CN111497366B - Interface-controllable non-layered multi-level graphene conformal folds and preparation method thereof - Google Patents
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Abstract
An interface-controllable non-layered multi-level graphene conformal fold and a preparation method thereof are disclosed, wherein a PMMA layer is coated on the surface of germanium-based graphene grown by a CVD method in a spinning mode, a germanium sheet/graphene/PMMA composite structure is placed in a container in a mode that PMMA faces upwards, uncured PDMS mixture is poured in for a post-curing process and a gradient interface layer is formed, a germanium sheet is etched, and finally a sample which is cleaned and fully dried in the air is triggered to form the multi-level graphene conformal fold by a method of heating and loading mechanical stress. The multilayer hard film-soft base system prepared by introducing the PDMS post-curing process has strong interface strength between different layers, and generates high-quality non-layered and multi-scale graphene conformal wrinkle patterns under the action of heating and mechanical stress. A Raman spectrum detection means is used for verifying that the graphene keeps a high-quality single layer in the transfer process. In addition, the method is not only suitable for the graphene two-dimensional material, but also suitable for preparing conformal folds of other two-dimensional materials.
Description
Technical Field
The invention relates to a technology in the field of graphene, in particular to an interface-controllable non-layered multi-level graphene conformal fold and a preparation method thereof.
Background
Due to the fact that the functional surface of the graphene wrinkle has excellent characteristics of large specific surface area, remarkable bearing capacity, abnormal chemical activity, adjustable wettability, chemical transmittance and the like, the graphene wrinkle is widely applied to the fields of flexible electronics, nano-electromechanical systems (NEMS), flexible sensing and actuators, energy storage devices and the like. At present, graphene wrinkles mainly include the following three types: the method comprises the steps of drawing stress induced single-layer graphene wrinkles, double-layer graphene wrinkles with graphene as a surface hard layer, and multi-layer graphene conformal wrinkles with graphene compounded with an intermediate layer as a surface hard layer. Compared with graphene folds in a single-layer system and a double-layer system, the conformal folds in the multi-layer system can control key characteristic parameters such as wavelength, direction and amplitude of the graphene folds by controlling the thickness of the intermediate layer. One of the conformal wrinkle triggering conditions within the hierarchy is: good conformal contact between different layers. However, interfacial slippage and partial separation phenomena between graphene and the substrate can greatly inhibit wrinkle formation, limit the long-term stability of the wrinkle pattern, and can even lead to overall device failure.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an interface-controllable non-layered multilayer graphene conformal fold and a preparation method thereof, which can ensure that the interface between graphene and polymethyl methacrylate (PMMA) and the interface between PMMA and Polydimethylsiloxane (PDMS) have enough interface adhesion energy, so that the non-layered graphene conformal fold is prepared in a three-layer system.
The invention is realized by the following technical scheme:
the invention relates to a non-layered multi-level graphene conformal fold, which is a composite structure of surface folds formed by a PDMS layer, a PMMA layer and a graphene layer in sequence, wherein: a gradient interface layer is arranged between the PMMA layer and the PDMS layer, and the gradient interface is formed by combining a PDMS molecular chain and a PMMA molecular chain in the curing process of the PDMS layer so as to improve the interface adhesion energy.
The invention relates to a preparation method of a non-layered multi-level graphene conformal wrinkle, which comprises the steps of spin-coating a PMMA layer on the surface of germanium-based graphene grown by Chemical Vapor Deposition (CVD), placing a germanium sheet/graphene/PMMA composite structure in a container in a manner that PMMA faces upwards, pouring an uncured PDMS mixture for post-curing process and forming a gradient interface layer, etching a germanium sheet, and triggering the multi-level graphene conformal wrinkle by heating and loading a mechanical stress method on a sample which is cleaned and fully dried in the air.
The spin coating is to coat the PMMA solution on the surface of the graphene by a spin coater at a speed of 3000-5000 rpm.
