CN107739027A - A kind of continuous method and device for preparing porous graphene film - Google Patents
A kind of continuous method and device for preparing porous graphene film Download PDFInfo
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- CN107739027A CN107739027A CN201711030395.XA CN201711030395A CN107739027A CN 107739027 A CN107739027 A CN 107739027A CN 201711030395 A CN201711030395 A CN 201711030395A CN 107739027 A CN107739027 A CN 107739027A
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Abstract
A kind of continuous method and device for preparing porous graphene film is provided, methods described comprises the following steps：(1) thin polymer film along its length transmit in the machining area of thin polymer film by continuously and smoothly；(2) laser brought into focus in advance does straight reciprocating motion along predetermined direction, and thin polymer film described in ablation, forms continuous porous graphene in the machining area of the thin polymer film.The specific thin polymer film of ablation is processed by laser direct-writing, acted on using photothermal laser, in polymeric film surface inductive formation porous graphene, the large area that described method is advantageous to carry out porous graphene film using the laser of low-power continuously quickly produces, device requirement is reduced, and is advantageous to improve the production efficiency and membrane quality of porous graphene processing.
Description
Technical field
The present invention relates to field of preparation of graphene, more particularly to a kind of continuous method and dress for preparing porous graphene film
Put.
Background technology
Graphene has numerous good characteristics, such as high carrier mobility, high heat conduction as quasi- two-dimensional nano-carbon material
Rate, high mechanical properties, splendid translucency etc., thus in electronic device of new generation, wearable device, micro-nano sensing, new energy
The various fields such as battery possess great development potentiality, it is considered to be " the magical material " that " will thoroughly change 21 century ".
The a member of porous graphene as graphene family, not only possess a variety of good characteristics of graphene, because it is more
Pore structure and substantial amounts of nanometer hole defect so that it possesses bigger surface area and Geng Gao surface-active.Porous graphene quilt
It is widely used in the fields such as flexible sensor, super capacitor, Molecular Detection and gas sensing.Yet with inexpensive high-volume
The technology for producing porous graphene lacks, and porous graphene thin-film material still can not obtain extensive commercial application.
The content of the invention
It is an object of the invention to provide a kind of continuous method and device for preparing porous graphene film, can polymerize
In thing film substrate, continuous batch, the industrialization production of large area porous graphene film are carried out.
The purpose of the present invention is achieved through the following technical solutions：
A kind of continuous method for preparing porous graphene film, comprises the following steps：
(1) thin polymer film along its length transmit in the machining area of thin polymer film by continuously and smoothly；
(2) laser brought into focus in advance does straight reciprocating motion along predetermined direction, in adding for the thin polymer film
Thin polymer film described in ablation, forms continuous porous graphene in the domain of work area.
A kind of continuous device for preparing porous graphene film, including laser head, discharge mechanism, receiving mechanism and guide rail,
The discharge mechanism and receiving mechanism are provided commonly for driving a thin polymer film along its length in the processing of thin polymer film
Continuously and smoothly is transmitted in region, and the discharge mechanism and receiving mechanism are located at the two of the machining area of the thin polymer film respectively
Side, the laser head are located at the top of the machining area of the thin polymer film, and on the guide rail, and can be described
Moved on guide rail along the direction of the machining area perpendicular to the thin polymer film to adjust the focal length of its laser beam, and in institute
State and do straight reciprocating motion along predetermined direction on guide rail, with polymerization described in the ablation in the machining area of the thin polymer film
Thing film, form continuous porous graphene.
Beneficial effects of the present invention include：The present invention can be carried out big by induced with laser on polymer film base
The continuous batch of area porous graphene film, industrialization production.
Brief description of the drawings
Fig. 1 is the continuous process schematic for preparing porous graphene film in the specific embodiment of the invention；
Fig. 2 is the forms of motion schematic top plan view of the laser facula and thin polymer film in the specific embodiment of the invention；
Fig. 3 is the SEM figures of the porous graphene prepared in the specific embodiment of the invention；
Fig. 4 is the light microscopic figure of the porous graphene prepared in the specific embodiment of the invention；
Fig. 5 is the cross-sectional view of the thin polymer film used in the specific embodiment of the invention；
Fig. 6 is that the cross section of storing state after the porous graphene being prepared in the specific embodiment of the invention is wound shows
It is intended to；
Fig. 7 is the schematic device that porous graphene film is continuously prepared in the specific embodiment of the invention.
