CN106829936A - The horizontal continuous growth apparatus of Graphene volume to volume - Google Patents

The horizontal continuous growth apparatus of Graphene volume to volume Download PDF

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Publication number
CN106829936A
CN106829936A CN201710186762.9A CN201710186762A CN106829936A CN 106829936 A CN106829936 A CN 106829936A CN 201710186762 A CN201710186762 A CN 201710186762A CN 106829936 A CN106829936 A CN 106829936A
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graphene
volume
vacuum
chamber
horizontal continuous
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CN106829936B (en
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李占成
伍俊
史浩飞
李昕
朱鹏
黄德萍
段银武
余杰
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Chongqing Graphene Technology Co Ltd
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Chongqing Graphene Technology Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02P20/00Technologies relating to chemical industry
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Abstract

Being capable of improve production efficiency, reducing energy consumption the invention discloses one kind, it is ensured that the horizontal continuous growth apparatus of Graphene volume to volume of product quality.The horizontal continuous growth apparatus of Graphene volume to volume, including vacuum feeding room, high-temperature technology chamber, vacuum material extracting chamber, drive device;The vacuum feeding room and vacuum material extracting chamber are provided with vavuum pump;Nonstorage calorifier is provided with the high-temperature technology chamber;The high-temperature technology chamber is connected and connects with vacuum feeding room, and the other end is connected and connects with vacuum material extracting chamber;The two ends of the high-temperature technology chamber are provided with uniform flow thermal insulation board and quickly cooling device;The tension detecting apparatus for detecting graphene growth substrate tension are provided with the vacuum feeding room, the cooling device for cooling down detection graphene growth substrate is provided between the graphene-based bottom material receiving roller and rewinding guide roller.Product quality can be improved using the horizontal continuous growth apparatus of Graphene volume to volume, production cost is saved.