The post-curing process specifically comprises the steps of mixing the oligomer and the cross-linking agent in a ratio of 10:1, slowly pouring the mixture into a container with a germanium/graphene/PMMA composite structure, and heating the mixture in a heating furnace for four hours at 70 ℃ to fully cure PDMS.
The etching germanium sheet is obtained by adopting HF H to the sample stripped of PDMS glue2O2:H2And (3) preparing an etching solvent at a ratio of 1:1:10 for etching for 2-3 hours, and fully etching away the residual germanium sheet.
The heating is carried out for 5-10 minutes at 70-120 ℃ by adopting a heating table, and different thermal stresses and wrinkle amplitudes are controlled by controlling the heating temperature.
The mechanical stress is uniaxial compressive stress and biaxial compressive stress loaded on the sample, and the amplitude of the wrinkles is controlled by controlling the magnitude of the compressive stress.
The gradient interface layer is formed by accelerating the molecular chain movement of uncured PDMS in the high-temperature curing process, so that the PDMS molecular chain moves to the PMMA layer.
The maximum interface stress which can be borne by the gradient interface is
Wherein:
is the modulus of elasticity of the surface layer,
is the modulus of elasticity of the substrate,νsis the poisson's ratio of the substrate.
The invention relates to application of the interface-controllable multi-level graphene conformal folds, which are applied to the aspects of diffraction gratings, surface wettability regulation and control methods of micro-nano devices, chemical modification and modification technologies and the like in the field of optical communication.
Technical effects
The method integrally solves the problem that the interface adhesion energy between layers is insufficient in the preparation process of the multi-layer graphene folds, so that the layering failure is caused between layers;
compared with the prior art, the gradient interface is formed between the PDMS layer and the PMMA/graphene layer, the multi-layer hard film-soft base system prepared by adopting the curing process has strong interface strength between different layers, and high-quality non-layering multi-scale graphene conformal fold patterns are generated under the action of heating and mechanical stress. A Raman spectrum detection means is used for verifying that the graphene keeps a high-quality single layer in the transfer process. In addition, the method is not only suitable for the graphene two-dimensional material, but also suitable for preparing conformal folds of other two-dimensional materials.
Drawings
FIG. 1 is a flow chart of the preparation process of this example;
in the figure: the preparation method comprises the following steps of (1) a germanium sheet, a graphene layer 2, a PMMA layer 3, a container 4, PDMS5, an etching solvent 6, a PMMA molecular chain 7 and a PDMS molecular chain 8;
FIG. 2 is a schematic view of the distribution of polymer chains between PMMA and PDMS;
in the figure: a is a schematic diagram of a traditional wet transfer method; b is a schematic diagram of the embodiment;
FIG. 3 is a comparative graph of samples subjected to compressive stress;
in the figure: c is an action graph of the compressive stress; d is a layering schematic diagram formed by the traditional wet transfer method; e is a schematic view of the surface wrinkles formed in the embodiment; a surface hard layer 9 and a soft substrate 10;
FIG. 4 is a cross-sectional view of the LSCM of this embodiment;
in the figure: f. g and h are three different positions.
Detailed Description
As shown in fig. 1, the non-delamination multi-level graphene conformal wrinkles are obtained by the following steps:
firstly, growing a high-quality single-layer graphene layer 2 on a crystal face of a germanium sheet 1 by a CVD method.
② the PMMA solution with the concentration of 120mg/mL is spin-coated on the graphene for 30 seconds at the speed of 5000rpm, and is heated for 10 minutes at 115 ℃ to form the PMMA layer 3.
③ mixing the PDMS5 oligomer and the cross-linking agent in a mass ratio of 10:1, and removing air bubbles in vacuum.
Putting the PMMA/graphene/germanium sheet into a container 4, slowly pouring the uncured PDMS5 mixed liquid prepared in the third step into the container 4, and putting the whole container 4 into a heating furnace to heat for four hours at 70 ℃.
