CN104140092A - Wrinkled graphene lamella and making method thereof - Google Patents
Wrinkled graphene lamella and making method thereof Download PDFInfo
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- CN104140092A CN104140092A CN201310169410.4A CN201310169410A CN104140092A CN 104140092 A CN104140092 A CN 104140092A CN 201310169410 A CN201310169410 A CN 201310169410A CN 104140092 A CN104140092 A CN 104140092A
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- polystyrene
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Abstract
The invention relates to a wrinkled graphene lamella and a making method thereof, and belongs to the graphene preparation field. The method is characterized in that laser irradiates a graphene lamella covering a polystyrene layer to obtain wrinkles. The method generating wrinkles on the graphene lamella can control the generation positions of the wrinkles, can generate wrinkles at the edges of the graphene lamella, and can also generate wrinkles in the middle position of the graphene lamella; and the method has the advantages of simple operation, and easy control of operation conditions.
Description
Technical field
The present invention relates to the preparation field of Graphene, be specifically related to a kind of graphene sheet layer with fold and preparation method thereof, described in there is the graphene sheet layer of fold preparation method can control the growth position of fold in graphene sheet layer.
Background technology
Graphene has Colloidal particles, and the carbon atom in plane is with sp
2hybridized orbital is connected to form hexagonal lattice structure, be that carbon atom passes through very strong σ key and is connected with three adjacent carbon atoms, C-C key makes Graphene have good structure rigidity, a remaining p electronic orbit is perpendicular to Graphene plane, form π key with carbon atom around, the delocalization of π-electron in lattice, makes Graphene have good electroconductibility, and the electronic mobility on room temperature lower plane is 1.5 * 10
4cm
2/ Vs, the conduction velocity considerably beyond electronics in general conductor, thereby in the middle of microelectronics, space flight military project, energy storing device, nano electron device, nano composite material, have wide potential application space.
Graphene is a kind of " metallic film " of " the softest ", and surface is easy to wrinkling, as paving silks and satins on the table.The performances such as the intrinsic mechanics of these " folds " meeting change Graphene, electricity.For adjusting and control the electric property of Graphene, in graphene sheet layer, generating fold is a kind of important method that Graphene is carried out to structure processing, and the method for still controlling the growth of Graphene fold is very limited.
In prior art, the main method that generates fold in graphene sheet layer is by the whole heating of the substrate of load Graphene and Graphene, at the edge of Graphene, obtains fold after cooling.But this method is because have no idea to accomplish local heating, and fold is only created in edge; And the lower stress producing of whole heating can, in the boundary effect of two individual system (Graphene and polymeric substrates), so only produce fold at the edge of Graphene, can not be controlled the position that fold generates effectively.
A kind of method that can control Graphene fold generation position need to be developed in this area, not only makes the edge of graphene sheet layer can generate fold, also can generate fold in the middle part of graphene sheet layer.
Summary of the invention
For prior art, cannot in the middle of graphene sheet layer, generate the problem of fold, a kind of method that can generate fold on graphene sheet layer is proposed, described method can be controlled the position that generates fold on graphene sheet layer, both can generate fold at the edge of graphene sheet layer, also can generate fold in any position in the centre of graphene sheet layer.
On the one hand, the invention provides a kind of method that generates fold on graphene sheet layer, described method is to utilize laser to carry out irradiation to the graphene sheet layer covering on polystyrene layer, obtains fold.
The present invention is melted by laser irradiation the polystyrene layer covering under graphene sheet layer, obtain the hole corresponding with laser facula, the graphene sheet layer covering on described hole subsides, and under the effect of mechanical stress, makes the graphene layer not subsiding produce fold.
Laser power of the present invention is 3～15mW, such as 3.3mW, 3.6mW, 3.9mW, 4.3mW, 4.8mW, 5.3mW, 5.6mW, 5.9mW, 6.5mW, 7.8mW, 8.4mW, 8.8mW, 9.2mW, 9.6mW, 12mW, 13mW, 14mW etc.Described unit " mW " is the abbreviation of unit of power milliwatt.
Described laser power is too large, and polystyrene layer is easily out of shape, and the graphene sheet layer covering on it is out of shape thereupon, is unfavorable for follow-up application; Laser power is too small, polystyrene layer fusing difficulty.
