CN103864046B - A kind of method preparing hydrogenation Graphene - Google Patents
A kind of method preparing hydrogenation Graphene Download PDFInfo
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- CN103864046B CN103864046B CN201410114921.0A CN201410114921A CN103864046B CN 103864046 B CN103864046 B CN 103864046B CN 201410114921 A CN201410114921 A CN 201410114921A CN 103864046 B CN103864046 B CN 103864046B
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Abstract
The present invention provides a kind of method preparing hydrogenation Graphene, it is suspended in the mixing solutions that the fluorographite dispersant liquid drop made in liquid amine is added to Na-K alloy and nonaqueous liquid amine is mixed to get reaction by fluorographite, adds fatty alcohol cancellation after 1-15 is little and be obtained by reacting hydrogenation Graphene. The method reaction conditions of the present invention is gentle, simply efficient, with low cost, it is possible to prepare the adjustable hydrogenation Graphene of band gap on a large scale.
Description
Technical field
The present invention relates to the method regulating Graphene band gap, it is specifically related to a kind of method preparing hydrogenation Graphene.
Background technology
2004, Britain graceful Chester college professor A.Geim and K.Novoselov utilized simple mechanically peel method, prepares and has observed single-layer graphene. Perfect Graphene is a kind of desirable two dimensional crystal, has the cellular lattice structure of two-dimension periodic of carbon six-ring composition, and thickness is only the diameter of a carbon atom, is material the thinnest in the world at present. Since this kind of material in 2004 is found, the physical and chemical performance of its uniqueness makes researchist shock. These two scientists also because this breakthrough discovery, are awarded Nobel prize for physics in 2010.
Chemically seeing in the bonding mode of key, the carbon atom forming Graphene two-dirnentional structure is with sp2Mode hydridization, and contribute a remaining p orbital electron to form the �� key of delocalization, ��-electron can move freely in plane, imparts the electroconductibility of Graphene excellence; And owing to only having the thickness of a carbon atom, Graphene also shows as typical two dimension quantum material. The mobility of electronics in Graphene can reach 15000cm2/ (V s), higher than silicon materials more than 10 times, and almost not by the impact of temperature variation. In addition, it also has a series of excellent physical propertys such as the high capacity of heat transmission, extra specific surface area, zero mass dirac-fermion behavior and abnormal quantum Hall effect, make it have application potential in nano electron device field, can be used to preparation novel field effect transistor, spin electric device and opto-electronic device etc.
Geim group successfully have developed Graphene monoatomic layer transistor, and this is transistor minimum in the world; IBM company have developed graphene field effect transistor fastest in the world, can run under 26GHz frequency. These antetype devices fully illustrate the great potential that Graphene is applied in nano electron device field, are also considered as the surrogate of a kind of potential conventional semiconductors microelectronic device based on the nano electron device of Graphene.
But, different from semiconductor silicon, there is no band gap between the valence band of Graphene and conduction band. And band gap is the key of electronic application, because it can make material realize the Push And Release of stream of electrons, development regulation and control Graphene electronic structure and energy gap technology are significant.
At present, it is possible to the method changing Graphene band gap has photolithography, edge to modify method, the assorted element method of doping, hydrogenation Graphene method and extending and growing graphene method etc. on different substrates.
Compared with other method, hydrogenation Graphene method is a kind of method of effective adjustment Graphene band gap. Through hydrogenation, in single-layer graphene, carbon atom is by sp2Hydridization is changed into sp3Hydridization, causes the migration of fermi level, and energy gap is increased, it is possible to the electrical property realizing Graphene by metallicity to the transformation of semiconductive. Further, the band gap of hydrogenation Graphene can be regulated by degree of hydrogenation, and band gap variable range is big, can meet the application requirement of different components. Energy gap increases with degree of hydrogenation and increases, and when complete hydrogenation, Graphene band gap increases to about 5.4eV.
Graphene is mainly carried out hydrogenation by the physical means such as hydrogen plasma, beamwriter lithography by the method preparing hydrogenation Graphene reported at present. This kind of method needs to use the means such as plasma technique and electron beam lithography, and experimental installation and experiment condition are had relatively high requirement; And it needs taking Graphene is raw material, and the preparation cost of Graphene is high, makes the large-scale application of this kind of preparation method be restricted.
