CN110673247A - Flexible grating with composite structure, preparation method and application thereof - Google Patents
Flexible grating with composite structure, preparation method and application thereof Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
- G02B5/1852—Manufacturing methods using mechanical means, e.g. ruling with diamond tool, moulding
Abstract
The invention discloses a flexible grating with a composite structure, a preparation method and application thereof. The preparation method comprises the following steps: preparing a rigid-flexible double-layer film with a rigid layer with uniform thickness in a flexible thin film on a rigid substrate; peeling the rigid-flexible double-layer film from the substrate to enable the surface of the rigid layer of the rigid-flexible double-layer film to generate parallel equal-width cracks; and uniformly stretching the rigid-flexible double-layer film along the direction vertical to the crack to enable the surface of the rigid layer of the rigid-flexible double-layer film to generate folds with orderly appearance and height vertical to the crack, so as to form a micro-nano structure with the folds vertically orthogonal to the crack, and obtain the flexible orthogonal composite sinusoidal grating and rectangular grating. The method effectively manages the crack distribution in the surface microstructure of the rigid-flexible double-layer film, so that the orientation of the cracks which are inevitably and randomly distributed is along a specific direction, the intervals of the cracks are uniform, and common defects in a fold structure, such as inconsistent appearance, inconsistent structures at two sides of the cracks and the like, are eliminated.
Description
Technical Field
The invention relates to a flexible grating, in particular to a flexible grating with a composite structure and a preparation method and application thereof, belonging to the technical field of flexible electronics and nano technology.
Background
Currently, flexible electronic devices and wearable devices are in the key period of practical application, and for example, flexible display screens (including mobile phone screens and television screens) are already in the commercial stage. However, most of the core components of the existing flexible electronic devices are still rigid and inflexible. For example, it has been reported that modules such as CPUs of foldable cellular phones are still formed of conventional silicon (Si) -based devices. In general, we are currently doing much more work away from the commercial applications that enable truly flexible electronics. The most critical of these is: flexible semiconductor devices that can replace traditional silicon (Si) -based devices are sought. However, in addition to the construction and fabrication of flexible semiconductor devices, many other flexible elements are required, which are all essential components for the fabrication of flexible electronic devices. This is the most critical component than a transistor or diode with Si as the semiconductor layer in conventional electronics, but Si-based devices alone are far from adequate for carrying the entire modern electronic circuitry. There is still a need for devices that receive or transmit signals (a special metal structure), devices that control the propagation of signals or light (e.g., gratings), etc. For the same reason, in addition to finding a flexible semiconductor device that can replace the Si device, we need to fabricate some other components necessary for the flexible electronic circuit in our way to realize commercial application of flexible electronic devices. Among these, a flexible information transmission device, i.e., a flexible grating, is indispensable.
The ordered micro-nano structure is a reliable flexible grating. Unlike conventional electronic circuits, flexible electronics require gratings that must also have the basic properties of flexibility, stretchability, etc. And the PDMS (poly (dimethylsiloxane) film-based micro-nano structure can just meet the requirements, so the micro-nano structure has high attention in the field of flexible electronics. At present, a PDMS film-based flexible micro-nano structure is mainly prepared by two methods. The first approach is related to the good tensile properties of PDMS films. Firstly, a double-layer film system of a PDMS film and a rigid film is prepared, and then a self-assembled microstructure is induced on the surface of the double-layer film through mechanical control or thermal treatment by utilizing the characteristic that the stress response of the two films in the double-layer film is not matched. The second method mainly utilizes the castable characteristic of PDMS pre-polymerized liquid (PDMS main liquid and cross-linking agent mixed liquid), the PDMS mixed liquid is poured on a template with a microstructure, and after solidification, the microstructure can be copied on the surface of the PDMS film.
The existing method relies on the inconsistent stress response characteristic of a rigid-flexible double-layer membrane system, and a fold structure is self-assembled on the surface under heating or mechanical stretching/extrusion, so that the structure is used as a flexible grating. However, the reported flexible grating mainly has the problem that a great number of defects exist in the structure, such as inconsistent morphology of folds, wherein the most critical point is that the fold structure is mixed with randomly distributed crack structures under the external control. Due to the interfering effect of random cracks on light propagation, it has been reported that such corrugated structures have practically no practical application value in the field of light propagation manipulation.
The inconsistency of the wrinkle morphology is caused by the non-uniformity of any film property of the rigid-flexible double-layer film, such as the non-uniformity of the thickness of the rigid layer film. In addition, due to the determination of the surface self-assembly characteristic of the rigid-flexible double-layer film, when the surface of the double-layer film is subjected to self-assembly to form wrinkles under external control, cracks which are randomly distributed inevitably appear.
