KR101761010B1 - Nanotransfer printing method and surface-enhanced raman scattering substrate, surface-enhanced raman scattering vial and surface-enhanced raman scattering patch manufactured using the same - Google Patents
Nanotransfer printing method and surface-enhanced raman scattering substrate, surface-enhanced raman scattering vial and surface-enhanced raman scattering patch manufactured using the same Download PDFInfo
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- H—ELECTRICITY
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- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
- H01L21/02288—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating printing, e.g. ink-jet printing
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- H01L21/0271—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers
- H01L21/0273—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers characterised by the treatment of photoresist layers
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/702—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof of thick-or thin-film circuits or parts thereof
- H01L21/707—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof of thick-or thin-film circuits or parts thereof of thin-film circuits or parts thereof
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- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0657—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
- H01L29/0665—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body the shape of the body defining a nanostructure
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Abstract
According to an embodiment of the present invention, there is provided a nano-transfer printing method comprising: coating a polymer thin film on a template substrate having a surface pattern formed thereon; Fabricating the polymer thin film as a duplicate thin film mold using the polymer thin film and the adhesive film; Forming a nanostructure on the duplicate thin film mold; Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold; And transferring the nanostructure to a target object.
Description
The present invention relates to a nanotransfer printing method and a surface-enhanced Raman scattering substrate, a surface-enhanced Raman scattering vial and a SERS patch (surface-enhanced Raman scattering patch) More specifically, a polymer thin film is used to duplicate a surface pattern of a template substrate to fabricate a duplicate thin film mold, nanostructures are formed on a duplicate thin film mold, and a nanostructure is transferred to various target objects to form SERS Substrates, SERS vials or techniques for making SERS patches.
When light is emitted to a specific molecule, inelastic scattering occurs between the light and the molecule with a probability of 1/1000000, and the wavelength can be changed as the light component loses energy due to the component and structure of the molecule. Raman spectroscopy is a technique that uses this principle to launch a single wavelength laser on a molecule and analyze the intensity of the reflected light (Raman signal) by wavelength band to obtain information on the composition and structure of the molecule to be. This Raman spectroscopy technique is emerging as a next-generation analytical technology because it can perform fast, accurate and non-destructive analysis.
However, since Raman spectroscopy generates very low probability of inelastic scattering of 1/1000000, there is a disadvantage in that the intensity of reflected light is very weak. When the amount of molecules to be analyzed is very small, ), It is not suitable for the analysis of trace amounts of substances.
In order to solve the problem of low signal intensity, a method using a surface-enhanced Raman scattering (SERS) effect has been proposed. The SERS effect locally concentrates the light emitted by the surface plasmon resonance (SPR) effect of nanostructures such as Au or Ag, greatly increasing the intensity of light on the surface of the nanostructure It is a technique to increase the Raman signal obtained from the molecules adsorbed on the surface of the nanostructure to 103 to 1015 times.
The nanostructure using the SERS effect is generally placed on a flat substrate, and a small amount of molecules to be analyzed may be coated on the surface by a drop casting method, and then the SERS substrate may be fabricated to be analyzed by a laser . In this case, the SERS substrate should have a high signal enhancement effect so that a trace amount can be analyzed, a uniformity of the nanostructure on the substrate is high, signal uniformity and reproducibility should be excellent, and recycling is difficult.
Conventional SERS substrates can be fabricated in two ways. One method is to form a pattern using a lithography process such as photolithography or E-beam lithography and form a nanostructure by depositing Au or Ag to form a uniform nanostructure, Is not only very expensive, but also has a disadvantage in that the cost of the process itself is also high. The other is that the process is simple and inexpensive by synthesizing the nanostructure in solution and then scattering it on the substrate to make the SERS substrate. However, since the nanostructures are randomly distributed on the substrate, the signal uniformity and reproducibility are remarkably deteriorated .
Therefore, in order to utilize Raman spectroscopy using SERS widely for trace analysis, a SERS substrate fabrication technique having a high signal enhancement effect, excellent signal uniformity and reproducibility, and low fabrication cost is required.
In one embodiment of the present invention, instead of performing the lithography process, a nanostructure printing process is performed in which a nanostructure is formed and transferred to a target object. Thus, a signal enhancing effect at a low cost is high and excellent signal uniformity and reproducibility (SERS substrate, SERS vial and / or SERS patch) of high performance.
In addition, one embodiment of the present invention provides a method of using a nano-transfer printing process capable of controlling the adhesive force with high resolution without a preprocessing process in the process of manufacturing the SERS device.
In addition, one embodiment of the present invention provides a SERS device having a structure in which nanostructure thin films are stacked to utilize a coupling effect between nanostructure thin films in order to secure a high Raman signal.
According to one embodiment, a nano-transfer printing method includes: coating a polymer thin film on a template substrate having a surface pattern formed thereon; Fabricating the polymer thin film as a duplicate thin film mold using the polymer thin film and the adhesive film; Forming a nanostructure on the duplicate thin film mold; Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold; And transferring the nanostructure to a target object.
