CN102730677B - Equipment and method for preparing graphene and prepared graphene - Google Patents
Equipment and method for preparing graphene and prepared graphene Download PDFInfo
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- CN102730677B CN102730677B CN201210254193.4A CN201210254193A CN102730677B CN 102730677 B CN102730677 B CN 102730677B CN 201210254193 A CN201210254193 A CN 201210254193A CN 102730677 B CN102730677 B CN 102730677B
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Abstract
The invention relates to equipment for preparing graphene, comprising a reaction room (1) and a sample collecting room (5) arranged under the reaction room, wherein the walls of the reaction room (1) are provided with a first gas inlet, a second gas inlet and a first material inlet except a bottom wall, and the bottom wall of the reaction room (1) can be opened. The method for preparing the graphene comprises the following steps of: (a) putting graphite oxide into a reaction room (3) from a material inlet (8), and charging inert gas into the reaction room through a gas inlet (7), so that the inert gas is filled with the whole room; (b) charging hot inert gas into the reaction room (3) from another gas inlet (12), so that the graphite oxide is reacted; and (c) blowing the inert gas to the bottom wall (4) of the reaction room from the gas inlet (7), so that the bottom wall of the reaction room is opened, and the generated graphene is charged into the sample collecting room (5) under the blowing of the inert gas. Finally, the invention further relates to the graphene prepared by the equipment and the method.
Description
Technical field
The Graphene that the present invention relates to a kind of equipment of continuous production Graphene, prepares the method for Graphene and make thus by described equipment.
background technology:graphene has excellent physics and chemistry performance, is expected in fields such as high-performance nano electron device, matrix material, field emmision material, gas sensors, and particularly stored energy field (ultracapacitor, battery etc.), obtain widespread use.
The preparation method of Graphene has a lot, and wherein oxidation reduction process can be prepared a tonne grapheme material, reproducible, and the Graphene of preparing is quality controllable, is considered to one of important method that can realize continuous production Graphene.The preparation principle of oxidation reduction process is generally: with strong oxidizer (as SODIUMNITRATE, the vitriol oil, potassium permanganate, hydrogen peroxide etc.) graphite oxide starting material, form graphite oxide; Then Van der Waals force graphite oxide being overcome between graphite flake layer by reduction method deoxidation makes original lamella graphite separately, forms grapheme material.Described reduction method has a lot, and wherein thermal shocking reduction method completes dispersion and reduction graphite oxide one step, has improved production efficiency and has had the possibility of accomplishing scale production.The process that thermal shocking reduction graphite oxide is prepared Graphene is generally: after the graphite oxide preparing is ground, be placed in rapidly the high-temperature zone of protection of inert gas and keep for some time; graphite oxide deoxidation is reduced; become black by brown color, prepare grapheme material.But the method mainly relies on manual operation, operating process has unstable inevitably; In addition, due to main dependence manual operation, cannot realize continuous production, limit thus the large-scale production of Graphene.
summary of the invention:for the problems referred to above, the invention provides a kind of equipment of preparing Graphene, it comprises:
(1) reaction chamber, has the first gas inlet, the second gas inlet and a material inlet, and described three entrances are positioned at other any walls except diapire, and its diapire is openable, and
(2) one are positioned at the sample collection room of reaction chamber below.
In addition, the invention provides a kind of method of preparing Graphene, it comprises the following steps:
(a) graphite oxide is dropped into reaction chamber from the material inlet of reaction chamber, described reaction chamber has the first gas inlet, the second gas inlet and a described material inlet, described three entrances are positioned at other any walls except diapire, and its diapire is to open; And in reaction chamber, pass into rare gas element by the first gas inlet of reaction chamber;
(b) close the first gas inlet, in reaction chamber, pass into hot inert gas by the second gas inlet, make graphite oxide reaction, and
(c) the diapire blown inert gas facing to reaction chamber by the first gas inlet, opens this diapire, and the Graphene of generation enters sample collection room under the blowing of rare gas element.
The present invention also provides a kind of Graphene, and its specific surface area can reach 300-500m
2/ g, preferred 350-480m
2/ g; Carbon-to-oxygen ratio (atomic ratio) can reach 7:1 to 10:1, preferably 8:1 to 10:1.