So in order to eliminate the disturbing effect of such cracks on light propagation, it is only possible to better manage such cracks. For example, ordering the distribution of such cracks. Effective management of the morphology of the wrinkles and the distribution of cracks, and elimination of defects in such microstructures as far as possible, are the direction in which researchers in the industry have been working for a long time.
Disclosure of Invention
The invention mainly aims to provide a flexible grating with a composite structure and a preparation method thereof, so as to overcome the defects of the prior art.
Another object of the present invention is to provide the use of said flexible grating with a composite structure.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a flexible grating with a composite structure, which comprises the following steps:
preparing a rigid-flexible double-layer film with a rigid layer with uniform thickness on a substrate;
peeling the rigid-flexible double-layer film from the substrate to enable the surface of the rigid layer of the rigid-flexible double-layer film to generate parallel equal-width cracks; and the number of the first and second groups,
and uniformly stretching the rigid-flexible double-layer film along the direction vertical to the crack, so that folds with ordered appearance and height perpendicular to the crack are generated on the surface of the rigid layer of the rigid-flexible double-layer film, a micro-nano structure with the folds perpendicular to the crack is formed, and the flexible orthogonal composite sinusoidal grating and rectangular grating are prepared.
The embodiment of the invention also provides the flexible grating with the composite structure prepared by the method.
The embodiment of the invention also provides application of the flexible grating with the composite structure in the field of flexible electronic devices.
Compared with the prior art, the invention has the advantages that at least:
1. the preparation method of the flexible grating with the composite structure effectively manages the crack distribution in the surface microstructure of the rigid-flexible double-layer film, so that the orientation of randomly distributed cracks is along a specific direction, and the intervals of the cracks are uniform;
2. according to the invention, the high-quality rigid-flexible double-layer film is prepared, the parallel equal-width cracks are prepared on the rigid-flexible double-layer film by using a peeling method, the corrugated structure with ordered appearance and height can be prepared in the direction vertical to the cracks by further uniform stretching, and common defects in the corrugated structure, such as inconsistent appearance, inconsistent two-layer structure of the cracks and the like, are eliminated.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a process for preparing a rigid-flexible double-layer film with a uniform thickness of a thin rigid layer under uniform plasma treatment in an exemplary embodiment of the invention.
Fig. 2 a-2 d are schematic diagrams of a process for peeling a rigid-flexible bilayer film from a substrate according to an exemplary embodiment of the present invention.
FIG. 3 is a confocal laser microscopy image of surface microstructure of the surface of the rigid-flexible overlayer after delamination in a relaxed and 40% stretched state in accordance with an exemplary embodiment of the invention.
Detailed Description
The inventor of the present invention can detect the technical scheme of the present invention through long-term research and practice, and the main purpose of the present invention is to prepare an orthogonal composite phase sine grating and a phase rectangular grating by depending on the inconsistent stress response characteristic of a rigid-flexible double-layer membrane system, wherein the flexible composite grating is prepared for the first time. The technical solution, its implementation and principles, etc. will be further explained as follows.
Some terms involved in the present invention are explained as follows:
phase sine grating: a periodic sinusoidal structure.
Phase rectangular grating: a periodic groove structure.
As one aspect of the technical solution of the present invention, a method for manufacturing a flexible grating having a composite structure includes:
preparing a rigid-flexible double-layer film with a rigid layer with uniform thickness on a substrate;
peeling the rigid-flexible double-layer film from the substrate to enable the surface of the rigid layer of the rigid-flexible double-layer film to generate parallel equal-width cracks; and the number of the first and second groups,
and uniformly stretching the rigid-flexible double-layer film along the direction vertical to the crack, so that folds with ordered appearance and height perpendicular to the crack are generated on the surface of the rigid layer of the rigid-flexible double-layer film, a micro-nano structure with the folds perpendicular to the crack is formed, and the flexible orthogonal composite sinusoidal grating and rectangular grating are prepared.
Further, the cracks are oriented in a selected direction and the crack spacing is uniform.
Further, the folds have a consistent sinusoidal shape, and the folds on both sides of the crack correspond one to one.
As one of the preferred embodiments, the preparation method comprises: when the stretching of the rigid-flexible double-layer film is stopped, the wrinkle structure of the rigid layer surface of the rigid-flexible double-layer film is kept unchanged, and when the stretching degree is 0%, the wrinkle of the rigid layer surface of the rigid-flexible double-layer film disappears and the rigid-flexible double-layer film completely returns to the initial state before stretching.