The step of forming the nanostructure may include depositing a functional material on the duplicate thin film mold using an inclined deposition method.
Wherein the step of depositing the functional material on the duplicate thin film mold includes the step of depositing the functional thin film on the surface where the duplicate thin film mold is deposited, And then tilting the duplicate thin film mold so as to have an angle to deposit the functional material.
The surface pattern of the concave-convex pattern is formed on the template substrate using a patterning process including at least one of photolithography, block copolymer self-assembly-based lithography and E-beam lithography, and a reactive ion etching (RIE) .
The step of coating the polymer thin film may include coating a single-layer thin film to form the polymer thin film; Or sequentially coating the first thin film and the second thin film to form the polymer thin film as a multilayer thin film.
The coating of the polymer thin film may be performed using at least one of spin coating, deep coating, and spray coating.
The step of fabricating the polymer thin film as a duplicate thin film mold includes: uniformly adhering the adhesive film to one surface of the polymer thin film; And separating the polymer thin film having the adhesive film from the template substrate.
Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold may include injecting organic solvent vapor between the adhesive film and the duplicate thin film mold to reduce the separation energy between the interfaces.
Injecting the organic solvent vapor between the adhesive film and the duplicate thin film mold comprises contacting the duplicate thin film mold with a polymeric pad containing an organic solvent to provide the organic solvent vapor; Or providing the organic solvent vapor vaporized from an organic solvent in a liquid state.
The organic solvent may have a similar solubility parameter within a predetermined range to the solubility parameter of the polymeric thin film constituting the duplicate thin film mold and / or the solubility parameter of the adhesive film.
The step of transferring the nanostructure to a target object comprises: contacting the duplicate thin film mold having the nanostructure formed thereon and the adhesive film to the polymer pad so that the nanostructure contacts the polymer pad; Separating the duplicate thin film mold and the adhesive film from the polymer pad so that the nanostructure remains on the polymer pad; Contacting the polymer pad on which the nanostructure remains so that the nanostructure contacts the target object; And separating the polymer pad from the object so that the nanostructure is transferred to the object.
Separating the duplicate thin film mold and the adhesive film from the polymer pad comprises: separating the adhesive film from the duplicate thin film mold that is in contact with the polymer pad; And removing the duplicate thin film mold that is in contact with the polymer pad using an organic solvent.
Wherein the step of transferring the nanostructure to a target object comprises the steps of: contacting the duplicate thin film mold having the nanostructure formed thereon and the adhesive film so that the nanostructure contacts the target object; And separating the duplicate thin film mold and the adhesive film from the object so that the nanostructure is transferred to the object.
Separating the duplicate thin film mold and the adhesive film from the object object comprises: separating the adhesive film from the duplicate film mold contacted with the object object; And removing the duplicate thin film mold contacted with the object using an organic solvent.
The nano-transfer printing method may further include repeatedly performing the step of transferring the nanostructure to the object to generate a SERS device having a structure of a three-dimensional nanostructure in which a plurality of the nanostructures are stacked .
The step of transferring the nanostructure to a target object may further include transferring the nanostructure onto a metal thin film.
According to one embodiment, a SERS device using a nanostructure is formed by the following steps of: coating a polymer thin film on a template substrate on which a surface pattern is formed; Fabricating the polymer thin film as a duplicate thin film mold using the polymer thin film and the adhesive film; Forming a nanostructure on the duplicate thin film mold; Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold; And transferring the nanostructure to a target object.
The SERS device using the nanostructure may be formed in the form of a substrate, a vial, or a patch according to the object to which the nanostructure is transferred, and may be utilized for analyzing the composition of the material.
The SERS device using the nanostructure may include at least one of a surface-enhanced Raman scattering substrate, a surface-enhanced Raman scattering vial, or a SERS patch (surface-enhanced Raman scattering patch).
The SERS apparatus using the nanostructure may have a structure of a three-dimensional nanostructure in which the above-described processes are repeatedly performed to form a plurality of nanostructures.
The step of transferring the nanostructure to a target object may further include transferring the nanostructure onto a metal thin film. The SERS device using the nanostructure may have a hybrid structure in which the nanostructure is transferred onto the metal thin film .
In one embodiment of the present invention, instead of performing the lithography process, a nanostructure printing process is performed in which a nanostructure is formed and transferred to a target object. Thus, a signal enhancing effect at a low cost is high and excellent signal uniformity and reproducibility A method of manufacturing a high performance SERS device (SERS substrate, SERS vial and / or SERS patch) can be provided.
In addition, one embodiment of the present invention can provide a method of using a nano-transfer printing process which has a high resolution and can control an adhesive force without a pretreatment process in the process of manufacturing a SERS device.
Accordingly, embodiments of the present invention can produce various types of SERS devices by performing nano-transfer printing on various objects.
In addition, one embodiment of the present invention can provide a SERS device having a structure in which nanostructure thin films are stacked to utilize a coupling effect between nanostructure thin films in order to secure a high Raman signal.