Optical maser wavelength of the present invention is 500～800nm, such as 505nm, 512nm, 520nm, 535nm, 578nm, 596nm, 621nm, 658nm, 668nm, 731nm, 754nm, 768nm, 770nm, 784nm, 792nm, 798nm etc., preferred 514～785nm, further preferably 514nm, in 633nm or 785nm any 1.
The diameter of the hot spot of described laser is 1～5 μ m, such as 1.2 μ m, 1.8 μ m, 2.2 μ m, 2.5 μ m, 2.7 μ m, 3.3 μ m, 3.8 μ m, 4.2 μ m, 4.6 μ m, 4.9 μ m etc.Spot diameter is too little, and existing techniques in realizing is more difficult; Hot spot is too large, and laser power is disperseed very much, can not effectively melt decomposition polystyrene.
The described laser irradiation time is 5～100s, such as 6s, 13s, 25s, 36s, 42s, 50s, 55s, 68s, 75s, 86s, 94s etc.
The weight-average molecular weight of polystyrene of the present invention is 100 * 10
3～1000 * 10
3, for example 150 * 10
3, 180 * 10
3, 240 * 10
3, 280 * 10
3, 340 * 10
3, 375 * 10
3, 456 * 10
3, 530 * 10
3, 588 * 10
3, 620 * 10
3, 670 * 10
3, 750 * 10
3, 780 * 10
3, 800 * 10
3, 880 * 10
3, 950 * 10
3, 980 * 10
3deng, preferably 200 * 10
3～500 * 10
3.
Preferably, the thickness of described polystyrene lamella is 100～500nm, such as 105～115nm, 112～118nm, 125～136nm, 136～148nm, 150～160nm, 168～178nm, 176～189nm, 185～196nm, 204～215nm, 265～276nm, 271～283nm, 306～316nm, 347～357nm, 382～393nm, 406～416nm, 438～447nm, 469～479nm, 486～496nm etc.
As optimal technical scheme, the method that generates fold on graphene sheet layer of the present invention comprises the steps:
(1) on silicon chip, form polystyrene layer;
(2) on the polystyrene layer obtaining in step (1), form graphene sheet layer;
(3) graphene sheet layer that laser irradiation step (2) obtains, obtains fold.
Wherein, the described method that forms polystyrene layer on silicon chip of step (1), for polystyrene solution is spun on silicon chip, is dried and is obtained polystyrene layer; The thickness of described polystyrene layer is 100～500nm; The weight-average molecular weight of described polystyrene is 100 * 10
3～1000 * 10
3, preferably 200 * 10
3～500 * 10
3.
Wherein, the mass concentration of described polystyrene solution is 2～20%, such as 2.1%, 2.6%, 3.0%, 4%, 7.5%, 10.3%, 12%, 14.5%, 15.6%, 16.8%, 17.9%, 18.2%, 19.2%, 19.6% etc.; The bake out temperature that described oven dry obtains polystyrene layer is 120～200 ℃, such as 124 ℃, 128 ℃, 135 ℃, 138 ℃, 142 ℃, 156 ℃, 168 ℃, 175 ℃, 186 ℃, 196 ℃ etc.The thickness that the polystyrene solution of 2～20% mass concentrations can be easy to control the polystyrene layer generating is between 100～500nm.
The solvent of described polystyrene solution is any organic solvent that polystyrene can be dissolved, preferred easy volatile solvent, typical but non-limiting example has the combination of any a kind or at least 2 kinds in methyl ethyl ketone, toluene, benzene, chlorobenzene, methylene dichloride, chloroform etc., concrete which kind of solvent of selecting, those skilled in the art can select according to practical situation voluntarily.
Preferably, the described silicon chip of step (1) cleans before using; Described cleaning as drying up scavenging solution with nitrogen after ultrasonic cleaning.
Alternatively, before the described silicon chip of step (1) is used, with acetone and dehydrated alcohol, carry out ultrasonic cleaning, with nitrogen, dry up afterwards, standby.
About the preparation of Graphene and the aspects such as transfer of big size graphene lamella, those skilled in the art have done certain research.Typical but non-limiting " on polystyrene layer, forming the method for graphene sheet layer " can be by process for preparing graphenes by chemical vapour deposition lamella, and is transferred on polystyrene layer by polydimethylsiloxane (PDMS) method; Or directly by micromechanical forces stripping method, directly on polystyrene layer, form graphene sheet layer; Deng.
