An automated apparatus for mechanical exfoliation of graphene and methods of use thereof

Abstract

The application discloses an automatic device for graphene mechanical stripping and a use method thereof, and belongs to the technical field of graphene mechanical stripping. The base is provided with the object table device, the right side of the object table device is provided with the slide glass cleaning device, the rear side of the object table device is provided with the adhesive tape transmission device, the pressing device and the monitoring device, the left side of the object table device is provided with the observation device, and the front side of the object table device is provided with the slide glass transfer device; and the heating device is arranged below the object table device. The automatic device for graphene mechanical stripping can strip graphene through multiple automatic stripping until single-layer graphene crystals are observed under a microscope.

Description

Technical Field

[0001] This invention relates to the field of graphene production equipment technology, and in particular to an automated device for mechanically exfoliating graphene and its method of use. Background Technology

[0002] Since the discovery of graphene, it has become a research hotspot in the fields of materials science and nanotechnology due to its unique physical, chemical and mechanical properties. Among them, research on monolayer graphene is particularly popular. After monolayer graphene was produced by foreign scholars using the mechanical exfoliation method, more and more people have devoted themselves to the development of preparation schemes for monolayer graphene.

[0003] Several methods are known for preparing monolayer graphene, including mechanical exfoliation, chemical vapor deposition, silicon substrate exfoliation, liquid phase exfoliation, and thermal reduction. Among these, mechanical exfoliation can produce high-quality monolayer graphene, but its efficiency is relatively low. Summary of the Invention

[0004] In order to overcome the above-mentioned defects and deficiencies in the prior art, the present invention provides an automated device for mechanical exfoliation of graphene.

[0005] To address the aforementioned technical problems, this invention provides an automated device for the mechanical exfoliation of graphene, comprising a stage, a belt drive, a slide cleaning device, a monitoring device, a pressing device, a heating device, an observation device, and a slide transfer device. The stage is mounted on a base; the slide cleaning device is located on the right side of the stage; the belt drive, monitoring device, and pressing device are located at the rear of the stage; the observation device is located on the left side of the stage; and the slide transfer device is located at the front of the stage. A heating device is located below the stage.

[0006] The belt drive device includes a belt unwinding device, a belt guiding device, a belt take-up device, and a belt roller assembly. The belt unwinding device includes two first straight bars, a first rotary motor, a first rotary motor connector, and a first roller. The two first straight bars are disposed on the upper surface of the base. The first rotary motor is connected to the two first straight bars through the first rotary motor connector. The first rotary motor is provided with a first roller, on which multiple layers of belt are disposed. One end of the multiple layers of belt is connected to the belt unwinding device, and the other end of each layer of belt passes through the belt guiding device and one or more rollers in the belt roller assembly before being connected to the belt take-up device.

[0007] Furthermore, the tape guiding device includes a first drive source, a guide bracket, a first linear moving slide, and guide wheels. The first drive source is provided at the top of the guide bracket, the first linear moving slide is slidably provided on the guide bracket, the first linear moving slide is provided with guide wheels, and the first drive source drives the first linear moving slide to move up and down.

[0008] Furthermore, the tape winding device includes a second drive source, a tape winding bracket, a second linear moving slide, a second rotary motor, and a second roller. The top of the tape winding bracket is provided with the second drive source, and the second linear moving slide is slidably provided on the tape winding bracket. The second drive source drives the second linear moving slide to move up and down. The second linear moving slide is provided with a second rotary motor and a second roller, and the second rotary motor drives the second roller to rotate.

[0009] Furthermore, the tape roller assembly includes two second straight bars, four rollers, and roller connectors. One roller is mounted on the second straight bar near the stage device via the roller connectors, and the three rollers arranged from top to bottom are mounted on the second straight bar away from the stage device via the roller connectors.

[0010] Furthermore, the platform device includes a lifting platform, a rotating disk shaft, a third rotating motor, a pad, a rotating disk, disk feet, and fixing plates. The lifting platform is fixedly connected to the rotating disk shaft, the rotating disk shaft is connected to the third rotating motor, the third rotating motor is connected to the pad, the pad is connected to the rotating disk, the rotating disk is connected to four disk feet, and two fixing plates are provided on the upper surface of the disk feet.