1 is a schematic view illustrating a process of fabricating a SERS device using nano-transfer printing according to an embodiment.
2A is an SEM image showing a surface pattern of a template substrate used in a SERS device fabrication process according to an embodiment.
2B is an SEM image showing a surface pattern of a template substrate used in a SERS device manufacturing process according to another embodiment.
2C is an SEM image showing a surface pattern of a template substrate used in a SERS device fabrication process according to another embodiment.
2D is an SEM image showing a surface pattern of a template substrate formed using a photolithography process according to an embodiment.
3A is a schematic view illustrating a process of fabricating a duplicate thin film mold in the SERS device manufacturing process according to one embodiment.
3B is a SEM image showing the surface of a duplicate thin film mold according to one embodiment.
3C is an SEM image showing the surface of a duplicate thin film mold according to another embodiment.
4A is a schematic view illustrating a process of forming a nanostructure in a SERS device manufacturing process according to an embodiment.
4B is an SEM image showing a nanostructure according to an embodiment.
5 is a graph showing a weight change rate with time at each temperature condition when the polymer pad according to one embodiment is immersed in an organic solvent.
6 is an SEM image showing a polymer pad in which the nanostructure remains by the first method of the S-
7 is a schematic diagram illustrating a process of using an organic solvent vapor vaporized from a liquid organic solvent according to an embodiment.
8A is an SEM image of a SERS substrate according to an embodiment.
8B is a diagram showing a Raman signal of the SERS substrate of FIG. 8A.
8C is an SEM image of a SERS substrate according to another embodiment.
8D is a GISAXS pattern image of an Al nanostructure included in a SERS substrate according to an embodiment.
9 is a SEM image of a three-dimensional SERS device having a structure in which nanostructure thin films are stacked according to an embodiment.
FIG. 10 is a graph showing the SERS Raman signal according to the number of the nanostructure thin films of FIG. 9 stacked. FIG.
11 is an SEM image showing a three-dimensional SERS device having a hybrid structure according to an embodiment.
FIG. 12 is a chart showing the SERS Raman signal according to the number of the nanostructures of FIG. 11 stacked. FIG.
13 is an SEM image of a three-dimensional SERS device having a hybrid structure according to another embodiment.
14 is optical images and SEM images showing various types of SERS devices according to one embodiment.
Hereinafter, embodiments according to the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to or limited by the embodiments. In addition, the same reference numerals shown in the drawings denote the same members.
Also, terminologies used herein are terms used to properly represent preferred embodiments of the present invention, which may vary depending on the user, intent of the operator, or custom in the field to which the present invention belongs. Therefore, the definitions of these terms should be based on the contents throughout this specification.
The present invention relates to a technique for fabricating a SERS device including a SERS substrate, a SERS vial, and a SERS patch by using a nano-transcription printing method in which a nanostructure is formed and transferred to a target object.
According to one embodiment of the present invention, a polymer thin film is coated on a template substrate having a surface pattern formed thereon, and a polymer thin film is formed from a thin film mold using a polymer thin film and an adhesive film, and then a nanostructure And then transferred to a target object to perform nano-transfer printing, thereby fabricating a SERS device. Hereinafter, the SERS device may be fabricated in the form of a substrate, a vial, or a patch according to an object to which the nanostructure is transferred, and may be utilized for analyzing a component of the substance. A detailed description thereof will be given below with reference to the drawings.
1 is a schematic view illustrating a process of fabricating a SERS device using nano-transfer printing according to an embodiment.
Referring to FIG. 1, a system for fabricating a SERS device according to an embodiment (hereinafter referred to as a SERS device manufacturing system) includes a solvent-vapor-injection nanotransfer printing (S-nTP ) To produce a SERS device.
Specifically, the S-nTP process may comprise a two-step continuous process. In the first process (S-
At this time, a surface pattern of concave-convex shape is formed on the template substrate by using a patterning process including at least one of photolithography, block copolymer self-assembly based lithography and E-beam lithography, and a reactive ion etching (RIE) .
For example, in the SERS device fabrication system, a surface pattern of a predetermined size is formed on a template substrate by using a patterning process, and then a surface etching is performed through an RIE process so that the surface pattern has a concavo-convex shape. More specifically, the SERS device fabrication system can fabricate a template substrate through patterning of block copolymer self-assembly based lithography on silicon wafers to form ultra-fine surface patterns below 20 nm. A detailed description thereof will be described with reference to FIG. 2A.
The SERS device manufacturing system can coat the polymer thin film by applying the polymer thin film on the template substrate using at least one of spin coating, deep coating, and spray coating. have. Here, the polymer to be coated with the polymer thin film is 20 to 40
In addition, the SERS device fabrication system can form a polymer thin film by applying a single layer thin film or sequentially form a first thin film and a second thin film to form a polymer thin film as a multilayer thin film. A detailed description thereof will be described with reference to Figs. 3A and 3B.
The SERS device fabrication system can form a nanostructure by depositing a functional material on a duplicate thin film mold using an in-line deposition method. A detailed description thereof will be described with reference to Fig. 4A.