Equipment of the present invention and method can continuous production Graphenes.In addition, equipment of the present invention is the basis of Graphene of accomplishing scale production, and is conducive to scale operation Graphene.The Graphene being obtained by the present invention has good quality, for example, have high specific surface area and high carbon-to-oxygen ratio.
brief description of the drawings:
Fig. 1 is a schematic diagram of present device.
embodiment:in the present invention, term " top ", " top ", " bottom ", " level ", " inclination " etc. are all for level ground.
" rare gas element " refers to the material of not participating in Graphene reaction under reaction conditions directly, for example, and one or more rare gas.
If no special instructions, " rare gas element " is in room temperature or approach room temperature (room temperature ± 5 DEG C).
" hot inert gas " refers to that temperature is the rare gas element of 500-2000 DEG C.
The invention provides a kind of equipment of preparing Graphene, it comprises:
(1) reaction chamber, has the first gas inlet, the second gas inlet and a material inlet, and described three entrances are positioned at other any walls except diapire, and its diapire is openable, and
(2) one are positioned at the sample collection room of reaction chamber below.
Fig. 1 is a schematic diagram of present device, below in connection with Fig. 1, present device is described in detail.But should be understood that described accompanying drawing, only for exemplary, should not be construed as and limits by any way the scope of the invention.
As shown in Figure 1, present device comprises a reaction chamber 3.Its shape is not particularly limited, and can be spherical, cube shaped as (preferably cube shaped) such as the octahedral bodily form, the square bodily forms; Its wall thickness is generally 6-120mm, but is not limited to this, is preferably 50-100mm.
On the wall (except diapire 4) of reaction chamber 3, there is material inlet 8, be preferably placed on the roof of reaction chamber 3, can directly be connected with reaction chamber, be preferably connected by one section of passage, as shown in Figure 1.
Preferably this material inlet is connected with an automatic feeding system.This automatic feeding system can comprise that transport unit 11 and reaction mass 10(are graphite oxide in the present invention).
Described transport unit 11 can be travelling belt, head tank etc., but is not limited to this.This transport unit can be level or tilt, be preferably level.In the situation that it is inclination, preferably inclination angle is below 60 degree.
On the wall (except diapire 4) of reaction chamber 3, also have the first gas inlet 7 and the second gas inlet 12, they join with a compressed air source unit separately, control gas flow rate by the valve of controlling compressed air source unit.
The first gas inlet 7 is preferably placed on the sidewall except diapire 4, for blowing room temperature to reaction chamber or approaching the rare gas element of room temperature; The second gas inlet 12 is preferably placed on diapire top the close sidewall of diapire (for 7), for blowing hot inert gas to reaction chamber.
The diapire of reaction chamber 3 (thickness is 6-120mm, preferably 50-100mm) is openable: can pneumaticly open that (being pneumatic diapire), electronic opening (being electronic diapire) or hydraulic pressure are moving opens (being the moving diapire of hydraulic pressure); Preferably can pneumaticly open.
In a specific embodiments, described diapire is pneumatic diapire, this diapire is divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with pressure pneumatic sensor (it being had no special requirements, as long as can implement the present invention), in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
In a specific embodiments, described diapire is electronic diapire, this diapire is divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with pressure electrodynamictransducer (it being had no special requirements, as long as can implement the present invention), when referred to the seam crossing of two diapires facing to this diapire leading portion by the first gas inlet 7) when blown inert gas, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
In a specific embodiments, described diapire is the moving diapire of hydraulic pressure, this diapire is divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with hydrauliccapsule (it being had no special requirements, as long as can implement the present invention), in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
Preferably, the compressed air source unit that described the second gas inlet 12 connects is connected with a well heater 2, for heating the rare gas element being entered by gas inlet 1, then enters in reaction chamber 3 via the second gas inlet 12 through the gas of heating, makes graphite oxide reaction.It can be maybe electrically heated, magnetic heating, Electromagnetic Heating, steam heating etc. that wherein said well heater can heat by Cowper stove.
Should be parallel or away from reaction chamber diapire, in order to avoid diapire is opened in the time having reacted, preferred parallel is in diapire to the direction of the rare gas element being blown in reaction chamber by the second gas inlet 12.
The below of diapire is a sample collection room 5.The Graphene generating enters this collecting chamber by the diapire of opening, and cooling with inert gas flow in the process of entering.
Preferably, sample collection room 5 is connected with a final sampling hut 6 with a sample channel 13 successively.The Graphene generating enters sample channel 13 under air-flow and action of gravity, and through further cooling in the process of this passage, the type of cooling is naturally cooling or cooling by heat-eliminating medium.Be connected with a final sampling hut 6 at the end (lower end) of sample channel 13, sample is finally cooled to the temperature that can take out therein.