[0011] Furthermore, the pressing device includes a third drive source, two slide rods, a pressing connector, and a pressing component. The third drive source is connected to the two slide rods via the pressing connector. The third drive source is connected to the pressing component, and the third drive source drives the pressing component to move up and down.

[0012] Furthermore, the monitoring device includes a camera, a monitoring bracket, and two third rods, with the camera connected to the two third rods via the monitoring bracket; the observation device includes a microscope, a CCD camera, and a microscope bracket, with the microscope mounted on the microscope bracket and the CCD camera mounted on the microscope.

[0013] Furthermore, the slide cleaning device includes a cleaning device support and an ultrasonic cleaner, with the ultrasonic cleaner mounted on the cleaning device support.

[0014] Furthermore, the slide transfer device is provided in two sets, including a robot arm base and two robot arms. The robot arm base is provided on the base, and the robot arm base is provided with two robot arms. The robot arms rotate relative to the robot arm base.

[0015] A method of using an automated device for mechanical exfoliation of graphene includes the following steps:

[0016] Step 1: The slide cleaning device cleans the slides. The slide transfer device transfers the cleaned slides from the slide cleaning device to the stage device. The fixing plate of the stage device fixes the slides. The prepared graphene crystals are placed on the clean slides. The stage device is then rotated 90° counterclockwise.

[0017] Step 2: Control the belt drive device to drive the belt for a certain length so that the multi-layered belt stops above the glass slide carrying the graphene crystals.

[0018] Step 3: Control the pressing device to lower the multi-layer tape into the monitoring range of the monitoring device. The monitoring device monitors whether the pressed multi-layer tape is in a flat and stacked state. If so, control the pressing device to continue lowering, pressing the multi-layer tape onto the glass slide with graphene for 5-10 seconds to allow the tape to better adhere to the graphene crystals. If not, control the tape winding device and tape guiding device to move the tape to adjust the multi-layer tape to a flat and stacked state.

[0019] Step 4: After the pressing process is complete, release the pressing device. At this time, a thin layer of graphene crystals will be attached to the tape.

[0020] Step 5: Control the stage to rotate 90° counterclockwise so that a new, clean glass slide is rotated under the tape with a thin layer of graphene attached.

[0021] Step 6: Activate the pressing device to hold down the tape; activate the heating device to heat the glass slide, causing the thin graphene layer to detach from the tape; after the thin graphene layer has detached from the tape, release the pressing device.

[0022] Step 7: Rotate the stage device counterclockwise by 90° so that the slide carrying the thin layer of graphene is positioned below the microscope lens.

[0023] Step 8: Observe the structure of graphene on the glass slide using the observation device. If a single layer of graphene is obtained, remove the glass slide. If it is not a single layer of graphene, rotate the glass slide 90° clockwise to below the tape and repeat steps 2 to 8 until a single layer of graphene structure is obtained.

[0024] The beneficial technical effects achieved by this invention are as follows: The tape conveyor device enables automatic tape feeding and winding, which is faster and more convenient than manual operation, while avoiding human-caused contamination of the graphene material. This invention innovatively uses a three-layer tape stack to peel off graphene, allowing for better tape adsorption of the graphene. The multiple layers of tape provide a buffering effect, and a monitoring device monitors the tape's state, preventing unpredictable damage to the graphene crystals during mechanical pressing, thus ensuring better integrity of the peeled thin layer of graphene. The rotating stage device allows for rapid alternation of slides and quick correction of slide height. The integrated CCD high-magnification microscope enables real-time imaging and manual observation of the graphene crystals. The heating device allows for rapid detachment of the graphene from the tape. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of an automated device for the mechanical exfoliation of graphene.

[0026] Figure 2 This is a schematic diagram of the belt drive device.

[0027] Figure 3 This is a schematic diagram of the stage device.