In the method that generates fold on graphene sheet layer of the present invention, the described method that forms graphene sheet layer on polystyrene layer of step (2) is micromechanical forces stripping method.
Micromechanics stripping method is to prepare the method that graphene sheet layer is conventional, prior art has also been done a lot of research, such as people such as Xu Xiujuan in " Graphene progress " (Graphene progress, Xu Xiujuan etc., 2009, the 12nd phase, 2559-2566 page) in (1) part of 3.2.1 mono-joint of a literary composition, micromechanical forces is peeled off and is described; (mechanically peel legal system is for the preliminary study of high-quality graphene in " mechanically peel legal system is for the preliminary study of high-quality graphene " for the people such as Tang Duochang, Tang Duochang etc., 2010, the 3rd phase, 16th～18 pages and the 59th page) in " 1 experimental technique " part of a literary composition, for adopting mechanically peel to prepare being described in detail of Graphene.No longer micromechanics being peeled off to the method for preparing Graphene herein repeats.
The concrete operations that typical but non-limiting micromechanics stripping method forms the method for graphene sheet layer on polystyrene layer are:
(1) for example, with adhesive tape (3M thinks high board adhesive tape), be attached to highly oriented pyrolytic graphite sheet surface, compacting gently, tightly attaches adhesive tape and graphite, then adhesive tape is slowly torn;
(2) adhesive tape can adhere to the graphite flake that one deck is very thin, and then will adhere to the adhesive tape doubling of graphite flake, and compacting gently, tightly attaches adhesive tape and graphite, then adhesive tape is slowly torn;
(3) repeating step is (2) 3～10 times, until the graphite flake on adhesive tape is evenly distributed;
(4) carefully the adhesive tape with graphene platelet is attached on the silicon chip of silicon-dioxide zone of oxidation, squeeze gently the air between adhesive tape and silicon chip, silicon chip and adhesive tape are attached completely, after pushing gently 10min, adhesive tape is slowly torn from silicon chip surface, thereby obtain being attached to the graphene sheet layer on silicon chip.
Preferably, the power of the described laser irradiation of step (3) is 3～15mW, and wavelength is 500～800nm; The diameter of laser facula is 1～5 μ m, and the laser irradiation time is 5～100s.
As optimal technical scheme, the method that generates fold on graphene sheet layer provided by the invention comprises the steps:
(1) will after silicon chip washing, use drying for standby; Then by polystyrene heating for dissolving in organic solvent, preparation polystyrene solution; Afterwards polystyrene solution is spun on silicon chip, dries and obtain polystyrene layer;
(2) use micromechanical forces stripping method that Graphene is stripped on the above-mentioned silicon chip that has a polystyrene layer;
(3) load there is is the silicon chip of single-layer graphene be for example placed in, under the laser optical system (laser Raman spectrometer) with opticmicroscope, by opticmicroscope, find Graphene position, then utilize the laser of laser optical system to carry out irradiation to above-mentioned Graphene, obtain the Graphene with pleated structure.
On the other hand, the invention provides the graphene sheet layer with fold that a kind of foregoing method prepares, the fold position of described graphene sheet layer is controlled;
Preferably, the fold of described graphene sheet layer is positioned at edge or the centre of graphene sheet layer.
When the middle part of laser irradiation graphene sheet layer, the polystyrene of laser facula corresponding zone is melted, the graphene sheet layer of laser facula corresponding zone subsides, and makes the graphene sheet layer outside laser facula corresponding zone bear certain stress of pullling, thereby produces fold.
Compared with prior art, the present invention has following beneficial effect:
(1) method that generates fold on graphene sheet layer provided by the invention, can control the generation position of fold, both can generate fold at the edge of graphene sheet layer, also can generate fold in the middle part of graphene sheet layer;
(2) method that generates fold on graphene sheet layer provided by the invention, easy and simple to handle, operational condition is easily controlled.