As one of the preferred embodiments, the preparation method comprises: the rigid-flexible double-layer film is prepared by any one method of directly treating the flexible film by adopting oxygen plasma, evaporating and plating rigid substances on the flexible film, directly treating the flexible film by ultraviolet light or ozone, irradiating the flexible film by electron beams or heavy ion beams, directly treating the flexible film by strong acid or strong alkali, spin-coating two substances with different elastic moduli and the like.
For example, the method for preparing the rigid-flexible bilayer film is preferably a method of directly treating the PDMS thin film with oxygen plasma, but not only this, for example, there are various methods as follows:
1) depositing inorganic matters or organic matters which are rigid after film formation on the flexible film through evaporation to form a rigid-flexible double-layer film;
2) attaching a rigid film to a flexible film by adopting an attaching method to prepare a rigid-flexible double-layer film;
3) directly treating the flexible film by using UV/ozone to prepare a rigid-flexible double-layer film;
4) preparing a rigid-flexible double-layer film by irradiating the flexible film with electron beams and heavy ion beams;
5) directly treating the flexible film by strong acid and strong base to directly prepare a rigid-flexible double-layer film;
6) an organic film having a modulus of elasticity which is not uniform with that of the flexible film after film formation is spin-coated on the flexible film by a spin coating method.
Further, the flexible film may be a PDMS film, or may be any other flexible film.
In some more specific embodiments, the method for preparing the rigid-flexible double-layer film specifically comprises the following steps:
providing a substrate, and modifying the substrate by adopting a modifying material capable of reducing the activation energy of the substrate so as to form a modifying layer on the surface of the substrate;
preparing a flexible film on the surface of the modification layer of the substrate by adopting a spin-coating method, wherein the flexible film is made of polydimethylsiloxane; and the number of the first and second groups,
and directly treating the flexible film by adopting oxygen plasma, thereby preparing a silicon oxide layer with uniform thickness on the surface of the flexible film.
Further, to produce a rigid-flexible double-layer film having a silicon oxide layer with a uniform thickness, the following two conditions need to be satisfied. One is that the oxygen plasma treatment must be uniform. To achieve this, the invention chooses an apparatus with a plasma treatment chamber having the following characteristics: the plane of the plasma source is parallel to the sample bearing table surface. The device can ensure that the same distance is kept between any position of the surface of the sample and the plasma source, and ensures the uniformity of the plasma on the surface of the sample. Further, the oxygen plasma treatment conditions are: the plasma source plane is parallel to the flexible membrane surface. In a second aspect, the properties of the PDMS flexible film are made isotropic.
Further, the preparation method comprises the following steps:
uniformly mixing polydimethylsiloxane and a cross-linking agent, and stirring for more than 10min to obtain a precursor solution; and the number of the first and second groups,
and applying the precursor solution to the surface of the modified layer of the substrate by adopting a spin coating method, and then curing to obtain the flexible film.
Further, the preparation method comprises the following steps: modifying the substrate for 30-90 min in a vacuum environment at 30-60 ℃ by adopting a modifying material capable of reducing the activation energy of the substrate. The surface of the substrate is modified by a modifying material capable of reducing the activation energy of the substrate, preferably by perfluorosilane (1H,1H,2H, 2H-perfluoroethylene), so that the bonding force between PDMS and the substrate is greatly reduced, and the rigid-flexible double-layer film can be conveniently stripped from the substrate.
Further, the substrate includes, but is not limited to, a rigid substrate such as a silicon wafer, a glass plate, a glass slide, and any rigid sheet such as a metal sheet.
In the stripping process of the invention, the strength and speed of stripping are also related to the occurrence of cracks. Therefore, the PDMS film is stressed uniformly as much as possible in the whole stripping process, and the stripping speed is kept consistent.
As one of the preferred embodiments, the preparation method specifically comprises: uniformly stripping the rigid-flexible double-layer film from the substrate at a uniform stripping speed (preferably 0.3-1 cm/s) and a uniform force (the applied force is larger than the bonding force between the film and the substrate, and the bonding force refers to intermolecular force between the film and the substrate), so that parallel cracks with equal width are generated on the surface of the rigid layer of the rigid-flexible double-layer film. The biggest characteristic of the crack array is that the cracks are parallel and equal in width.
As one of the preferred embodiments, the preparation method specifically comprises: and uniformly stretching the rigid-flexible double-layer film along the direction vertical to the crack by using uniform force. Wherein the applied force is approximately linear with the pleat amplitude.