[0028] Figure 4 A schematic diagram of the monitoring device, pressing device, and observation device;

[0029] Figure 5 This is a schematic diagram of the slide cleaning device and the slide transfer device. Detailed Implementation

[0030] The present invention will be further described below with reference to specific embodiments. These embodiments are only used to more clearly illustrate the technical solutions of the present invention and should not be construed as limiting the scope of protection of the present invention.

[0031] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0032] like Figure 1-5As shown, an automated device for mechanically exfoliating graphene includes a stage device 1, a belt drive device, a slide cleaning device 2, a monitoring device 3, a pressing device 4, a heating device 5, an observation device 6, and a slide transfer device 7. The stage device 1 is mounted on a base. The slide cleaning device 2 is located to the right of the stage device 1. The belt drive device, monitoring device 3, and pressing device 4 are located to the rear of the stage device. The heating device 5 is located below the stage device. The observation device 6 is located to the left of the stage device, and the slide transfer device 7 is located to the front of the stage device. The stage device 1, belt drive device, slide cleaning device 2, monitoring device 3, pressing device 4, heating device 5, observation device 6, and slide transfer device 7 are all connected to a computer 8. The computer 8 contains software that controls each device to operate as needed. The heating device 5 heats the slides, enabling rapid detachment of the graphene from the belt. The heating temperature is 70~80 degrees Celsius, and can be changed according to specific requirements; the heating time is 10~20 seconds, and can be changed according to specific requirements.

[0033] The tape drive device includes a tape unwinding device 9, a tape guiding device 10, a tape take-up device 11, and a tape roller assembly 12. The tape unwinding device 9 includes two first straight rods 91, a first rotary motor 92, a first rotary motor connector, and a first roller 93. The two first straight rods 91 are disposed on the upper surface of the base. The first rotary motor 92 is connected to the two first straight rods 91 through the first rotary motor connector. The first roller 93 is provided on the first rotary motor 92. The first roller 93 is provided with multiple layers of tape. The first rotary motor 92 drives the first roller 93 to rotate, which can unwind multiple layers of tape. One end of the multiple layers of tape is connected to the tape unwinding device. The other end of each layer of tape in the multiple layers of tape is connected to the tape take-up device after passing through the tape guiding device and one or more rollers in the tape roller assembly. Multi-layer tape can be set to three layers. Using three layers of tape to peel off graphene allows the graphene to be better absorbed by the tape. The multi-layer tape also provides a buffering effect, preventing unpredictable damage to the graphene crystals during mechanical pressing, thus ensuring better integrity of the peeled thin layer of graphene.

[0034] The tape guiding device 10 includes a first drive source 101, a guide bracket 102, a first linear moving slide 103, and guide wheels 104. The first drive source 101 is located at the top of the guide bracket 102, and the first linear moving slide 103 is slidably mounted on the guide bracket 102. The first linear moving slide 103 is equipped with guide wheels 104, and the first drive source 101 drives the first linear moving slide 103 to move up and down. The first drive source can be a hydraulic cylinder or a pneumatic cylinder, etc. The guide wheels move up and down with the first linear moving slide 103 to adjust the position of the tape, thereby facilitating better flat overlapping of multiple layers of tape and preventing unevenness between the multiple layers of tape, which would affect the quality of the thin-layer graphene.

[0035] The tape winding device 11 includes a second drive source 111, a tape winding bracket 112, a second linear moving slide 113, a second rotary motor 114, and a second roller 115. The second drive source 111 is located at the top of the tape winding bracket 112. The second linear moving slide 113 slides slidably on the tape winding bracket 112. The second drive source 111 drives the second linear moving slide 113 to move up and down. The second linear moving slide 113 is equipped with the second rotary motor 114 and the second roller 115. The second rotary motor 114 drives the second roller 115 to rotate. The second roller 115 is used to wind up multi-layer tape. The second roller 115 can move up and down with the second linear moving slide 113, facilitating better flattening and overlapping of the multi-layer tape to prevent unevenness between the tape layers, which would affect the quality of the thin-layer graphene. The second drive source can be a hydraulic cylinder or a pneumatic cylinder, etc.

