CN205295454U - Continuous scale deposition equipment of graphene films - Google Patents

Continuous scale deposition equipment of graphene films Download PDF

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Publication number
CN205295454U
CN205295454U CN201520927920.8U CN201520927920U CN205295454U CN 205295454 U CN205295454 U CN 205295454U CN 201520927920 U CN201520927920 U CN 201520927920U CN 205295454 U CN205295454 U CN 205295454U
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China
Prior art keywords
graphene
foil
deposition
vacuum chamber
deposit
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CN201520927920.8U
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Chinese (zh)
Inventor
王宏飞
戚顺昌
吴洪
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XIANYANG HONGFENG KLINE EQUIPMENT CO Ltd
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XIANYANG HONGFENG KLINE EQUIPMENT CO Ltd
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Abstract

The utility model discloses a continuous scale deposition equipment of graphene films, include: inclosed real empty room (1), be used for the sedimentary deposit foil strips of graphite alkene (2) and locate the thing receive and releasing of graphite alkene deposit foil strips a roll storehouse (3) at real empty room both ends, and with drive arrangement (4) that graphite alkene deposit foil strips (2) is connected, drive arrangement (4) include that driving motor and graphite alkene deposit foil strips receive and release winding up roller (5), just real empty room (1) is used for graphite alkene deposit foil strips heating device (7) with receiving and releasing to be equipped with in the middle of a roll storehouse (3), and it is along graphite alkene deposit foil strips's (2) direction of motion, it is equipped with and is used for cooling off quick cooling device (8) that the deposit has the deposit foil strips of graphite alkene to receive and release roll hatch opening to make the graphite alkene deposit foil strips (2) of high temperature cool off fast to normal atmospheric temperature, and the follow -up preparation process that makes is gone on fast consecutively.

Description

The continuous scale depositing device of a kind of graphene film
Technical field
The utility model relates to the continuous scale depositing device of a kind of graphene film.
Background technology
Graphene (Graphene) is a kind ofly to form with sp2 hybridized orbit the flat film that hexangle type is honeycomb lattice by carbon atom, only has the two-dimensional material of a carbon atom thickness. Graphene is the new material that integrates the excellent properties such as superelevation mechanical strength, thermal conductive resin, high optical transparency and superpower electric conductivity, it is not only applicable to basic physics research, as integer quantum hall effect under fractional quantum hall effect, room temperature etc., and have broad application prospects in fields such as demonstration, the energy, detection, photoelectrons, as molecular detector, thermal conductance/thermal interfacial material, field emission source, ultracapacitor, solar cell, Graphene lithium battery, field-effect transistor and integrated circuit, transparency conductive electrode etc.
The industrial chemical vapor deposition (CVD) legal system that generally adopts is for graphene film sheet at present; but the equipment of process for preparing graphenes by chemical vapour deposition is all periodic deposition at present; primary depositing a slice, cannot large-scale production, lack a kind of can be for the equipment of the continuous fast deposition of Graphene.
In view of above reason, my company's utility model the continuous scale of a kind of Graphene deposition special equipment.
Utility model content
The technical problems to be solved in the utility model be propose a kind of scale graphene film Preparation equipment, this scale graphene film Preparation equipment can realize Graphene rapidly, continuously and large-scale industrialized production.
It is as follows that the utility model solves the problems of the technologies described above taked technical scheme:
The continuous scale depositing device of a kind of graphene film, comprise: airtight vacuum chamber (1), deposit the unwinding and rewinding storehouse (3) of foil for the deposition foil (2) of Graphene deposition and the Graphene of being located at vacuum chamber two ends, and the drive unit (4) being connected with described Graphene deposition foil (2), described drive unit (4) comprises drive motors and Graphene deposition foil unwinding and rewinding rollers (5), and described vacuum chamber (1) is provided with for Graphene deposition foil heater (7) with unwinding and rewinding storehouse (3) is middle, it deposits the direction of motion of foil (2) along Graphene, described unwinding and rewinding Hatch Opening is provided with the quickly cooling device (8) for the cooling deposition foil that deposits Graphene, be quickly cooled to normal temperature with the Graphene deposition foil (2) that makes high temperature, and the follow-up preparation process making is in extremely rapid succession carried out.
