratio are 4g:1g, and deionized water and expanded graphite ratio are 60ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5ml:1g.
Embodiment three
A kind of preparation method of mono-layer graphite oxide alkene, comprise following process: be expanded graphite and the vitriol oil of 200 μ m with granularity, strong phosphoric acid is mixed in ice-water bath, add strong oxidizer potassium permanganate, ice-water bath mix and blend 1h, mixture is warming up to 50 ℃ and the lasting 0.5h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, in the above-mentioned reaction process, acid is 25ml:1g with the expanded graphite ratio, and wherein the vitriol oil and strong phosphoric acid volume ratio are 4:1, and potassium permanganate and expanded graphite ratio are 5g:1g, deionized water and expanded graphite ratio are 50ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5ml:1g.
Claims (6)
1. the preparation method of a mono-layer graphite oxide alkene, it is characterized in that, comprise following process: expanded graphite is mixed in ice-water bath with acid, add strong oxidizer, ice-water bath mix and blend 10min ~ 1h, mixture is warming up to 30 ~ 50 ℃ and the lasting 0.5 ~ 2h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, it is dissolved in deionized water is prepared into the preservation of graphene oxide liquid; In the above-mentioned reaction process, acid is 20-40ml:1g with the expanded graphite ratio, and strong oxidizer and expanded graphite ratio are 2-5g:1g, and deionized water and expanded graphite ratio are 40-150ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5-10ml:1g.
2. the preparation method of a kind of mono-layer graphite oxide alkene according to claim 1 is characterized in that, the granularity of described expanded graphite is at 2 ~ 500 μ m.
3. the preparation method of a kind of mono-layer graphite oxide alkene according to claim 1 is characterized in that, the described acid that mixes with expanded graphite is the vitriol oil, phosphoric acid, nitric acid or their mixing acid, and strong oxidizer is potassium permanganate, NaNO
3, KNO
3, perchloric acid, high chromic acid content or their mixture.
4. the preparation method of a kind of mono-layer graphite oxide alkene according to claim 1 and 2, it is characterized in that, be that the expanded graphite micro mist of 2 μ m mixes in ice-water bath with the vitriol oil with granularity, add strong oxidizer potassium permanganate, ice-water bath mix and blend 1h, mixture is warming up to 30 ℃ and the lasting 1h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, in the above-mentioned reaction process, acid is 25ml:1g with the expanded graphite ratio, and potassium permanganate and expanded graphite ratio are 3g:1g, deionized water and expanded graphite ratio are 50ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 10ml:1g.
5. the preparation method of a kind of mono-layer graphite oxide alkene according to claim 1 and 2, it is characterized in that, be that the expanded graphite micro mist of 10 μ m mixes in ice-water bath with the vitriol oil with granularity, add strong oxidizer potassium permanganate, ice-water bath mix and blend 10min, mixture is warming up to 40 ℃ and the lasting 2h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, in the above-mentioned reaction process, acid is 30ml:1g with the expanded graphite ratio, and potassium permanganate and expanded graphite ratio are 4g:1g, deionized water and expanded graphite ratio are 60ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5ml:1g.
6. the preparation method of a kind of mono-layer graphite oxide alkene according to claim 1 and 2, it is characterized in that, be expanded graphite and the vitriol oil of 200 μ m with granularity, strong phosphoric acid is mixed in ice-water bath, add strong oxidizer potassium permanganate, ice-water bath mix and blend 1h, mixture is warming up to 50 ℃ and the lasting 0.5h of stirring, add subsequently the deionized water hydrolysis, add hydrogen peroxide after the stable reaction, products therefrom cleans repeatedly with 5% dilute hydrochloric acid and deionized water, centrifugation obtains mono-layer graphite oxide alkene, and in the above-mentioned reaction process, acid is 25ml:1g with the expanded graphite ratio, wherein the vitriol oil and strong phosphoric acid volume ratio are 4:1, potassium permanganate and expanded graphite ratio are 5g:1g, and deionized water and expanded graphite ratio are 50ml:1g during hydrolysis reaction, and hydrogen peroxide and expanded graphite ratio are 5ml:1g.
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| CN102173414A (en) * | 2011-03-18 | 2011-09-07 | 中国地质大学（武汉） | Method for preparing graphene oxide by chemical peeling |
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