CN103771401A - Preparation method for single-layered graphene - Google Patents
Preparation method for single-layered graphene Download PDFInfo
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- CN103771401A CN103771401A CN201310739904.1A CN201310739904A CN103771401A CN 103771401 A CN103771401 A CN 103771401A CN 201310739904 A CN201310739904 A CN 201310739904A CN 103771401 A CN103771401 A CN 103771401A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a preparation method for single-layered graphene. The preparation method for the single-layered graphene comprises the following steps: carrying out purification treatment on graphite powder; adding the purified graphite powder into a high-pressure kettle or dispersing the purified graphite powder into a solvent, and then adding into the high-pressure kettle; heating and pumping supercritical fluid into the high-pressure kettle after the temperature in the high-pressure kettle reaches to a pre-set temperature; after raising the pressure in the high-pressure kettle to a pre-set value, agitating and stripping the graphite by a shearing force generated by the supercritical fluid which flows at a high speed, and rapidly reducing the pressure; sampling from the high-pressure kettle to obtain the single-layered graphene. The invention further provides the single-layered graphene which is prepared by the preparation method provided by the invention. The invention further provides a device for producing the single-layered graphene. The preparation method for the single-layered graphene provided by the invention is green and environment-friendly, low in production cost, short in reaction period and simple in preparation process; the sheet layer integrity of the prepared single-layered graphene is good.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene, particularly a kind of preparation method of few layer graphene, belongs to chemical materials preparation field.
Background technology
Since being found from Graphene in 2004, extremely physics and Material Field investigator's generally favor always.Graphene is a kind of by the tightly packed bi-dimensional cellular shape crystalline network carbonaceous material forming of monolayer carbon atom.Although Graphene only has a carbon atomic layer thickness, and is one the thinnest in known materials, 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 Graphene how to prepare high quality, high yield has become the research topic of this area hot topic.
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 all there is familiar lacunas in aforesaid method, and mostly belong to the preparation method of multi-layer graphene in the time of concrete application.
As can be seen here, developing a kind of preparation facilities and method of few layer graphene, is one of this area problem demanding prompt solution.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of preparation method of few layer graphene, the preparation technology of the method is simple, can prepare in a large number, efficiently the Graphene of few layer.
The present invention also aims to provide a kind of few layer graphene and the device for the preparation of above-mentioned few layer graphene.
In order to achieve the above object, first the present invention provides a kind of preparation method of few layer graphene, and it comprises the following steps:
Step 1: Graphite Powder 99 is carried out to purification process;
Step 2: the Graphite Powder 99 after purifying is directly added in autoclave or after being dispersed in solvent and added in autoclave, heat, reach after 35-60 ℃ until the temperature in autoclave, supercutical fluid is pumped in autoclave;
Step 3: by pumping into supercutical fluid, autoclave internal pressure is raised to after 75atm-300atm, stirs 30min-20h, then by pressure at the preferred 10s of 5s-20s() in reduce to 1atm, concrete step-down mode can be carried out according to ordinary method;
Step 4: sample in autoclave, obtain described few layer graphene.
According to specific embodiment of the invention scheme, preferably, the supercutical fluid adopting is CO
2supercutical fluid.
According to specific embodiment of the invention scheme, preferably, the Graphite Powder 99 adopting comprises crystalline graphite powder and/or expanded graphite powder etc.
According to specific embodiment of the invention scheme, preferably, the solvent adopting comprises sodium lauryl sulphate and/or Sodium dodecylbenzene sulfonate etc.
According to specific embodiment of the invention scheme, preferably, the stirring velocity in described step 3 is 1000-10000r/min.
In the preparation method of above-mentioned few layer graphene, the gas that described supercutical fluid can be obtained after step-down is put into gas tank and is reclaimed storage use to be recycled.
According to specific embodiment of the invention scheme, preferably, the purification process of concrete Graphite Powder 99 comprises the following steps:
Step 1: by Graphite Powder 99 ultrasonic cleaning, remove impurity;
Step 2: remove dephasign material and impurity element through chemical treatment or alternate manner.
The present invention also provides a kind of few layer graphene, and it is prepared by above-mentioned preparation method.
According to specific embodiment of the invention scheme, the ratio of the few layer graphene of the number of plies of preparing by aforesaid method below 10 layers is more than 60%, and preferably, the number of plies of described few layer graphene is 1-10 layer.