When the first process is completed, the SERS device manufacturing system selectively weakens the adhesive force between the adhesive film and the duplicate thin film mold, and then performs a second process (S-
At this time, the SERS device fabrication system can selectively weaken the adhesive force between the adhesive film and the replication thin-film mold by injecting organic solvent vapor between the adhesive film and the replication thin-film mold in order to reduce the separation energy between the interfaces.
In the S-
According to the first mode of the S-
Here, the polymer pad is a flat PDMS (polydimethylsiloxane) pad having a thickness of 0.5 to 2 cm which is expanded by absorbing an organic solvent. A mixture of a precursor and a curing agent is placed on a silicon wafer, Followed by separation, crosslinking, and separation. At this time, the polymer pad has a solubility parameter ranging from 10 to 40
Organic solvent vapors provided by the polymer pads in contact with the duplicate thin film mold are injected between the adhesive film and the duplicate thin film mold to weaken the adhesion between the adhesive film and the duplicate thin film mold. When such a process is performed, the SERS device fabrication system can separate the duplicate thin film mold and the adhesive film from the polymer pad so that the nanostructure remains on the polymer pad. Here, in the SERS device manufacturing system, after separating the adhesive film from the duplicate thin film mold which is in contact with the polymer pad, the duplicate thin film mold which is in contact with the polymer pad can be removed by using the organic solvent.
For example, the SERS device fabrication system can separate only the contact film after the duplicate thin film mold and the adhesive film are brought into contact with the nanostructure and the polymer pad. Subsequently, the SERS device manufacturing system is designed to wash the duplicate thin film mold with an organic solvent such as toluene, acetone, and IPA solvent so that only the nanostructure remains on the polymer pad, or to deposit the polymer pad on which the duplicate thin film mold is in contact with the organic solvent The duplicate thin film mold can be removed from the polymer pad. A detailed description thereof will be described with reference to Fig.
Therefore, the polymer pad remaining in the nanostructure can be transferred to the object. For example, a SERS device fabrication system is a system in which a nanostructure is brought into contact with a target object (for example, for 1 to 5 seconds) so that the nanostructure contacts the target object, The pad can be separated from the object.
On the other hand, according to the second mode of the S-
When such a process is performed, the SERS device fabrication system can bring the duplicate thin film and the adhesive film, in which the nanostructure is formed, into contact with the object (for example, for 1 to 5 seconds) so that the nanostructure contacts the object. Subsequently, the SERS device manufacturing system can separate the duplicate thin film and the adhesive film from the object so that the nanostructure is transferred to the object.
For example, in the SERS device manufacturing system, a duplicate thin film mold and an adhesive film are brought into contact with a target object so that the nano structure is in contact with the target object, only the contact film is separated, and the duplicate thin film mold contacted with the target object is removed using an organic solvent . More specifically, for example, the SERS device fabrication system can remove the duplicate thin film mold from the object by rinsing the duplicate thin film mold with an organic solvent, or by depositing the object on which the duplicate thin film mold is in contact with the organic solvent .
As described above, a nanostructure of a metal material such as Au, Ag, Cu, Ni, Pt, Cr, Co, or Pd is formed through the S-
In particular, the SERS device fabrication system can perform a nano-transfer printing process (S-
Here, since the area of the nanostructure of the SERS device is formed on the basis of the surface area of the template substrate, the surface area of the template substrate is increased, so that a nanostructure of a large-area nanowire thin film can be realized in the SERS device.
2A is an SEM (scanning electron microscope) image showing a surface pattern of a template substrate used in a SERS device fabricating process according to an exemplary embodiment, and FIG. 2B is a scanning electron microscope FIG. 2C is a SEM image showing a surface pattern of a template substrate used in a SERS device fabrication process according to another embodiment, FIG. 2D is an SEM image showing a surface pattern using a photolithography process according to an embodiment Is an SEM image showing a surface pattern of a template substrate to be formed. Hereinafter, the SEM image means an image photographed by a SEM of 200 nm scale.
2A, a SERS device fabrication system according to an embodiment includes self-assembling a PS-PDMS (poly (stryene-b-dimethylsiloxane)) block copolymer on a silicon trench substrate having a width of 1 to 1 cm and a depth of 1 nm to 1 cm After the linear surface pattern is formed, a RIE process is performed under an oxygen environment to produce a template substrate having a surface pattern of concavo-convex shape with a line width of 20 nm.
In addition, the SERS device fabrication system has a hydrophobic SAM (self-assembled monolayer) such as a PDMS brush polymer or HMDS (hexa methylene di silazane) having low surface energy on the surface of a template substrate manufactured through the above- A coating process is performed so that the template substrate surface is 30
2B, which is a SEM image showing the surface pattern of the template substrate used in the SERS device manufacturing process according to another embodiment, and a SEM image showing the surface pattern of the template substrate used in the SERS device manufacturing process according to another embodiment 2C, the SERS device fabrication system self-assemble a PS-PDMS block copolymer on a silicon trench substrate having a width of 1 to 1 cm and a depth of 1 to 1 cm to form a linear surface pattern, The template substrate having the surface pattern of the concavo-convex shape of 15 nm line width and 8 nm line width can be produced.