Embodiment
Below against accompanying drawing and with reference to preferred embodiment, the invention will be further described.Under it should be noted that
State it is bright be merely exemplary, the scope being not intended to be limiting of the invention and its application, in the case where not conflicting, this Shen
Please in embodiment and embodiment in feature can be mutually combined.
The present invention provides a kind of continuous method for preparing porous graphene film, and it is that a kind of large area continuously manufactures work
Skill, by controlling the specific thin polymer film of laser ablation of certain wavelength, using photothermal laser effect can inductive formation it is more
Hole graphene.
In a particular embodiment, comprise the following steps：
(1) thin polymer film along its length transmit in the machining area of thin polymer film by continuously and smoothly；
(2) laser brought into focus in advance does straight reciprocating motion along predetermined direction, in the processing district of thin polymer film
Ablative polymer film in domain, form continuous porous graphene.
As shown in figure 1, the laser that 1 expression laser head, 11 expression laser heads are sent, 2 signal discharge mechanisms, 3 represent polymerization
Thing film, the porous graphene film of 4 expression generations, 5 signal receiving mechanisms, the XYZ coordinate system shown in figure, hereinafter：
" X-direction " and " thin polymer film length direction " is to represent same direction, " Y direction " and " thin polymer film width side
To " it is to represent same direction, " Z-direction " and it is to represent same " perpendicular to the direction of the machining area of thin polymer film "
Direction.Thin polymer film (X-direction i.e. shown in figure along its length under the drive of discharge mechanism 2 and receiving mechanism 5
On) continuously and smoothly is transmitted in the machining area of thin polymer film.Laser head 1 can be perpendicular to the processing district of thin polymer film
It is predetermined that the laser edge to adjust the focal length of its laser beam, brought into focus is moved (in the Z-direction i.e. shown in figure) in the direction in domain
Direction do straight reciprocating motion, the ablative polymer film in the machining area of thin polymer film, form continuous porous stone
Black alkene, that is, can be moved on laser head XYZ direction of principal axis shown in the figure, in process, laser head is kept in Z
It is fixed on direction of principal axis, moved along a straight line in X/Y plane.
Wherein, preferably it is that the predetermined direction of laser motion refers to：The direction of motion of laser and the width of thin polymer film
Spend direction (Y direction i.e. shown in figure) θ, 0 ° of 1 ° of ＜ θ ＜ at an angle, it is preferable that 0 ° of 0.52 ° of ＜ θ ＜；Done in laser
During straight reciprocating motion, in the machining area of the thin polymer film, when speed of the laser on thin polymer film length direction
It is process when the direction of degree component is identical with the direction of motion of thin polymer film, in process, laser is opened；When
Laser is backhaul when the direction of the velocity component on thin polymer film length direction is opposite with the direction of motion of thin polymer film
Process, in return stroke, laser shutdown.Further, in process, laser is on thin polymer film length direction
Velocity component VxSize in the range of 0.006mm/s~0.455mm/s；Speed of the laser on thin polymer film width
Spend component VySize in the range of 50mm/s~250mm/s.As shown in Fig. 2 the motion for laser facula and thin polymer film
Form schematic top plan view, in the example, laser facula (shown in a in such as figure, a ') along with Y direction θ at an angle
Straight reciprocating motion is done in direction, and a → a ' illustrated in figure is process, and a ' → a is return stroke.
