CN101549864A - Method for simply and innoxiously preparing single-layer graphene - Google Patents
Method for simply and innoxiously preparing single-layer graphene Download PDFInfo
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Abstract
The invention relates to a method for simply and innoxiously preparing single-layer graphene, belonging to the chemical field of inorganic field. The technical processes of the invention are as follows: adopting a fixed amount of natural graphite powder; oxidizing the natural graphite powder in a strong oxidizing condition to obtain the graphite oxide; dispersing the obtained graphite oxide in the de-ionized water; then ultrasonically processing for a certain period in an ultrasonic machine to peel the graphite oxide off into single-layer graphite oxide sheet; then dispersing the graphite oxide sheet in the dimethylsulfoxide solution; transferring the mixture solution to a reaction kettle and reacting for 10 to 16 hours in 150 to 200 degrees centigrade; after filtered, obtaining the mass colour product, that is, single-layer grapheme. The invention adopts nontoxic reducing agent, dimethylsulfoxide, so it is good for environment protection. The invention has simple technique, operation convenience, and low manufacturing cost.
Description
Technical field
The present invention relates to a kind of method of simple innoxiously preparing single-layer graphene, belong to the inorganic materials chemical field.
Background technology
Since finding that it independently existed in 2004, Graphene (Graphene) is as a kind of new allotropic substance of carbon, and it has more special cellular two-dirnentional structure, is made up of the monolayer carbon atom, it not only has the favorable mechanical performance, and unique electrical properties is also arranged.It is a zero gap semiconductor, have unique current carrier characteristic and excellent electricity quality, and electronics wherein aspect a lot of as the electronic mobility of immeasurable dirac fermion, Brillouin scatter and superelevation, higher 100 times than the electronic mobility of silicon semiconductor, higher 20 times than gallium arsenide.In view of it has so many unusual characteristic, therefore receive much concern recently, be considered to have great application prospect, comprising electron device, energy storage etc. at wide spectrum.
The method of existing preparation Graphene (Graphene) mainly is mechanically peel method, heating SiC method, chemical dispersion method, and method respectively has its advantage, and shortcoming is separately also arranged simultaneously.Mechanically peel method, heating SiC method all need the temperature condition of superelevation, complex process, and preparation time is long, the more high shortcoming of cost.Chemical dispersion method is as a kind of important preparation method, select a kind of method of the suitable former graphite oxide of ring to become to attach most importance to, present method of reducing mainly comprises reduction such as hydrazine hydrate, dimethylhydrazine, but one closes hydrazine, dimethylhydrazine and is faced with supervirulent huge unfavourable condition again.So, prepare in the mono-layer graphite oxide sheet process in the applied chemistry dispersion method, it is very urgent to seek a kind of novel simple method of reducing.
Summary of the invention
The method that the objective of the invention is a kind of simple innoxiously preparing single-layer graphene.
The method of a kind of simple innoxiously preparing single-layer graphene of the present invention is characterized in that having following process and step:
A. mono-layer graphite oxide sheet solution and graphene oxide solid preparation: with natural graphite powder is raw material, adds a certain amount of vitriol oil, Potassium Persulphate and Vanadium Pentoxide in FLAKES, at 80 ℃ of following uniform mixing, makes its reaction 4.5 hours; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that stir on the graphite limit of preoxidation, the limit adds in the mixing solutions of the cold vitriol oil and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of superoxol again; Then above-mentioned solution is filtered, and remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality with the dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally make graphite oxide; The graphite oxide of gained is mixed with the aqueous solution of 0.5 mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide sheet solution; Again this mono-layer graphite oxide sheet solution is placed on centrifugation in the supercentrifuge, resulting solid is carried out vacuum-drying, be the graphene oxide solid;
B. the preparation of single-layer graphene: in dimethyl sulfoxide solution, both amount ratios are 1: 1 with the graphene oxide solid dispersed of above-mentioned gained; Be that per 1 milligram of graphene oxide solid adds 1 milliliter dimethyl sulfoxide solution; After stirring it is transferred in the reactor, and reacted 10～16 hours down, after filtering, obtain the black product and be single-layer graphene, product is placed under the vacuum-drying condition preserves at 150～200 ℃.
The product single-layer graphene that the inventive method makes has the individual layer two-dirnentional structure, and the principal feature of the inventive method is: do not use common poisonous and hazardous chemical substance commonly used to be nearly former dose.The present invention has adopted methyl-sulphoxide as dispersion medium, so environmentally safe helps environment protection.Technology of the present invention is simple, be convenient to operation, and manufacturing cost is lower.
Description of drawings
Fig. 1 is atomic force microscope (AFM) the photo figure of the mono-layer graphite oxide sheet of gained of the present invention.
