CN103553030A - Preparation method of few-layer graphene - Google Patents
Preparation method of few-layer graphene Download PDFInfo
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- CN103553030A CN103553030A CN201310542269.8A CN201310542269A CN103553030A CN 103553030 A CN103553030 A CN 103553030A CN 201310542269 A CN201310542269 A CN 201310542269A CN 103553030 A CN103553030 A CN 103553030A
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Abstract
The invention provides a preparation method of few-layer graphene. The preparation method at least comprises the following steps: mixing a graphite sheet with a solvent, shearing and stirring a mixed solution of the graphite sheet and the solvent in a shear rate of 500-300000r/min for 30min to 30 hours to obtain a reacted mixed solution, standing the reacted mixed solution, filtering supernatant to obtain filter residue, and then obtaining the few-layer graphene. The preparation method can be used for efficiently and fast preparing the few-layer graphene in a large scale.
Description
Technical field
The preparation method who the present invention relates to a kind of few layer graphene, belongs to the Graphene technical field in field of nanometer material technology.
Background technology
Since being found from Graphene in 2004, just enjoyed the generally favor from physics and Material Field investigator always.Graphene be a kind of by carbon atom with sp
2the hexangle type that hybridized orbital forms is the flat film of honeycomb lattice.Although Graphene only has a carbon atomic layer thickness, and be the thinnest a kind of in known materials, however very firmly hard.Graphene is also the outstanding material of current known conductive.In addition, Graphene also has the performance of many excellences: as higher Young's modulus, thermal conductivity, huge specific surface area etc.Due to the property of Graphene, it is all widely used at aspects such as electronics, optics, magnetics, biomedicine, sensor, energy storage.And prepare Graphene how efficiently, fast, on a large scale, become the most popular research topic in this area.
At present, the method for preparing Graphene mainly comprises following several: oxidation reduction process, chemical Vapor deposition process, mechanically peel method, epitaxial growth method, solvent stripping method etc.But oxidation reduction process need experience the oxidising process of graphite, and Graphite Powder 99 is easily introduced a large amount of defects in the process of oxidation, is but difficult to repair these defects completely, so be difficult to prepare high-quality Graphene during reduction.The preparation condition harshness of chemical Vapor deposition process and epitaxial growth method, complicated operation, apparatus expensive, thereby be difficult to carry out scale operation.The complex operation of mechanically peel method, the amount of each product obtaining seldom and also cost very high, be unfavorable for extensive preparation.Although solvent stripping method can prepare high-quality Graphene, there is the shortcoming that productive rate is low, and be unfavorable for industrializing implementation.
Wang etc. have prepared few layer graphene (Graphene of the number of plies between 3 layers to 10 layers) by electrochemical method high yield, but the method must be used electrochemical appliance, and electrode complex disposal process, therefore do not possess possibility (the Wang et al. of scale operation, JAm Chem Soc, 2011,133,8888).
As can be seen here, develop a kind of preparation method of few layer graphene, be still one of this area problem demanding prompt solution.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of preparation method of few layer graphene.Preparation method of the present invention can prepare few layer graphene efficiently, fast, on a large scale.
For reaching above-mentioned purpose, the invention provides a kind of preparation method of few layer graphene, it at least comprises the following steps:
Admixed graphite thin slice and a solvent; Then with the shearing rate of 500-30000r/min, the mixed solution of graphite flake and solvent is carried out to shear agitation 30min to 30 hour, obtain a reacted mixed solution; Standing described reacted mixed solution, then carried out leaching filter residue by upper strata liquid, obtained described few layer graphene.
In above-mentioned preparation method, preferably, described shearing rate is 5000-20000r/min, and the time of described shear agitation is 1-10 hour.
In above-mentioned preparation method, preferably, described solvent comprises one or more the combination in nitrogen methyl-2-pyrrolidone (NMP), dimethyl phthalate (DMP), sodium lauryl sulphate (SDS) and nitrogen dimethylformamide (DMF) etc.
In above-mentioned preparation method, preferably, the ratio of described graphite flake and described solvent is 0.1g-10g:1L.
In above-mentioned preparation method, preferably, described graphite flake comprises one or more the combination in the graphite flake that expands again after Graphite thin slice, exfoliated graphite sheet and ball milling etc.Wherein, ball milling and expansion be this area prepare graphite flake the conventional method adopting.
In above-mentioned preparation method, preferably, the number of plies of described graphite flake is below 30 layers.
In above-mentioned preparation method, preferably, the graphite flake that described graphite flake is purified processing, and described purification process at least comprises ultrasonic cleaning.The ultrasonic frequency of this ultrasonic cleaning, power and ultrasonic cleaning time can be carried out conventional adjustment according to practical situation by those skilled in the art.Such as, hyperacoustic frequency can be 40KHz, and power can be 150W, and the ultrasonic cleaning time can be 5-10min.In addition,, except ultrasonic cleaning, can also use conventional other purification process modes of using in chemical treatment or this area to carry out purification process to graphite flake, to remove dephasign material and impurity element wherein.