The waste gas generating in reaction process is preferably discharged by an outlet port.Discharge and realize by the inert gas flow being passed into by least one first gas inlet 7.Described outlet port can be separately located in reaction chamber top relief outlet 9(as shown in fig. 1).In addition,, the in the situation that of more than one the first gas inlet 7, described outlet port also can be first gas inlet 7.
Preferably, outlet port is connected with a waste gas recovering device (preferably carbon trap setting), to reclaim waste gas and to be used.
Present device concrete structure is determined by design feature itself, is not limited to a kind of ad hoc structure.
Each parts of present device are preferably by identical or different high temperature alloy, for example high temperature steel or blast furnace hood steel form, and the temperature of fusion that wherein forms the material of reaction chamber 3 should be higher than the top temperature in reaction process (temperature of reaction in the present invention be 500-2000 DEG C).
In addition, the invention provides a kind of method of preparing Graphene, it comprises the following steps:
(a) graphite oxide is dropped into reaction chamber from the material inlet of reaction chamber, described reaction chamber has the first gas inlet, the second gas inlet and a described material inlet, described three entrances are positioned at other any walls except diapire, and its diapire is to open; And in reaction chamber, pass into rare gas element by the first gas inlet of reaction chamber;
(b) close the first gas inlet, in reaction chamber, pass into hot inert gas by the second gas inlet, make graphite oxide reaction, and
(c) the diapire blown inert gas facing to reaction chamber by the first gas inlet, opens this diapire, and the Graphene of generation enters sample collection room under the blowing of rare gas element.
Below in conjunction with Fig. 1, the inventive method specific embodiments is described.
Step (a): graphite oxide is dropped in the reaction chamber of present device via material inlet 8 by a transport unit 11, and pass into rare gas element by the first gas inlet 7 in reaction chamber 3, make to be full of rare gas element in whole reaction chamber.
Graphite oxide can utilize any method known in the art, preferably conventional H ummers method (Ha Mosi method) or improved Hummers method (improved Ha Mosi method), and graphite oxide starting material and making, or be commercially available.The purity of graphite raw material used is > 99%, 45 microns of granularity <, 25 microns of preferred size <.Graphite oxide should have high degree of oxidation, to prepare high-quality Graphene product, described degree of oxidation is C/O(atomic ratio) < 5:1, be preferably C/O=2:1.
The process that conventional H ummers method is prepared graphite oxide is: by powdered graphite and strong oxidizer, such as SODIUMNITRATE, the vitriol oil (for example 98 quality %), potassium permanganate, hydrogen peroxide etc. mix stirring, react some hours, after cleaning, dewater, drying, obtain brown color graphite oxide powder.
An operational instances of above-mentioned conventional H ummers method is: for example, by powdered graphite, the vitriol oil (98 % by weight concentration) and SODIUMNITRATE, (consumption is with three kinds of compound forms, by pure substance part by weight, graphite: sulfuric acid: SODIUMNITRATE=5-10:150-450:2-8) mix and blend, mixing solutions is remained in ice bath simultaneously; (consumption is by pure substance part by weight slowly to add potassium permanganate, graphite: potassium permanganate=5-10:10-35), stir, slowly add deionized water, now solution temperature rises sharply (temperature is 80-100 DEG C), keeps this temperature, and (consumption is by pure substance part by weight slowly to add deionized water and hydrogen peroxide, graphite: water: hydrogen peroxide=5-10:200-500:6-16), solution colour becomes golden yellow.Solution is carried out to centrifugal treating, then clean repeated washing process if desired with deionized water, hydrochloric acid and dehydrated alcohol.The centrifugal brown color solid obtaining is dried, finally obtain graphite oxide powder.
An operational instances of improved Hummers method is:
The first step, according to conventional H ummers method, adds graphite in the vitriol oil, strong phosphoric acid, Potcrate (consumption is by pure substance part by weight, graphite: sulfuric acid: phosphoric acid: Potcrate=(5-10): (100-400): (20-33): (10-35)); Or after graphite is for example immersed in, in the vitriol oil (98 % by weight concentration), add potassium permanganate (consumption is by pure substance part by weight, graphite: sulfuric acid: potassium permanganate=(5-10): (150-450): (10-35)),
Second step, at room temperature stirs, and adds water and hydrogen peroxide (consumption is by pure substance part by weight, graphite: water: hydrogen peroxide=(5-10): (200-500): (6-16)); Or at room temperature stir, heating (temperature is 80-100 DEG C), adds water and hydrogen peroxide (consumption is by pure substance part by weight, graphite: water: hydrogen peroxide=(5-10): (200-500): (6-16)).