Preferably, described drive unit is also provided with tensioning running roller (6).
Preferably, in described vacuum chamber (1), be provided with the air-channel system (9) of preparing desired gas for passing into Graphene, and the peripheral hardware of vacuum chamber (1) is useful on the vavuum pump group (10) that vacuum chamber (1) is vacuumized, described vavuum pump group (10) vacuumizes described vacuum chamber (1), and makes vacuum chamber (1) in Graphene preparation process, keep constant vacuum.
Preferably, described folding and unfolding winding up roller (5) and tensioning pressure roller (6), and unwinding and rewinding storehouse is the foil rolling wheel of outer wall mirror finish metal or quartzy material, high temperature deposition storehouse is quartzy material.
Preferably, described Graphene deposition foil is Copper Foil, and Graphene sedimentary condition is 1000 degree left and right.
Preferably, described drive system adopts continuous-moving type or pulsed to move, and while adopting continuous moving, need to regulate the rate travel of Graphene foil (2), makes it in high temperature service (7) is located the mobile time, can complete the deposition of Graphene; Adopt pulsed while moving, stop when Graphene foil moves to when high temperature service (7) is located, until Graphene deposited, then the foil that does not deposit Graphene is moved to high temperature service (7) locate to deposit Graphene.
Preferably, described heater (7) is circumferential Omnidirectional heating; Described quickly cooling device (8), adopts cooling water circulation cooling; On described heater (7) and quickly cooling device (8), be equipped with temperature sensor, heat for Graphene foil provides circular Omnibearing even by heater (7), make graphene uniform deposition, quickly cooling device can be cooled to normal temperature so that follow-up rolling by the Graphene foil having deposited fast.
Preferably, between described vavuum pump group (10) and vacuum chamber (1), be provided with valve (11), can effectively improve and vacuumize efficiency and in Graphene manufacture process, keep the vacuum in vacuum chamber (1).
Preferably, in described vacuum chamber (1), be also provided with the vacuum meter (12) of measuring positive reciprocal of duty cycle, for the vacuum in Real-time Feedback and monitoring vacuum chamber (1).
The beneficial effects of the utility model are:
Continous way scale graphene film depositing device of the present utility model, first the foil volume that needs preparation size is arranged on and is unreeled in storehouse, remove the foreign gas in cavity by vacuumizing the whole cavity of repeated washing and pipeline again, pass into again catalytic gas, form a stable Graphene and prepare environment, Graphene is deposited to foil to be heated to Graphene and to deposit required temperature, and after temperature stabilization, in vacuum cavity, evenly pass into Graphene and prepare needed carbon-source gas, in that section of corresponding Graphene deposition foil of heater, carbon-source gas decomposes under acting in catalytic substrate and catalytic gas, and deposit Graphene in the corresponding section of heater Graphene deposition foil, the preparation technology that Graphene is prepared in scale of the present utility model is by local heat, and Graphene deposition foil at the uniform velocity by high-temperature heating equipment, realizes Graphene successive sedimentation in foil under high-temperature temperature under needed pressure and atmospheric condition, according to type of drive difference, can deposit piecemeal, intermittently deposition, successive sedimentation, until the Graphene in whole Graphene deposition foil all deposit, the utility model can realize Graphene continuously, quick, scale industrialization production.
Other features and advantages of the utility model will be set forth in the following description, and, partly from description, become apparent, or understand by implementing the utility model. The purpose of this utility model and other advantages can be realized and be obtained by specifically noted structure in write description, claims and accompanying drawing.
Brief description of the drawings
Below in conjunction with accompanying drawing, the utility model is described in detail, to make above-mentioned advantage of the present utility model clearer and more definite.
Fig. 1 is the structural representation of the continuous scale depositing device of the utility model graphene film.