Have recently emerged wet chemistry hydride process and prepare hydrogenation Graphene, namely utilize the liquid ammonia solution of basic metal that graphite or graphite oxide are carried out reduction and obtain hydrogenation Graphene. This kind of method raw material sources are extensive, with low cost, and reaction conditions is gentle, simple, are applicable to the extensive preparation of hydrogenation Graphene.
To sum up, still needing and continue the preparation method of research and development hydrogenation Graphene in this area, simply efficiently, and can reduce costs, it is possible to prepare on a large scale.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of novel hydrogenation Graphene.
A first aspect of the present invention, it is provided that a kind of method preparing hydrogenation Graphene, comprises the following steps:
A Na-K alloy and nonaqueous liquid amine under an inert atmosphere, are mixed to get mixing solutions by ();
B fluorographite dispersant liquid drop is added in the mixing solutions of step (a) gained and reacts by ();
C () reaction 1-15 is little after, in the reaction system of step (b), adds fatty alcohol cancellation be obtained by reacting hydrogenation Graphene,
Wherein, described fluorographite dispersion liquid is suspended in liquid amine by fluorographite and makes.
In another preference, described method also comprises step:
D () is separated described hydrogenation Graphene after cancellation is reacted.
In another preference, described separation comprises the following steps:
(d1) in reaction system, add normal hexane and water, form aqueous phase and normal hexane phase;
(d2) remove described aqueous phase, wash described normal hexane with water mutually to neutral;
(d3) filter described normal hexane and obtain filtrate mutually;
(d4) dry described filtrate obtains described hydrogenation Graphene.
In another preference, in described Na-K alloy, the mass ratio of sodium and potassium is 1:0.5-8.
In another preference, in potassium and fluorographite, the mol ratio of fluorine is 10-50:1.
In another preference, described liquid amine is selected from: liquefied ammonia, quadrol.
In another preference, described fatty alcohol is selected from: ethanol, Virahol, the trimethyl carbinol.
In another preference, in step (c), the feed postition of described fatty alcohol is once all add or add with the speed of 3-10ml/h.
In another preference, the ratio 1:1-20 of the quality (g) of described Na-K alloy and nonaqueous liquid amine volume (ml).
In another preference, in described fluorographite dispersion liquid, the quality (mg) of fluorographite is 0.5-20:1 with the ratio of the volume (ml) of liquid amine.
The present invention adopts fluorographite as raw material, and raw material sources are extensive, with low cost, and reaction conditions is gentle, simply efficiently, be applicable to the extensive preparation of hydrogenation Graphene; And the hydrogen richness of gained hydrogenation Graphene is controlled, and namely band gap can effectively regulate, and has potential application in nano electron device field.
It will be understood that within the scope of the present invention, above-mentioned each technology characteristic sum of the present invention can combine mutually between specifically described each technology feature in below (eg embodiment), thus form new or preferred technical scheme. As space is limited, tired no longer one by one state at this.
Accompanying drawing explanation
Fig. 1 is the image of gained hydrogenation Graphene, the transmission electron microscope image that wherein (a) and (b) is gained hydrogenation Graphene; C () is the high resolution transmission electron microscope image of gained hydrogenation Graphene; D () is the selected area electron diffraction figure of gained hydrogenation Graphene.
Fig. 2 is fluorographite and the infrared spectrogram of gained hydrogenation Graphene.
Fig. 3 is the Raman spectrogram of hydrogenation Graphene.
Fig. 4 is the absorbance curve of hydrogenation Graphene.
Fig. 5 is the band gap mensuration figure of hydrogenation Graphene.
Embodiment
Present inventor, through studying extensively and deeply, surprisingly develops a kind of method of hydrogenation Graphene first, it may also be useful to fluorographite, as raw material, prepares hydrogenation Graphene with the reduction of the amine aqueous solution of basic metal. This method is simply efficient, it is possible to low cost, prepare hydrogenation Graphene on a large scale, and the hydrogen richness of gained hydrogenation Graphene is controlled, and namely band gap can effectively regulate, and has potential application in nano electron device field. On this basis, the present invention is completed.