Accompanying drawing explanation
Fig. 1 is the local atomic power shape appearance figure of the graphene sheet layer with fold that obtains of embodiment 1; In figure, fine strip shape projection is pleated structure;
Fig. 2 is the Local Phase bitmap of the graphene sheet layer with fold that obtains of embodiment 1; In figure, fine strip shape projection is pleated structure.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
On graphene sheet layer, generate a method for fold, described method comprises the steps:
(1) by silicon chip after acetone and absolute ethanol washing, with nitrogen, dry up standby;
By weight-average molecular weight, be 100 * 10
3polystyrene heating for dissolving in chlorobenzene, the preparation mass concentration polystyrene solution that is 5%;
Polystyrene solution is spun on silicon chip, at 180 ℃, dries and obtain polystyrene layer, thickness is 230nm;
(2) use micromechanical forces stripping method Graphene to be stripped on the silicon chip of the polystyrene layer that step (1) obtains;
(3) load there is is the silicon chip of graphene sheet layer be placed under the laser optical system (Reinshaw inVia laser Raman spectrometer) with opticmicroscope, by opticmicroscope, find graphene sheet layer position, then utilize the laser that wavelength is 514nm to carry out irradiation to described graphene sheet layer, laser power is 5mW, laser spot diameter is 1 μ m, irradiation time is 60s, can obtain the graphene sheet layer with pleated structure;
Performance test:
The graphene sheet layer with pleated structure preparing is characterized by atomic force microscope, as depicted in figs. 1 and 2, Fig. 1 is the local atomic power shape appearance figure with the graphene sheet layer of pleated structure, and Fig. 2 is the Local Phase bitmap with the graphene sheet layer of pleated structure; Fine strip shape projection in Fig. 1 and Fig. 2 is the pleated structure in graphene sheet layer.
Embodiment 2
Be with the difference of embodiment 1:
The weight-average molecular weight of step (1) polystyrene used is 600 * 10
3, the polystyrene solution mass concentration of preparation is 3%; The thickness of polystyrene layer is 150nm;
Step (3) sharp light wavelength used is 633nm, and laser power is 10mW, and the laser irradiation time is 20s.
Embodiment 3
Be with the difference of embodiment 1:
The weight-average molecular weight of step (1) polystyrene used is 900 * 10
3, the polystyrene solution mass concentration of preparation is 8%; The thickness of polystyrene layer is 460nm;
Step (3) optical maser wavelength used is 785nm, and laser power is 15mW, and irradiation time is 90s.
Embodiment 4
On graphene sheet layer, generate a method for fold, described method comprises the steps:
(1) on silicon chip, form polystyrene layer;
Silicon chip, after acetone and absolute ethanol washing, is dried up standby with nitrogen;
By weight-average molecular weight, be 1000 * 10
3polystyrene heating for dissolving in toluene, the preparation mass concentration polystyrene solution that is 2%;
Polystyrene solution is spun on silicon chip, at 120 ℃, dries and obtain polystyrene layer, thickness is 100nm;
(2) use micromechanical forces stripping method Graphene to be stripped on the silicon chip of the polystyrene layer that step (1) obtains;
(3) take power as 3mW, wavelength is 500～800nm, and the diameter of hot spot is the graphene sheet layer 100s that the laser irradiation step (2) of 1 μ m obtains, and obtains fold.
Embodiment 5
On graphene sheet layer, generate a method for fold, described method comprises the steps:
(1) on silicon chip, form polystyrene layer;
Silicon chip, after acetone and absolute ethanol washing, is dried up standby with nitrogen;
By weight-average molecular weight, be 300 * 10
3polystyrene heating for dissolving in toluene, the preparation mass concentration polystyrene solution that is 20%;
Polystyrene solution is spun on silicon chip, at 200 ℃, dries and obtain polystyrene layer, thickness is 500nm;
(2) use micromechanical forces stripping method Graphene to be stripped on the silicon chip of the polystyrene layer that step (1) obtains;
(3) take power as 10mW, wavelength is 500～800nm, and the diameter of hot spot is the graphene sheet layer 5s that the laser irradiation step (2) of 5 μ m obtains, and obtains fold.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. on graphene sheet layer, generate a method for fold, it is characterized in that, described method is to utilize laser to carry out irradiation to the graphene sheet layer covering on polystyrene layer, obtains fold.
2. the method for claim 1, is characterized in that, described laser power is 3～15mW.
3. method as claimed in claim 1 or 2, is characterized in that, described optical maser wavelength is 500～800nm, preferred 514～785nm, further preferred 514nm, in 633nm or 785nm any 1;
Preferably, the diameter of described laser facula is 1～5 μ m;
Preferably, the described laser irradiation time is 5～100s;
Preferably, the weight-average molecular weight of described polystyrene is 100 * 10
3～1000 * 10
3, preferably 200 * 10
3～500 * 10
3;
Preferably, the thickness of described polystyrene lamella is 100～500nm.