[0036] The tape roller assembly 12 includes two second straight bars 121, four rollers 122, and roller connectors 123. One roller 122 is mounted on the second straight bar 121 near the platform device via the roller connectors 123, and the three rollers 122 arranged from top to bottom are mounted on the second straight bar 121 away from the platform device via the roller connectors 123.

[0037] One end of the multi-layer tape is connected to the first roller 93. After passing through the tape guide device, the multi-layer tape separates and winds sequentially onto the rollers of the tape guide device, ensuring that the three layers overlap during pressing. For example, with three layers of tape, the top layer passes through the tape guide device, then winds upwards from the bottom end of the top roller of the second straight bar 121 on the side away from the platform device, and connects to the tape winding device. The middle layer passes through the tape guide device and then winds sequentially from the bottom end of the middle roller and the right end of the top roller of the second straight bar 121 on the side away from the platform device, and connects to the tape winding device. The bottom layer passes through the tape guide device and then winds sequentially from the bottom ends of the two parallel rollers at the lowest position of the two second straight bars, then winds upwards to the right ends of the two top rollers of the second straight bar 121 on the side away from the platform device, and connects to the tape winding device.

[0038] The stage device 1 includes a lifting platform 1001, a rotating disk shaft, a third rotary motor 1002, a pad 1003, a rotating disk 1004, disk feet 1005, and fixing plates 1006. The lifting platform 1001 is fixedly connected to the rotating disk shaft and provides lifting functionality. The rotating disk shaft is connected to the third rotary motor 1002, which is connected to the pad 1003, driving the pad 1003 to rotate. The pad 1003 is connected to the rotating disk 1004, which is connected to four disk feet 1005, for example, using screws. Two fixing plates 1006 are provided on the upper surface of each disk foot 1005. The two fixing plates can slide along the grooves on the upper surface of the disk feet to adjust their position. A computer 8 controls the stage device 1 to lift, rotate, etc., enabling rapid alternation of slides and rapid correction of slide height.

[0039] The pressing device 4 includes a third drive source 41, two slide rods 42, a pressing connector 43, and a pressing component 44. The third drive source 41 is connected to the two slide rods 42 via the pressing connector 43. The third drive source 41 is connected to the pressing component 44, and the third drive source 41 drives the pressing component 44 to move up and down. The pressing device 4 is connected to a computer 8, which controls the pressing device to perform pressing and lifting movements. The pressing device also has a temperature sensor that detects the temperature of the glass slide below the pressing device.

[0040] The monitoring device 3 includes a camera 31, a monitoring bracket 32, and two third straight rods 33. The camera 31 is connected to the two third straight rods 33 via the monitoring bracket 32. The camera 31 is connected to a computer 8. When the pressing device lowers the tape into the monitoring range of the monitoring device 3, the monitoring device monitors whether the pressed multi-layer tape is in a flat and stacked state. If so, it controls the pressing device to continue lowering, pressing the multi-layer tape onto the glass slide with graphene for 5-10 seconds to allow the tape to better adhere to the graphene crystals. If not, it controls the tape winding device and tape guiding device to move the tape to adjust it to a flat and stacked state. To determine whether the multi-layer tape is in a flat and stacked state, image processing and other technologies can be used for comparison. For example, reference images of unevenly stacked tape, such as wrinkled tape, can be pre-stored in the computer, and the images captured by the camera can be compared with the reference images using computer software.

[0041] The observation device 6 includes a microscope 61, a CCD camera 62, and a microscope support 63. The microscope 61 is mounted on the microscope support 63, and the CCD camera 62 is mounted on the microscope 61. The single-layer graphene structure can be observed through the microscope or transmitted to a computer for observation via the CCD camera. The observation device 6 enables real-time imaging and manual observation of graphene crystals.

[0042] The slide cleaning device 2 includes a cleaning device support 21 and an ultrasonic cleaner 22, with the ultrasonic cleaner 22 mounted on the cleaning device support 21. The slide cleaning device provides clean slides and enables rapid cleaning of slides, thereby increasing work efficiency.