Description

The horizontal continuous growth apparatus of Graphene volume to volume
Technical field
The present invention relates to a kind of growth apparatus of Graphene, especially a kind of horizontal Graphene volume to volume, continuously growth sets It is standby.
Background technology
It is well-known:Graphene is due to its superpower heat endurance, chemical stability, mechanical stability and printing opacity high The advantages of property and electron mobility, thus be considered as to prepare one of optimal material of conducting membrane material.
Chemical meteorology deposition method CVD:
CVD is a kind of most common method of controllable preparation large-area graphene.Its cardinal principle is to utilize plane Metal is passed through a certain amount of carbon source presoma and hydrogen, in gold after interaction as substrate and catalyst in hot environment Metal surface is deposited and obtains Graphene.
CVD tube furnaces:Equipment is simple, and operation is easy, but reaction temperature is high, and the time is more long, and consuming energy is larger, by stone The diameter and flat-temperature zone effect length of English tube furnace cannot prepare the Graphene of large area;Further, since base material is not pressed Power/tension force, film growth easily forms fold, reduces flatness.
The diameter and body of heater constant temperature section length of prior art conventional CVD tube furnaces growth Graphene by quartz tube furnace Influence, graphene growth size of foundation base is limited, high additionally, due to graphene growth technological temperature, therefore technological process is:Metal Paillon foil is pre-processed, fills sample, vacuumize, heat, lead to protective gas, logical process gas, be warming up to 1000 degrees centigrades, and insulation is given birth to Long, logical protective gas, is cooled to room temperature, sampling.
Existing production technology has the disadvantage that:1) efficiency is low;2) consume energy high;3) exterior quality is poor;4) quality control Difficulty is high.
The content of the invention
The technical problems to be solved by the invention are to provide one kind being capable of improve production efficiency, reducing energy consumption, it is ensured that product The horizontal continuous growth apparatus of Graphene volume to volume of quality.
The technical solution adopted for the present invention to solve the technical problems is:The invention provides a kind of horizontal graphene roll pair Roll up continuous growth apparatus, including vacuum feeding room, high-temperature technology chamber, vacuum material extracting chamber, drive device;The vacuum feeding room Graphene growth substrate emptying roller is inside provided with, graphene-based bottom material receiving roller is provided with the vacuum material extracting chamber and rewinding is led To roller;The vacuum feeding room and vacuum material extracting chamber are provided with vavuum pump;The graphene growth substrate emptying roller and stone Mertenyl bottom material receiving roller drives and rotates by drive device;Nonstorage calorifier is provided with the high-temperature technology chamber;
The high-temperature technology chamber is connected and connects with vacuum feeding room, and the other end is connected and connects with vacuum material extracting chamber It is logical;The two ends of the high-temperature technology chamber are provided with uniform flow thermal insulation board and quickly cooling device;
The tension detecting apparatus for detecting graphene growth substrate tension are provided with the vacuum feeding room, it is described true The cooling device for cooling down detection graphene growth substrate is provided with empty material extracting chamber, the cooling device is located at graphene-based Between bottom material receiving roller and rewinding guide roller.
Further, the drive device includes first driving means and the second drive device;Described first drives dress Put and be connected with graphene growth substrate emptying roller;Second drive device is connected with graphene-based bottom material receiving roller.
Further, the rotating shaft that the graphene growth substrate emptying roller has passes through vacuum feeding room, and by clutch Device is connected with first driving means;The rotating shaft that the graphene-based bottom material receiving roller has passes through vacuum material extracting chamber, and passes through Clutch and the second drive device are connected.
Further, to be provided with vacuum moving between the rotating shaft of the graphene growth substrate emptying roller and vacuum feeding room close Seal apparatus;Vacuum dynamic seal device is provided between the rotating shaft of the graphene-based bottom material receiving roller and vacuum material extracting chamber.
Preferably, the first driving means and the second drive device use reducing motor.
Further, the described horizontal continuous growth apparatus of Graphene volume to volume, also including processor, the processor point Do not electrically connected with tension detecting apparatus and first driving means, and the processor, tension detecting apparatus and first drive Device forms feedback closed loop.
Further, the processor is electrically connected with speed detector and the second drive device respectively, and the place Reason device, speed detector and first driving means form feedback closed loop.
Further, the quickly cooling device is detachably connected with high-temperature technology chamber.
Preferably, the uniform flow heat-proof device includes at least two-layer thermal insulation board and support column, and the support column is arranged on Between adjacent two layers thermal insulation board;Central through hole is provided with the thermal insulation board, is provided with the thermal insulation board equally distributed Stomata, the air-vent on the adjacent two layers thermal insulation board is dislocatedly distributed.
The beneficial effects of the invention are as follows:The horizontal continuous growth apparatus of Graphene volume to volume of the present invention, with following Advantage:
