CN103588195A - Preparation method of graphene - Google Patents
Preparation method of graphene Download PDFInfo
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- CN103588195A CN103588195A CN201310539828.XA CN201310539828A CN103588195A CN 103588195 A CN103588195 A CN 103588195A CN 201310539828 A CN201310539828 A CN 201310539828A CN 103588195 A CN103588195 A CN 103588195A
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Abstract
The invention discloses a preparation method of graphene. The preparation method is implemented according to the following steps: mixing evenly sodium chloride, potassium chloride and zinc chloride, to prepare a molten salt with a low melting point, carrying out thermal intercalation of graphite fluoride by using the molten salt, and carrying out the intercalation process and a reaction process at the same time to obtain better intercalation effect; carrying out ultrasonic stripping of the intercalation composite; centrifuging to remove the intercalation composite which is not stripped, carrying out suction filtration of the centrifuged upper solution, and washing to obtain graphene. The preparation method does not require high temperature and high vacuum conditions and special reaction instruments; and compared with other preparation methods of the graphene material, the preparation method has simple preparation process and low preparation cost, and allows the obtained graphene to have large sheet area, fewer sheet layers, and high regularity.
Description
Technical field
The preparation method who the present invention relates to a kind of Graphene, belongs to field of nano material preparation.
Background technology
Within 2004, British scientist has been prepared the two-dimentional atomic crystal-Graphene consisting of carbon atom monoatomic layer first, and its thickness only has 0.3354nm, is the thin material of finding at present in the world.Graphene has special monoatomic layer structure and novel physical properties: intensity reaches 130GPa, the about 5000J/ of thermal conductivity (mKs), carrier mobility reaches 2 * 10
5cm
2/ (Vs), specific surface area calculated value is 2630m
2/ g, high-clarity (approximately 97.7%), energy gap are almost nil, and it also has the series of properties such as minimum electron conductivity under fractional quantum hall effect, quantum Hall ferromegnetism and the zero carrier concentration limit.In the past few years, Graphene has become a study hotspot in material science.
The preparation method of Graphene starts to develop gradually multiple preparation method from mechanically peel method the earliest, as: chemical Vapor deposition process, crystal epitaxy method, the direct stripping method of liquid phase, chemical reduction method and high temperature deoxidation method etc.Chemical Vapor deposition process is the common method of preparing at present big area Graphene, and the hydrocarbon gas that use (as CH more at present
4, C
2h
2, C
2h
4deng) as carbon source, also can utilize solid carbon aggressiveness to provide carbon source as presoma, as Sun etc. utilizes chemical Vapor deposition process that polymeric film is deposited on metal catalyst matrix, prepare the controlled Graphene (SunZ of the number of plies, YanZ, Yao J, etal.Growth of graphene from solid carbon sources[J] .Nature, 2010,468 (7323): 549 – 552).Compare with chemical Vapor deposition process, plasma enhanced chemical vapor deposition method can be prepared single-layer graphene within lower depositing temperature and shorter reaction times.In addition crystal epitaxy method can remove Si by heating monocrystalline 6H-SiC, thereby obtains at the epitaxially grown Graphene in SiC surface.But can there is reconstruct and surface tissue is changed in SiC plane of crystal in pyroprocess, so very difficult acquisition thickness is homogeneous, large-area graphene sheet layer (HannonJB, Tromp R M.Pit formation during graphene synthesis on SiC (0001): In situ electron microscopy[J] .Phys.Rev.B, 2008,77 (24): 241404.).
Different from above-mentioned synthetic method from bottom to top, top-down method can improve Graphene productive rate and be easy to preparation.As having become laboratory, simple graphite oxide reduction method prepares the simplest method of Graphene.Except chemical reduction method, also can graphite oxide be reduced into Graphene by electrochemical method, but in the Graphene that this method prepares C and O atomic ratio lower.In addition, microwave method is also used to prepare Graphene, as first Chen etc. is distributed to graphene oxide (GO) in the mixed solvent of N-N-N,N-DIMETHYLACETAMIDE and water (DMAc/H2O), then mixed reaction solution is carried out to microwave thermal reduction, the Graphene specific conductivity obtaining is 104 times of (ChenW of graphene oxide, YanL, BangalPR.Preparation of graphene by the rapid and mild thermal reduction of graphene oxide induced by microwaves.Carbon, 2010,48 (4): 1146 – 1152.).And next the basic metal intercalation stripping method of development is less than oxidation reduction process toxicity, and can not destroy the structure of Graphene.Owing to can preparing high-quality Graphene, therefore be also more and more subject to researchist's concern (Park K H, Kim B H, Song S H, et al.Exfoliation of non-oxidized graphene flakes for scalable conductive film[J] .Nano letters, 2012,12 (6): 2871-2876.).