[0043] The slide transfer device 7 has two sets, each including a robotic arm base 71 and two robotic arms 72. The robotic arm base 71 is mounted on the base, and the two robotic arms 72 are mounted on the robotic arm base 71. The robotic arms 72 rotate relative to the robotic arm base. The slide transfer device can automatically load slides and automatically transfer them to an ultrasonic cleaner for cleaning.

[0044] A method of using an automated device for mechanical exfoliation of graphene includes the following steps:

[0045] Step 1: The slide cleaning device cleans the slides. The slide transfer device transfers the cleaned slides from the slide cleaning device to the stage device. The fixing plate of the stage device fixes the slides. The prepared graphene crystals are placed on the clean slides. The stage device is then rotated 90° counterclockwise.

[0046] Step 2: Control the belt drive device to drive the belt for a certain length so that the multi-layered belt stops above the glass slide carrying the graphene crystals.

[0047] Step 3: Control the pressing device to lower the multi-layer tape into the monitoring range of the monitoring device. The monitoring device monitors whether the pressed multi-layer tape is in a flat and stacked state. If so, control the pressing device to continue lowering, pressing the multi-layer tape onto the glass slide with graphene for 5-10 seconds to allow the tape to better adhere to the graphene crystals. If not, control the tape winding device and tape guiding device to move the tape to adjust the multi-layer tape to a flat and stacked state.

[0048] Step 4: After the pressing process is complete, release the pressing device. At this time, a thin layer of graphene crystals will be attached to the tape.

[0049] Step 5: Control the stage to rotate 90° counterclockwise so that a new, clean glass slide is rotated under the tape with a thin layer of graphene attached.

[0050] Step 6: Activate the pressing device to hold down the tape; activate the heating device to heat the glass slide, causing the thin graphene layer to detach from the tape; after the thin graphene layer has detached from the tape, release the pressing device.

[0051] Step 7: Rotate the stage device counterclockwise by 90° so that the slide carrying the thin layer of graphene is positioned below the microscope lens.

[0052] Step 8: Observe the structure of graphene on the glass slide using the observation device. If a single layer of graphene is obtained, remove the glass slide. If it is not a single layer of graphene, rotate the glass slide 90° clockwise to below the tape and repeat steps 2 to 8 until a single layer of graphene structure is obtained.

[0053] The present invention has been disclosed above with reference to preferred embodiments, but it is not intended to limit the present invention. All technical solutions obtained by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the present invention.

Claims

1. An automated device for mechanically exfoliating graphene, comprising a stage, a belt drive, a slide cleaning device, a monitoring device, a pressing device, a heating device, an observation device, and a slide transfer device; the stage is mounted on a base, the slide cleaning device is located on the right side of the stage, the belt drive, monitoring device, and pressing device are located at the rear of the stage, the observation device is located on the left side of the stage, and the slide transfer device is located at the front of the stage; characterized in that… A heating device is installed below the stage assembly; The belt drive device includes a belt unwinding device, a belt guiding device, a belt winding device, and a belt roller assembly. The belt unwinding device includes two first straight bars, a first rotary motor, a first rotary motor connector, and a first roller. The two first straight bars are disposed on the upper surface of the base. The first rotary motor is connected to the two first straight bars through the first rotary motor connector. The first rotary motor is provided with a first roller, and the first roller is provided with multiple layers of belt. One end of the multiple layers of belt is connected to the belt unwinding device, and the other end of each layer of belt passes through the belt guiding device and one or more rollers in the belt roller assembly before being connected to the belt winding device. The tape guiding device includes a first drive source, a guide bracket, a first linear moving slide, and guide wheels. The first drive source is provided at the top of the guide bracket, the first linear moving slide is slidably provided on the guide bracket, the first linear moving slide is provided with guide wheels, and the first drive source drives the first linear moving slide to move up and down. The tape winding device includes a second drive source, a tape winding bracket, a second linear moving slide, a second rotary motor, and a second roller. The top of the tape winding bracket is provided with a second drive source, and the second linear moving slide is slidably provided on the tape winding bracket. The second drive source drives the second linear moving slide to move up and down. The second linear moving slide is provided with a second rotary motor and a second roller, and the second rotary motor drives the second roller to rotate. The tape roller assembly includes two second straight bars, four rollers, and roller connectors. One roller is mounted on the second straight bar near the stage device via the roller connectors, and the three rollers arranged from top to bottom are mounted on the second straight bar away from the stage device via the roller connectors.