The present invention also provides a kind of device for the preparation of above-mentioned few layer graphene, and it can be for the preparation method of above-mentioned few layer graphene.This device comprises agitator motor, heating jacket, autoclave, gas-circulating system, agitator arm, stirring-head, wherein,
Described agitator arm is vertically positioned at the centre at autoclave top, and described agitator arm connects agitator motor in one end of autoclave outside, and the other end that extends to described autoclave base connects stirring-head;
Be provided with injection port and gas inlet at the top of described autoclave; The be placed in both sides of agitator motor of described injection port and described gas inlet;
Described heating jacket is wrapped in the outside of described autoclave;
The bottom of described autoclave is provided with outlet;
Described gas-circulating system comprises gas tank, the first valve, the second valve, under meter, condensing equipment and the 3rd valve, the pipeline of drawing from gas inlet is communicated with the first valve, gas tank, the second valve, under meter, condensing equipment and the 3rd valve successively, the pipeline that end of line is drawn with gas inlet is communicated with, and forms gas-circulating system; Wherein, the first valve, the second valve and the 3rd valve are opened and closure for pilot piping, the amount of under meter for measuring gas, gas tank is for storing the gas of needed gas and recovery, condensing equipment carries out condensation to gas, work with ambient pressure pump one, make gas become supercritical state, can adopt any equipment that can realize this function;
Described gas-circulating system is communicated with described gas inlet.
While adopting said apparatus to prepare few layer graphene, first, the first valve, the second valve, the 3rd valve are in closure state, Graphite Powder 99 after purifying is directly joined in autoclave or after being dispersed in solvent and added in autoclave, heat by heating jacket, reach after 35-60 ℃ until the temperature in autoclave, open the second valve, the 3rd valve, gas in gas tank is by condensing equipment condensation, working with ambient pressure pump one, to make gas reforming be supercutical fluid, and supercutical fluid is pumped in autoclave; Then, by pumping into supercutical fluid, autoclave internal pressure is raised to after 75atm-300atm, close the second valve and the 3rd valve, opening agitator motor stirs, the shearing force of utilizing swiftly flowing supercutical fluid to produce is peeled away graphite, stir after 30min-20h, pressure is reduced in 5s-20s to 1atm, close again the first valve after opening the first valve gas recovery; Finally, in autoclave, sample, make few layer graphene.
The preparation method of few layer graphene provided by the present invention is the method for the few layer graphene of efficient preparation, can prepare in a large number high-quality few layer graphene, and the Graphene number of plies prepared by the method is few.
Preparation method's environmental protection of few layer graphene provided by the present invention, production cost is low, can recycle CO
2, reduce CO
2discharge and cost.Meanwhile, also have reaction time short, technique is simple, the advantage such as the lamella integrity of the few layer graphene preparing is good.
Accompanying drawing explanation
Fig. 1 is the preparation method's of few layer graphene provided by the present invention schema;
Fig. 2 is the structural representation of the few layer graphene device of preparation provided by the present invention;
Fig. 3 is transmission electron microscope (TEM) figure of the few layer graphene prepared of embodiment 1;
Fig. 4 is another transmission electron microscope (TEM) figure of the few layer graphene prepared of embodiment 1;
Fig. 5 is transmission electron microscope (TEM) figure of the few layer graphene prepared of embodiment 2;
Fig. 6 is another transmission electron microscope (TEM) figure of the few layer graphene prepared of embodiment 2.
Main drawing reference numeral:
1 autoclave 2 heating jacket 3 agitator motor 4 agitator arm 5 stirring-head 6 injection port 7 gas inlet 8 outlet 9 first valve 10 second valve 11 under meter 12 gas tank 13 condensing equipments 14 the 3rd valves
Embodiment
Understand for technical characterictic of the present invention, object and beneficial effect being had more clearly, referring now to Figure of description, 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.
Embodiment 1
The present embodiment provides a kind of device for the preparation of few layer graphene, and its structure as shown in Figure 2.This device comprises: agitator motor 3, heating jacket 2, autoclave 1, gas-circulating system, agitator arm 4, stirring-head 5, wherein,
Agitator arm 4 is vertically positioned at the centre at autoclave 1 top, and agitator arm 4 connects agitator motor 3 in one end of autoclave 1 outside, and the other end that extends to autoclave 1 bottom connects stirring-head 5;
Be provided with injection port 6 and gas inlet 7 at the top of autoclave 1; The be placed in both sides of agitator motor 3 of injection port 6 and gas inlet 7;
Heating jacket 2 is wrapped in the outside of autoclave 1;
The bottom of autoclave 1 is provided with outlet 8;
Gas-circulating system comprises gas tank 12, the first valve 9, the second valve 10, under meter 11, condensing equipment 13 and the 3rd valve 14, the pipeline of drawing from gas inlet 7 is communicated with the first valve 9, gas tank 12, the second valve 10, under meter 11, condensing equipment 13 and the 3rd valve 14 successively, end of line is communicated with the pipeline of drawing from gas inlet 7, forms gas-circulating system; Wherein, the first valve 9 and the second valve 10 opening and closure for pilot piping, under meter 11 is for measuring the amount of gas, gas tank 12 is for storing the gas of needed gas and recovery, condensing equipment 13 carries out condensation to gas, work with ambient pressure pump one, make gas become supercritical state, can adopt any equipment that can realize this function; Gas-circulating system is communicated with gas inlet 7.