In above-mentioned preparation method, preferably, described shear agitation is carried out in refiner.
In above-mentioned preparation method, preferably, the described standing time is 12-48 hour.
In above-mentioned preparation method, preferably, upper strata liquid was carried out after leaching filter residue, also comprise filter residue is cleaned and dry step.To the cleaning of filter residue, can adopt ethanol.The number of times of washing and each consumption can carry out conventional selection and adjustment by those skilled in the art.To the dry of the filter residue after washing, can be oven drying, drying temperature can be 80-100 ℃, and the time can be 12h.
According to the specific embodiment of the present invention, preferably, above-mentioned preparation method comprises the following steps:
(1) to the number of plies, be, that purification process is carried out in one or more combination in the graphite flake expanding again after 30 layers of following Graphite thin slice, exfoliated graphite sheet and ball milling, this purification process at least comprises ultrasonic cleaning, this ultrasonic cleaning is is 40KHz in hyperacoustic frequency, power is under the condition of 150W, ultrasonic cleaning 5-10min, obtains the graphite flake of purified processing;
(2), the ratio (graphite flake: solvent) put into refiner with 0.1g-10g:1L by the graphite flake of purified processing and solvent, then open refiner, shearing rate with 500-30000r/min is carried out shear agitation 30min to 30 hour to the mixed solution of graphite flake and solvent, utilize the shearing force of high-revolving different in flow rate fluid to peel off graphite flake, stop refiner, obtain a reacted mixed solution;
(3), pour described reacted mixed solution in beaker standing 12-48 hour, utilize the dispersion effect of solvent, will lack layer graphene and isolate, upper strata liquid was carried out to leaching filter residue, obtain described few layer graphene.
As shown in Figure 1, Fig. 1 is the preparation method's of few layer graphene of the present invention principle schematic, the preparation method of few layer graphene of the present invention utilizes the shearing force of different in flow rate fluid 2 to peel off graphite flake 1, can prepare efficiently, fast, on a large scale few layer graphene 3.Preparation method of the present invention is simple to operate, consuming time short, cost is low, be easy to realize large-scale industrialization produces; And the few layer graphene defect preparing is few, quality is high.
Accompanying drawing explanation
Fig. 1 is the preparation method's of few layer graphene of the present invention principle schematic.
Fig. 2 is the transmission electron microscope photo of few layer graphene product of embodiment 1.
Fig. 3 is the transmission electron microscope photo of few layer graphene product of embodiment 1.
Fig. 4 is the transmission electron microscope photo of few layer graphene product of embodiment 2.
Fig. 5 is the transmission electron microscope photo of few layer graphene product of embodiment 2.
Fig. 6 is the transmission electron microscope photo of few layer graphene product of embodiment 3.
Fig. 7 is the transmission electron microscope photo of few layer graphene product of embodiment 3.
Fig. 8 is the transmission electron microscope photo of few layer graphene product of embodiment 4.
Fig. 9 is the transmission electron microscope photo of few layer graphene product of embodiment 4.
Primary clustering nomenclature:
The few layer graphene 3 of graphite flake 1 fluid 2
Embodiment
For technical characterictic of the present invention, object and beneficial effect being had more clearly, understand, existing technical scheme of the present invention is carried out to following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
The present embodiment provides a kind of preparation method of few layer graphene, and it comprises the following steps:
(1) to the number of plies, be, that the graphite flake expanding again after 30 layers of following ball milling carries out purification process, this purification process at least comprises ultrasonic cleaning, this ultrasonic cleaning is is 40KHz in hyperacoustic frequency, power is under the condition of 150W, ultrasonic cleaning 5-10min, obtains the graphite flake of purified processing;
(2), the ratio (graphite flake: NMP) put into refiner with 0.5g:500mL by the graphite flake of purified processing and nitrogen methyl-2-pyrrolidone (NMP), then open refiner, shearing rate with 8000r/min is carried out shear agitation 1 hour to the mixed solution of graphite flake and NMP, utilize the shearing force of high-revolving different in flow rate fluid to peel off graphite flake, stop refiner, obtain a reacted mixed solution;
(3), described reacted mixed solution is poured in beaker standing 24 hours, utilize the dispersion effect of NMP, will lack layer graphene and isolate, upper strata liquid was carried out to leaching filter residue, obtain described few layer graphene.