In addition, the SERS device fabrication system can produce a template substrate used for duplicating the surface pattern during the SERS device manufacturing process through various patterning processes. For example, referring to FIG. 2D, which is an SEM image showing a surface pattern of a template substrate formed using a photolithography process according to one embodiment, the SERS device fabrication system includes a step of forming a linear surface pattern with a line width of several hundreds nm to several μm, Can be formed through a lithography process. However, without being limited thereto, the SERS device manufacturing system can form various surface patterns such as a dot surface pattern or a hole surface pattern through a photolithography process or a block copolymer self-assembly process in addition to the above-described linear surface pattern.
3A is a schematic view showing a process of fabricating a duplicate thin film mold in the SERS device manufacturing process according to one embodiment, FIG. 3B is an SEM image showing the surface of the duplicate thin film mold according to one embodiment, and FIG. 2 is an SEM image showing the surface of a duplicate thin film mold according to an example.
Referring to FIG. 3A, a SERS device manufacturing system according to an exemplary embodiment of the present invention includes a step of first coating a poly-4-vinyl pyridine (P4VP) thin film as a first thin film on a template substrate (coating with IPA (isopropyl alcohol) The polymer thin film can be formed of a P4VP-PS multilayer thin film or a P4VP-PMMA multilayer thin film by applying any one of PS (polystyrene) or PMMA (poly (methylmethacrylate)) as the second thin film. However, the present invention is not limited thereto, and the SERS device fabrication system can form a polymer thin film by applying either PS or PMMA on a template substrate as a single layer thin film.
The polymer thin film thus coated can replicate the surface pattern of the template substrate with a resolution of 10 nm or less in the process of being applied on the template substrate.
Although not shown in the drawings, the SERS device manufacturing system can uniformly adhere an adhesive film to one surface of the polymer thin film (the opposite side to the surface coated on the template substrate), then separate the polymer thin film having the adhesive film from the template substrate , A polymer thin film can be fabricated from a duplicate thin film mold.
Therefore, the duplicate thin film mold manufactured through the above-described processes can greatly reduce the material cost consumed in the fabrication process and does not require strong pressure, tension or heat treatment in the process of duplicating the surface pattern of the template substrate, ≪ / RTI >
The duplicate thin film mold thus produced may have a linear pattern of 20 nm as shown in FIG. 3B, which is an SEM image showing the surface of the duplicate thin film mold according to one embodiment according to the line width of the surface pattern of the template substrate, As shown in FIG. 3C, which is an SEM image showing the surface of the duplicate thin film mold according to the present invention.
FIG. 4A is a schematic view illustrating a process of forming a nanostructure in a SERS device fabrication process according to an exemplary embodiment of the present invention, and FIG. 4B is a SEM image illustrating a nanostructure according to an exemplary embodiment of the present invention.
Referring to FIG. 4A, in order to deposit a functional material on only a portion of the surface where deposition of the duplicate thin film mold is performed, the SERS apparatus manufacturing system according to an exemplary embodiment includes a surface on which the duplicate thin film mold is deposited, The functional thin film can be deposited by tilting the duplicate thin film mold. For example, the SERS device fabrication system can deposit functional materials only on the portion of the surface where the duplicate thin film mold is deposited using the E-beam lithography or thermal evaporation deposition technique with the duplicate thin film mold tilted. More concretely, for example, the SERS device fabrication system may use a co-deposition technique depending on the material of the functional material (metal material such as Au, Ag, Cu, Ni, Pt, Cr, Co or Pd). Therefore, the SERS device manufacturing system can form a nanostructure having the same size as the surface pattern of the duplicate thin film mold without a separate lift-off process.
Referring to FIG. 4B, which is an SEM image of a nanostructure according to an embodiment, Au nanostructures formed through the above-described process are formed by depositing a pattern of 20 nm line width on a duplicate thin film mold by E-beam evaporation .
The nanostructure formed on the duplicate thin film mold can be transferred to various object bodies, and various types of SERS devices can be manufactured. For example, when the nanostructure is transferred to a substrate, a SERS substrate can be fabricated, and when the nanostructure is transferred to the inner surface of the vial, a SERS vial can be fabricated, and the nanostructure can be fabricated A SERS patch can be made when transferring to a flexible patch-like object.
In the case of the SERS vials, the SERS nanostructures are formed on the vial interior surface, allowing the user to fill the vial with liquid analytes and perform laser analysis on the surface where the SERS nanostructures are formed have. Therefore, the SERS vial is capable of analyzing the liquid substance unlike the general SERS substrate and has the advantage that the Raman analysis is possible without exposing the harmful substance to the outside.
