CN106829936B - Horizontal type graphene roll-to-roll continuous growth equipment - Google Patents
Horizontal type graphene roll-to-roll continuous growth equipment Download PDFInfo
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Abstract
The invention discloses horizontal graphene roll-to-roll continuous growth equipment which can improve production efficiency, reduce energy consumption and ensure product quality. The horizontal graphene roll-to-roll continuous growth equipment comprises a vacuum feeding chamber, a high-temperature process chamber, a vacuum material taking chamber and a driving device; the vacuum feeding chamber and the vacuum material taking chamber are both provided with vacuum pumps; a rapid heating device is arranged on the high-temperature process chamber; one end of the high-temperature process chamber is connected and communicated with the vacuum feeding chamber, and the other end of the high-temperature process chamber is connected and communicated with the vacuum material taking chamber; two ends of the high-temperature process chamber are respectively provided with a uniform-flow heat insulation plate and a rapid cooling device; the vacuum feeding chamber is internally provided with a tension detection device for detecting the tension of the graphene growth substrate, and a cooling device for cooling and detecting the graphene growth substrate is arranged between the graphene bottom receiving roller and the receiving guide roller. By adopting the horizontal graphene roll-to-roll continuous growth equipment, the product quality can be improved, and the production cost is saved.
Description
Technical Field
The invention relates to a graphene growing device, in particular to a horizontal graphene roll-to-roll continuous growing device.
Background
It is well known that: graphene is considered to be one of the best materials for preparing conductive film materials due to its superior thermal stability, chemical stability, mechanical stability, high light transmittance and electron mobility.
Chemical vapor deposition CVD:
the CVD method is one of the most common methods for the controlled preparation of large-area graphene. The main principle of the method is that planar metal is used as a substrate and a catalyst, a certain amount of carbon source precursor and hydrogen are introduced into the substrate and the catalyst in a high-temperature environment, and after interaction, the carbon source precursor and the hydrogen are deposited on the surface of the metal to obtain the graphene.
CVD tube furnace: the method has the advantages that the equipment is simple, the operation is easy, but the reaction temperature is high, the time is long, the energy consumption is large, and large-area graphene cannot be prepared under the influence of the diameter of the quartz tube furnace and the length of a constant temperature area; in addition, since the base material is not pressure/tension controlled, wrinkles are easily formed in the film growth, reducing flatness.
The conventional CVD tubular furnace of prior art grows graphite alkene and receives the influence of the diameter of quartz tubular furnace and furnace body thermostatic zone length, and graphite alkene growth basement size is limited, in addition because graphite alkene growth technology temperature is high, therefore the process flow is: pretreating metal foil, loading sample, vacuumizing, heating, introducing protective gas, introducing process gas, heating to about 1000 ℃, keeping the temperature for growth, introducing protective gas, cooling to room temperature, and sampling.
The existing production process has the following defects: 1) the efficiency is low; 2) the energy consumption is high; 3) the appearance quality is poor; 4) the difficulty of quality control is high.
Disclosure of Invention
The technical problem to be solved by the invention is to provide horizontal graphene roll-to-roll continuous growth equipment which can improve production efficiency, reduce energy consumption and ensure product quality.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention provides horizontal graphene roll-to-roll continuous growth equipment which comprises a vacuum feeding chamber, a high-temperature process chamber, a vacuum material taking chamber and a driving device, wherein the vacuum feeding chamber is arranged in the vacuum feeding chamber; a graphene growth substrate discharging roller is arranged in the vacuum feeding chamber, and a graphene bottom receiving roller and a receiving guide roller are arranged in the vacuum taking chamber; the vacuum feeding chamber and the vacuum material taking chamber are both provided with vacuum pumps; the graphene growth substrate discharging roller and the graphene substrate receiving roller are driven to rotate through a driving device; a rapid heating device is arranged on the high-temperature process chamber;
one end of the high-temperature process chamber is connected and communicated with the vacuum feeding chamber, and the other end of the high-temperature process chamber is connected and communicated with the vacuum material taking chamber; two ends of the high-temperature process chamber are respectively provided with a uniform-flow heat insulation plate and a rapid cooling device;
the tension detection device for detecting the tension of the graphene growth substrate is arranged in the vacuum feeding chamber, the cooling device for cooling the graphene growth substrate is arranged in the vacuum material taking chamber, and the cooling device is located between the graphene bottom material receiving roller and the material receiving guide roller.