Wherein, the spot diameter of laser is 100 μm -200 μm, and width etc. can be generated on the polymer film after single induction
In the porous graphene lines 41 of laser spot diameter, after multiple process, the meeting in the machining area of thin polymer film
Continuous porous graphene is formed, as shown in figure 4, can see that continuous porous graphene parallel is connected by some under microcosmic
(edge line of i.e. every graphene lines is parallel to each other, and is to be close to or part per two adjacent graphene lines
It is overlapping) the porous graphene lines composition of arrangement.The center spacing of every two adjacent porous graphene lines is s, wall scroll
The line width of 2/3rds≤s of the line width (i.e. laser spot diameter) of porous graphene lines≤wall scroll porous graphene lines
(i.e. laser spot diameter), preferably it is that in 66 μm~100 μ ms, s can also be calculated to obtain s by below equation：
As shown in Fig. 2 setting the width d of the machining area of thin polymer film, the velocity component of laser processing procedure is VxWith
Vy, the velocity component of return stroke is Vx′And Vy′, the used time of return stroke is t, then has
By converting,
Wherein, the width d of the machining area of thin polymer film is 50mm~500mm, and the opening speed of laser can be to add
10 times of (V of the speed of work processx′It is Vx10 times and Vy′It is Vy10 times), the movement velocity V of thin polymer film0It can be equal to
X-component (the i.e. V of the speed of laser in processx)。
In above embodiment, laser is point-like light spot laser, using CO2Infrared laser, wavelength are 10.6 micro-
Rice；Laser power is 4W~10W；Thin polymer film is polyimides (PI) or PEI (PEI) film；Thin polymer film
Middle part be machining area, the width of thin polymer film two side portions be independently each the machining area width eight/
Between 1/1st to six；The thickness of the machining area of thin polymer film is 50-100 μm, the porous graphene for processing to obtain
Thickness is 5-40 μm.Processing method in embodiment of above can lift the uniformity and matter of the porous graphene film of generation
Measure, thin polymer film continuously moves in process, and light spot laser device does periodicity linear reciprocation fortune on fixed movement line
Dynamic, the kinematic accuracy and performance requirement to equipment be not high, and working range is small, can reduce plant bulk, and only need power very
Small point-like laser achieves that the continuous poriferous graphene film processing of large area, saves equipment cost, high in machining efficiency.Such as
Shown in Fig. 3, because the porous graphene being processed into has the characteristics of porous, loose, (porosity in porous graphene hole is 25%-
65%), easy fail in compression, therefore thin polymer film uses specific shape of cross section, as shown in figure 5, cross section two side portions
Part compared with intervening deposition graphene is higher by some sizes (for example, thickness of two sides can be higher by one than the thickness of machining area
Times), it after porous graphene winding, can play a supportive role, prevent that winding film from damaging porous graphene structure by pressure, the horizontal stroke after winding
Cross sectional shape is as shown in Figure 6.
As shown in fig. 7, continuously to prepare the schematic device of porous graphene film in the specific embodiment of the invention, its
Including laser head 1, discharge mechanism 2, receiving mechanism 5 and guide rail, discharge mechanism 2 and receiving mechanism 5 are provided commonly for driving a polymerization
Thing film 3 along its length transmit in the machining area 31 of thin polymer film by continuously and smoothly, discharge mechanism 2 and receiving mechanism
5 are located at the top of the machining area of thin polymer film 3 positioned at the both sides of the machining area 31 of thin polymer film, laser head 1 respectively,
And on guide rail, and can be moved on guide rail along the direction of the machining area perpendicular to thin polymer film to adjust its laser
The focal length of beam, and straight reciprocating motion is done along predetermined direction on guide rail, with the machining area 31 of thin polymer film
Ablative polymer film, form continuous porous graphene.Wherein, in this example, guide rail includes X guide rails 6, Y guide rail 7 and Z guide rails
8, Z guide rails can be fixed in frame (not shown), and laser head 1 is arranged in Y guide rail 7, and during focusing, X guide rails 6 drive Y guide rail 7
And the laser head 1 in Y guide rail 7 is slided on Z guide rails 8 and (moved along Z-direction), after the completion of focusing, the position of X guide rails 6 is fixed；
During straight reciprocating motion, Y guide rail 7 drives laser head 1 to slide and (move in the X-axis direction) on X guide rails 6, and laser
First 1 slides (being moved along Y direction) in Y guide rail 7, and the two directions have just synthesized process and the backhaul of laser head
The straight reciprocating motion of journey.Discharge mechanism 2 is roller discharge mechanism, including blowing live-roller 21 and the (this example of blowing help roll 22
In be two blowing help rolls), receiving mechanism 5 is roller receiving mechanism, including rewinding live-roller 51 and (this of rewinding help roll 52
It is two rewinding help rolls in example), blowing live-roller 21 and rewinding live-roller 51 are rolled and moved around drive thin polymer film 3 (in figure
Illustrated with arrow), blowing help roll 22 and rewinding help roll 52 keep thin polymer film 3 in motion thin polymer film plus
31 is tight in the domain of work area, to be advantageous to the growth of the porous graphene of high quality.