The SERS patch is a custom SERS device that can be easily used by users according to various analysis environments since the SERS nanostructure transferred on the patch can be transferred to the surface of the user's desired surface. At this time, the polymer constituting the patch for the SERS patch is 30
5 is a graph showing a weight change rate with time at each temperature condition when the polymer pad according to one embodiment is immersed in an organic solvent.
Referring to FIG. 5, when the polymer pad, which is a PDMS pad, is immersed in toluene within about 6 hours at room temperature, the saturated expansion rate is reached and the weight does not increase any more. Accordingly, the SERS device fabrication system according to one embodiment can immerse the polymer pad in an organic solvent such as toluene at room temperature within 6 hours to absorb the organic solvent, and then swell the polymer pad to a saturated expansion rate. The polymer pad thus produced can generate the same vapor pressure as the saturated vapor pressure of the pure liquid since the chemical potential of the solvent molecules contained therein is the same as that of the organic solvent in pure liquid state. Thus, polymer pads containing organic solvents can continuously release high solvent vapor at high flow rates.
6 is an SEM image showing a polymer pad in which the nanostructure remains by the first method of the S-
Referring to FIG. 6, the SERS device fabrication system may perform the first method of the S-
Further, when the polymer thin film of the duplicate thin film mold is formed as a multilayer thin film, it can be sequentially removed from the uppermost thin film.
7 is a schematic diagram illustrating a process of using an organic solvent vapor vaporized from a liquid organic solvent according to an embodiment.
Referring to FIG. 7, in the SERS apparatus manufacturing system according to an embodiment, an organic solvent is filled in a chamber manufactured according to an area of a duplicate thin film mold, an adhesive film of a duplicate thin film mold is attached to a lid of the chamber, So that the organic solvent vapor in the liquid organic solvent in the chamber is injected between the adhesive film and the duplicate thin film mold. After a certain period of time, the transfer process described above can be performed by separating the adhesive film and the duplicate thin film mold from the lid of the chamber.
8A is a SEM image of a SERS substrate according to an embodiment, FIG. 8B is a chart showing a Raman signal of the SERS substrate of FIG. 8A, FIG. 8C is a SEM image of a SERS substrate according to another embodiment, 8D is a GISAXS pattern image of the Al nanostructure included in the SERS substrate according to one embodiment.
Referring to FIG. 8A, the SERS substrate is a SERS device manufactured through the above-described S-
Such a SERS substrate can acquire a high Raman signal. For example, referring to FIG. 8B showing a Raman signal of the SERS substrate of FIG. 8A, when a drop of a solution containing Rhodamin 6G (R6G) molecules is dropped on the SERS substrate and Raman analysis is performed, It can have a strong SERS signal, and the SERS peak of the SERS signal can also be clearly indicated.
On the other hand, when a drop of a solution containing R6G molecules is dropped on a substrate using a conventional Raman spectroscopic method that does not include a nanostructure, and a Raman analysis is performed, a substrate using a conventional Raman spectroscopic technique has a weak SERS signal, The SERS peak of the signal may also not be apparent.
In addition, the SERS substrate may be formed of a nanostructure of various metal materials as well as an Au nanostructure depending on materials used as a functional material in the S-
As described above, the SERS device manufactured through the S-
8D, which is a GISAXS pattern image of an Al nanostructure included in a SERS substrate according to an embodiment, an Al nanostructure included in a SERS substrate manufactured through S-
In addition, since the SERS device is manufactured through a nano-transfer printing process which can achieve high resolution, control the adhesive force without a pretreatment process, and can perform continuous printing, the nanostructure thin films may be stacked. A detailed description thereof will be described with reference to FIG.
FIG. 9 is a SEM image of a three-dimensional SERS device having a structure in which nanostructure thin films are stacked according to an embodiment, and FIG. 10 is a diagram showing SERS Raman signals according to numbers in which nanostructure thin films of FIG. 9 are stacked.
Referring to FIG. 9, the SERS device according to one embodiment can be manufactured as a three-dimensional SERS device having a structure in which nanostructure thin films are stacked.
Here, the three-dimensional SERS device can be manufactured by successively performing the above-described nano-transfer printing process to successively laminate the nanostructure films on the object and transfer them.
For example, the SERS device fabrication system may be configured to transfer a first nanostructure thin film on a target object (substrate) by first nano-transcription printing, and then to cross the first nanostructure thin film in a direction perpendicular to the first nanostructure thin film by a second nano- By transferring the second nanostructure thin film onto the first nanostructure thin film, a three-dimensional SERS device having a crossed-wire structure can be manufactured. At this time, the number in which the nanostructure thin films are stacked can be set adaptively to a plurality of layers (a plurality of nanostructure thin film layers are formed so as to intersect with each other in a direction perpendicular to each other) without being limited to or limited to two layers.
Therefore, the three-dimensional SERS device having the structure in which the nanostructure thin films are stacked can obtain the SERS signal intensity significantly increased as compared with the SERS device including the single-layer nanostructure.