Preparation method
The method preparing hydrogenation Graphene provided by the invention, comprises the following steps:
A Na-K alloy and nonaqueous liquid amine under an inert atmosphere, are mixed to get mixing solutions by ();
B fluorographite dispersant liquid drop is added in the mixing solutions of step (a) gained and reacts by ();
C () reaction 1-15 is little after, in the reaction system of step (b), adds fatty alcohol cancellation be obtained by reacting hydrogenation Graphene,
Wherein, described fluorographite dispersion liquid is suspended in liquid amine by fluorographite and makes.
In addition, described method can also comprise step:
D () is separated described hydrogenation Graphene after cancellation is reacted.
Described separation can comprise the following steps:
(d1) in reaction system, add normal hexane and water, form aqueous phase and normal hexane phase;
(d2) remove described aqueous phase, wash described normal hexane with water mutually to neutral;
(d3) filter described normal hexane and obtain filtrate mutually;
(d4) dry described filtrate obtains described hydrogenation Graphene.
In the preparation method of the present invention, in described Na-K alloy, the mass ratio of sodium and potassium is 1:0.5-8, it is preferred that be 1:1-5, is more preferably 1:3.
Described liquid amine is selected from: liquefied ammonia, quadrol. In another preference, fluorographite dispersion liquid liquid amine used is identical with liquid amine in step (a).
The ratio 1:1-20 of the quality (g) of Na-K alloy and nonaqueous liquid amine volume (ml), it is preferred that be 1:1.5-15, be more preferably 1:2-10. In another preference, the ratio 1:2-5 of the quality (g) of described Na-K alloy and nonaqueous liquid amine volume (ml).
Step (a) carries out under an inert atmosphere, as nitrogen, helium, argon gas etc. do not participate in reaction gas atmosphere under carry out.
In fluorographite dispersion liquid, the quality (mg) of fluorographite is 0.5-20:1 with the ratio of the volume (ml) of liquid amine, it is preferred that is 1-15:1, is more preferred from 2-10:1. In another preference, the quality (mg) of fluorographite is 4-8:1 with the ratio of the volume (ml) of liquid amine.
In described potassium and fluorographite, the mol ratio of fluorine is 10-50:1, it is preferred that is 15-40:1, is more preferably 15-25:1.
The volume ratio 0.5-2:1 of the mixing solutions that step (a) obtains and fluorographite dispersion liquid, it is preferred that be 0.6-1.5:1. It is more preferably 0.8-1.2:1. In another preference, the volume ratio 1:1 of the mixing solutions that step (a) obtains and fluorographite dispersion liquid.
In step (c), described fatty alcohol is selected from: ethanol, Virahol, the trimethyl carbinol.
In step (c), the feed postition of described fatty alcohol is once all add or add taking the speed of 3-10ml/h (better as 3-8ml/h). Fatty alcohol add-on has no particular limits, and is enough to cancellation and reacts.
In the present invention one better embodiment, the method preparing hydrogenation Graphene of the present invention comprises the following steps:
(1) in the container of full rare gas element, add Na-K alloy and nonaqueous liquid amine, it is stirred to and dissolves completely, obtain dark blue solution;
(2) fluorographite is joined in nonaqueous liquid amine, ultrasonic it is uniformly suspended in liquid amine to fluorographite;
(3) the fluorographite dispersion liquid of step (2) gained is slowly added drop-wise in the solution of step (1) gained, stirs after 1-12 hour, in reaction system, add fatty alcohol cancellation reaction;
(4) in reaction system, add normal hexane and water, hydrogenation Graphene can be enriched to normal hexane mutually in; Divide phase of anhydrating, and wash normal hexane mutually to neutral with pure water;
(5) filter also dry, obtain hydrogenation Graphene.
The present invention adds ratio, the reaction times of fluorine element in potassium metal and fluorographite in reaction system and reacts cancellation mode by regulating, and regulates the hydrogen richness of generated hydrogenation Graphene, to obtain the hydrogenation Graphene that band gap can regulate.
The above-mentioned feature that the present invention mentions, or the feature that embodiment is mentioned can arbitrary combination. All features that this case specification sheets discloses can with any composition forms and use, each feature disclosed in specification sheets, it is possible to alternative characteristics that is identical by any offer, impartial or similar object replaces. Therefore apart from special instruction, the feature disclosed is only general example that is impartial or similar features.
