CN110357085A - A kind of graphene surface plasma modification processing unit and processing method - Google Patents
A kind of graphene surface plasma modification processing unit and processing method Download PDFInfo
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- CN110357085A CN110357085A CN201910753605.0A CN201910753605A CN110357085A CN 110357085 A CN110357085 A CN 110357085A CN 201910753605 A CN201910753605 A CN 201910753605A CN 110357085 A CN110357085 A CN 110357085A
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Abstract
The invention proposes a kind of graphene surface plasma modification processing unit and processing methods, belong to graphene surface technical field of modification, more particularly to a kind of graphene surface plasma modification processing unit and processing method.Solve the problems, such as it is existing the method low yield of graphene is managed by ultrasonic wave, heating or air-flow etc., lamella serious, long-time ultrasound of reuniting causes a large amount of faults of construction of graphene, needs to introduce more surfactant or surface active object and the problem of existing method of plasma processing can only act on the superficial layer of graphene accumulation.It include vacuum chamber, glass container, radio-frequency power system, to electrode and rotating mechanism, the vacuum chamber is horizontal type structure, and described is arc-shaped structure to electrode, described to placement circle tube glass container among electrode, the glass container is connected with rotating mechanism and corresponding processing method.It is mainly used for graphene surface modification.
Description
Technical field
The invention belongs to graphene surface technical field of modification, more particularly to a kind of graphene surface plasma modification
Processing unit and processing method.
Background technique
Plasma technique is usually used in material surface modifying, and graphene is also widely used in each field, has in aqueous solution
The graphene of effect dispersion surfactant-free is always the hope that material supply section scholar dreams of, however due to graphene surface
Hydrophobicity is difficult to be scattered in water with uniformly dividing, is easy to reunite, therefore also limit the application development of graphene, mainly borrow at present
The effect of ultrasonic wave, heating or air-flow is helped to obtain graphene solution, but there is also yields that not high, lamella is reunited for the preparation of these methods
Seriously, long-time ultrasound causes a large amount of faults of construction of graphene, needs to introduce more surfactant or surface active object etc.
Disadvantage, so that these preparation methods are by very big restriction.There is also the correlations of graphene surface plasma modification to grind at present
Study carefully, but take tiling accumulation mode generally for graphene, plasma can only act on the superficial layer of graphene accumulation, the inside
Graphene cannot achieve modification, be badly in need of a kind of device for being able to achieve industrialization production and processing method in the market.For
The hydrophilic plasma modification device of graphene surface and processing method are improved, is advantageously implemented at the modification of graphene surface
Reason and application.
Summary of the invention
The present invention in order to solve the problems in the prior art, proposes a kind of graphene surface plasma modification processing unit
And processing method.
To achieve the above object, the invention adopts the following technical scheme: a kind of graphene surface plasma modification is handled
Device, it include vacuum chamber, glass container, radio-frequency power system, to electrode and rotating mechanism, the vacuum chamber is horizontal knot
Structure offers aeration aperture and aspirating hole on the vacuum chamber, described to be connected to electrode with radio-frequency power system, described to be to electrode
Arc-shaped structure, inner arc part are discharge layer, and middle section is insulating layer, and outer arc part is shielded layer, described right
Circle tube glass container is placed among electrode, it is described that electrode is fixed in vacuum chamber interior walls by polytetrafluoroethylene (PTFE) block, and with
Glass container central coaxial, the glass container are connected with rotating mechanism, and described glass container one end is provided with through-hole.
Further, offer protected type observation window on the vacuum chamber, the vacuum chamber include vacuum chamber body and
Vacuum chamber end socket, the vacuum chamber body and vacuum chamber end socket are to be detachably connected.The vacuum chamber is Horizontal rectangular structure, long
Degree is 1500mm, width 1200mm, is highly 1000mm.
Further, the glass container includes vessel and vessel head, the vessel and vessel head
To be detachably connected.The glass container length is 1000mm, internal diameter 600mm, with a thickness of 5mm.
Further, the aeration aperture is connected with ventilatory control system, and the aspirating hole is connected with pumping control system.