Utilize said apparatus to prepare few layer graphene, as shown in Figure 1, this preparation process specifically can comprise the following steps preparation flow figure:
Step 1, prepare Graphite Powder 99: by 10g crystalline graphite powder ultrasonic cleaning (wash 1 time, ethanol is washed 2 times) to remove dephasign material and impurity element;
Step 2, supercritical CO
2intercalation: the first valve 9, the second valve 10, the 3rd valve 14 are in closure state, crystalline graphite powder after purifying is directly joined in autoclave 1 and heated, reach after 35 ℃ until the temperature in autoclave 1, open the second valve 10, the 3rd valve 14, by the CO in gas tank 12
2gas, by condensing equipment 13 condensations, works CO with one of ambient pressure pump
2gas reforming is CO
2supercutical fluid, by CO
2supercutical fluid pumps in autoclave 1, CO
2the consumption of supercutical fluid measures by under meter 11;
Step 3, supercritical CO
2shear: by pumping into CO
2supercutical fluid is raised to after 300atm autoclave 1 internal pressure, closes the second valve 10 and the 3rd valve 14, opens agitator motor 3 and stirs, and rotating speed is 10000r/min, utilizes swiftly flowing CO
2the shearing force that supercutical fluid produces is peeled away graphite, stirs after 30min and pressure is reduced in 10s to 1atm, closes the first valve 9 after opening the first valve 9 gas recoveries again;
Step 4, obtain Graphene: from the interior sampling of autoclave 1, obtain described few layer graphene.
The few layer graphene making is taken pictures by transmission electron microscope (TEM), as shown in Figure 3 and Figure 4.Can be clearly seen that the number of plies of few layer graphene prepared by the present embodiment from Fig. 3 and Fig. 4, the defect that can observe Graphene less simultaneously, by its number of plies is added up, the ratio of the number of plies of the Graphene that discovery embodiment 1 makes below 10 layers is about 60%.
Embodiment 2
The present embodiment provides a kind of preparation method of few layer graphene, and it is to utilize the device described in embodiment 1 to prepare, and the method specifically comprises the following steps:
Step 1, prepare Graphite Powder 99: by 1g expanded graphite powder ultrasonic cleaning (wash 1 time, ethanol is washed 2 times) to remove dephasign material and impurity element;
Step 2, supercritical CO
2intercalation: the first valve 9, the second valve 10, the 3rd valve 14 are in closure state, after expanded graphite powder after purifying is dispersed in the sodium lauryl sulphate that 200ml concentration is 1wt% (SDS), join in autoclave 1 and heat, reach after 60 ℃ until the temperature in autoclave 1, open the second valve 10, the 3rd valve 14, by the CO in gas tank 12
2gas, by condensing equipment 13 condensations, works CO with one of ambient pressure pump
2gas reforming is CO
2supercutical fluid, by CO
2supercutical fluid pumps in autoclave 1, CO
2the consumption of supercutical fluid measures by under meter 11;
Step 3, supercritical CO
2shear: by pumping into CO
2supercutical fluid is raised to after 75atm autoclave 1 internal pressure, closes the second valve 10 and the 3rd valve 14, opens agitator motor 3 and stirs, and rotating speed is 1000r/min, utilizes swiftly flowing CO
2the shearing force that supercutical fluid produces is peeled away graphite, stirs 20h, then pressure is reduced in 10s to 1atm, closes the first valve 9 after opening the first valve 9 gas recoveries again;
Step 4, obtain Graphene: from the interior sampling of autoclave 1, obtain described few layer graphene.
To make few for layer graphene transmission electron microscope (TEM) take pictures, as shown in Figure 5 and Figure 6.Can be clearly seen that the number of plies of few layer graphene prepared by the present embodiment from Fig. 5 and Fig. 6, the defect that can observe Graphene less simultaneously, by its number of plies is added up, the ratio of the number of plies of the Graphene that discovery embodiment 2 makes below 10 layers is about 80%.