Detailed description of the invention
Below in conjunction with specific embodiment, the utility model is described in detail.
Specifically, the utility model relates to the continuous scale deposition of a kind of graphene film special equipment, and equipment comprises that drive system, Graphene deposition foil unwinding and rewinding system, the Graphene of vacuum turnover volume storehouse, high temperature deposition storehouse, the motion of Graphene deposition foil deposit required external vacuum pump group; In described vacuum chamber, in deposition foil and the direction of motion thereof, should be provided with the heater for heating Graphene deposition foil; The direction of moving along described Graphene deposition foil, described rolling bin location should be provided with the quickly cooling device for the Graphene deposition foil of cooling deposition Graphene; Described whole vacuum cavity is provided with the air-channel system of preparing desired gas for passing into Graphene, and vacuum chamber peripheral hardware is useful on the vavuum pump group that described vacuum cavity is vacuumized. The continuous scale of Graphene of the present utility model deposition special equipment can realize Graphene rapidly, continuously and large-scale industrialized production. Beneficial effect is: manufacturing cycle is short, and equipment operating is simple, and output can continous way be produced in batches greatly, and economic benefit is high.
Wherein, scale method for preparing graphene membrane of the present utility model, comprises the steps:
1) the Graphene deposited foil roll coil of strip is fixed on and is unreeled in storehouse, foil is fixed to foil rolling storehouse through one section of bringing-up section corresponding to heater;
2) get rid of after the foreign gas in vacuum chamber, in vacuum chamber, pass into catalytic gas;
3) start heater and in vacuum chamber, pass into carbon-source gas, and the pressure controlling in vacuum chamber is the Graphene deposition pressure of setting simultaneously;
4) when Graphene starts to deposit, start foil folding and unfolding drive unit, make foil at the uniform velocity by high temperature carbon deposition zone, Negotiation speed regulates according to Graphene sedimentation time;
5) after the Graphene of Graphene deposition foil has deposited, in the whole collections of foil and foil rolling storehouse, utilize quickly cooling device that Graphene foil is cooled to normal temperature, open hatch door and take out the foil volume that has deposited Graphene;
6) put into new foil and start the deposition of new round graphene film.
Further, the described the 4th), in step, Graphene deposition foil moves for continous way at the uniform velocity with respect to the relative movement mode of heater.
Further, the speed that described Graphene deposition foil and heater relatively move equals the length of heater in the Graphene deposition foil direction of motion and the ratio of Graphene deposition required time.
Further, the flow of described carbon-source gas is 1-1000sccm, and the flow of catalytic gas is 1-1000sccm, Graphene deposition pressure 1Pa-3atm, and Graphene depositing temperature is 700-1050 DEG C.
Further, in the time that deposition pressure is greater than 1atm, in vacuum chamber, pass into inert dilution gas, the flow of described inert dilution gas is 100-2000sccm.
Further, described inert dilution gas is argon gas or nitrogen etc.;
Described carbon-source gas is the carbonaceous gas such as methane, ethene or acetylene;
Described catalytic gas is hydrogen.
Further, described 2) in step, the method of despumation gas is as follows: fix after foil volume in anti-roll storehouse, whole cavity is evacuated to equipment vacuum degree, with the whole air inlet pipeline of inert gas purge, cavity, unwinding and rewinding storehouse, after repeated washing at least twice, then cavity is evacuated to equipment vacuum degree.
Further, the described the 2nd) in step, in the time that Graphene deposition pressure is greater than 1atm, the method for despumation gas is as follows: more than passing into whole cavity the inert dilution gas half an hour that flow is more than or equal to 1000sccm.
Further, described quickly cooling device is cooled to normal temperature required time by described Graphene deposition foil and should be foil operation 50mm required time.
As shown in Figure 1, prepare the structural representation of the apparatus embodiments of graphene film for serialization scale of the present utility model. Graphene deposition Preparation equipment of the present utility model, comprise airtight vacuum chamber 1, for the deposition foil 2 of Graphene deposition, the unwinding and rewinding storehouse 3 of the Graphene deposition foil at vacuum chamber two ends, the drive unit 4 of Graphene deposition foil motion, drive unit 4 comprises drive motors and Graphene deposition foil unwinding and rewinding roller 5, and drive unit also needs to add tensioning running roller 6 as required.