The orthogonal crack and fold structures of the present invention are, in fact, typical orthogonal sinusoidal and rectangular gratings. The special feature of the grating is that all characteristic parameters can be regulated and controlled by mechanical stretching, such as the amplitude and the period of a sinusoidal structure and the width and the period of a rectangular structure, so that the optical manipulation behavior of the grating can be regulated and controlled by mechanical stretching.
As another aspect of the technical solution of the present invention, it also relates to a flexible grating having a composite structure prepared by the aforementioned method.
As another aspect of the technical solution of the present invention, it also relates to the application of the flexible grating with the composite structure in the field of flexible electronic devices.
In conclusion, the crack distribution in the surface microstructure of the rigid-flexible double-layer film is effectively managed, so that the orientation of the cracks which are inevitably and randomly distributed is along a specific direction, and the intervals of the cracks are uniform.
The technical solutions of the present invention will be described in further detail below with reference to several preferred embodiments and accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The test methods in the following examples, which are not specified under specific conditions, are generally carried out under conventional conditions.
Example 1
1. Preparation of rigid-flexible double-layer film with uniform thickness of rigid layer
In order to make the sinusoidal corrugation morphology consistent, a rigid-flexible double-layer film with a rigid layer with uniform thickness needs to be prepared. Firstly, the silicon wafer is decorated with primary perfluorosilane (trichloro (1H,1H,2H, 2H-perfluoroethylene)). Then, a PDMS film with any thickness is prepared by a spin coating method. Finally using O2The method for directly processing the PDMS film by the (oxygen) plasma is used for preparing the rigid-flexible double-layer film. Albeit O2The plasma treatment can oxidize the PDMS surface layer to form a silicon oxide layer in principle, but the following two conditions need to be satisfied in order to prepare a rigid-flexible double-layer film having a silicon oxide layer with a uniform thickness. One is that the plasma treatment must be uniform. To achieve this, the inventors have purposely selected an apparatus having a plasma processing chamber with the following characteristics: plasma source plane andthe sample support platforms were parallel. The device can ensure that the same distance is kept between any position of the surface of the sample and the plasma source, and ensures the uniformity of the plasma on the surface of the sample. In a second aspect, the properties of the PDMS film are made isotropic. The PDMS film is prepared by mixing two precursors (PDMS main liquid and cross-linking agent), stirring, and curing. During this process sufficient agitation (over 10 minutes) is necessary to allow sufficient mixing of the host liquid and the crosslinking agent.
The whole preparation process is shown in fig. 1, and after the preparation is strictly carried out according to the above process, a rigid-flexible double-layer film with a silicon oxide layer with uniform thickness is obtained. As shown in FIG. 1, under the uniform plasma treatment, a silicon oxide layer with uniform thickness appears on the surface of the isotropic PDMS film, and the blue layer represents a layer of perfluoro silane (1H,1H,2H, 2H-perfluoroethylene) modified on the surface of the silicon wafer.
2. Controlled preparation of cracks
The surface of the silicon wafer is modified by perfluorosilane (1H,1H,2H, 2H-perfluoroethylene), so that the bonding force between PDMS and the silicon wafer is greatly reduced. This facilitates peeling of the rigid-flexible bilayer film from the silicon wafer substrate. The modification condition selected in this example is that 10 μ l of perfluorosilane is continuously modified in a vacuum chamber at 30-60 ℃ for 30-90 min. The process of peeling is shown in fig. 2 a-2 d. The finished rigid-flexible bilayer film was first cut into equal width "tapes" with a razor blade (fig. 2 a). Then, an adhesive tape having the same width as the tape is attached to one end of the tape (FIG. 2 b). Then, the tape was held by a wide-head tweezers and peeled off at a constant speed at a peeling speed of 0.1cm/s to 1cm/s (FIG. 2 c). After peeling, the stretched "tape" was slowly released and the non-peeled portion was cut with a knife (FIG. 2 d). The inventors believe that the strength and speed of the peeling are also related to the occurrence of cracks. Therefore, the film is stressed uniformly as much as possible in the whole stripping process, and the stripping speed is kept consistent.
After the peeling-off in the above-mentioned steps, cracks having the same width in parallel appear on the rigid film side of the rigid-flexible double film. The biggest characteristic of the crack array is that the cracks are parallel and equal in width. If the rigid-flexible double-layer film is stretched along the direction vertical to the crack, a wrinkle vertical to the crack can appear on one side of the rigid film, a structure with the wrinkle vertical to the crack is formed, the surface microstructure pattern completely returns to the initial state after the surface microstructure pattern is relaxed, and as shown in fig. 3, the confocal laser microscope image of the surface microstructure is shown when the surface of the rigid-flexible upper-layer film is in a state of being relaxed and stretched by 40% after being peeled off. The folds have consistent sine-shaped appearance, the folds of the two layers of cracks correspond one to one, and the defects of uneven appearance and irregular distribution and arrangement are avoided.