1st, efficiency high:In the absence of frequently blow-on sampling/setting-out, the action, continuous volume to volume growth such as vacuumize;
2nd, consume energy low:In the absence of frequently heating/cooling procedure, consume energy low;
3rd, due to being provided with the tension detecting apparatus for detecting graphene growth substrate tension in vacuum feeding room, because This can be controlled to the tension force of graphene growth substrate, so that product appearance quality is high, it is to avoid fold occur;
4th, because the growth technique environment experienced with a roll growth base material is identical, therefore Graphene quality batch stabilization can Lean on.
Brief description of the drawings
Fig. 1 is the structural representation of the horizontal continuous growth apparatus of Graphene volume to volume in the embodiment of the present invention;
Fig. 2 is the left view of the horizontal continuous growth apparatus of Graphene volume to volume in the embodiment of the present invention;
Fig. 3 is the right view of the horizontal continuous growth apparatus of Graphene volume to volume in the embodiment of the present invention;
Fig. 4 is the stereogram of uniform flow heat-proof device in the embodiment of the present invention;
Indicated in figure:1- vacuum feedings room, 2- graphene growth substrate emptying rollers, 3- tension detecting apparatus, the fast quickly coolings of 4- But device, 5- nonstorage calorifiers, 6- uniform flow heat-proof devices, 7- high-temperature technology chambers, 8- vacuum material extracting chamber, the graphene-based bottoms of 9- Material receiving roller, 10- rewinding guide rollers, 11- speed detectors, 12- first driving means, the drive devices of 13- second, 14- clutches Device, 15- vacuum dynamic seal devices, 16- graphene growth substrates, 17- installing plates.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples.
As depicted in figs. 1 and 2, the horizontal continuous growth apparatus of Graphene volume to volume of the present invention, including vacuum feeding Room 1, high-temperature technology chamber 7, vacuum material extracting chamber 8, drive device;Graphene growth substrate is provided with the vacuum feeding room 1 Graphene-based bottom material receiving roller 9 and rewinding guide roller 10 are provided with emptying roller 2, the vacuum material extracting chamber 8;The vacuum feeding Room 1 and vacuum material extracting chamber 8 are provided with vavuum pump;The graphene growth substrate emptying roller 2 and graphene-based bottom material receiving roller 9 By drive device, drive and rotate;Nonstorage calorifier 5 is provided with the high-temperature technology chamber 7;
Described one end of high-temperature technology chamber 7 is connected and connects with vacuum feeding room 1, and the other end is connected with vacuum material extracting chamber 8 And connection;The two ends of the high-temperature technology chamber 7 are provided with uniform flow heat-proof device 6 and quickly cooling device 4;
The tension detecting apparatus 3 for detecting the tension force of graphene growth substrate 16, institute are provided with the vacuum feeding room 1 State the cooling device 11 being provided with vacuum material extracting chamber 8 for cooling down detection graphene growth substrate 16, the cooling device position Between graphene-based bottom material receiving roller 9 and rewinding guide roller 10.
The Main Function of the nonstorage calorifier 5 is to realize the heating to high-temperature technology chamber 7 so that high-temperature technology chamber Temperature in room 7 can reach the temperature of technological requirement.The nonstorage calorifier 5 can use resistance heater, in order to just In the maintenance of high-temperature technology chamber 7, a kind of preferred embodiment is specifically, the nonstorage calorifier 5 uses retractable heating Stove, at least dual temperature area are controlled.
The Main Function of the quickly cooling device 4 is to realize the quick cooling to graphene growth substrate 16, specifically, Specifically, the quickly cooling device 4 can include outer water jacket and inner water sleeve flange using cold water jacket, the cooling device 4, outward Water jacket is sleeved on high-temperature technology chamber 7, and inner water sleeve flange is arranged on high-temperature technology chamber 7 and vacuum feeding room 1 and vacuum The junction of material extracting chamber 8.
The high-temperature technology chamber 7 is arranged between vacuum feeding room 1 and vacuum material extracting chamber 8;The vacuum feeding room 1 In the lower end of high-temperature technology chamber 7, the vacuum material extracting chamber 8 is arranged on the upper end of high-temperature technology chamber 7;The high-temperature technology chamber The two ends of room 7 are provided with quickly cooling device 4.Specifically, vacuum feeding room 1, vacuum material extracting chamber 8 and high-temperature technology chamber 7 The quickly cooling device 4 of junction, is connected using the flange with water cooling plant.Specifically, the high-temperature technology chamber 7 is typically adopted Use quartz ampoule.
During use:
Tinsel is pre-processed and enters first and then in vacuum feeding room 1 and vacuum material extracting chamber 8 luggage sample, dress sample is complete Vacuumized into the rear vavuum pump by vacuum feeding room 1 and vacuum material extracting chamber 8;Then by fast on high-temperature technology chamber 7 Fast heater 5 is heated, while lead to protective gas and be passed through process gas, until temperature heats up in high-temperature technology chamber 7 To 1000 degrees centigrades;Start graphene-based bottom material receiving roller 9 and batch graphene growth substrate 16;Due in high-temperature technology chamber 7 two ends are provided with quickly cooling device 4, therefore, it is possible to ensure graphene growth substrate 16 so as to high-temperature technology chamber 7 is to very The temperature of empty material extracting chamber 8 is reduced, then the cooling device 11 in by vacuum material extracting chamber 8 so that graphene growth substrate 16 is arrived It is sampled after normal temperature.