In addition, also can prepare graphite oxide by other improved Hummers methods.
Described transport unit can be travelling belt or head tank etc., but is not limited to this.The transfer rate of transport unit is 0.5-3 m/s, preferably 1-2 m/s.
The preferred argon gas of described rare gas element.The time that passes into rare gas element is generally 10-30 minute; Flow velocity is 1-5 L/min/L chamber volume.In this step, in reaction chamber, the pressure of rare gas element is generally 0.5-2 normal atmosphere, is preferably 1-1.5 normal atmosphere.
Step (b): hot inert gas is passed in reaction chamber 3 and the reaction times of lasting 5-60s by the second gas inlet 12, makes graphite oxide reaction.
The preferred argon gas of rare gas element described herein, is heated to 500-2000 DEG C via well heater 2, preferably 800-1800 DEG C, further preferred 1000-1800 DEG C; Then pass in reaction chamber 3 through the second gas inlet 12, make graphite oxide reaction.Described well heater can be maybe electrically heated, magnetic heating, Electromagnetic Heating, steam heating etc. by the heating of internal combustion type hot blast reaction chamber, preferably electrically heated.The flow velocity that hot inert gas passes in reaction chamber 3 is 0.1-10 L/min/L chamber volume, preferably 1-5 L/min/L chamber volume.In addition, the direction of the rare gas element being passed into by the second gas inlet 12 should not face toward diapire, and should be parallel or away from diapire, in order to avoid diapire is opened in the time having reacted, preferred parallel is in diapire.
Graphite oxide reacts on the diapire 4 that is positioned at reaction chamber 3, and the reaction times, depending on the amount of the graphite oxide that adds, is generally 5-60s, preferably 10-40 s.Reaction pressure is generally 0.5-2 normal atmosphere, is preferably 1-1.5 normal atmosphere.
Step (c): diapire 4 blown inert gas by the first gas inlet 7 facing to reaction chamber 3, this diapire is opened, the Graphene of generation enters sample collection room 5 under the blowing of rare gas element.
Described diapire is preferably pneumatic diapire, be divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with pressure pneumatic sensor, in the time being blown into rare gas element by the first gas inlet 7 facing to this diapire leading portion (referring to the seam crossing of two diapires), produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.The temperature of the rare gas element being blown at least should, lower than the temperature in reaction chamber after reaction, be preferably room temperature or the gas lower than room temperature.Gas flow rate is so that diapire 4 braking is opened is limited, and its flow velocity is 0.1-10 L/min/L chamber volume conventionally, preferably 1-5 L/min/L chamber volume.
For electronic diapire, opening procedure is as follows: diapire is divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with pressure electrodynamictransducer, in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
For the moving diapire of hydraulic pressure, opening procedure is as follows: diapire is divided into two, be connected on the sidewall of reaction chamber 3 by two rotatable shafts respectively, below every diapire, be equipped with hydrauliccapsule, in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
The temperature of rare gas element at least should, lower than the temperature in reaction chamber now, be preferably room temperature or the gas lower than room temperature.
The Graphene generating after reaction enters in sample collection room 5 with inert gas flow via the diapire 4 of opening, and cooling with inert gas flow in the process of entering.
Preferably, the Graphene in sample collection room 5 enters in final sampling hut 6 by a coupled sample channel 13.Object is to make Graphene further cooling in the process process of sample channel 13, and the type of cooling is naturally cooling or cooling by heat-eliminating medium.
In addition,, under the blowing of rare gas element, the waste gas producing in reaction is discharged via an outlet port.Described outlet port can be separately located in reaction chamber top relief outlet 9(as shown in Figure 1).In addition,, the in the situation that of more than one the first gas inlet 7, described outlet port also can be first gas inlet 7.Preferably, outlet port is connected with a waste gas recovering device, to reclaim waste gas and to be used.Described waste gas recovering device is preferably a carbon trap setting.
Implement above-mentioned steps (a) to (c) by circulation, can realize the continuous production of Graphene.
Can continuous production Graphene by present device and method, be conducive to the large-scale production of Graphene.In addition, obviously, automated operation process is more stable than manual operation.Its specific surface area of Graphene being made by described equipment and method can reach 300-500m
2/ g, preferred 350-480m
2/ g; Carbon-to-oxygen ratio (atomic ratio) can reach 7:1 to 10:1, preferably 8:1 to 10:1.