2. The automated device for mechanical exfoliation of graphene according to claim 1, characterized in that, The platform device includes a lifting platform, a rotating shaft of a disc, a third rotating motor, a pad, a rotating disc, disc feet, and fixing plates. The lifting platform is fixedly connected to the rotating shaft of the disc, the rotating shaft of the disc is connected to the third rotating motor, the third rotating motor is connected to the pad, the pad is connected to the rotating disc, the rotating disc is connected to four disc feet, and two fixing plates are provided on the upper surface of the disc feet.

3. The automated device for mechanical exfoliation of graphene according to claim 1, characterized in that, The pressing device includes a third drive source, two slide rods, a pressing connector, and a pressing component. The third drive source is connected to the two slide rods through the pressing connector. The third drive source is connected to the pressing component and drives the pressing component to move up and down.

4. The automated device for mechanical exfoliation of graphene according to claim 1, characterized in that, The monitoring device includes a camera, a monitoring bracket, and two third rods. The camera is connected to the two third rods via the monitoring bracket. The observation device includes a microscope, a CCD camera, and a microscope bracket. The microscope is mounted on the microscope bracket, and the CCD camera is mounted on the microscope.

5. The automated device for mechanical exfoliation of graphene according to claim 1, characterized in that, The slide cleaning device includes a cleaning device bracket and an ultrasonic cleaner, with the ultrasonic cleaner mounted on the cleaning device bracket.

6. The automated device for mechanical exfoliation of graphene according to claim 1, characterized in that, The slide transfer device is provided in two sets. The slide transfer device includes a robot arm base and two robot arms. The robot arm base is provided on the base, and the robot arm base is provided with two robot arms. The robot arms rotate relative to the robot arm base.

7. A method of using an automated device for mechanical exfoliation of graphene as described in any one of claims 1-6, characterized in that, Includes the following steps: Step 1: The slide cleaning device cleans the slides. The slide transfer device transfers the cleaned slides from the slide cleaning device to the stage device. The fixing plate of the stage device fixes the slides. The prepared graphene crystals are placed on the clean slides. The stage device is controlled to rotate 90° counterclockwise. Step 2: Control the belt drive device to drive the belt for a certain length so that the multi-layered belt stops above the glass slide carrying the graphene crystals. Step 3: Control the pressing device to lower the multi-layer tape into the monitoring range of the monitoring device. The monitoring device monitors whether the pressed multi-layer tape is in a flat and stacked state. If so, control the pressing device to continue lowering, pressing the multi-layer tape onto the glass slide with graphene for 5-10 seconds to allow the tape to better adhere to the graphene crystals. If not, control the tape winding device and tape guiding device to move the tape to adjust the multi-layer tape to a flat and stacked state. Step 4: After the pressing process is complete, release the pressing device. At this time, a thin layer of graphene crystals will be attached to the tape. Step 5: Control the stage to rotate 90° counterclockwise so that a new, clean glass slide is rotated under the tape with a thin layer of graphene attached. Step 6: Activate the pressing device to press down the tape; The heating device is activated to heat the glass slide, causing the thin graphene layer to detach from the tape; after the thin graphene layer has detached from the tape, the pressing device is released. Step 7: Rotate the stage device counterclockwise by 90° so that the slide carrying the thin layer of graphene is positioned below the microscope lens. Step 8: Observe the structure of graphene on the glass slide using the observation device. If a single layer of graphene is obtained, remove the glass slide. If it is not a single layer of graphene, rotate the glass slide 90° clockwise to below the tape and repeat steps 2 to 8 until a single layer of graphene structure is obtained.

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