Below by way of a specific example, the present invention will be described in detail.
Embodiment 1
As shown in Fig. 1~7, laser uses wavelength as 10.6 μm of infrared laser, power 5.5W.Thin polymer film is
Polyimides (PI) film.By thin polymer film on discharge mechanism and receiving mechanism, the center section of thin polymer film
For machining area, its thickness is 50 μm, width 300mm, and the width of the both sides of thin polymer film is respectively 50mm, and thickness is respectively
100μm.Control laser head 1 to be moved in Z-direction, carry out laser focusing, be 100 μm to defocused laser spot diameter.It is processed
Laser work in journey (a → a ' process in such as Fig. 2), laser shutdown in return stroke (a ' → a process in such as Fig. 2), set
The transmission speed V of thin polymer film0=0.045mm/s, continuously and smoothly are driven, in process, laser facula and polymer thin
Film speed of related movement Vy=150mm/s, Vx=0.045mm/s, laser spot velocity V in backhaulx′=0.45mm/s, Vy′=
1500mm/s.Such periodic straight lines move back and forth, and obtain the porous graphene film of continuous large-area.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For those skilled in the art, do not taking off
On the premise of from present inventive concept, some equivalent substitutes or obvious modification can also be made, and performance or purposes are identical, all should
When being considered as belonging to protection scope of the present invention.
Claims (10)
- A kind of 1. continuous method for preparing porous graphene film, it is characterised in that comprise the following steps：(1) thin polymer film along its length transmit in the machining area of thin polymer film by continuously and smoothly；(2) laser brought into focus in advance does straight reciprocating motion along predetermined direction, in the processing district of the thin polymer film Thin polymer film described in ablation in domain, forms continuous porous graphene.
- 2. the method as described in claim 1, it is characterised in that in the step (2), the predetermined direction refers to：Laser The direction of motion and the thin polymer film width θ, 0 ° of 1 ° of ＜ θ ＜ at an angle.
- 3. method as claimed in claim 1 or 2, it is characterised in that when doing the straight reciprocating motion, in the polymer In the machining area of film, direction and thin polymer film when velocity component of the laser on thin polymer film length direction The direction of motion it is identical when, be process, in the process, laser open；When the laser is in thin polymer film It is return stroke, in the backhaul when direction of velocity component on length direction is opposite with the direction of motion of thin polymer film During, laser shutdown.
- 4. method as claimed in claim 3, it is characterised in that in the process, the laser is in thin polymer film Velocity component V on length directionxSize in the range of 0.006mm/s~0.455mm/s；The laser is in thin polymer film Velocity component V on widthySize in the range of 50mm/s~250mm/s.
- 5. method as claimed in claim 3, it is characterised in that in process each time, in the thin polymer film The porous graphene lines that a width is 100 μm -200 μm are formed in machining area, after multiple process, described poly- Form continuous porous graphene in the machining area of compound film, the continuous porous graphene parallel is connected by some The porous graphene lines composition of arrangement；The center spacing of every two adjacent porous graphene lines is s, wall scroll porous graphite The line width of 2/3rds≤s of the line width of alkene lines≤wall scroll porous graphene lines；The width of wall scroll porous graphene lines Equal to the spot diameter of laser used.
- 6. method as claimed in claim 5, it is characterised in that the s is in 66 μm~100 μ ms.
- 7. method as claimed in claim 4, it is characterised in that in the return stroke, opening speed is process 5-10 times of speed.
- 8. method as claimed in claim 1 or 2, it is characterised in that the laser is point-like light spot laser, and spot diameter is 100 μm -200 μm, using CO2Infrared laser, wavelength are 10.6 microns；The laser power is 4W~10W；The polymer thin Film is polyimides or PEI film；The middle part of the thin polymer film is machining area, the thin polymer film The width d of machining area is 50mm~500mm, and the width of the thin polymer film two side portions is independently each the processing Between 1st/1st to six/8th of peak width, the thickness of the thin polymer film two side portions is more than the machining area Thickness；The thickness of the machining area of the thin polymer film is 50-100 μm, and the thickness of the porous graphene is 5-40 μm.