Further, the driving device comprises a first driving device and a second driving device; the first driving device is in transmission connection with the graphene growth substrate discharging roller; and the second driving device is in transmission connection with the graphene base material receiving roller.
Further, a rotating shaft of the graphene growth substrate discharging roller penetrates through the vacuum feeding chamber and is in transmission connection with the first driving device through a clutch; and a rotating shaft of the graphene substrate material receiving roller penetrates through the vacuum material taking chamber and is in transmission connection with the second driving device through a clutch.
Further, a vacuum dynamic sealing device is arranged between the rotating shaft of the graphene growth substrate discharging roller and the vacuum feeding chamber; and a vacuum dynamic sealing device is arranged between the rotating shaft of the graphene base material receiving roller and the vacuum material taking chamber.
Preferably, the first driving device and the second driving device both use a reduction motor.
Furthermore, the horizontal graphene roll-to-roll continuous growth equipment further comprises a processor, wherein the processor is electrically connected with the tension detection device and the first driving device respectively, and the processor, the tension detection device and the first driving device form a feedback closed loop.
Further, the processor is electrically connected with the speed detection device and the second driving device respectively, and the processor, the speed detection device and the first driving device form a feedback closed loop.
Furthermore, the rapid cooling device is detachably connected with the high-temperature process chamber.
Preferably, the uniform-flow heat insulation device comprises at least two layers of heat insulation boards and a support column, and the support column is arranged between two adjacent layers of heat insulation boards; the heat insulation board is provided with a central through hole, the heat insulation board is provided with air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards are distributed in a staggered mode.
The invention has the beneficial effects that: the horizontal graphene roll-to-roll continuous growth equipment disclosed by the invention has the following advantages:
1. the efficiency is high: the continuous roll-to-roll growth does not have the actions of frequent furnace opening sampling/lofting, vacuum pumping and the like;
2. the energy consumption is low: frequent heating/cooling processes do not exist, and energy consumption is low;
3. because the tension detection device for detecting the tension of the graphene growth substrate is arranged in the vacuum feeding chamber, the tension of the graphene growth substrate can be controlled, so that the appearance quality of a product is high, and wrinkles are avoided;
4. because the same growth process environment is experienced by the same roll of growth substrate, the quality of the graphene is stable and reliable in batches.
Drawings
Fig. 1 is a schematic structural diagram of a horizontal graphene roll-to-roll continuous growth apparatus in an embodiment of the present invention;
fig. 2 is a left side view of a horizontal graphene roll-to-roll continuous growth apparatus in an embodiment of the present invention;
fig. 3 is a right side view of the horizontal graphene roll-to-roll continuous growth apparatus in the embodiment of the present invention;
FIG. 4 is a perspective view of a uniform flow insulation apparatus in an embodiment of the present invention;
the following are marked in the figure: the method comprises the following steps of 1-a vacuum feeding chamber, 2-a graphene growth substrate discharging roller, 3-a tension detection device, 4-a rapid cooling device, 5-a rapid heating device, 6-a uniform flow heat insulation device, 7-a high-temperature process chamber, 8-a vacuum material taking chamber, 9-a graphene bottom material receiving roller, 10-a material receiving guide roller, 11-a speed detection device, 12-a first driving device, 13-a second driving device, 14-a clutch, 15-a vacuum dynamic sealing device, 16-a graphene growth substrate and 17-a mounting plate.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1 and fig. 2, the horizontal graphene roll-to-roll continuous growth apparatus of the present invention includes a vacuum feeding chamber 1, a high temperature process chamber 7, a vacuum discharging chamber 8, and a driving device; a graphene growth substrate discharging roller 2 is arranged in the vacuum feeding chamber 1, and a graphene bottom receiving roller 9 and a receiving guide roller 10 are arranged in the vacuum taking chamber 8; the vacuum feeding chamber 1 and the vacuum material taking chamber 8 are both provided with vacuum pumps; the graphene growth substrate discharging roller 2 and the graphene growth substrate receiving roller 9 are driven to rotate by a driving device; the high-temperature process chamber 7 is provided with a rapid heating device 5;
one end of the high-temperature process chamber 7 is connected and communicated with the vacuum feeding chamber 1, and the other end of the high-temperature process chamber is connected and communicated with the vacuum material taking chamber 8; the two ends of the high-temperature process chamber 7 are respectively provided with a uniform flow heat insulation device 6 and a rapid cooling device 4;
the tension detection device 3 for detecting the tension of the graphene growth substrate 16 is arranged in the vacuum feeding chamber 1, the cooling device for cooling the graphene growth substrate 16 is arranged in the vacuum material taking chamber 8, and the cooling device is located between the graphene substrate material receiving roller 9 and the material receiving guide roller 10.