Fig. 2 is X-ray diffraction (XRD) spectrogram of the Graphene of gained of the present invention.
Fig. 3 is x-ray photoelectron spectroscopy (XPS) data plot of the Graphene of gained of the present invention.
Fig. 4 is the thermogravimetric and differential scanning calorimetric analysis (TG-DSC) the data and curves figure of the Graphene of gained of the present invention.
Embodiment
After now specific embodiments of the invention being discussed in.
Embodiment 1
Preparation process and step in the present embodiment are as described below:
1, mono-layer graphite oxide sheet solution and graphene oxide solid preparation: with natural graphite powder is raw material, get the natural graphite powder of 3 grams, 325 order fineness, add 12 milliliters of vitriol oils, 2.5 gram Potassium Persulphates and 2.5 gram Vanadium Pentoxide in FLAKESs,, make its reaction 4.5 hours at 80 ℃ of following uniform mixing; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that the graphite limit stirring of preoxidation, 120 milliliters of the vitriol oils and the potassium permanganate 15 that the limit slowly adds 0 ℃ of refrigerative restrain in the mixing solutions of forming, after stirring 2 hours under 35 ℃, release with 250 ml deionized water alkene, continue stirring and add 700 ml deionized water again after 2 hours, after stirring, add 20 milliliters of superoxols again; Then above-mentioned solution is filtered, and remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality with 1: 10 dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally obtain graphite oxide; The graphite oxide of gained is mixed with the aqueous solution of 0.5 mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide sheet solution; Again this mono-layer graphite oxide sheet solution is placed on centrifugation in the supercentrifuge, resulting solid is carried out vacuum-drying, be the graphene oxide solid;
2, the preparation of single-layer graphene: in dimethyl sulfoxide solution, both amount ratios are 1: 1 with the graphene oxide solid dispersed of above-mentioned gained; Be that per 1 milligram of graphene oxide solid adds 1 milliliter dimethyl sulfoxide solution; After stirring it is transferred in the reactor, and reacted 14 hours down, after filtering, obtain the black product and be single-layer graphene, product is placed under the vacuum-drying condition preserves at 180 ℃.
Embodiment 2
Preparation process in the present embodiment and step and the foregoing description 1 are identical.Different is: the temperature that heats in reactor is 150 ℃, and the reaction times is 10 hours, finally makes single-layer graphene.
Embodiment 3
Preparation process in the present embodiment and step and the foregoing description 1 are identical.Different is: the temperature that heats in reactor is 200 ℃, and the reaction times is 16 hours, finally makes single-layer graphene
The instrument detecting of products therefrom be the results are shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4 in the accompanying drawing.
Fig. 1 is atomic force microscope (AFM) the photo figure of gained mono-layer graphite oxide sheet among the embodiment.Its crystal formation form is the two-dimensional sheet structure as we know from the figure.
Fig. 2 is X-ray diffraction (XRD) spectrogram of gained Graphene among the embodiment.Its peak value place explanation has the existence of Graphene as seen from the figure.
Fig. 3 is x-ray photoelectron spectroscopy (XPS) data plot of gained Graphene among the embodiment.
Fig. 4 is the thermogravimetric and differential scanning calorimetric analysis (TG-DSC) the data and curves figure of gained Graphene among the embodiment.
Claims (1)
1, a kind of method of simple innoxiously preparing single-layer graphene is characterized in that having following process and step:
A. mono-layer graphite oxide sheet solution and graphene oxide solid preparation: with natural graphite powder is raw material, adds a certain amount of vitriol oil, Potassium Persulphate and Vanadium Pentoxide in FLAKES, at 80 ℃ of following uniform mixing, makes its reaction 4.5 hours; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that stir on the graphite limit of preoxidation, the limit adds in the mixing solutions of the cold vitriol oil and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of superoxol again; Then above-mentioned solution is filtered, and remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality with the dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally make graphite oxide; The graphite oxide of gained is mixed with the aqueous solution of 0.5mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide sheet solution; Again this mono-layer graphite oxide sheet solution is placed on centrifugation in the supercentrifuge, resulting solid is carried out vacuum-drying, be the graphene oxide solid;
B. the preparation of single-layer graphene: in dimethyl sulfoxide solution, both amount ratios are 1: 1 with the graphene oxide solid dispersed of above-mentioned gained; Be that per 1 milligram of graphene oxide solid adds 1 milliliter dimethyl sulfoxide solution; After stirring it is transferred in the reactor, and reacted 10～16 hours down, after filtering, obtain the black product and be single-layer graphene, product is placed under the vacuum-drying condition preserves at 150～200 ℃.
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