Few layer graphene product of gained is carried out to transmission electron microscope (TEM) and characterize, as shown in Figures 2 and 3, Fig. 2 and Fig. 3 are respectively the TEM photo of the few layer graphene product under the different visuals field to the TEM photo of gained.By Fig. 2 and Fig. 3, can know the number of plies of seeing Graphene product, the defect that simultaneously can observe Graphene product is less, according to the known method of Fig. 2, Fig. 3 and this area (number of plies statistical technique), calculates and in known Graphene product, is less than the Graphene (few layer graphene) of 10 layers and accounts for 87%(to take the gross weight of described Graphene product be benchmark).
The present embodiment provides a kind of preparation method of few layer graphene, and it comprises the following steps:
(1) to the number of plies, be, that the graphite flake expanding again after 30 layers of following ball milling carries out purification process, this purification process at least comprises ultrasonic cleaning, this ultrasonic cleaning is is 40KHz in hyperacoustic frequency, power is under the condition of 150W, ultrasonic cleaning 5-10min, obtains the graphite flake of purified processing;
(2), the ratio (graphite flake: SDS) put into refiner with 5g:500mL by the graphite flake of purified processing and sodium lauryl sulphate (SDS), then open refiner, shearing rate with 20000r/min is carried out shear agitation 2 hours to the mixed solution of graphite flake and SDS, utilize the shearing force of high-revolving different in flow rate fluid to peel off graphite flake, stop refiner, obtain a reacted mixed solution;
(3), described reacted mixed solution is poured in beaker standing 12 hours, utilize the dispersion effect of SDS, will lack layer graphene and isolate, upper strata liquid was carried out to leaching filter residue, obtain described few layer graphene.
Few layer graphene product of gained is carried out to transmission electron microscope (TEM) and characterize, as shown in Figure 4 and Figure 5, Fig. 4 and Fig. 5 are respectively the TEM photo of the few layer graphene product under the different visuals field to the TEM photo of gained.By Fig. 4 and Fig. 5, can know the number of plies of seeing Graphene product, the defect that simultaneously can observe Graphene product is less, according to the known method of Fig. 4, Fig. 5 and this area (number of plies statistical technique), calculates and in known Graphene product, is less than the Graphene (few layer graphene) of 10 layers and accounts for 83%(to take the gross weight of described Graphene product be benchmark).
The present embodiment provides a kind of preparation method of few layer graphene, and it comprises the following steps:
(1) to the number of plies, be, that the graphite flake expanding again after 30 layers of following ball milling carries out purification process, this purification process at least comprises ultrasonic cleaning, this ultrasonic cleaning is is 40KHz in hyperacoustic frequency, power is under the condition of 150W, ultrasonic cleaning 5-10min, obtains the graphite flake of purified processing;
(2), the ratio (graphite flake: DMP) put into refiner with 0.05g:500mL by the graphite flake of purified processing and dimethyl phthalate (DMP), then open refiner, shearing rate with 500r/min is carried out shear agitation 30 hours to the mixed solution of graphite flake and DMP, utilize the shearing force of high-revolving different in flow rate fluid to peel off graphite flake, stop refiner, obtain a reacted mixed solution;
(3), described reacted mixed solution is poured in beaker standing 48 hours, utilize the dispersion effect of DMP, will lack layer graphene and isolate, upper strata liquid was carried out to leaching filter residue, obtain described few layer graphene.
Few layer graphene product of gained is carried out to transmission electron microscope (TEM) and characterize, as shown in Figure 6 and Figure 7, Fig. 6 and Fig. 7 are respectively the TEM photo of the few layer graphene product under the different visuals field to the TEM photo of gained.By Fig. 6 and Fig. 7, can know the number of plies of seeing Graphene product, the defect that simultaneously can observe Graphene product is less, according to the known method of Fig. 6, Fig. 7 and this area (number of plies statistical technique), calculates and in known Graphene product, is less than the Graphene (few layer graphene) of 10 layers and accounts for 72%(to take the gross weight of described Graphene product be benchmark).
Embodiment 4
The present embodiment provides a kind of preparation method of few layer graphene, and it comprises the following steps:
(1) to the number of plies, be, that the graphite flake expanding again after 30 layers of following ball milling carries out purification process, this purification process at least comprises ultrasonic cleaning, this ultrasonic cleaning is is 40KHz in hyperacoustic frequency, power is under the condition of 150W, ultrasonic cleaning 5-10min, obtains the graphite flake of purified processing;
(2), the ratio (graphite flake: DMF) put into refiner with 1g:500mL by the graphite flake of purified processing and nitrogen dimethylformamide (DMF), then open refiner, shearing rate with 30000r/min is carried out shear agitation 30 minutes to the mixed solution of graphite flake and DMF, utilize the shearing force of high-revolving different in flow rate fluid to peel off graphite flake, stop refiner, obtain a reacted mixed solution;
(3), described reacted mixed solution is poured in beaker standing 12 hours, utilize the dispersion effect of DMF, will lack layer graphene and isolate, upper strata liquid was carried out to leaching filter residue, obtain described few layer graphene.
