CN110357085B - Graphene surface plasma modification treatment device and treatment method - Google Patents
Graphene surface plasma modification treatment device and treatment method Download PDFInfo
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- CN110357085B CN110357085B CN201910753605.0A CN201910753605A CN110357085B CN 110357085 B CN110357085 B CN 110357085B CN 201910753605 A CN201910753605 A CN 201910753605A CN 110357085 B CN110357085 B CN 110357085B
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The invention provides a graphene surface plasma modification treatment device and method, belongs to the technical field of graphene surface modification, and particularly relates to a graphene surface plasma modification treatment device and method. The method solves the problems that the existing method for processing graphene by ultrasonic wave, heating or air flow and the like has low yield, serious sheet agglomeration, a large number of structural defects of the graphene caused by long-time ultrasonic and more surfactants or surface activators need to be introduced, and the existing plasma processing method can only act on the surface layer accumulated by the graphene. The device comprises a vacuum chamber, a glass container, a radio frequency power supply system, a counter electrode and a rotating mechanism, wherein the vacuum chamber is of a horizontal structure, the counter electrode is of an arc-shaped structure, the cylindrical glass container is placed in the middle of the counter electrode, and the glass container is connected with the rotating mechanism. The method is mainly used for graphene surface modification treatment.
Description
Technical Field
The invention belongs to the technical field of graphene surface modification, and particularly relates to a graphene surface plasma modification treatment device and method.
Background
The plasma technology is commonly used for material surface modification, graphene is widely applied to various fields, graphene without a surfactant is always a desire of material scientists to find in an aqueous solution, however, due to the hydrophobicity of the surface of the graphene, the graphene is difficult to uniformly disperse in water and easy to agglomerate, application development of the graphene is limited, the graphene solution is obtained mainly under the action of ultrasonic waves, heating or air flows at present, but the preparation methods have the defects that the yield is low, the sheet agglomeration is serious, a large number of structural defects of the graphene are caused by long-time ultrasonic waves, more surfactants or surface activators need to be introduced, and the like, so that the preparation methods are greatly restricted. At present, related researches on graphene surface plasma modification also exist, but generally, a tiled stacking mode is adopted for graphene, plasma can only act on a stacked surface layer of the graphene, the graphene in the plasma cannot be modified, and a device and a processing method capable of realizing industrial production are urgently needed in the market. The plasma modification device and the plasma modification method for improving the surface hydrophilicity of the graphene are beneficial to realizing the modification treatment and application of the surface of the graphene.
Disclosure of Invention
The invention provides a graphene surface plasma modification treatment device and a graphene surface plasma modification treatment method, which aim to solve the problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: the utility model provides a graphite alkene surface plasma modified treatment device, it includes real empty room, glass container, radio frequency power supply system, counter electrode and rotary mechanism, real empty room is horizontal structure, gas charging hole and aspirating hole have been seted up on the real empty room, the counter electrode links to each other with radio frequency power supply system, the counter electrode is convex structure, and inboard circular arc part is the discharge layer, and the middle part is the insulating layer, and outside circular arc part is the shielding layer, place cylindrical glass container in the middle of the counter electrode, the counter electrode passes through the polytetrafluoroethylene piece to be fixed on the real empty room inner wall to coaxial with glass container center, glass container links to each other with rotary mechanism, glass container one end is provided with the through-hole.
Furthermore, a shielding type observation window is arranged on the vacuum chamber, the vacuum chamber comprises a vacuum chamber body and a vacuum chamber end socket, and the vacuum chamber body and the vacuum chamber end socket are detachably connected. The vacuum chamber is of a horizontal rectangular structure, the length of the vacuum chamber is 1500mm, the width of the vacuum chamber is 1200mm, and the height of the vacuum chamber is 1000 mm.
Furthermore, the glass container comprises a container body and a container sealing head, wherein the container body is detachably connected with the container sealing head. The glass container has a length of 1000mm, an inner diameter of 600mm and a thickness of 5 mm.
Furthermore, the inflation hole is connected with a ventilation control system, and the exhaust hole is connected with an exhaust control system.