For example, referring to FIG. 10, which is a diagram showing a SERS Raman signal according to the number of nanostructure thin films stacked in FIG. 9, when SERS analysis is performed by applying the same amount of R6G molecules to a SERS device, It can be seen that the intensity of the SERS Raman signal becomes stronger as the number of the nanostructure thin films stacked in the device increases.
In addition, as described above, the SERS device manufacturing system can perform a continuous nano-transfer printing process on various objects. For example, a SERS device fabrication system can produce a SERS substrate, a SERS vial, or a SERS patch by performing a continuous nanosecond printing process on a substrate, vial, food or part of the body.
FIG. 11 is a SEM image showing a three-dimensional SERS device having a hybrid structure according to an embodiment, and FIG. 12 is a diagram showing a SERS Raman signal according to a number in which the nanostructure of FIG. 11 is stacked.
Referring to FIG. 11, the SERS device according to one embodiment can be fabricated as a three-dimensional SERS device having a hybrid structure in which a nanostructure is printed on a metal thin film by nano-transfer printing. Such a three-dimensional SERS device having a hybrid structure can have a very strong SERS Raman signal enhancement effect by plasmonic coupling between the nanostructure and the underlying metal thin film.
For example, a SERS device fabrication system can deposit a silver layer on a silicon substrate to a thickness of several tens nm, and then print a silver nanostructure on the silver nano structure to fabricate a three-dimensional SERS device having a hybrid structure. At this time, the SERS device fabrication system can stack the nanostructure into a plurality of layers.
12, which is a chart showing the SERS Raman signal according to the number of the nanostructures stacked in FIG. 11, when SERS analysis is performed by applying the same amount of R6G molecules to a SERS device, a three-dimensional SERS device having a hybrid structure It can be seen that the higher the number of layers of the nanostructures stacked in the SERS Raman signal enhancement effect is, the stronger the SERS Raman signal enhancement effect is.
These Raman signal enhancement effects can be quantified as averaged enhancement factor (AEF) as shown in Table 1. The AEF can also be calculated using the ratio of the Raman signal intensity from the R6G molecule applied on the SERS device to the Raman signal intensity obtained on the substrate using the conventional Raman spectroscopy technique without nanostructure formation have.
In addition, the SERS device manufacturing system can produce a three-dimensional SERS device having another type of hybrid structure. A detailed description thereof will be described with reference to FIG.
13 is an SEM image of a three-dimensional SERS device having a hybrid structure according to another embodiment.
Referring to FIG. 13, a SERS device manufacturing system according to another embodiment of the present invention is a system for manufacturing a three-dimensional SERS device having a hybrid structure by printing a nanostructure on a silicon substrate having a trench- A three-dimensional SERS device having a hybrid structure can be manufactured by nano-transfer printing the structure.
14 is optical images and SEM images showing various types of SERS devices according to one embodiment.
Referring to FIG. 14, the SERS device manufacturing system according to an exemplary embodiment of the present invention includes Au, Ag, Cu, Ni, Pt, Cr, Co, or Pd through the nano transfer printing process (S-
For example, the SERS device fabrication system can create a SERS vial by nano-transfer printing a nanostructure onto a vial, and nano-transfer the nanostructure onto a part of the body (nail or wrist) or food surface, Can be produced. In addition, the SERS device fabrication system can fabricate a flexible SERS substrate by nano-transfer printing the nanostructure onto a flexible substrate.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. For example, it is to be understood that the techniques described may be performed in a different order than the described methods, and / or that components of the described systems, structures, devices, circuits, Lt; / RTI > or equivalents, even if it is replaced or replaced.
Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.
Claims (21)
Fabricating the polymer thin film as a duplicate thin film mold using the polymer thin film and the adhesive film;
Forming a nanostructure on the duplicate thin film mold;
Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold; And
Transferring the nanostructure to a target object
Wherein the nano-transfer printing method comprises the steps of:
The step of forming the nanostructure comprises:
Depositing a functional material on the duplicate thin film mold using an inclined deposition method
≪ / RTI >
The step of depositing the functional material on the duplicate thin film mold
The duplicate thin film mold is tilted so that the surface on which the duplicate thin film mold is deposited and the deposition direction are at an angle so as to deposit the functional material only on the portion derived from the surface on which the duplicate thin film mold is deposited, The step of depositing
≪ / RTI >
The template substrate
A nano transfer printing process in which the surface pattern of the concave-convex shape is formed using a patterning process including at least one of photolithography, block copolymer self-assembly based lithography, and E-beam lithography, and a reactive ion etching (RIE) Way.
The step of coating the polymer thin film
Forming a polymer thin film by applying a monolayer thin film; or
Sequentially coating the first thin film and the second thin film to form the polymer thin film as a multilayer thin film
≪ / RTI > wherein the method comprises any one of the following steps:
The step of coating the polymer thin film
Wherein the polymer thin film is applied using at least one of spin coating, deep coating, and spray coating.