Few layer graphene product of gained is carried out to transmission electron microscope (TEM) and characterize, as shown in Figure 8 and Figure 9, Fig. 8 and Fig. 9 are respectively the TEM photo of the few layer graphene product under the different visuals field to the TEM photo of gained.By Fig. 8 and Fig. 9, can know the number of plies of seeing Graphene product, the defect that simultaneously can observe Graphene product is less, according to the known method of Fig. 8, Fig. 9 and this area (number of plies statistical technique), calculates and in known Graphene product, is less than the Graphene (few layer graphene) of 10 layers and accounts for 79%(to take the gross weight of described Graphene product be benchmark).
Claims (10)
1. lack a preparation method for layer graphene, it at least comprises the following steps:
Admixed graphite thin slice and a solvent; Then with the shearing rate of 500-30000r/min, the mixed solution of graphite flake and solvent is carried out to shear agitation 30min to 30 hour, obtain a reacted mixed solution; Standing described reacted mixed solution, then carried out leaching filter residue by upper strata liquid, obtained described few layer graphene.
2. preparation method according to claim 1, wherein, described shearing rate is 5000-20000r/min, the time of described shear agitation is 1-10 hour.
3. preparation method according to claim 1, wherein, described solvent comprises one or more the combination in nitrogen methyl-2-pyrrolidone, dimethyl phthalate, sodium lauryl sulphate and nitrogen dimethylformamide.
4. preparation method according to claim 1, wherein, the ratio of described graphite flake and described solvent is 0.1g-10g:1L.
5. preparation method according to claim 1, wherein, described graphite flake comprises one or more the combination in the graphite flake expanding again after Graphite thin slice, exfoliated graphite sheet and ball milling.
6. preparation method according to claim 1 or 5, wherein, the number of plies of described graphite flake is below 30 layers.
7. according to the preparation method described in claim 1,5 or 6, wherein, the graphite flake that described graphite flake is purified processing, and described purification process at least comprises ultrasonic cleaning.
8. preparation method according to claim 1, wherein, described shear agitation is carried out in refiner.
9. preparation method according to claim 1, wherein, the described standing time is 12-48 hour.
10. preparation method according to claim 1, wherein, carried out upper strata liquid after leaching filter residue, also comprises filter residue is cleaned and dry step.
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| CN104003375A (en) * | 2014-05-05 | 2014-08-27 | 北京航空航天大学 | Preparation method for small-size graphene |
| CN105347332A (en) * | 2015-11-25 | 2016-02-24 | 山东科技大学 | Preparation method for graphene |
| CN106115679A (en) * | 2016-07-04 | 2016-11-16 | 济南大学 | A kind of low cost prepares the method for Graphene |
| CN106995212A (en) * | 2017-05-05 | 2017-08-01 | 李源作 | A kind of mechanical shearing peels off the dilute method of production graphite |
| CN108439390A (en) * | 2018-05-29 | 2018-08-24 | 武汉科技大学 | Based on the method for isolating and purifying graphene from Pintsch process charcoal |
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| EP3204223A4 (en) * | 2014-10-05 | 2018-12-19 | EOS GmbH Electro Optical Systems | 3d printers and feedstocks for 3d printers |
| US10926326B2 (en) | 2014-10-05 | 2021-02-23 | Yazaki Corporation | 3D printers and feedstocks for 3D printers |
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| CN109694529B (en) * | 2017-10-23 | 2020-11-06 | 中国科学院理化技术研究所 | Preparation method of graphene PVC (polyvinyl chloride) antistatic composite material |
| CN109694529A (en) * | 2017-10-23 | 2019-04-30 | 中国科学院理化技术研究所 | A kind of preparation method of graphene PVC anti-static composite material |
| CN108439390A (en) * | 2018-05-29 | 2018-08-24 | 武汉科技大学 | Based on the method for isolating and purifying graphene from Pintsch process charcoal |
| CN108706577A (en) * | 2018-06-19 | 2018-10-26 | 于峰 | A kind of method for separating and preparing of graphene nano material |
| CN109384219A (en) * | 2018-11-16 | 2019-02-26 | 新奥石墨烯技术有限公司 | Nano-fluid towards high efficient heat exchanging working medium and preparation method thereof and heat exchange equipment |
| CN109607516A (en) * | 2018-11-26 | 2019-04-12 | 天元羲王控股有限公司 | A kind of layer graphene production equipment and its control method less |
| CN111137880A (en) * | 2019-12-18 | 2020-05-12 | 武汉科技大学 | Separation and purification method of graphene |
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Application publication date: 20140205 |