The main function of the rapid heating device 5 is to heat the high-temperature process chamber 7, so that the temperature in the high-temperature process chamber 7 can reach the temperature required by the process. The rapid heating device 5 may be a resistance heater, and in order to facilitate maintenance of the high-temperature process chamber 7, a preferred mode is specifically that the rapid heating device 5 is a heating furnace which can be opened and closed, and at least two temperature zones are controlled.
The main function of the rapid cooling device 4 is to realize rapid cooling of the graphene growth substrate 16, specifically, the rapid cooling device 4 may adopt a cold water jacket, the rapid cooling device 4 includes an outer water jacket and an inner water jacket flange, the outer water jacket is sleeved on the high-temperature process chamber 7, and the inner water jacket flange is arranged at the connection between the high-temperature process chamber 7 and the vacuum feeding chamber 1 and the vacuum material taking chamber 8.
The high-temperature process chamber 7 is arranged between the vacuum feeding chamber 1 and the vacuum material taking chamber 8; the vacuum feeding chamber 1 is positioned at the lower end of the high-temperature process chamber 7, and the vacuum material taking chamber 8 is arranged at the upper end of the high-temperature process chamber 7; and the two ends of the high-temperature process chamber 7 are provided with the rapid cooling devices 4. Specifically, the rapid cooling device 4 at the joint of the vacuum feeding chamber 1, the vacuum material taking chamber 8 and the high-temperature process chamber 7 is connected by a flange with a water cooling device. In particular, the high-temperature process chamber 7 generally adopts a quartz tube.
In the process of use:
firstly, pretreating a metal foil, then loading the sample in a vacuum loading chamber 1 and a vacuum material taking chamber 8, and vacuumizing through vacuum pumps on the vacuum loading chamber 1 and the vacuum material taking chamber 8 after the sample loading is finished; then heating by a rapid heating device 5 on the high-temperature process chamber 7, and simultaneously introducing a protective gas and a process gas until the temperature in the high-temperature process chamber 7 is raised to about 1000 ℃; starting a graphene base material receiving roller 9 to roll up a graphene growth base 16; because all be provided with quick cooling device 4 at high temperature process chamber 7 both ends, thereby can guarantee that graphite alkene growth substrate 16 high temperature process chamber 7 reduces to 8 temperature in vacuum material taking chamber, then through the cooling device in the vacuum material taking chamber 8 for sample after 16 to the normal atmospheric temperature of graphite alkene growth substrate.