In sum, the horizontal continuous growth apparatus of Graphene volume to volume of the present invention, due to during production Frequently blow-on sampling/setting-out need not be carried out, the action such as vacuumizes such that it is able to realize the continuous growth of volume to volume, thus it is raw Produce efficiency high;Simultaneously in the absence of frequently heating/cooling procedure, therefore it is low to consume energy.Secondly as being set in vacuum feeding room 1 The tension detecting apparatus 3 for detecting graphene growth substrate tension are equipped with, therefore, it is possible to the tension force to graphene growth substrate It is controlled, so that product appearance quality is high, it is to avoid fold occur;And due to the growth with a roll of growth base material experience Process environments are identical, therefore Graphene quality batch is reliable and stable.Again, due to the cooling device 11 in vacuum material extracting chamber 8, because It is normal temperature that this ensure that graphene growth substrate 16 is crimped onto temperature when on graphene-based bottom material receiving roller 9.
The uniform flow heat-proof device 6 can be using the uniform flow thermal insulation board of monolithic, in order to improve effect of heat insulation and cause gas It is uniformly distributed in high-temperature technology chamber, it is preferred that as shown in figure 4, the uniform flow heat-proof device 6 includes at least two-layer thermal insulation board 61 And support column 62, the support column 62 is arranged between adjacent two layers thermal insulation board 61;Center is provided with the thermal insulation board 61 Through hole 63, and equally distributed air-vent, the air-vent on the adjacent two layers thermal insulation board 61 are dislocatedly distributed.Specifically, every Hot plate can be the unlike materials such as quartz, ceramics, molybdenum, stainless steel, copper, preferred quartz thermal insulation board in the present invention.
Further, for the ease of to being passed through process gas in high-temperature technology chamber 7, being set in high-temperature technology chamber 7 No less than two process gas connectors, being passed through on pipeline for external process gas has flowmeter to monitor.
For the ease of detecting the growing environment of graphene growth substrate, further, there is pressure in high-temperature technology chamber 7 Detection, temperature-detecting device.
The Main Function of the drive device is to drive graphene growth substrate emptying roller 2 and graphene-based bottom material receiving roller 9 Rotate;For the ease of the independent control to graphene growth substrate emptying roller 2 and the graphene-based rotating speed of bottom material receiving roller 9, further , the drive device includes the drive device 13 of first driving means 12 and second;The first driving means 12 and graphite Alkene growth substrate emptying roller 2 is connected;Second drive device 13 is connected with graphene-based bottom material receiving roller 9.
For the ease of quick despatch substrate or coiled material, without driving or stopping drive device, further, the graphite The rotating shaft that alkene growth substrate emptying roller 2 has passes through vacuum feeding room 1, and is driven with first driving means 12 by clutch 14 Connection;The rotating shaft that the graphene-based bottom material receiving roller 9 has passes through vacuum material extracting chamber 8, and is driven by clutch 14 and second Device 13 is connected.
In order to avoid between the rotating shaft of graphene growth substrate emptying roller 2 and vacuum feeding room 1 and graphene-based bottom is received Expect occur leaking out between the rotating shaft of roller 9 and vacuum material extracting chamber 8, further, the rotating shaft of the graphene growth substrate emptying roller 2 Vacuum dynamic seal device 15 is provided between vacuum feeding room 1;The rotating shaft of the graphene-based bottom material receiving roller 9 and vacuum feeding Vacuum dynamic seal device 15 is provided between room 8.
For the ease of the rotating speed control to graphene growth substrate emptying roller 2 and graphene-based bottom material receiving roller 9, it is preferred that The drive device 13 of first driving means 12 and second uses servomotor acceleration and deceleration device;Preferably, clutch 14 selects magnetic Powder clutch.
For the ease of the guiding of graphene growth substrate 16, further, in the vacuum feeding room 1 it is provided with blowing and leads To rod 4;Graphene growth substrate 16 on graphene growth substrate emptying roller 2 bypasses tension detecting apparatus 3, blowing guiding successively Rod 4 enters high-temperature technology chamber 7.
In order to realize the Aulomatizeted Detect of the tension force of graphene growth substrate 16, while passing through graphene growth substrate emptying roller 2 rotating speed realizes the Automated condtrol to tension force, further, the described horizontal continuous growth apparatus of Graphene volume to volume, and also Including processor, the processor is electrically connected with tension detecting apparatus 8 and first driving means respectively, and the processor, Tension detecting apparatus 8 and first driving means 12 form feedback closed loop.Tension detecting apparatus 8 detect that the data feedback for obtaining is arrived Processor, the processor can use CPU or single-chip microcomputer, then control turning for first driving means 12 by processor Speed, so as to the automation for realizing tension force is adjusted.
In order to realize the graphene-based rotating speed of bottom material receiving roller 9 automation adjust, further, the processor respectively with speed The degree drive device 13 of detection means 11 and second is electrically connected, and the processor, speed detector 11 and first drive Device 15 forms feedback closed loop.
Safeguard and change, further, the quickly cooling device 4 and high-temperature technology for the ease of high-temperature technology chamber 7 Chamber 7 is detachably connected.