The usefulness of the present invention is:
(1) the present invention provides the preparation method of a kind of new hydrogenation Graphene;
(2) using fluorographite as raw material, method is simply efficient, it is possible to low cost, prepare hydrogenation Graphene on a large scale;
(3) hydrogen richness of gained hydrogenation Graphene is controlled, and namely band gap can effectively regulate, and has potential application in nano electron device field.
Below in conjunction with specific embodiment, set forth the present invention further. Limit the scope of the invention it will be understood that these embodiments are only not used in for illustration of the present invention. The experimental technique of unreceipted concrete condition in the following example, usually conveniently condition or the condition advised according to manufacturer. Unless otherwise indicated, otherwise per-cent and part number calculate by weight.
Unless otherwise defined, the same meaning that in literary composition, all specialties of using and science term and one skilled in the art are familiar with. In addition, any method similar or impartial to described content and material all can be applicable in the inventive method. Literary composition described in better implementation method and what material only was used as to demonstrate.
Universal method
All constituent contents of the present invention are recorded by ultimate analysis; The structure of hydrogenation Graphene is confirmed by transmission electron microscope, FT-IR & FT-RAMAN spectra; The band gap of hydrogenation Graphene is recorded by uv-visible absorption spectroscopy.
Specifically, joining in 5mL chloroform by 1mg hydrogenation Graphene sample, ultrasonic 1h makes it evenly disperse. Gained liquid pipettes in supernatant liquid to quartz colorimetric utensil after leaving standstill 24 hours and leaving standstill and measures the absorbance curve within the scope of 190-700nm by uv-visible absorption spectroscopy. To curve carry out mathematics manipulation to obtain the longitudinal axis be that absorbancy square is multiplied by photon energy square, transverse axis is the curve of photon energy. Making the tangent line increased closest to its sudden change on curve, the intercept of this tangent line on transverse axis is exactly the band gap of sample.
Embodiment 1
The synthesis of hydrogenation Graphene
The reaction flask of full argon gas adds Na-K alloy (1.9g, wherein sodium content is 25%) and 5mL anhydrous ethylenediamine, is stirred to dark blue solution.
37mg fluorographite is joined in 5mL anhydrous ethylenediamine, ultrasonic it is dispersed in quadrol to fluorographite. The mol ratio throwing material potassium/fluorine is 30.0:1.
Slowly being added drop-wise in the ethylenediamine solution of Na-K alloy by the quadrol dispersion liquid of fluorographite, stirring at room temperature, after 2 hours, is slowly dripped and is added (rate of addition is 5mL/h) 10mL Virahol cancellation reaction.
Add 30mL normal hexane and 50mL deionized water extracts, remove aqueous phase; Organic phase repeats with deionized water wash to neutral. Filtering with the filtering membrane of 0.22 micron, gained solid, 60 DEG C of dryings 24 hours, obtains 11.9mg hydrogenation Graphene, and ratio of carbon-hydrogen is 1.08:1.
The transmission electron microscope image that in Fig. 1, (a) and (b) is the present embodiment gained hydrogenation Graphene; C () is the high resolution transmission electron microscope image of gained hydrogenation Graphene; D () is the selected area electron diffraction figure of gained hydrogenation Graphene, show the hydrogenation graphene sheet layer of gained possess thickness thin, have the features such as curling fold, illustrate that this hydrogenation Graphene meets the shape looks feature of two-dimensional material really.
Fig. 2 is the present embodiment gained fluorographite and the infrared spectrogram of gained hydrogenation Graphene, illustrates to there is the distinctive lard type C-H bond of a large amount of alkane in this hydrogenation Graphene, also consistent with the C-H bond type in hydrogenation Graphene (graphite alkane) theoretical model.
Fig. 3 is the Raman spectrogram of the present embodiment gained hydrogenation Graphene, and in Raman spectrum, higher than G peak, D peak intensity then illustrates that in this hydrogenation Graphene, lard type carbon atom proportion is bigger.
Fig. 4 is the absorbance curve of the present embodiment gained hydrogenation Graphene; Fig. 5 is the band gap mensuration figure of the present embodiment gained hydrogenation Graphene, by experimental data being processed, it is possible to the band gap drawing this hydrogenation Graphene is 4.3eV.