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Graphene, this grapheme material, has good uniformity, regularity advantages of higher.Its preparation method process is simple, productive rate is high, the cycle is short, is applicable to scale operation.
Technical purpose of the present invention is achieved by following technical proposals:
A preparation method for Graphene, carries out according to following step:
Step 1, carries out melting after sodium-chlor, Repone K, zinc chloride are mixed according to mass ratio 1:1:3;
In described step 1, while selecting melting, at 250 ℃, make it melting, keep 30 minutes
Step 2, adds fluorographite in the melting salt of step 1, at 200 ℃-350 ℃, heats 6h-12h, carries out hot intercalation; In described step 2, the mass ratio of the melting salt of described fluorographite and step 1 is (1-5): 50;
Step 3, naturally cools to 20-25 ℃ of room temperatures by the intercalated compound of step 2, adds organic solvent ultrasonic centrifugal, removes lower floor's solid; In described step 3, described organic solvent is N-Methyl pyrrolidone, dimethyl formamide, Virahol, pyridine or dimethyl sulfoxide (DMSO), be chosen in ultrasonic 2h-12h under 200W power, centrifugal 5min – 30min under the rotating speed of 500r/min – 4000r/min, removes lower floor's solid;
Step 4, obtains filter cake by washing after gained solution suction filtration, after being dried, obtains Graphene; In described step 4, by after gained solution suction filtration, with deionized water, wash 3 times, obtain filter cake, filter cake is dried at 60 ℃, obtain Graphene.
The present invention uses an alkali metal salt intercalation fluorographite to prepare grapheme material, do not need high temperature, high vacuum condition and special reaction kit, in the process of an alkali metal salt intercalation fluorographite, the fluorine generation reduction reaction on an alkali metal salt and fluorographite, intercalation process and reaction process are carried out simultaneously, there is better intercalation effect, simple with other preparation methods' comparison preparation process of grapheme material, preparation cost is cheap, and resulting graphene film area is large, lamella is few, and regularity is high.In addition, resulting product is pure, is easy to realize scale operation.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the Graphene prepared of the present invention.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention.Fluorographite manufacturer is that Hubei Zhuo Xi fluoridizes Science and Technology Ltd..
Embodiment 1:
By sodium-chlor, Repone K, zinc chloride mixes according to mass ratio 1:1:3, at 250 ℃, heat 30min and make it melting, then 100mg fluorographite is mixed with the above-mentioned melting salt of 5g, at 300 ℃, heat 10h, carry out hot intercalation, after finishing heat-up time, above-mentioned intercalated compound is added in 200mLN-methyl-2-pyrrolidone, then by gained suspension ultrasonic 12h under 200W power, after ultrasonic time finishes by the centrifugal 20min under the rotating speed of 2000r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, with deionized water, wash 3 times, then the filter cake obtaining is dried at 60 ℃, obtain grapheme material.
Embodiment 2:
By sodium-chlor, Repone K, zinc chloride mixes according to mass ratio 1:1:3, at 250 ℃, heat 30min and make it melting, then 200mg fluorographite is mixed with the above-mentioned melting salt of 5g, at 280 ℃, heat 12h, carry out hot intercalation, after finishing heat-up time, above-mentioned intercalated compound is added in 200mL dimethyl formamide, then by gained suspension ultrasonic 10h under 200W power, after ultrasonic time finishes by the centrifugal 20min under the rotating speed of 1000r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, with deionized water, wash 3 times, then the filter cake obtaining is dried at 60 ℃, obtain grapheme material.
Embodiment 3:
By sodium-chlor, Repone K, zinc chloride mixes according to mass ratio 1:1:3, at 250 ℃, heat 30min and make it melting, then 100mg fluorographite is mixed with the above-mentioned melting salt of 5g, at 200 ℃, heat 12h, carry out hot intercalation, after finishing heat-up time, above-mentioned intercalated compound is added in 200mL Virahol, then by gained suspension ultrasonic 12h under 200W power, after ultrasonic time finishes by the centrifugal 15min under the rotating speed of 3000r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, with deionized water, wash 3 times, then the filter cake obtaining is dried at 60 ℃, obtain grapheme material.
Embodiment 4:
By sodium-chlor, Repone K, zinc chloride mixes according to mass ratio 1:1:3, at 250 ℃, heat 30min and make it melting, then 500mg fluorographite is mixed with the above-mentioned melting salt of 5g, at 220 ℃, heat 6h, carry out hot intercalation, after finishing heat-up time, above-mentioned intercalated compound is added in 200mL pyridine, then by gained suspension ultrasonic 8h under 200W power, after ultrasonic time finishes by the centrifugal 10min under the rotating speed of 4000r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, with deionized water, wash 3 times, then the filter cake obtaining is dried at 60 ℃, obtain grapheme material.