In the middle of vacuum chamber and unwinding and rewinding storehouse, be provided with for Graphene deposition foil heater 7, along Graphene deposition foil 2 directions of motion, unwinding and rewinding Hatch Opening is provided with the quickly cooling device 8 for the cooling deposition foil 2 that deposits Graphene, can make the Graphene deposition foil 2 of high temperature be quickly cooled to normal temperature, contribute to the raising of Graphene quality of forming film, and the follow-up preparation process making is in extremely rapid succession carried out.
In vacuum chamber 1, be provided with the air-channel system 9 of preparing desired gas for passing into Graphene, and vacuum chamber 1 peripheral hardware is useful on the vavuum pump group 10 that vacuum chamber 1 is vacuumized, vavuum pump group 10 can vacuumize vacuum chamber 1, and makes vacuum chamber 1 in Graphene preparation process, keep constant vacuum.
The Graphene deposition continuous production equipment of the present embodiment provides required vacuum environment by airtight vacuum chamber 1 is set for Graphene deposits, air-channel system 9 can deposit needed gas to passing into Graphene in vacuum chamber 1, by being set, running roller drive unit drive Graphene deposition foil 2 to move, being positioned at the middle heater 7 of vacuum chamber provides deposition temperature required for the Graphene by this section deposits foil, and deposit Graphene in this section of Graphene deposition foil 2, Graphene has deposited rear driven device and has moved to quickly cooling device 8 places and be cooled to normal temperature, finally completed the preparation of Graphene by 4 rollings of unwinding and rewinding storehouse. therefore, under the effect of drive system, what Graphene deposition foil 2 can continuously and smoothly passes through heater 7 place's heating deposition Graphenes, then through rolling after cooling, can meet Graphene rapidly, continuously with the demand of large-scale production.
Further, after quickly cooling device 8, be provided with compacting tensioning apparatus 6, to ensure that foil normally moves.
Further, folding and unfolding winding up roller 5, tensioning pressure roller 6, and unwinding and rewinding storehouse is the foil rolling wheel of outer wall mirror finish metal or quartzy material, high temperature deposition storehouse is that quartzy material is made and can be born Graphene and deposit required high temperature. The Graphene deposition foil preferably copper paper tinsel of preferred the present embodiment, Graphene sedimentary condition is 1000 degree left and right, if directly adopt external force to hale Copper Foil motion, may cause at high temperature Graphene foil fracture, cannot realize continuous production, deposit as under low temperature, can not prepare Graphene, therefore unwinding and rewinding storehouse, will realize a rolling foil, one discharges the effect of foil, can ensure the proper motion of foil simultaneously, again can not be by its drawing crack, and then realize Graphene serialization deposition.
Further, drive system adopts continuous-moving type or pulsed to move, while adopting continuous moving, need to regulate the rate travel of Graphene foil 2, make can complete in its time of moving at high temperature service 7 places the deposition of Graphene, while adopting pulsed to move, in the time that Graphene foil moves to high temperature service 7 place, stop, until Graphene deposited, then the foil that does not deposit Graphene is moved to high temperature service 7 places' deposition Graphenes; The mode of employing continuous-moving type or pulse movable type can realize in Graphene foil and deposit Graphene, and the present embodiment adopts the mode of continuous moving to drive foil 2 to deposit Graphene.
Further, heater 7 is circumferential Omnidirectional heating; Quickly cooling device 8, adopts cooling water circulation cooling; Heater 7 is equipped with temperature sensor with on quickly cooling device 8, heat for Graphene foil provides circular Omnibearing even by heater 7, make graphene uniform deposition, quickly cooling device can be cooled to normal temperature so that follow-up rolling by the Graphene foil having deposited fast.