Furthermore, the rotating mechanism comprises a rotating shaft and an active motor, wherein the output end of the active motor is connected with the rotating shaft, and the rotating shaft is connected with the glass container.
Furthermore, the maximum power of the radio frequency power supply system is 1000W, and the frequency is 13.56 MHz.
Furthermore, the discharge layer is made of 304 stainless steel, the insulating layer is made of polytetrafluoroethylene, and the shielding layer is made of 304 stainless steel.
Furthermore, the thickness of the discharge layer is 3mm, the thickness of the insulating layer is 50mm, and the thickness of the shielding layer is 3 mm.
The invention also provides a graphene surface plasma modification treatment method, which comprises the following steps:
the method comprises the following steps: loading graphene to be treated into a glass container, closing a container end socket and a vacuum chamber end socket, starting an air suction control system, and keeping the background vacuum degree of the vacuum chamber at 0.01-1 Pa;
step two: opening a ventilation control system, filling mixed gas into the vacuum chamber, maintaining the air extraction and inflation states of the vacuum chamber, keeping the working vacuum degree in the vacuum chamber stable at 10-20 Pa, and starting a radio frequency power supply system to enable a glow discharge area to be bound in the glass container;
step three: starting a driving motor, rotating the glass container through transmission of a rotating shaft, and driving graphene placed in the glass container to continuously roll in a glow discharge area, wherein the processing time is 2-5min, and the discharge radio frequency power is 80-120W;
step four: and after the treatment is finished, closing the radio frequency power supply system, the ventilation control system and the air extraction control system, introducing air to atmospheric pressure, and taking out the treated graphene.
Furthermore, the mixed gas in the second step is oxygen and helium, and the volume ratio of the oxygen to the helium is 10: 1-5: 1.
Compared with the prior art, the invention has the beneficial effects that: the method solves the problems that the existing method for processing the graphene by ultrasonic wave, heating or airflow and the like has low yield, serious sheet agglomeration, a large number of structural defects of the graphene caused by long-time ultrasonic and more surfactants or surface activators need to be introduced, and the existing plasma processing method can only act on the surface layer of the accumulated graphene. The device is used for improving the hydrophilicity of the surface of the graphene, is beneficial to realizing the modification treatment of the surface of the graphene, and has the advantages of reasonable structure, good stability and simple operation.
Drawings
FIG. 1 is a schematic structural diagram of a graphene surface plasma modification processing apparatus according to the present invention
FIG. 2 is a schematic cross-sectional structure diagram of a graphene surface plasma modification processing apparatus according to the present invention
FIG. 3 is a schematic view of the structure of the counter electrode according to the present invention
1-vacuum chamber, 2-glass container, 3-container end socket, 4-vacuum chamber end socket, 5-inflation hole, 6-air suction hole, 7-rotating shaft, 8-active motor, 9-radio frequency power supply system, 10-counter electrode, 11-through hole, 12-polytetrafluoroethylene block, 13-discharge layer, 14-insulating layer, 15-shielding layer
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely explained below with reference to the drawings in the embodiments of the present invention.
Referring to fig. 1-3 to illustrate the present embodiment, a graphene surface plasma modification processing apparatus includes a vacuum chamber 1, a glass container 2, a radio frequency power supply system 9, a counter electrode 10 and a rotating mechanism, where the vacuum chamber 1 is of a horizontal structure, the vacuum chamber 1 is provided with an inflation hole 5 and an air exhaust hole 6, the counter electrode 10 is connected with the radio frequency power supply system 9, the counter electrode 10 is of an arc structure, an inner arc portion is a discharge layer 13, a middle portion is an insulating layer 14, an outer arc portion is a shielding layer 15, the cylindrical glass container 2 is placed in the middle of the counter electrode 10, the counter electrode 10 is fixed on the inner wall of the vacuum chamber 1 through a teflon block 12 and is coaxial with the center of the glass container 2, the glass container 2 is connected with the rotating mechanism, and one end of the glass container 2 is provided with a through.