Embodiment 5:
By sodium-chlor, Repone K, zinc chloride mixes according to mass ratio 1:1:3, at 250 ℃, heat 30min and make it melting, then 300mg fluorographite is mixed with the above-mentioned melting salt of 5g, at 350 ℃, heat 8h, carry out hot intercalation, after finishing heat-up time, above-mentioned intercalated compound is added in 200mL dimethyl sulfoxide (DMSO), then by gained suspension ultrasonic 8h under 200W power, after ultrasonic time finishes by the centrifugal 30min under the rotating speed of 2500r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, with deionized water, wash 3 times, then the filter cake obtaining is dried at 60 ℃, obtain grapheme material.
Utilize the Dutch TecnaiG2F20 of FEI Co. to carry out TEM (transmission electron microscope) analysis, as shown in Figure 1, carry out corresponding eds analysis, result is as follows:
Fluorographite raw material energy stave
Fluorinated graphene energy stave
Above the present invention has been done to exemplary description; should be noted that; in the situation that not departing from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (5)
1. a preparation method for Graphene, is characterized in that, according to following step, carries out:
Step 1, carries out melting after sodium-chlor, Repone K, zinc chloride are mixed according to mass ratio 1:1:3;
Step 2, adds fluorographite in the melting salt of step 1, at 200 ℃-350 ℃, heats 6h-12h, carries out hot intercalation; In described step 2, the mass ratio of the melting salt of described fluorographite and step 1 is (1-5): 50;
Step 3, naturally cools to 20-25 ℃ of room temperatures by the intercalated compound of step 2, adds organic solvent ultrasonic centrifugal, removes lower floor's solid;
Step 4, obtains filter cake by washing after gained solution suction filtration, after being dried, obtains Graphene.
2. the preparation method of a kind of Graphene according to claim 1, is characterized in that, in described step 1, while selecting melting, at 250 ℃, makes it melting, keeps 30 minutes.
3. the preparation method of a kind of Graphene according to claim 1, is characterized in that, in described step 3, described organic solvent is N-Methyl pyrrolidone, dimethyl formamide, Virahol, pyridine or dimethyl sulfoxide (DMSO).
4. the preparation method of a kind of Graphene according to claim 1, is characterized in that, in described step 3, is chosen in ultrasonic 2h-12h under 200W power, and centrifugal 5min – 30min under the rotating speed of 500r/min – 4000r/min removes lower floor's solid.
5. the preparation method of a kind of Graphene according to claim 1, is characterized in that, in described step 4, by after gained solution suction filtration, with deionized water, washes 3 times, obtains filter cake, and filter cake is dried at 60 ℃, obtains Graphene.
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| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
| CN104445160A (en) * | 2014-11-07 | 2015-03-25 | 孙旭阳 | Method for preparing graphene through molten inorganic salt reaction bed |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
| CN104876218A (en) * | 2015-06-10 | 2015-09-02 | 北京化工大学 | Room-temperature preparation method for water-soluble functionalized graphene |
| CN105366658A (en) * | 2015-11-13 | 2016-03-02 | 哈尔滨工程大学 | Method for preparing porous carbon for super capacitor by waste plastic carbonization |
| WO2016070396A1 (en) * | 2014-11-07 | 2016-05-12 | 孙旭阳 | Method for preparing graphene by molten state inorganic salt reaction bed |
| CN105668530A (en) * | 2016-01-14 | 2016-06-15 | 苏州微格纳米科技有限公司 | Preparation method of two-dimensional nanomaterial |
| CN106784547A (en) * | 2016-12-10 | 2017-05-31 | 浙江大学 | The preparation method of gel polymer lithium ion battery |
| CN107055515A (en) * | 2016-11-03 | 2017-08-18 | 孙旭阳 | A kind of method that atomized molten medium prepares graphene |
| CN107176600A (en) * | 2016-03-11 | 2017-09-19 | 北京大学 | A kind of cube pattern graphene powder and preparation method and application |
| CN108423661A (en) * | 2018-03-29 | 2018-08-21 | 武汉科技大学 | It is a kind of to derive the graphene that charcoal prepares the method for graphene and its prepares with mesophase pitch |