Further, the rotating mechanism includes rotary shaft and active motor, the output end of the active motor and rotation
Shaft is connected, and the rotary shaft is connected with glass container.
Further, the maximum power of the radio-frequency power system is 1000W, frequency 13.56MHz.
Further, the discharge layer is 304 stainless steel materials, and the insulating layer is polytetrafluoroethylene (PTFE) material, described
Shielded layer is 304 stainless steel materials.
Further, the discharge layer is 50mm with a thickness of 3mm, the thickness of insulating layer, and the shielding thickness is
3mm。
The present invention also provides a kind of graphene surface plasma modification processing method, it the following steps are included:
Step 1: graphene to be processed is packed into glass container, closes vessel head and vacuum chamber end socket, and starting is taken out
Gas control system keeps the background vacuum 0.01-1Pa of vacuum chamber；
Step 2: ventilatory control system is opened, mixed gas is filled with into vacuum chamber, maintains the pumping and inflation of vacuum chamber
State makes the indoor working vacuum degree of vacuum be kept stable at 10~20Pa, opens radio-frequency power system, makes glow discharge zone beam
It is tied in glass container；
Step 3: opening active motor, rotate glass container by transmission of rotary axis, drives and places inside glass container
Graphene continuously roll in glow discharge zone, the processing time be 2-5min, electric discharge radio-frequency power be 80-120W；
Step 4: after the completion of processing, radio-frequency power system, ventilatory control system and pumping control system is closed, sky is passed through
Gas is to atmospheric pressure, the graphene that takes out that treated.
Further, mixed gas is oxygen and helium in the step 2, and the volume ratio of oxygen and helium is 10:
1-5:1.
Compared with prior art, the beneficial effects of the present invention are: the present invention solve it is existing by ultrasonic wave, heating or gas
Stream etc. manages the method low yield of graphene, lamella is reunited, and serious, long-time ultrasound causes a large amount of faults of construction of graphene, needs
The problem of introducing more surfactant or surface active object and existing method of plasma processing can only act on graphite
The problem of superficial layer of alkene accumulation.The present invention is used to improve the hydrophily of graphene surface, is advantageously implemented graphene surface
Modification, the apparatus structure is reasonable, stability is good, easy to operate, and the processing method is modified for pure physical method, processing method
Environmental protection, without introducing surfactant or surface active object, processing result is reproducible, high production efficiency.
Detailed description of the invention
Fig. 1 is a kind of graphene surface plasma modification processing device structure diagram of the present invention
Fig. 2 is a kind of graphene surface plasma modification processing unit schematic cross-sectional view of the present invention
Fig. 3 is of the present invention to electrode structure schematic diagram
1- vacuum chamber, 2- glass container, 3- vessel head, 4- vacuum chamber end socket, 5- aeration aperture, 6- aspirating hole, 7- rotation
Axis, 8- active motor, 9- radio-frequency power system, 10- is to electrode, 11- through-hole, 12- polytetrafluoroethylene (PTFE) block, 13- discharge layer, 14-
Insulating layer, 15- shielded layer
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation illustrates.
Illustrate present embodiment referring to Fig. 1-3, a kind of graphene surface plasma modification processing unit, it includes vacuum
Room 1, glass container 2, radio-frequency power system 9, to electrode 10 and rotating mechanism, the vacuum chamber 1 is horizontal type structure, the vacuum
Aeration aperture 5 and aspirating hole 6 are offered on room 1, described to be connected to electrode 10 with radio-frequency power system 9, described is circle to electrode 10
Arcuate structure, inner arc part are discharge layer 13, and middle section is insulating layer 14, and outer arc part is shielded layer 15, institute
It states to placement circle tube glass container 2 among electrode 10, it is described that vacuum chamber 1 is fixed on by polytetrafluoroethylene (PTFE) block 12 to electrode 10
On inner wall, and with 2 central coaxial of glass container, the glass container 2 is connected with rotating mechanism, and described 2 one end of glass container is set
It is equipped with through-hole 11.