Further, between vavuum pump group 10 and vacuum chamber 1, be provided with valve 11, can effectively improve and vacuumize efficiency and keep the vacuum in vacuum chamber 1 in Graphene manufacture process. Preferably, in system, be provided with the vacuum meter 12 of measuring positive reciprocal of duty cycle, for the vacuum in Real-time Feedback and monitoring vacuum vacuum chamber 1.
Below the method that adopts the present embodiment Graphene depositing device to prepare Graphene is described.
Adopt the Graphene Preparation equipment of the present embodiment to prepare the method for Graphene, comprise the following steps:
1) open unwinding and rewinding door the Graphene deposited foil roll coil of strip is installed, get rid of the foreign gas in whole vacuum vacuum chamber 1, in vacuum chamber 1, pass into catalytic gas by air-channel system 9, under condition of normal pressure, also need to pass into the inert dilution gas for regulating vacuum chamber 1 interior pressure simultaneously, inert dilution gas can be argon gas, nitrogen etc., catalytic gas is hydrogen; And the method for despumation gas is, system is evacuated to 1Pa, with the whole pipeline of inert gas purge and cavity, repeated washing more than at least twice, is being evacuated to low vacuum by vacuum chamber 1. Can directly first pass into a large amount of inert gases for Graphene deposition in normal temperature situation and discharge the foreign gas in vacuum chamber.
2) by the heater of Graphene depositional phase, be heated to 700-1000 degree, Graphene deposits needed temperature.
3) in vacuum chamber 1, pass into carbon-source gas by air-channel system 9, and the pressure controlling in whole vacuum system is that Graphene deposits required pressure, carbon-source gas uses methane, ethene or acetylene, and carbon-source gas flow is 1-1000sccm, and hydrogen flowing quantity is 1-1000sccm.
4) start heater 7 and start Graphene foil drive unit, make it Graphene deposition foil and heater 7 and produce displacement, the time is set as Graphene deposition required time, after Graphene has deposited, go out at quickly cooling device 8 cooling fast, rolling afterwards.
The beneficial effects of the utility model are:
Continous way scale graphene film depositing device of the present utility model, first the foil volume that needs preparation size is arranged on and is unreeled in storehouse, remove the foreign gas in cavity by vacuumizing the whole cavity of repeated washing and pipeline again, pass into again catalytic gas, form a stable Graphene and prepare environment, Graphene is deposited to foil to be heated to Graphene and to deposit required temperature, and after temperature stabilization, in vacuum cavity, evenly pass into Graphene and prepare needed carbon-source gas, in that section of corresponding Graphene deposition foil of heater, carbon-source gas decomposes under acting in catalytic substrate and catalytic gas, and deposit Graphene in the corresponding section of heater Graphene deposition foil, the preparation technology that Graphene is prepared in scale of the present utility model is by local heat, and Graphene deposition foil at the uniform velocity by high-temperature heating equipment, realizes Graphene successive sedimentation in foil under high-temperature temperature under needed pressure and atmospheric condition, according to type of drive difference, can deposit piecemeal, intermittently deposition, successive sedimentation, until the Graphene in whole Graphene deposition foil all deposit, the utility model can realize Graphene continuously, quick, scale industrialization production.
Finally it should be noted that: the foregoing is only preferred embodiment of the present utility model, be not limited to the utility model, although the utility model is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement. All within spirit of the present utility model and principle, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.

Claims (9)

1. the continuous scale depositing device of graphene film, it is characterized in that, comprise: airtight vacuum chamber (1), deposit the unwinding and rewinding storehouse (3) of foil for the deposition foil (2) of Graphene deposition and the Graphene of being located at vacuum chamber two ends, and the drive unit (4) being connected with described Graphene deposition foil (2), described drive unit (4) comprises drive motors and Graphene deposition foil unwinding and rewinding rollers (5), and described vacuum chamber (1) is provided with for Graphene deposition foil heater (7) with unwinding and rewinding storehouse (3) is middle, it deposits the direction of motion of foil (2) along Graphene, described unwinding and rewinding Hatch Opening is provided with the quickly cooling device (8) for the cooling deposition foil that deposits Graphene, be quickly cooled to normal temperature with the Graphene deposition foil (2) that makes high temperature, and the follow-up preparation process making is in extremely rapid succession carried out.