This embodiment the shielding formula observation window has been seted up on vacuum chamber 1, vacuum chamber 1 includes vacuum chamber body and vacuum chamber head 4, vacuum chamber body and vacuum chamber head 4 are for dismantling the connection. The vacuum chamber 1 is of a horizontal rectangular structure, the length is 1500mm, the width is 1200mm, the height is 1000mm, a shielding type observation window can be used for observing the conditions of transmission and glow discharge in the vacuum chamber 1, the shielding type observation window can be arranged on the vacuum chamber end socket 4, and the structure that the vacuum chamber body is detachably connected with the vacuum chamber end socket 4 is convenient for the installation in the vacuum chamber 1 and the opening and closing of the vacuum chamber; the glass container 2 comprises a container body and a container seal head 3, wherein the container body is detachably connected with the container seal head 3. The length of the glass container 2 is 1000mm, the inner diameter of the glass container is 600mm, the thickness of the glass container is 5mm, and the container body and the container end enclosure 3 are detachably connected so as to be convenient for taking and placing graphene; the inflation hole 5 is connected with a ventilation control system, the exhaust hole 6 is connected with an exhaust control system, and the vacuum degree of the vacuum chamber 1 is ensured through the ventilation control system and the exhaust control system; the rotating mechanism comprises a rotating shaft 7 and an active motor 8, the output end of the active motor 8 is connected with the rotating shaft 7, the rotating shaft 7 is connected with the glass container 2, and the rotating speed is adjustable so as to control and realize cylinder rotation and continuous graphene rolling; the maximum power of the radio frequency power supply system 9 is 1000W, the frequency is 13.56MHz, and glow discharge under different powers can be realized according to requirements; discharge layer 13 is 304 stainless steel material, insulating layer 14 is the polytetrafluoroethylene material, shielding layer 15 is 304 stainless steel material, discharge layer 13 thickness is 3mm, insulating layer 14 thickness is 50mm, shielding layer 15 thickness is 3mm, and 11 quantity of through-holes are a plurality of, and 2 centre of a circle direction equipartitions are followed to a plurality of through-holes 11.
The invention also provides a graphene surface plasma modification treatment method, which comprises the following steps:
the method comprises the following steps: loading graphene to be processed into a glass container 2, closing a container end enclosure 3 and a vacuum chamber end enclosure 4, starting an air extraction control system, and keeping the background vacuum degree of a vacuum chamber 1 at 0.01-1 Pa;
step two: opening a ventilation control system, filling mixed gas into the vacuum chamber 1, maintaining the air extraction and inflation states of the vacuum chamber 1, keeping the working vacuum degree in the vacuum chamber 1 stable at 10-20 Pa, and starting a radio frequency power supply system 9 to enable a glow discharge area to be bound in the glass container 2;
step three: starting a driving motor 8, driving the glass container 2 to rotate through a rotating shaft 7, and driving graphene placed in the glass container 2 to continuously roll in a glow discharge area, wherein the processing time is 2-5min, and the discharge radio frequency power is 80-120W;
step four: and after the treatment is finished, closing the radio frequency power supply system 9, the ventilation control system and the air extraction control system, introducing air to atmospheric pressure, and taking out the treated graphene.
In the second step of this embodiment, the mixed gas is oxygen and helium, and the volume ratio of oxygen to helium is 10: 1-5: 1.
The graphene surface plasma modification processing apparatus and the processing method provided by the present invention are introduced in detail, and the principle and the implementation manner of the present invention are explained in the present document by applying specific examples, and the description of the above examples is only used to help understanding the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (7)
1. A graphene surface plasma modification processing device is characterized in that: the device comprises a vacuum chamber (1), a glass container (2), a radio frequency power supply system (9), a counter electrode (10) and a rotating mechanism, wherein the vacuum chamber (1) is of a horizontal structure, an inflation hole (5) and an air suction hole (6) are formed in the vacuum chamber (1), the counter electrode (10) is connected with the radio frequency power supply system (9), the counter electrode (10) is of an arc-shaped structure, the inner arc part is a discharge layer (13), the middle part is an insulating layer (14), the outer arc part is a shielding layer (15), the cylindrical glass container (2) is placed in the middle of the counter electrode (10), the counter electrode (10) is fixed on the inner wall of the vacuum chamber (1) through a polytetrafluoroethylene block (12) and is coaxial with the center of the glass container (2), the glass container (2) is connected with the rotating mechanism, one end of the glass container (2) is provided with a, discharge layer (13) are 304 stainless steel, insulating layer (14) are the polytetrafluoroethylene material, shielding layer (15) are 304 stainless steel, discharge layer (13) thickness is 3mm, insulating layer (14) thickness is 50mm, shielding layer (15) thickness is 3 mm.