The present embodiment vacuum chamber 1 realizes radio-frequency power system 9 to electrode 10 in the case where setting vacuum degree condition, by arc-shaped
Glow discharge is strapped in plasma glow discharge region in glass container 2, improves the validity of graphene processing, passes through
Rotating mechanism drives glass container 2 to rotate, so that the internal graphene loaded be driven continuously to be rolled, carries out to graphene equal
Even surface treatment, through-hole 11 pass through aeration aperture 5 and aspirating hole 6 for realizing the connection between vacuum chamber 1 and glass container 2
Guarantee the vacuum degree of vacuum chamber 1.
Protected type observation window is offered on vacuum chamber 1 described in the present embodiment, the vacuum chamber 1 is including vacuum chamber body and very
Empty room end socket 4, the vacuum chamber body and vacuum chamber end socket 4 are to be detachably connected.The vacuum chamber 1 is Horizontal rectangular structure,
Length is 1500mm, width 1200mm, is highly 1000mm, and protected type observation window can be used for observing transmission in vacuum chamber 1
And the case where glow discharge, protected type observation window may be provided on vacuum chamber end socket 4, vacuum chamber body and vacuum chamber end socket 4 can
The structure of dismantling connection is convenient for the installation inside vacuum chamber 1 and the opening and closing of vacuum chamber；The glass container 2 include vessel and
Vessel head 3, the vessel and vessel head 3 are to be detachably connected.2 length of glass container is 1000mm, internal diameter
For 600mm, with a thickness of 5mm, vessel and vessel head 3 are the pick-and-place being detachably connected convenient for graphene；The aeration aperture 5
It is connected with ventilatory control system, the aspirating hole 6 is connected with pumping control system, passes through ventilatory control system and pumping control system
The vacuum degree of blanket insurance card vacuum chamber 1；The rotating mechanism includes rotary shaft 7 and active motor 8, the output of the active motor 8
End be connected with rotary shaft 7, the rotary shaft 7 is connected with glass container 2, and rotation speed is adjustable, with control realization cylinder rotate with
Graphene continuously rolls；The maximum power of the radio-frequency power system 9 be 1000W, frequency 13.56MHz, as needed can be real
Glow discharge under existing different capacity；The discharge layer 13 is 304 stainless steel materials, and the insulating layer 14 is polytetrafluoroethylene (PTFE) material
Matter, the shielded layer 15 are 304 stainless steel materials, the discharge layer 13 with a thickness of 3mm, the insulating layer 14 with a thickness of 50mm,
The shielded layer 15 with a thickness of 3mm, 11 quantity of through-hole be it is multiple, multiple through-holes 11 are uniformly distributed along 2 center of circle direction of glass container.
The present invention also provides a kind of graphene surface plasma modification processing method, it the following steps are included:
Step 1: graphene to be processed is packed into glass container 2, is closed vessel head 3 and vacuum chamber end socket 4, is opened
Dynamic pumping control system, keeps the background vacuum 0.01-1Pa of vacuum chamber 1；
Step 2: opening ventilatory control system, and mixed gas is filled with into vacuum chamber 1, maintains the pumping of vacuum chamber 1 and fills
Gaseity makes the working vacuum degree in vacuum chamber 1 be kept stable at 10~20Pa, opens radio-frequency power system 9, makes glow discharge
Area is strapped in glass container 2；
Step 3: opening active motor 8, rotates glass container 2 by the transmission of rotary shaft 7, drives inside glass container 2
The graphene of placement continuously rolls in glow discharge zone, and the processing time is 2-5min, and electric discharge radio-frequency power is 80-120W；
Step 4: after the completion of processing, radio-frequency power system 9, ventilatory control system and pumping control system is closed, sky is passed through
Gas is to atmospheric pressure, the graphene that takes out that treated.
Mixed gas is oxygen and helium in step 2 described in the present embodiment, and the volume ratio of oxygen and helium is 10:1-5:
1。
Above to a kind of graphene surface plasma modification processing unit provided by the present invention and processing method, carry out
It is discussed in detail, used herein a specific example illustrates the principle and implementation of the invention, above embodiments
Explanation be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art,
According to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion in this specification
Appearance should not be construed as limiting the invention.