The step of fabricating the polymer thin film as a duplicate thin film mold
Uniformly adhering the adhesive film to one surface of the polymer thin film; And
Separating the polymer thin film having the adhesive film from the template substrate
≪ / RTI >
Selectively weakening the adhesive force between the adhesive film and the duplicate thin film mold
Injecting an organic solvent vapor between the adhesive film and the duplicate thin film mold to reduce the separation energy between the interfaces
≪ / RTI >
The step of injecting the organic solvent vapor between the adhesive film and the duplicate thin film mold
Contacting the polymeric pad containing an organic solvent with the duplicate thin film mold to provide the organic solvent vapor; or
Providing said organic solvent vapor which is vaporized from an organic solvent in a liquid state
≪ / RTI > wherein the method comprises any one of the following steps:
The step of transferring the nanostructure to a target object
Contacting the duplicate thin film mold having the nanostructure formed thereon and the adhesive film to the polymer pad so that the nanostructure contacts the polymer pad;
Separating the duplicate thin film mold and the adhesive film from the polymer pad so that the nanostructure remains on the polymer pad;
Contacting the polymer pad on which the nanostructure remains so that the nanostructure contacts the target object; And
Separating the polymer pad from the object so that the nanostructure is transferred to the object;
≪ / RTI >
The step of separating the duplicate thin film mold and the adhesive film from the polymer pad
Separating the adhesive film from the duplicate thin film mold that is in contact with the polymeric pad; And
Removing the duplicate thin film mold that is in contact with the polymer pad using an organic solvent
Wherein the nano-transfer printing method further comprises:
The step of transferring the nanostructure to a target object
Contacting the duplicate thin film mold having the nanostructure formed thereon and the adhesive film to the object so that the nanostructure contacts the object; And
Separating the duplicate thin film mold and the adhesive film from the object so that the nanostructure is transferred to the object;
≪ / RTI >
Wherein said step of separating said duplicate thin film mold and said adhesive film from said object comprises
Separating the adhesive film from the duplicate thin film mold in contact with the object; And
Removing the duplicate thin film mold that is in contact with the object using an organic solvent
Wherein the nano-transfer printing method further comprises:
The step of transferring the nanostructure to the target object is repeatedly performed to generate a SERS device having a structure of a three-dimensional nanostructure in which a plurality of the nanostructures are stacked
Wherein the nano-transfer printing method further comprises:
The step of transferring the nanostructure to a target object
Transferring the nanostructure onto a metal thin film
Wherein the nano-transfer printing method further comprises:
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| KR1020150129896A KR101761010B1 (en) | 2015-09-14 | 2015-09-14 | Nanotransfer printing method and surface-enhanced raman scattering substrate, surface-enhanced raman scattering vial and surface-enhanced raman scattering patch manufactured using the same |
| US14/884,529 US10507604B2 (en) | 2014-10-29 | 2015-10-15 | Nanotransfer printing method and surface-enhanced raman scattering substrate, surface-enhanced raman scattering vial and surface-enhanced raman scattering patch manufactured using the same |
| PCT/KR2015/011082 WO2016068538A1 (en) | 2014-10-29 | 2015-10-20 | Nanotransfer printing method and sers substrate, sers vial, and sers patch manufactured using same |
| EP15191672.3A EP3015918B1 (en) | 2014-10-29 | 2015-10-27 | Nanotransfer printing method and surface-enhanced raman scattering substrate |
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| US10981301B2 (en) | 2018-01-30 | 2021-04-20 | Samsung Display Co., Ltd. | Mold for wire grid polarizer and manufacturing method thereof |
| KR20230072290A (en) | 2021-11-17 | 2023-05-24 | 한국과학기술원 | Dielectrophoresis-based Dynamic SERS Device for Separation and Analysis of Metabolites |
| KR20230072291A (en) | 2021-11-17 | 2023-05-24 | 한국과학기술원 | Method and Apparatus for Electrochemically Extracting Metabolites Using Nanotransfer Printing-based SERS Device |
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| KR102377588B1 (en) * | 2017-10-17 | 2022-03-24 | 한국과학기술원 | Fabrication of self-assembled quantum dot array in single-quantum-particle resolution using block-copolymer as template and nanotransfer printing of the array |
| US20230288341A1 (en) * | 2019-05-20 | 2023-09-14 | Pico Foundry Inc. | Carboxylic acid functionalized 3-dimensional sers substrate |
| KR20240042871A (en) | 2022-09-26 | 2024-04-02 | 한국과학기술원 | Deep learning and self-assembled monolayer-based alzheimer's disease diagnosis method and sers substrate for the same |
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| US10981301B2 (en) | 2018-01-30 | 2021-04-20 | Samsung Display Co., Ltd. | Mold for wire grid polarizer and manufacturing method thereof |
| KR20230072290A (en) | 2021-11-17 | 2023-05-24 | 한국과학기술원 | Dielectrophoresis-based Dynamic SERS Device for Separation and Analysis of Metabolites |
| KR20230072291A (en) | 2021-11-17 | 2023-05-24 | 한국과학기술원 | Method and Apparatus for Electrochemically Extracting Metabolites Using Nanotransfer Printing-based SERS Device |
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