2. The graphene surface plasma modification processing apparatus according to claim 1, wherein: the vacuum chamber is characterized in that a shielding type observation window is arranged on the vacuum chamber (1), the vacuum chamber (1) comprises a vacuum chamber body and a vacuum chamber end socket (4), the vacuum chamber body and the vacuum chamber end socket (4) are detachably connected, the vacuum chamber (1) is of a horizontal rectangular structure, the length of the vacuum chamber is 1500mm, the width of the vacuum chamber is 1200mm, and the height of the vacuum chamber is 1000 mm.
3. The graphene surface plasma modification processing apparatus according to claim 1, wherein: the glass container (2) comprises a container body and a container sealing head (3), the container body is detachably connected with the container sealing head (3), the length of the glass container (2) is 1000mm, the inner diameter of the glass container is 600mm, and the thickness of the glass container is 5 mm.
4. The graphene surface plasma modification processing apparatus according to claim 1, wherein: the inflation hole (5) is connected with a ventilation control system, and the exhaust hole (6) is connected with an exhaust control system.
5. The graphene surface plasma modification processing apparatus according to claim 1, wherein: the rotating mechanism comprises a rotating shaft (7) and a driving motor (8), the output end of the driving motor (8) is connected with the rotating shaft (7), and the rotating shaft (7) is connected with the glass container (2).
6. The graphene surface plasma modification processing apparatus according to claim 1, wherein: the maximum power of the radio frequency power supply system (9) is 1000W, and the frequency is 13.56 MHz.
7. The processing method of the graphene surface plasma modification processing apparatus according to claim 1, characterized in that: it comprises the following steps:
the method comprises the following steps: loading graphene to be processed into a glass container (2), closing a container end enclosure (3) and a vacuum chamber end enclosure (4), starting an air exhaust control system, and keeping the background vacuum degree of a vacuum chamber (1) at 0.01-1 Pa;
step two: opening a ventilation control system, filling mixed gas into the vacuum chamber (1), maintaining the air extraction and inflation states of the vacuum chamber (1), keeping the working vacuum degree in the vacuum chamber (1) stable at 10-20 Pa, and starting a radio frequency power supply system (9) to enable a glow discharge area to be bound in the glass container (2);
step three: starting a driving motor (8), driving the glass container (2) to rotate through a rotating shaft (7), driving graphene placed in the glass container (2) to roll continuously in a glow discharge area, wherein the processing time is 2-5min, and the discharge radio frequency power is 80-120W;
step four: after the treatment is finished, closing the radio frequency power supply system (9), the ventilation control system and the air extraction control system, introducing air to atmospheric pressure, and taking out the treated graphene;
and in the second step, the mixed gas is oxygen and helium, and the volume ratio of the oxygen to the helium is 10: 1-5: 1.
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| CN111430724A (en) * | 2020-05-16 | 2020-07-17 | 武汉理工大学 | Current collector, preparation method thereof and soft package lithium ion battery |
| CN112724710A (en) * | 2021-01-15 | 2021-04-30 | 贵州玖碳科技有限公司 | Plasma graphene powder surface modification process |
| CN115069168B (en) * | 2022-06-14 | 2023-09-22 | 西安交通大学 | Carbon nanotube material fluorination device based on plasma and application method thereof |
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| CN104671237B (en) * | 2015-02-04 | 2016-08-17 | 浙江大学 | A kind of devices and methods therefor preparing graphene film based on plasma |
| CN205542695U (en) * | 2016-04-15 | 2016-08-31 | 常州机电职业技术学院 | Improve modified device of hydrophilic plasma in powder material surface |
| CN105742143B (en) * | 2016-04-15 | 2017-07-04 | 常州机电职业技术学院 | Improve the hydrophilic plasma modification device of powder body material surface and processing method |
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