Embodiment
Below with reference to specific embodiment and comparative example, the present invention is described in more detail, but the invention is not restricted to these embodiment.
In embodiment, graphite oxide used all utilizes following conventional H ummers method to make:
By powdered graphite (5 g, granularity is 44 microns), the vitriol oil (concentration is 98 quality %, 115 ml) and SODIUMNITRATE, (2.5 g) pack in the container of 1 L, this container are remained in the ice bath of 0 DEG C simultaneously, mix and stir; Then (15 g), continues to stir 30 minutes in the situation that stirring, slowly to add potassium permanganate; Slowly add afterwards deionized water (230 ml), now solution temperature rises sharply 98 DEG C.After 15 minutes, slowly add deionized water (230 ml) and hydrogen peroxide (5 ml), solution colour becomes golden yellow.Solution is carried out in whizzer (3200 revs/min) to the centrifugal treating of 5 minutes, the deionized water for product (500ml) of centrifugation, hydrochloric acid (concentration is 20 volume %, 500ml) and dehydrated alcohol (500ml) are cleaned successively.Repeated washing 3 times, obtains brown color solid graphite oxide compound, is dried (40 DEG C, 12 hours), grinds, stand-by.
embodiment1, adopt Fig. 1 shown device (two the first gas inletes 7, second gas inlet 12, whole equipment is made up of high temperature steel (GB4238-2007), wall thickness is 50mm) carry out: gained graphite oxide is dropped in reaction chamber via material inlet with the flow velocity of 1m/s by travelling belt, and in reaction chamber 3, pass into room temperature argon gas 10 minute with the flow velocity of 1L/min/L chamber volume by the first gas inlet 7, make to be full of argon gas in whole reaction chamber; In well heater 2, input argon gas by gas inlet 1 afterwards, heater 2, by flowing through, its argon gas is heated to 1000 DEG C; Then make be parallel to diapire and pass in reaction chamber 3 via the second gas inlet 12 through the argon gas of heating, and continue to pass into 30 seconds, make graphite oxide fully reaction in reaction chamber; Open afterwards two the first gas inletes 7, flow velocity with 10L/min/L chamber volume is blown into room temperature argon gas facing to diapire direction in reaction chamber: diapire is divided into two, below every diapire, be equipped with pressure pneumatic sensor (for example KAL08-U01 KAL08-U01, purchased from Dongguan Xing Ke industrial automation equipment company limited), in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.The Graphene generating enters in the sample collection room 5 below diapire under air-flow and action of gravity, then enters final sampling hut 6 via a coupled sample channel 13.Open in the process of diapire being blown into argon gas, the waste gas in reaction chamber is discharged in a carbon trap setting by outlet port 9.
embodiment2, to be undertaken by the process identical with embodiment 1, difference is, the argon gas gas of the well heater 2 of flowing through is heated to 500 DEG C, and it is continued to pass into 60 seconds in reaction chamber 3.
embodiment3
,undertaken by the process identical with embodiment 1, difference is, the argon gas gas of the well heater 2 of flowing through is heated to 2000 DEG C, and it is continued to pass into 5 seconds in reaction chamber 3.
embodiment4
,undertaken by the process identical with embodiment 1, difference is, diapire is electronic diapire, open by electric device: diapire is divided into two, below every diapire, be equipped with pressure electrodynamictransducer (for example KAL08-U01 KAL08-U01, purchased from Dongguan Xing Ke industrial automation equipment company limited), in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
embodiment5, undertaken by the process identical with embodiment 1, difference is, diapire is the moving diapire of hydraulic pressure, opens: diapire is divided into two by hydraulic efficiency plant, is equipped with hydrauliccapsule (for example KAL08-U01 KAL08-U01 below every diapire, purchased from Dongguan Xing Ke industrial automation equipment company limited), in the time facing toward this diapire leading portion (referring to the seam crossing of two diapires) blown inert gas by the first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
Sample analysis to embodiment 1-5 is as follows: from final sampling hut, respectively get 1 g sample, it,, in 150 DEG C of vacuum-dryings 12 hours, is then analyzed: adopt its specific surface area of Quantachrome AUTOSORB-1 test system and test; Adopt PHI 5000 Versa Probe. x-ray photoelectron energy spectrum testing systems and MultiPak V 9.0 digital simulation softwares to measure its carbon/Sauerstoffatom ratio.The results are shown in following table:
| Numbering | Specific surface area (m 2/g） | C/O ratio |
| 500 | 10:1 | |
| Embodiment 2 | 507 | 9.8:1 |
| Embodiment 3 | 495 | 9.5:1 |
| Embodiment 4 | 498 | 9.9:1 |
| Embodiment 5 | 489 | 10:1 |
Although describe the present invention with reference to particular, but what those skilled in the art will recognize that is, in the situation that not departing from purport of the present invention and scope, can described embodiment be changed or be improved, the scope of the invention limits by appended claims.