Fifthly, washing off residual PDMS5 formed by the infiltration of the liquid on the rough surface of the germanium sheet 1 in the third step.
Sixthly, after the curing, placing the PDMS 5/PMMA/graphene/germanium sheet 1 composite structure stripped of the residual PDMS5 into a container 4, and adopting HF H2O2:H2And etching the germanium sheet for 1 to three hours by using an etching solvent 6 prepared in a ratio of 1:1:10 of 0 to obtain the PDMS 5/PMMA/graphene composite structure.
And seventhly, placing the PDMS 5/PMMA/graphene composite structure obtained in the step (sixthly) into deionized water for cleaning, and fully drying in the air.
Heating the PDMS 5/PMMA/graphene composite structure to over 70 ℃ to trigger the multi-scale graphene conformal folds.
As shown in fig. 2a, the interface between the PMMA layer and the PDMS layer in the graphene/PMMA/PDMS sample obtained by the conventional wet transfer is obvious; as shown in fig. 2b, a gradient interface layer exists between the PMMA layer 3 and the PDMS5 layer of the graphene co-type wrinkled sample obtained by post-curing transfer, and the gradient interface layer is formed by accelerating the molecular chain movement of uncured PDMS5 in the high-temperature curing process, so that the PDMS molecular chain 8 moves to the PMMA layer 3 and is combined with the PMMA molecular chain 7.
As shown in fig. 3, a graphene/PMMA/PDMS sample obtained by conventional wet transfer is delaminated due to insufficient interfacial adhesion energy under uniaxial compressive stress, as shown in fig. 3 d; under the action of uniaxial compressive stress, a graphene/PMMA/PDMS 5 sample obtained by post-curing transfer generates a gradient interface layer and enough interface adhesion energy due to a post-curing process, so that delamination caused by desorption is not generated between PMMA and PDMS5, and only a surface wrinkle phenomenon occurs, as shown in fig. 3e, a surface hard layer 9 and a soft substrate 10 are tightly attached without separation.
The interface between the PMMA and PDMS prepared by the traditional wet transfer method can bear the maximum interface stress, and the following requirements are met:
wherein:
and
critical stresses generated by buckling-induced delamination and surface-destabilization-induced wrinkling, respectively; the interface between the PMMA layer 3 and the PDMS5 layer of the post-cured sample provided by the invention can bear the maximum interface stress, and the following requirements are met:
wherein:
is the modulus of elasticity of the surface layer,
is the elastic modulus, v, of the substratesIs the poisson's ratio of the substrate.
As shown in fig. 4f to 4h, the cross-sectional geometries of the multi-scale graphene co-formed wrinkles at three different positions are measured by a confocal laser microscope, and as shown in the figure, the wavelength and the amplitude of the graphene co-formed wrinkles are multi-scale.
In this embodiment, the experimental sample obtained by the above preparation process is heated to 110 ℃, cooled to room temperature, and measured by a Laser Scanning Confocal Microscope (LSCM), a multi-scale graphene co-form fold with an amplitude of 10 nm to 2 microns and a wavelength of 5 microns to 100 microns is obtained, and no delamination failure behavior is observed.
Compared with the traditional wet transfer technology, the post-curing process provided by the invention can introduce a gradient interface layer, and the gradient interface layer is formed by utilizing the diffusion capability enhancement effect of uncured PDMS high molecular molecules at high temperature, so that the sufficient interface adhesion energy is ensured, the interface strength between sample layers is evaluated by the buckling surface instability theory, and the phenomenon of layering is avoided, and the continuity of wrinkle patterns is prevented from being influenced.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. The utility model provides a conformal fold of no layered multi-level graphene which characterized in that, the composite construction of the surface fold that forms by PDMS layer, PMMA layer and graphite alkene layer in proper order, wherein: a gradient interface layer is arranged between the PMMA layer and the PDMS layer, and the gradient interface layer is formed by combining a PDMS molecular chain and a PMMA molecular chain in the curing process of the PDMS layer so as to improve the interface adhesion energy.