Claims (9)
1. a preparation method for few layer graphene, it comprises the following steps:
Step 1: Graphite Powder 99 is carried out to purification process;
Step 2: the Graphite Powder 99 after purifying is directly added in autoclave or after being dispersed in solvent and added in autoclave, heat, reach after 35-60 ℃ until the temperature in autoclave, supercutical fluid is pumped in autoclave;
Step 3: by pumping into supercutical fluid, autoclave internal pressure is raised to after 75atm-300atm, stirs 30min-20h, then pressure is reduced in 5s-20s to 1atm;
Step 4: sample in autoclave, obtain described few layer graphene.
2. preparation method according to claim 1, wherein, described supercutical fluid is CO
2supercutical fluid.
3. preparation method according to claim 1, wherein, described Graphite Powder 99 comprises crystalline graphite powder and/or expanded graphite powder.
4. preparation method according to claim 1, wherein, described solvent comprises sodium lauryl sulphate and/or Sodium dodecylbenzene sulfonate.
5. preparation method according to claim 1, wherein, the stirring velocity in described step 3 is 1000-10000r/min.
6. preparation method according to claim 1, wherein, puts into gas tank by the gas obtaining after described supercutical fluid step-down and stores use to be recycled.
7. preparation method according to claim 1, wherein, the purification process of described Graphite Powder 99 comprises the following steps:
Step 1: by Graphite Powder 99 ultrasonic cleaning, remove impurity;
Step 2: remove dephasign material and impurity element through chemical treatment or alternate manner.
8. a few layer graphene, it is to be made by the preparation method described in claim 1-7 any one.
9. for the preparation of a device for few layer graphene claimed in claim 8, it comprises, agitator motor, heating jacket, autoclave, gas-circulating system, agitator arm, stirring-head, wherein,
Described agitator arm is vertically positioned at the centre at autoclave top, and described agitator arm connects agitator motor in one end of autoclave outside, and the other end that extends to described autoclave base connects stirring-head;
Be provided with injection port and gas inlet at the top of described autoclave; The be placed in both sides of agitator motor of described injection port and described gas inlet;
Described heating jacket is wrapped in the outside of described autoclave;
The bottom of described autoclave is provided with outlet;
Described gas-circulating system comprises gas tank, the first valve, the second valve, under meter, condensing equipment and the 3rd valve, the pipeline of drawing from gas inlet is communicated with the first valve, gas tank, the second valve, under meter, condensing equipment and the 3rd valve successively, the pipeline that end of line is drawn with gas inlet is communicated with, and forms gas-circulating system;
Described gas-circulating system is communicated with described gas inlet.
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| CN201310739904.1A CN103771401B (en) | 2013-12-26 | 2013-12-26 | A kind of preparation method of few layer graphene and device |
| PCT/CN2014/075917 WO2015096317A1 (en) | 2013-12-26 | 2014-04-22 | Method for preparing single-layered graphene |
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| CN104229787A (en) * | 2014-09-18 | 2014-12-24 | 上海交通大学 | Method for increasing yield of graphene prepared by supercritical fluid through pretreatment of natural graphite |
| CN105084347A (en) * | 2014-05-08 | 2015-11-25 | 北京航空航天大学 | Graphene preparation method |
| CN106044765A (en) * | 2016-08-17 | 2016-10-26 | 新奥科技发展有限公司 | Apparatus and method of supercritically preparing graphene |
| CN106044764A (en) * | 2016-08-17 | 2016-10-26 | 新奥科技发展有限公司 | Apparatus and method of supercritically preparing graphene |
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| CN114426269A (en) * | 2020-10-13 | 2022-05-03 | 中国石油化工股份有限公司 | Graphene and preparation method thereof |
| CN114426269B (en) * | 2020-10-13 | 2023-10-10 | 中国石油化工股份有限公司 | Graphene and preparation method thereof |
| CN113750910A (en) * | 2021-08-27 | 2021-12-07 | 南京公诚节能新材料研究院有限公司 | Alkali metal carbon preparation facilities in supercritical fluid reaction system |
| CN114672156A (en) * | 2022-03-04 | 2022-06-28 | 上海交通大学 | Preparation method of graphene/PA 6 composite material |
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| CN103771401B (en) | 2015-09-09 |
| WO2015096317A1 (en) | 2015-07-02 |
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