2. the continuous scale depositing device of graphene film according to claim 1, is characterized in that, described drive unit is also provided with tensioning running roller (6).
3. the continuous scale depositing device of graphene film according to claim 1; it is characterized in that; in described vacuum chamber (1), be provided with the air-channel system (9) of preparing desired gas for passing into Graphene; and the peripheral hardware of vacuum chamber (1) is useful on the vavuum pump group (10) that vacuum chamber (1) is vacuumized; described vavuum pump group (10) vacuumizes described vacuum chamber (1), and makes vacuum chamber (1) in Graphene preparation process, keep constant vacuum.
4. the continuous scale depositing device of graphene film according to claim 1; it is characterized in that; described folding and unfolding winding up roller (5) and tensioning pressure roller (6), and unwinding and rewinding storehouse is the foil rolling wheel of outer wall mirror finish metal or quartzy material, high temperature deposition storehouse is quartzy material.
5. the continuous scale depositing device of graphene film according to claim 3, is characterized in that, described Graphene deposition foil is Copper Foil, and Graphene sedimentary condition is 1000 degree left and right.
6. the continuous scale depositing device of graphene film according to claim 3, it is characterized in that, described drive system adopts continuous-moving type or pulsed to move, while adopting continuous moving, need to regulate the rate travel of Graphene foil (2), make it in high temperature service (7) is located the mobile time, can complete the deposition of Graphene; Adopt pulsed while moving, stop when Graphene foil moves to when high temperature service (7) is located, until Graphene deposited, then the foil that does not deposit Graphene is moved to high temperature service (7) locate to deposit Graphene.
7. the continuous scale depositing device of graphene film according to claim 3, is characterized in that, described heater (7) is circumferential Omnidirectional heating; Described quickly cooling device (8), adopts cooling water circulation cooling; On described heater (7) and quickly cooling device (8), be equipped with temperature sensor, heat for Graphene foil provides circular Omnibearing even by heater (7), make graphene uniform deposition, quickly cooling device can be cooled to normal temperature so that follow-up rolling by the Graphene foil having deposited fast.
8. the continuous scale depositing device of graphene film according to claim 1; it is characterized in that; between described vavuum pump group (10) and vacuum chamber (1), be provided with valve (11), can effectively improve and vacuumize efficiency and in Graphene manufacture process, keep the vacuum in vacuum chamber (1).
9. the continuous scale depositing device of graphene film according to claim 1, is characterized in that, is also provided with the vacuum meter (12) of measuring positive reciprocal of duty cycle in described vacuum chamber (1), for the vacuum in Real-time Feedback and monitoring vacuum chamber (1).
CN201520927920.8U 2015-11-20 2015-11-20 Continuous scale deposition equipment of graphene films Expired - Fee Related CN205295454U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107236938A (en) * 2017-07-11 2017-10-10 江苏星特亮科技有限公司 A kind of continous way membrane production equipment
CN112723347A (en) * 2021-01-28 2021-04-30 孙华 Large-scale preparation equipment for CVD deposited graphene
CN114703466A (en) * 2022-02-07 2022-07-05 常州第六元素半导体有限公司 Continuous CVD film manufacturing apparatus and method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107236938A (en) * 2017-07-11 2017-10-10 江苏星特亮科技有限公司 A kind of continous way membrane production equipment
CN112723347A (en) * 2021-01-28 2021-04-30 孙华 Large-scale preparation equipment for CVD deposited graphene
CN114703466A (en) * 2022-02-07 2022-07-05 常州第六元素半导体有限公司 Continuous CVD film manufacturing apparatus and method
CN114703466B (en) * 2022-02-07 2024-04-09 常州第六元素半导体有限公司 Continuous CVD film manufacturing apparatus and method

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