- 9. a kind of continuous device for preparing porous graphene film, it is characterised in that including laser head, discharge mechanism, collecting machine Structure and guide rail, the discharge mechanism and receiving mechanism are used to drive a thin polymer film jointly along its length in polymer thin Continuously and smoothly is transmitted in the machining area of film, and the discharge mechanism and receiving mechanism are located at the processing of the thin polymer film respectively The both sides in region, the laser head are located at the top of the machining area of the thin polymer film, and on the guide rail, and It can be moved on the guide rail along the direction of the machining area perpendicular to the thin polymer film to adjust the focal length of its laser beam, And straight reciprocating motion is done along predetermined direction on the guide rail, with the ablation in the machining area of the thin polymer film The thin polymer film, form continuous porous graphene.
- 10. device as claimed in claim 9, it is characterised in that the discharge mechanism is roller discharge mechanism, including blowing passes Dynamic roller and blowing help roll, the receiving mechanism are roller receiving mechanism, including rewinding live-roller and rewinding help roll, described to put Expect that live-roller and rewinding live-roller drive the thin polymer film motion, the blowing help roll and rewinding help roll keep motion In the thin polymer film it is tight in the machining area of the thin polymer film；The guide rail includes X guide rails, Y guide rail and Z Guide rail, the laser head is arranged in the Y guide rail, and during focusing, the X guide rails are driven in the Y guide rail and the Y guide rail Laser head is slided on the Z guide rails, and after the completion of focusing, the X guide rail positions are fixed；In the straight reciprocating motion, institute Stating Y guide rail drives the laser head to be slided on the X guide rails, and the laser head slides in the Y guide rail.
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Cited By (8)
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| CN109632905A (en) * | 2019-01-14 | 2019-04-16 | 南京邮电大学 | A kind of flexible non-enzymatic glucose sensor of graphene-supported copper nano particles and preparation method thereof |
| CN109686501A (en) * | 2018-12-30 | 2019-04-26 | 苏州碳素集电新材料有限公司 | A kind of graphene/aluminum composite conducting material and preparation method thereof |
| CN110246880A (en) * | 2019-06-14 | 2019-09-17 | 武汉华星光电半导体显示技术有限公司 | The preparation method and display panel of display panel |
| CN112798472A (en) * | 2020-12-24 | 2021-05-14 | 广东工业大学 | Quality online detection method and device for graphene-based composite material production |
| CN114211831A (en) * | 2021-12-24 | 2022-03-22 | 中科合肥智慧农业协同创新研究院 | Preparation method of degradable thickened graphene photothermal conversion mulching film |
| CN114228182A (en) * | 2021-12-24 | 2022-03-25 | 中科合肥智慧农业协同创新研究院 | Method for rapidly preparing graphene sandwich type photothermal conversion mulching film |
| CN114275771A (en) * | 2021-12-06 | 2022-04-05 | 喆烯新材(北京)科技有限公司 | Scanning device for laser-induced graphene |
| CN115819824A (en) * | 2022-12-27 | 2023-03-21 | 中科合肥智慧农业协同创新研究院 | Graphene/polyimide water seepage mulching film and preparation method thereof |
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| CN109686501A (en) * | 2018-12-30 | 2019-04-26 | 苏州碳素集电新材料有限公司 | A kind of graphene/aluminum composite conducting material and preparation method thereof |
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| CN114211831A (en) * | 2021-12-24 | 2022-03-22 | 中科合肥智慧农业协同创新研究院 | Preparation method of degradable thickened graphene photothermal conversion mulching film |
| CN114228182A (en) * | 2021-12-24 | 2022-03-25 | 中科合肥智慧农业协同创新研究院 | Method for rapidly preparing graphene sandwich type photothermal conversion mulching film |
| CN115819824A (en) * | 2022-12-27 | 2023-03-21 | 中科合肥智慧农业协同创新研究院 | Graphene/polyimide water seepage mulching film and preparation method thereof |
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