Such orthogonal crack and corrugation structures are in fact typical of orthogonal sinusoidal and rectangular gratings. The special feature of the grating is that all characteristic parameters can be regulated and controlled by mechanical stretching, such as the amplitude and the period of a sinusoidal structure and the width and the period of a rectangular structure, so that the optical manipulation behavior of the grating can be regulated and controlled by mechanical stretching.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
It should be noted that the above-mentioned embodiments are only some of the embodiments of the present invention, and it is apparent to those skilled in the art that other variations and modifications can be made without departing from the inventive concept of the present invention, and these are within the scope of the present invention.
Claims (15)
1. A method for preparing a flexible grating with a composite structure is characterized by comprising the following steps:
preparing a rigid-flexible double-layer film with a rigid layer with uniform thickness on a substrate;
peeling the rigid-flexible double-layer film from the substrate to enable the surface of the rigid layer of the rigid-flexible double-layer film to generate parallel equal-width cracks; and the number of the first and second groups,
and uniformly stretching the rigid-flexible double-layer film along the direction vertical to the crack, so that folds with ordered appearance and height perpendicular to the crack are generated on the surface of the rigid layer of the rigid-flexible double-layer film, a micro-nano structure with the folds perpendicular to the crack is formed, and the flexible orthogonal composite sinusoidal grating and rectangular grating are prepared.
2. The method of claim 1, wherein: the orientation of the cracks is along the selected direction, and the crack spacing is uniform and consistent.
3. The method of claim 1, wherein: the folds have consistent sine-shaped appearance, and the folds on two sides of the crack correspond one to one.
4. The production method according to claim 1, characterized by comprising: when the stretching of the rigid-flexible double-layer film is stopped, the wrinkle structure of the rigid layer surface of the rigid-flexible double-layer film remains unchanged, and when the stretching degree is 0%, wrinkles disappear.
5. The production method according to claim 1, characterized by comprising: the rigid-flexible double-layer film is prepared by any one method of directly treating a flexible film by adopting oxygen plasma, evaporating and plating a rigid substance on the flexible film, directly treating the flexible film by ultraviolet light or ozone, irradiating the flexible film by an electron beam or heavy ion beam, directly treating the flexible film by strong acid or strong alkali and spin-coating two substances with different elastic moduli.
6. The preparation method according to claim 5, characterized by specifically comprising:
providing a substrate, and modifying the substrate by adopting a modifying material capable of reducing the activation energy of the substrate so as to form a modifying layer on the surface of the substrate;
preparing a flexible film on the surface of the modification layer of the substrate by adopting a spin-coating method, wherein the flexible film is made of polydimethylsiloxane; and the number of the first and second groups,
and directly treating the flexible film by adopting oxygen plasma, thereby preparing a silicon oxide layer with uniform thickness on the surface of the flexible film.
7. The production method according to claim 6, wherein the oxygen plasma treatment conditions are: the plasma source plane is parallel to the flexible membrane surface.
8. The method of claim 6, wherein: the flexible film has isotropy.
9. The production method according to claim 6, characterized by comprising:
uniformly mixing polydimethylsiloxane and a cross-linking agent, and stirring for more than 10min to obtain a precursor solution; and the number of the first and second groups,
and applying the precursor solution to the surface of the modified layer of the substrate by adopting a spin coating method, and then curing to obtain the flexible film.
10. The production method according to claim 6, characterized by comprising: modifying the substrate for 30-90 min in a vacuum environment at 30-60 ℃ by adopting a modifying material capable of reducing the activation energy of the substrate; preferably, the modifying material capable of reducing the activation energy of the substrate comprises perfluorosilane.
11. The production method according to claim 1 or 6, characterized in that: the substrate comprises a rigid substrate, preferably a silicon wafer, glass sheet, glass slide or metal foil.
12. The method according to claim 1, comprising: and under the conditions that the peeling speed is 0.1-1 cm/s and the applied force degree is greater than the intermolecular force between the film and the substrate, uniformly peeling the rigid-flexible double-layer film from the substrate, so that parallel equal-width cracks are generated on the surface of the rigid layer of the rigid-flexible double-layer film.
13. The method according to claim 1, comprising: and uniformly stretching the rigid-flexible double-layer film along the direction of the vertical crack, wherein the applied force degree is nearly linear with the wrinkle amplitude.
14. A flexible grating having a composite structure produced by the method of any one of claims 1-13.
15. Use of a flexible grating with a composite structure according to claim 14 in the field of flexible electronics.
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