Claims (10)
1. a kind of graphene surface plasma modification processing unit, it is characterised in that: it includes vacuum chamber (1), glass container
(2), radio-frequency power system (9), to electrode (10) and rotating mechanism, the vacuum chamber (1) is horizontal type structure, the vacuum chamber
(1) aeration aperture (5) and aspirating hole (6) are offered on, it is described to be connected to electrode (10) with radio-frequency power system (9), it is described to electricity
Pole (10) is arc-shaped structure, and inner arc part is discharge layer (13), and middle section is insulating layer (14), outer arc part
It is described to place circle tube glass container (2) among electrode (10) for shielded layer (15), it is described that polytetrafluoro is passed through to electrode (10)
Ethylene block (12) is fixed on vacuum chamber (1) inner wall, and with glass container (2) central coaxial, the glass container (2) and rotation
Mechanism is connected, and described glass container (2) one end is provided with through-hole (11).
2. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: described true
Offer protected type observation window in empty room (1), the vacuum chamber (1) includes vacuum chamber body and vacuum chamber end socket (4), described true
Empty room ontology and vacuum chamber end socket (4) are to be detachably connected.The vacuum chamber (1) be Horizontal rectangular structure, length 1500mm,
Width is 1200mm, is highly 1000mm.
3. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: the glass
Glass container (2) includes vessel and vessel head (3), and the vessel and vessel head (3) are to be detachably connected.It is described
Glass container (2) length is 1000mm, internal diameter 600mm, with a thickness of 5mm.
4. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: described to fill
Stomata (5) is connected with ventilatory control system, and the aspirating hole (6) is connected with pumping control system.
5. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: the rotation
Rotation mechanism includes rotary shaft (7) and active motor (8), and the output end of the active motor (8) is connected with rotary shaft (7), described
Rotary shaft (7) is connected with glass container (2).
6. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: described to penetrate
The maximum power of frequency power system (9) is 1000W, frequency 13.56MHz.
7. a kind of graphene surface plasma modification processing unit according to claim 1, it is characterised in that: described to put
Electric layer (13) is 304 stainless steel materials, and the insulating layer (14) is polytetrafluoroethylene (PTFE) material, and the shielded layer (15) is not 304 not
Rust steel material.
8. a kind of graphene surface plasma modification processing unit according to claim 7, it is characterised in that: described to put
Electric layer (13) is with a thickness of 3mm, and the insulating layer (14) is with a thickness of 50mm, and the shielded layer (15) is with a thickness of 3mm.
9. a kind of processing method of graphene surface plasma modification processing unit as described in claim 1, feature exist
In: it the following steps are included:
Step 1: graphene to be processed is packed into glass container (2), closes vessel head (3) and vacuum chamber end socket (4),
Starting pumping control system, keeps the background vacuum 0.01-1Pa of vacuum chamber (1)；
Step 2: opening ventilatory control system, and mixed gas is filled with into vacuum chamber (1), maintains the pumping of vacuum chamber (1) and fills
Gaseity makes the working vacuum degree in vacuum chamber (1) be kept stable at 10~20Pa, opens radio-frequency power system (9), makes aura
Region of discharge is strapped in glass container (2)；
Step 3: opening active motor (8), rotates glass container (2) by rotary shaft (7) transmission, drives glass container (2)
The graphene that inside is placed continuously rolls in glow discharge zone, and the processing time is 2-5min, and electric discharge radio-frequency power is 80-120W；
Step 4: after the completion of processing, radio-frequency power system (9), ventilatory control system and pumping control system is closed, air is passed through
To atmospheric pressure, the graphene that takes out that treated.
10. a kind of graphene surface plasma modification processing method according to claim 9, it is characterised in that: described
Mixed gas is oxygen and helium in step 2, and the volume ratio of oxygen and 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 |
| CN115069168A (en) * | 2022-06-14 | 2022-09-20 | 西安交通大学 | Plasma-based carbon nanotube material fluorination device and use method thereof |
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