In conclusion, the horizontal graphene roll-to-roll continuous growth equipment disclosed by the invention has the advantages that the roll-to-roll continuous growth can be realized due to the fact that frequent furnace opening sampling/lofting, vacuumizing and other actions are not required in the production process, and the production efficiency is high; and meanwhile, frequent heating/cooling processes do not exist, so that the energy consumption is low. Secondly, as the tension detection device 3 for detecting the tension of the graphene growth substrate is arranged in the vacuum feeding chamber 1, the tension of the graphene growth substrate can be controlled, so that the appearance quality of a product is high, and wrinkles are avoided; and because the growth process environment experienced by the same roll of growth substrate is the same, the quality of the graphene is stable and reliable in batches. Thirdly, due to the cooling device in the vacuum material taking chamber 8, the temperature of the graphene growth substrate 16 can be guaranteed to be normal temperature when the graphene growth substrate is curled onto the graphene substrate receiving roller 9.
In order to improve the heat insulation effect and enable the gas to be uniformly distributed in the high-temperature process chamber, it is preferable that the uniform flow heat insulation device 6 comprises at least two layers of heat insulation boards 61 and a supporting column 62, and the supporting column 62 is arranged between two adjacent layers of heat insulation boards 61, as shown in fig. 4; the heat insulation board 61 is provided with a central through hole 63 and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards 61 are distributed in a staggered mode. Specifically, the thermal insulation plate can be made of different materials such as quartz, ceramics, molybdenum, stainless steel, copper and the like, and the quartz thermal insulation plate is preferred in the invention.
Furthermore, in order to facilitate the introduction of the process gas into the high-temperature process chamber 7, at least two process gas connectors are arranged in the high-temperature process chamber 7, and a flow meter is arranged on an introduction pipeline of the external process gas for monitoring.
In order to facilitate detection of the growth environment of the graphene growth substrate, further, a pressure detection device and a temperature detection device are arranged in the high-temperature process chamber 7.
The driving device is mainly used for driving the graphene growth substrate discharging roller 2 and the graphene growth substrate receiving roller 9 to rotate; in order to facilitate the independent control of the rotation speed of the graphene growth substrate discharging roller 2 and the graphene substrate receiving roller 9, further, the driving device comprises a first driving device 12 and a second driving device 13; the first driving device 12 is in transmission connection with the graphene growth substrate discharging roller 2; and the second driving device 13 is in transmission connection with the graphene base material receiving roller 9.
In order to facilitate the rapid loading and unloading of the substrate or the coiled material without driving or stopping the driving device, further, the graphene growth substrate discharging roller 2 has a rotating shaft which penetrates through the vacuum loading chamber 1 and is in transmission connection with the first driving device 12 through a clutch 14; the graphene-based bottom material receiving roller 9 has a rotating shaft which passes through the vacuum material taking chamber 8 and is in transmission connection with a second driving device 13 through a clutch 14.
In order to avoid air leakage between the rotating shaft of the graphene growth substrate discharging roller 2 and the vacuum feeding chamber 1 and between the rotating shaft of the graphene substrate receiving roller 9 and the vacuum taking chamber 8, a vacuum dynamic sealing device 15 is further arranged between the rotating shaft of the graphene growth substrate discharging roller 2 and the vacuum feeding chamber 1; and a vacuum dynamic sealing device 15 is arranged between the rotating shaft of the graphene-based bottom receiving roller 9 and the vacuum material taking chamber 8.
In order to facilitate the control of the rotation speed of the graphene growth substrate discharging roller 2 and the graphene bottom receiving roller 9, preferably, the first driving device 12 and the second driving device 13 both adopt a servo motor and a reducer; preferably, the clutch 14 is a magnetic particle clutch.
In order to facilitate the guiding of the graphene growth substrate 16, a discharging guide rod 4 is further arranged in the vacuum feeding chamber 1; the graphene growth substrate 16 on the graphene growth substrate discharging roller 2 sequentially bypasses the tension detection device 3 and the discharging guide rod 4 and enters the high-temperature process chamber 7.
In order to realize the automatic detection of the tension of the graphene growth substrate 16 and realize the automatic control of the tension through the rotating speed of the graphene growth substrate discharging roller 2, the horizontal type graphene roll-to-roll continuous growth equipment further comprises a processor, wherein the processor is electrically connected with the tension detection device 3 and the first driving device respectively, and the processor, the tension detection device 3 and the first driving device 12 form a feedback closed loop. The data obtained by the tension detection device 3 is fed back to the processor, the processor can adopt a CPU or a single chip microcomputer, and then the rotation speed of the first driving device 12 is controlled by the processor, so that the automatic adjustment of the tension is realized.