2. The preparation method of the multi-layer graphene conformal wrinkles as claimed in claim 1, wherein a PMMA layer is spin-coated on the surface of germanium-based graphene grown by a CVD method, a germanium sheet/graphene/PMMA composite structure is placed in a container in a manner that PMMA faces upwards, uncured PDMS mixture is poured to perform a post-curing process and form a gradient interface layer, the germanium sheet is etched, and finally the multi-layer graphene conformal wrinkles are triggered by a method of heating and loading mechanical stress on a sample which is cleaned and fully dried in air;
the gradient interface layer is formed by accelerating the molecular chain movement of uncured PDMS in the curing process so that the PDMS molecular chain moves to the PMMA layer.
3. The method as claimed in claim 2, wherein the spin coating is carried out by applying the PMMA solution on the surface of the graphene by a spin coater at a speed of 3000-5000 rpm.
4. The method as claimed in claim 2, wherein the post-curing process comprises mixing the oligomer and the cross-linking agent at a ratio of 10:1, slowly pouring the mixture into a container with a germanium sheet/graphene/PMMA composite structure, and heating the mixture in a heating furnace at 70 ℃ for four hours to fully cure the PDMS.
5. The method as claimed in claim 2, wherein the heating is performed by heating the sheet at 70-120 ℃ for 5-10 minutes in a heating stage, and the heating temperature is controlled to control the different thermal stresses and the wrinkle amplitudes.
6. The method of claim 2, wherein the mechanical stress is uniaxial or biaxial compressive stress applied to the sample, and the amplitude of the wrinkles is controlled by controlling the magnitude of the compressive stress.
7. The method of claim 2, wherein said gradient interface is capable of withstanding a maximum interface stress of
Wherein:
is the modulus of elasticity of the surface layer,
is the elastic modulus, v, of the substratesIs the poisson's ratio of the substrate.
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| CN104597230A (en) * | 2015-01-29 | 2015-05-06 | 国家纳米科学中心 | Functional polymer thin film, preparation method and application thereof |
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| CN109627476A (en) * | 2018-11-30 | 2019-04-16 | 国家纳米科学中心 | A kind of two-dimensional material and its preparation method and application with orderly fold strain structure |
| CN110155961A (en) * | 2018-06-25 | 2019-08-23 | 中国科学院物理研究所 | A method of preparing stratified material fold |
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| KR101680761B1 (en) * | 2010-09-17 | 2016-11-30 | 삼성전자주식회사 | Graphene-polymer layered composite and process for preparing the same |
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Patent Citations (7)
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|---|---|---|---|---|
| JP2014034503A (en) * | 2012-08-10 | 2014-02-24 | Fuji Electric Co Ltd | Method for producing graphene film and graphene film |
| CN104477886A (en) * | 2014-11-20 | 2015-04-01 | 中山大学 | Folded graphene and controllable preparation method thereof |
| CN104597230A (en) * | 2015-01-29 | 2015-05-06 | 国家纳米科学中心 | Functional polymer thin film, preparation method and application thereof |
| CN106883438A (en) * | 2017-02-24 | 2017-06-23 | 天津大学 | A kind of controllable method for preparing of the chill mark micro-structural of photoresponse type |
| CN107607240A (en) * | 2017-08-31 | 2018-01-19 | 上海交通大学 | Graphene mechanical property synchronous meter sign implementation method based on fold formation basic theory |
| CN110155961A (en) * | 2018-06-25 | 2019-08-23 | 中国科学院物理研究所 | A method of preparing stratified material fold |
| CN109627476A (en) * | 2018-11-30 | 2019-04-16 | 国家纳米科学中心 | A kind of two-dimensional material and its preparation method and application with orderly fold strain structure |
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