4. the method as described in one of claim 1～3, is characterized in that, described method comprises the steps:
(1) on silicon chip, form polystyrene layer;
(2) on the polystyrene layer that transfer graphene sheet layer to step (1) obtains;
(3) graphene sheet layer that laser irradiation step (2) obtains, obtains fold.
5. method as claimed in claim 4, is characterized in that, the described method that forms polystyrene layer on silicon chip of step (1), for polystyrene solution is spun on silicon chip, is dried and obtained polystyrene layer;
Preferably, the thickness of described polystyrene layer is 100～500nm.
6. method as claimed in claim 5, is characterized in that, the weight-average molecular weight of described polystyrene is 100 * 10
3～1000 * 10
3, preferably 200 * 10
3～500 * 10
3;
Preferably, the mass concentration of described polystyrene solution is 2～20%;
Preferably, to obtain the bake out temperature of polystyrene layer be 120～200 ℃ in described oven dry.
7. the method as described in one of claim 4～6, is characterized in that, before the described silicon chip of step (1) is used, cleans;
Preferably, described cleaning as drying up scavenging solution with nitrogen after ultrasonic cleaning.
8. the method as described in one of claim 4～7, is characterized in that, the method for the described transfer graphene sheet layer of step (2) is micromechanical forces stripping method.
9. the method as described in one of claim 4～8, is characterized in that, the power of the described laser irradiation of step (3) is 3～15mW, and wavelength is 500～800nm; The diameter of laser facula is 1～5 μ m, and the laser irradiation time is 5～100s.
10. the graphene sheet layer with fold that the method as described in one of claim 1～9 prepares, is characterized in that, the fold position of described graphene sheet layer is controlled;
Preferably, the fold of described graphene sheet layer is positioned at edge or the centre of graphene sheet layer.
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| CN104477886A (en) * | 2014-11-20 | 2015-04-01 | 中山大学 | Folded graphene and controllable preparation method thereof |
| CN105261671A (en) * | 2015-09-08 | 2016-01-20 | 苏州华维纳纳米科技有限公司 | Method for preparing thin-film antireflection structure employing laser direct writing |
| CN106093000A (en) * | 2016-05-31 | 2016-11-09 | 中山大学 | A kind of stretchable surface reinforced Raman active substrate and preparation method thereof |
| CN107117607A (en) * | 2017-06-20 | 2017-09-01 | 成都新柯力化工科技有限公司 | It is a kind of that the method that stripping prepares graphene is classified based on ray |
| CN110734037A (en) * | 2019-10-25 | 2020-01-31 | 哈尔滨工业大学 | Construction method of polymer material surface fold structure |
| WO2020151276A1 (en) * | 2019-01-21 | 2020-07-30 | 广东工业大学 | Method and device for processing polystyrene and graphene nanocomposite microstructure array |
| CN114768104A (en) * | 2022-03-24 | 2022-07-22 | 安徽格兰科新材料技术有限公司 | Preparation method of graphene heating body with adjustable broadband thermal radiation emissivity |
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| CN106093000A (en) * | 2016-05-31 | 2016-11-09 | 中山大学 | A kind of stretchable surface reinforced Raman active substrate and preparation method thereof |
| CN107117607A (en) * | 2017-06-20 | 2017-09-01 | 成都新柯力化工科技有限公司 | It is a kind of that the method that stripping prepares graphene is classified based on ray |
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| WO2020151276A1 (en) * | 2019-01-21 | 2020-07-30 | 广东工业大学 | Method and device for processing polystyrene and graphene nanocomposite microstructure array |
| CN110734037A (en) * | 2019-10-25 | 2020-01-31 | 哈尔滨工业大学 | Construction method of polymer material surface fold structure |
| CN110734037B (en) * | 2019-10-25 | 2023-01-24 | 哈尔滨工业大学 | Method for constructing surface fold structure of high polymer material |
| CN114768104A (en) * | 2022-03-24 | 2022-07-22 | 安徽格兰科新材料技术有限公司 | Preparation method of graphene heating body with adjustable broadband thermal radiation emissivity |
| CN114768104B (en) * | 2022-03-24 | 2023-03-21 | 安徽格兰科新材料技术有限公司 | Preparation method of graphene heating body with adjustable broadband thermal radiation emissivity |
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