Claims (5)
1. a method of preparing Graphene, it comprises the following steps:
(a) graphite oxide is dropped into reaction chamber (3) from the material inlet (8) of reaction chamber (3), described reaction chamber has the first gas inlet (7), the second gas inlet (12) and a described material inlet (8), described three entrances are positioned at other any walls except diapire (4), and its diapire (4) is to open; And in reaction chamber, pass into rare gas element by first gas inlet (7) of reaction chamber (3);
(b) close the first gas inlet (7), in reaction chamber (3), pass into hot inert gas by the second gas inlet (12), make graphite oxide reaction; It is parallel with reaction chamber diapire or away from diapire that guarantee passes into the direction of described hot inert gas, and the temperature of described hot inert gas is that 500-2000 DEG C, pressure are 0.5-2 normal atmosphere, the time of passing into be that 5-60s, flow velocity are 0.1-10 L/min/L chamber volume;
(c) the diapire blown inert gas facing to reaction chamber (3) by the first gas inlet (7), opens this diapire, and the Graphene of generation enters sample collection room (5) under the blowing of rare gas element.
2. the process of claim 1 wherein that graphite oxide described in step (a) prepared by conventional Ha Mosi method or improved Ha Mosi method.
3. the process of claim 1 wherein that described in step (a) to (c), rare gas element is one or more rare gas.
4. the process of claim 1 wherein that the pressure of hot inert gas described in step (b) is 1-1.5 normal atmosphere, the time of passing into is 10-40s, and flow velocity is 1-5 L/min/L chamber volume.
5. the method for claim 1, wherein described in step (c), diapire is pneumatic diapire, this diapire is divided into two, be connected on the sidewall of reaction chamber (3) by two rotatable shafts respectively, below every diapire, be equipped with pressure pneumatic sensor, in the time facing toward this diapire leading portion blown inert gas by the first gas inlet (7), produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs; Or be electronic diapire, this diapire is divided into two, be connected on the sidewall of reaction chamber (3) by two rotatable shafts respectively, below every diapire, be equipped with pressure electrodynamictransducer, in the time facing toward this diapire leading portion blown inert gas by the first gas inlet (7), produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs; Or be the moving diapire of hydraulic pressure, this diapire is divided into two, be connected on the sidewall of reaction chamber (3) by two rotatable shafts respectively, below every diapire, be equipped with pressure electrodynamictransducer, in the time facing toward this diapire leading portion blown inert gas by the first gas inlet (7), produce pressure, diapire is outwarded winding to both sides from centre around two axle along continuous straight runs.
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| CN106829935B (en) * | 2017-03-27 | 2023-03-24 | 重庆墨希科技有限公司 | Multi-cavity graphene continuous growth equipment arranged transversely |
| CN112661141B (en) * | 2021-01-08 | 2023-05-05 | 常州机电职业技术学院 | Equipment for preparing graphene |
| CN112875690B (en) * | 2021-04-29 | 2021-08-31 | 中国恩菲工程技术有限公司 | Graphene synthesis device and graphene synthesis method using same |
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| CN101287679A (en) * | 2005-10-14 | 2008-10-15 | 普林斯顿大学理事会 | Thermally exfoliated graphite oxide |
| CN102471068A (en) * | 2009-08-10 | 2012-05-23 | 新正直技术株式会社 | A method of producing nano-size graphene-based material and an equipment for producing the same |
| CN102001642A (en) * | 2009-09-02 | 2011-04-06 | 中国科学院金属研究所 | Method for producing graphene belts in controllable macroscopic quantity by chemically cutting grapheme |
| CN102120572A (en) * | 2011-01-24 | 2011-07-13 | 南京大学 | Method for preparing nitrogen-doped graphene |
| CN102139873A (en) * | 2011-02-17 | 2011-08-03 | 无锡第六元素高科技发展有限公司 | Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment |
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