Claims (9)

1. horizontal continuous growth apparatus of Graphene volume to volume, including vacuum feeding room (1), high-temperature technology chamber (7), vacuum feeding Room (8), drive device;Graphene growth substrate emptying roller (2), the vacuum feeding are provided with the vacuum feeding room (1) Graphene-based bottom material receiving roller (9) and rewinding guide roller (10) are provided with room (8);The vacuum feeding room (1) and vacuum take Material room (8) is provided with vavuum pump;The graphene growth substrate emptying roller (2) and graphene-based bottom material receiving roller (9) lead to Over-driving device, drives and rotates;Nonstorage calorifier (5) is provided with the high-temperature technology chamber (7);
It is characterized in that:Described high-temperature technology chamber (7) one end is connected and connects with vacuum feeding room (1), the other end and vacuum Material extracting chamber (8) connects and connects;The two ends of the high-temperature technology chamber (7) are provided with uniform flow heat-proof device (6) and quick Cooling device (4);
The tension detecting apparatus (3) for detecting graphene growth substrate (16) tension force are provided with the vacuum feeding room (1), The cooling device (11) for cooling down detection graphene growth substrate (16) is provided with the vacuum material extracting chamber (8), it is described cold But device is located between graphene-based bottom material receiving roller (9) and rewinding guide roller (10).
2. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 1, it is characterised in that:The drive device bag Include first driving means (12) and the second drive device (13);The first driving means (12) are put with graphene growth substrate Material roller (2) drive connection;Second drive device (13) is connected with graphene-based bottom material receiving roller (9).
3. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 2, it is characterised in that:The graphene growth The rotating shaft that substrate emptying roller (2) has passes through vacuum feeding room (1), and is passed by clutch (14) and first driving means (12) Dynamic connection;The rotating shaft that the graphene-based bottom material receiving roller (9) has pass through vacuum material extracting chamber (8), and by clutch (14) with Second drive device (13) is connected.
4. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 3, it is characterised in that:The graphene growth Vacuum dynamic seal device (15) is provided between the rotating shaft of substrate emptying roller (2) and vacuum feeding room (1);The graphene-based bottom Vacuum dynamic seal device (15) is provided between the rotating shaft of material receiving roller (9) and vacuum material extracting chamber (8).
5. horizontal continuous growth apparatus of Graphene volume to volume as described in claim 2,3 or 4, it is characterised in that:Described first Drive device (12) and the second drive device (15) use reducing motor.
6. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 5, it is characterised in that:Also include processor, The processor is electrically connected with tension detecting apparatus (8) and first driving means respectively, and the processor, tension force detection dress Put (8) and first driving means (12) form feedback closed loop.
7. horizontal continuous growth apparatus of Graphene volume to volume as described in claim 2,3 or 4, it is characterised in that:The treatment Device is electrically connected with speed detector (11) and the second drive device (13) respectively, and the processor, speed detector (11) and the second drive device (13) formed feedback closed loop.
8. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 1, it is characterised in that:The quick cooling dress (4) are put to be detachably connected with high-temperature technology chamber (7).
9. horizontal continuous growth apparatus of Graphene volume to volume as claimed in claim 1, it is characterised in that:The heat-insulated dress of uniform flow Putting (6) includes at least two-layer thermal insulation board (61) and support column (62), and the support column (62) is arranged on adjacent two layers thermal insulation board (61) between;Central through hole (63) is provided with the thermal insulation board (61), is provided with the thermal insulation board (61) equally distributed Air-vent, the air-vent on the adjacent two layers thermal insulation board (61) is dislocatedly distributed.
CN201710186762.9A 2017-03-27 2017-03-27 Horizontal type graphene roll-to-roll continuous growth equipment Active CN106829936B (en)

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KR20130114523A (en) * 2012-04-09 2013-10-18 엘지전자 주식회사 Apparatus for growing graphene using joule heating
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CN105624640A (en) * 2016-01-31 2016-06-01 安徽贝意克设备技术有限公司 Roll-to-roll continuous grapheme film growth device and technique
US20160186320A1 (en) * 2014-12-26 2016-06-30 Metal Industries Research And Development Centre Apparatus for continuously forming a film through chemical vapor deposition
CN105908149A (en) * 2016-06-30 2016-08-31 青岛赛瑞达电子科技有限公司 Reel-to-reel continuous growth equipment for graphene films
CN207030960U (en) * 2017-03-27 2018-02-23 重庆墨希科技有限公司 The horizontal continuous growth apparatus of graphene volume to volume

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202297140U (en) * 2011-11-01 2012-07-04 海洋王(东莞)照明科技有限公司 Device capable of continuously preparing grapheme film
KR20130114523A (en) * 2012-04-09 2013-10-18 엘지전자 주식회사 Apparatus for growing graphene using joule heating
CN103276372A (en) * 2013-06-03 2013-09-04 重庆绿色智能技术研究院 Preparation method of graphene and preparation method thereof
CN103305806A (en) * 2013-06-28 2013-09-18 重庆墨希科技有限公司 Device for continuously growing graphene at high temperature
CN203569183U (en) * 2013-11-21 2014-04-30 青岛赛瑞达电子科技有限公司 Normal pressure CVD (Chemical Vapor Deposition) film continuous growth furnace
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