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| CN110294470A (en) * | 2018-03-22 | 2019-10-01 | 中国科学院上海硅酸盐研究所 | It is a kind of to vulcanize three-dimensional porous grapheme material and preparation method thereof |
| CN111620326A (en) * | 2020-04-27 | 2020-09-04 | 福建江夏学院 | Preparation method of fluorinated graphene material with adjustable fluorine content |
| CN112830479A (en) * | 2021-02-25 | 2021-05-25 | 山东大学 | Method for preparing easy-to-strip near-free graphene by using sulfur beam decoupling technology |
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| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
| US10392256B2 (en) * | 2014-11-07 | 2019-08-27 | Xuyang SUN | Method for preparing graphene by using molten inorganic salt reaction bed |
| CN104445160A (en) * | 2014-11-07 | 2015-03-25 | 孙旭阳 | Method for preparing graphene through molten inorganic salt reaction bed |
| EP3216757A4 (en) * | 2014-11-07 | 2018-04-04 | Sun, Xuyang | Method for preparing graphene by molten state inorganic salt reaction bed |
| WO2016070396A1 (en) * | 2014-11-07 | 2016-05-12 | 孙旭阳 | Method for preparing graphene by molten state inorganic salt reaction bed |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
| CN104876218B (en) * | 2015-06-10 | 2017-06-20 | 北京化工大学 | A kind of room temperature preparation method of water-soluble functionalized graphite's alkene |
| CN104876218A (en) * | 2015-06-10 | 2015-09-02 | 北京化工大学 | Room-temperature preparation method for water-soluble functionalized graphene |
| CN105366658A (en) * | 2015-11-13 | 2016-03-02 | 哈尔滨工程大学 | Method for preparing porous carbon for super capacitor by waste plastic carbonization |
| CN105668530A (en) * | 2016-01-14 | 2016-06-15 | 苏州微格纳米科技有限公司 | Preparation method of two-dimensional nanomaterial |
| CN105668530B (en) * | 2016-01-14 | 2018-01-19 | 苏州微格纳米科技有限公司 | A kind of preparation method of two-dimension nano materials |
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| CN107055515A (en) * | 2016-11-03 | 2017-08-18 | 孙旭阳 | A kind of method that atomized molten medium prepares graphene |
| CN106784547A (en) * | 2016-12-10 | 2017-05-31 | 浙江大学 | The preparation method of gel polymer lithium ion battery |
| CN106784547B (en) * | 2016-12-10 | 2019-04-02 | 浙江大学 | The preparation method of gel polymer lithium ion battery |
| CN110294470B (en) * | 2018-03-22 | 2022-10-14 | 中国科学院上海硅酸盐研究所 | Vulcanized three-dimensional porous graphene material and preparation method thereof |
| CN110294470A (en) * | 2018-03-22 | 2019-10-01 | 中国科学院上海硅酸盐研究所 | It is a kind of to vulcanize three-dimensional porous grapheme material and preparation method thereof |
| CN108423661A (en) * | 2018-03-29 | 2018-08-21 | 武汉科技大学 | It is a kind of to derive the graphene that charcoal prepares the method for graphene and its prepares with mesophase pitch |
| CN108976433A (en) * | 2018-07-13 | 2018-12-11 | 江南大学 | A kind of method that liquid phase stripping method prepares metal organic frame nanometer sheet |
| CN108976433B (en) * | 2018-07-13 | 2020-08-04 | 江南大学 | Method for preparing metal organic framework nanosheet by liquid phase stripping method |
| CN109750316A (en) * | 2018-09-12 | 2019-05-14 | 东莞理工学院 | Electrochemistry formated ammonia catalyst based on graphene quantum dot and preparation method thereof |
| CN109323896B (en) * | 2018-09-12 | 2021-09-03 | 东莞理工学院 | Pesticide detection method based on graphene quantum dots |
| CN109323896A (en) * | 2018-09-12 | 2019-02-12 | 东莞理工学院 | Pesticide detection method based on graphene quantum dot |
| CN111620326A (en) * | 2020-04-27 | 2020-09-04 | 福建江夏学院 | Preparation method of fluorinated graphene material with adjustable fluorine content |
| CN111620326B (en) * | 2020-04-27 | 2022-09-02 | 福建江夏学院 | Preparation method of fluorinated graphene material with adjustable fluorine content |
| CN112877038A (en) * | 2021-01-13 | 2021-06-01 | 中盐金坛盐化有限责任公司 | Chloride-based molten salt heat transfer and storage medium and preparation method and application thereof |
| CN113004875A (en) * | 2021-02-09 | 2021-06-22 | 中盐金坛盐化有限责任公司 | Chloride-based nano molten salt heat transfer and storage medium and application and preparation method thereof |
| CN112830479A (en) * | 2021-02-25 | 2021-05-25 | 山东大学 | Method for preparing easy-to-strip near-free graphene by using sulfur beam decoupling technology |
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