Embodiment 2-8
The synthesis of hydrogenation Graphene
Repeating embodiment 1, difference is to throw mol ratio, reaction times and the cancellation mode of expecting potassium/fluorine.
The detection data of embodiment 1-8 hydrogenation Graphene of preparation under the different condition such as reaction times and cancellation mode are as shown in table 1.
Table 1 different reaction times and cancellation mode affect result
Comparative example 1-3
The synthesis of hydrogenation Graphene
The method adopting embodiment 1 substantially identical prepares hydrogenation Graphene, and difference is to throw mol ratio, reaction times and the cancellation mode of expecting potassium/fluorine.
Table 2 comparative example result
Result shows, adopts the mol ratio of above-mentioned potassium/fluorine, reaction times and cancellation mode, and degree of hydrogenation does not meet it is contemplated that namely the band gap of gained hydrogenation Graphene can not control, and these methods can not be used for the controlled synthesis of hydrogenation Graphene.
On the contrary, the method for the present invention, reaction conditions is gentle, simply efficient, is applicable to the extensive preparation of hydrogenation Graphene; And the hydrogen richness of gained hydrogenation Graphene is controlled, and namely band gap can effectively regulate, and has potential application in nano electron device field.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document. In addition it will be understood that after the above-mentioned teachings having read the present invention, the present invention can be made various changes or modifications by those skilled in the art, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. prepare the method for hydrogenation Graphene for one kind, it is characterised in that, described method comprises the following steps:
A Na-K alloy and nonaqueous liquid amine under an inert atmosphere, are mixed to get mixing solutions by ();
B fluorographite dispersant liquid drop is added in the mixing solutions of step (a) gained and reacts by ();
C () reaction 1-15 is little after, in the reaction system of step (b), adds fatty alcohol cancellation be obtained by reacting hydrogenation Graphene,
Wherein, described fluorographite dispersion liquid is suspended in liquid amine by fluorographite and makes.
2. the method for claim 1, it is characterised in that, described method also comprises step:
D () is separated described hydrogenation Graphene after cancellation is reacted.
3. method as claimed in claim 2, it is characterised in that, described separation comprises the following steps:
(d1) in reaction system, add normal hexane and water, form aqueous phase and normal hexane phase;
(d2) remove described aqueous phase, wash described normal hexane with water mutually to neutral;
(d3) filter described normal hexane and obtain filtrate mutually;
(d4) dry described filtrate obtains described hydrogenation Graphene.
4. method as described in item as arbitrary in claim 1-3, it is characterised in that, in described Na-K alloy, the mass ratio of sodium and potassium is 1:0.5-8.
5. method as described in item as arbitrary in claim 1-3, it is characterised in that, in potassium and fluorographite, the mol ratio of fluorine is 10-50:1.
6. method as described in item as arbitrary in claim 1-3, it is characterised in that, described liquid amine is selected from: liquefied ammonia, quadrol.
7. method as described in item as arbitrary in claim 1-3, it is characterised in that, described fatty alcohol is selected from: ethanol, Virahol, the trimethyl carbinol.
8. method as described in item as arbitrary in claim 1-3, it is characterised in that, in step (c), the feed postition of described fatty alcohol is once all add or add with the speed of 3-10ml/h.
9. method as described in item as arbitrary in claim 1-3, it is characterised in that, the ratio 1g:1-20mL of the quality of described Na-K alloy and nonaqueous liquid amine volume.
10. method as described in item as arbitrary in claim 1-3, it is characterised in that, in described fluorographite dispersion liquid, the quality of fluorographite is 0.5-20mg:1mL with the ratio of the volume of liquid amine.
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| CN103555326A (en) * | 2013-10-17 | 2014-02-05 | 厦门大学 | Preparation method of oxygen-free graphene fluorescence quantum dots |
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| CN101783366A (en) * | 2010-02-11 | 2010-07-21 | 复旦大学 | Preparation method of graphene MOS transistor |
| CN103555326A (en) * | 2013-10-17 | 2014-02-05 | 厦门大学 | Preparation method of oxygen-free graphene fluorescence quantum dots |
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