In order to realize the automatic adjustment of the rotation speed of the graphene-based bottom material receiving roller 9, further, the processor is electrically connected with the speed detection device 11 and the second driving device 13, and the processor, the speed detection device 11 and the first driving device 12 form a feedback closed loop.
In order to facilitate the maintenance and replacement of the high-temperature process chamber 7, further, the rapid cooling device 4 is detachably connected with the high-temperature process chamber 7.
Claims (8)
1. The horizontal graphene roll-to-roll continuous growth equipment comprises a vacuum feeding chamber (1), a high-temperature process chamber (7), a vacuum material taking chamber (8) and a driving device; a graphene growth substrate discharging roller (2) is arranged in the vacuum feeding chamber (1), and a graphene substrate receiving roller (9) and a receiving guide roller (10) are arranged in the vacuum taking chamber (8); the vacuum feeding chamber (1) and the vacuum material taking chamber (8) are both provided with vacuum pumps; the graphene growth substrate discharging roller (2) and the graphene substrate receiving roller (9) are driven to rotate by a driving device; a rapid heating device (5) is arranged on the high-temperature process chamber (7);
the method is characterized in that: one end of the high-temperature process chamber (7) is connected and communicated with the vacuum feeding chamber (1), and the other end of the high-temperature process chamber is connected and communicated with the vacuum material taking chamber (8); both ends of the high-temperature process chamber (7) are provided with a uniform flow heat insulation device (6) and a rapid cooling device (4);
a tension detection device (3) for detecting the tension of the graphene growth substrate (16) is arranged in the vacuum feeding chamber (1), a cooling device for cooling the graphene growth substrate (16) is arranged in the vacuum taking chamber (8), and the cooling device is positioned between the graphene substrate receiving roller (9) and the receiving guide roller (10);
the uniform-flow heat insulation device (6) comprises at least two layers of heat insulation boards (61) and a supporting column (62), wherein the supporting column (62) is arranged between two adjacent layers of heat insulation boards (61); the heat insulation plate (61) is provided with a central through hole (63), the heat insulation plate (61) is provided with air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation plates (61) are distributed in a staggered mode.
2. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 1, wherein: the drive means comprise a first drive means (12) and a second drive means (13); the first driving device (12) is in transmission connection with the graphene growth substrate discharging roller (2); and the second driving device (13) is in transmission connection with the graphene base material receiving roller (9).
3. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 2, wherein: the graphene growth substrate discharging roller (2) is provided with a rotating shaft which penetrates through the vacuum feeding chamber (1) and is in transmission connection with the first driving device (12) through a clutch (14); the graphene-based bottom material receiving roller (9) is provided with a rotating shaft which penetrates through the vacuum material taking chamber (8) and is in transmission connection with a second driving device (13) through a clutch (14).
4. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 3, wherein: a vacuum dynamic sealing device (15) is arranged between the rotating shaft of the graphene growth substrate discharging roller (2) and the vacuum feeding chamber (1); and a vacuum dynamic sealing device (15) is arranged between the rotating shaft of the graphene base receiving roller (9) and the vacuum material taking chamber (8).
5. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 2, 3 or 4, wherein: the first driving device (12) and the second driving device (13) both adopt speed reducing motors.
6. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 5, wherein: the tension detection device is characterized by further comprising a processor, wherein the processor is electrically connected with the tension detection device (3) and the first driving device respectively, and the processor, the tension detection device (3) and the first driving device (12) form a feedback closed loop.
7. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 6, wherein: the processor is electrically connected with the speed detection device (11) and the second driving device (13) respectively, and the processor, the speed detection device (11) and the second driving device (13) form a feedback closed loop.
8. The horizontal graphene roll-to-roll continuous growth apparatus according to claim 1, wherein: the rapid cooling device (4) is detachably connected with the high-temperature process chamber (7).
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