KR20170036896A - Surface enhanced raman scattering sensor, method of forming the same, and analyzing method using the same - Google Patents

Surface enhanced raman scattering sensor, method of forming the same, and analyzing method using the same Download PDF

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KR20170036896A
KR20170036896A KR1020150135213A KR20150135213A KR20170036896A KR 20170036896 A KR20170036896 A KR 20170036896A KR 1020150135213 A KR1020150135213 A KR 1020150135213A KR 20150135213 A KR20150135213 A KR 20150135213A KR 20170036896 A KR20170036896 A KR 20170036896A
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metal layer
nanoparticles
analyte
substrate
raman scattering
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KR101724271B1 (en
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위정섭
이태걸
손진경
박지수
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한국표준과학연구원
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • 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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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

A surface enhanced Raman scattering sensor of the present invention comprises: at least one metal layer disposed on a substrate having a circular shape; nanoparticles disposed along the edges of the metal layer; and a sample supplier providing a solution containing an analyte to correspond to a size of the metal layer on the metal layer on which the nanoparticles are arranged.

Description

Technical Field [0001] The present invention relates to a surface enhanced Raman scattering sensor, a method of manufacturing the same, and a measurement method using the same. [0002]

The present invention relates to a surface enhanced Raman scattering sensor, And more particularly, to a surface enhanced Raman scattering sensor using metal nanostructures, And a measurement method using the surface enhanced Raman scattering sensor.

Surface Enhanced Raman Scattering (SERS) is a phenomenon in which Raman scattering of molecules is greatly amplified by plasmon resonance appearing on a metal surface. Since the sensor using the SERS is highly sensitive, it can detect chemical substances and biochemically As a method of analysis.

The surface enhancement Raman scattering can be detected as a high response when the analyte is bound to the surface of the metal nanostructure or when the analyte exists in the vicinity, the signal is greatly increased. Thus, in a sensor using it, it is necessary to amplify the Raman signal by providing hot-spots in which the collective oscillation of free electrons, known as surface plasmon resonance, is maximized, thereby enhancing local electromagnetic fields. Therefore, to manufacture a surface enhanced Raman scattering sensor having a high strengthening effect, it is essential to control a nanostructure providing a hot spot. There is a need for a technique capable of producing such nanostructures with high integration and reproducibility, easy manufacturing process and low manufacturing cost.

One of the technical problems to be solved by the technical idea of the present invention is to provide a surface enhanced Raman scattering sensor using a metal nanostructure, A manufacturing method thereof, and a measuring method using the same.

A surface enhanced Raman scattering sensor according to an embodiment of the present invention includes at least one metal layer disposed on a substrate and having a circular shape, nanoparticles disposed along an edge of the metal layer, And a sample providing unit for providing a solution containing an analyte on the metal layer so as to correspond to the size of the metal layer.

In some embodiments of the present invention, the nanoparticles may be arranged in a ring shape along the shape of the metal layer.

In some embodiments of the present invention, the apparatus may further include a signal measuring unit for measuring a Raman signal from the analyte after the solvent of the solution provided by the sample preparation unit is evaporated.

In some embodiments of the present invention, the metal layer has a hydrophilic surface, and the substrate may have a hydrophobic surface.

In some embodiments of the present invention, the metal layer and the nanoparticles may be made of the same material.

In some embodiments of the present invention, a plurality of the metal layers may be arranged in rows and columns on the substrate.

A method of fabricating a surface enhanced Raman scattering sensor according to an embodiment of the present invention includes forming at least one metal layer having a circular shape on a substrate, providing a solution containing nanoparticles on the metal layer, And evaporating the solvent of the solution so that the nanoparticles remain, wherein the nanoparticles are spontaneously arranged in a ring shape along the edge of the metal layer by a coffee-ring effect.

In some embodiments of the present invention, the step of evaporating the solvent may further comprise cleaning the surface of the nanoparticles arranged on the metal layer.

In some embodiments of the present invention, the upper surface of the substrate exposed around the metal layer is treated to have hydrophobicity, and the surface of the metal layer may be formed to have hydrophilicity.

A method of measuring a surface enhanced Raman scattering sensor according to an embodiment of the present invention includes the steps of providing a substrate on which at least one metal layer having a circular shape and nanoparticles disposed along an edge of the metal layer are formed, Providing a solution containing the analyte so as to correspond to the size of the metal layer on the metal layer on which the analyte is disposed; evaporating the solvent of the solution so that the analyte remains, And a step of measuring.

In some embodiments of the present invention, the analyte may spontaneously be located between and above the nanoparticles along the edge of the metal layer by a coffee-ring effect.

In some embodiments of the present invention, the metal layer has a hydrophilic surface, and the substrate is provided with a hydrophobic surface, whereby the solution forms droplets confined on the metal layer.

A surface enhanced Raman scattering sensor with improved sensitivity and a measurement method using the same can be provided by inducing the analyte to spontaneously reach and adsorb between the nanoparticles.

By arranging and cleaning nanoparticles, a method of manufacturing a surface enhanced Raman scattering sensor that is easy to carry and has improved sensitivity can be provided.

The various and advantageous advantages and effects of the present invention are not limited to the above description, and can be more easily understood in the course of describing a specific embodiment of the present invention.

1 is a schematic perspective view showing a surface enhanced Raman scattering sensor according to an embodiment of the present invention.
2 is a flowchart illustrating a measurement method using a surface enhanced Raman scattering sensor according to an embodiment of the present invention.
FIGS. 3A to 3C are cross-sectional views illustrating major steps of a method of manufacturing a surface enhanced Raman scattering sensor according to an embodiment of the present invention.
FIGS. 4A to 4C are cross-sectional views schematically showing major steps of a measurement method using a surface enhanced Raman scattering sensor according to an embodiment of the present invention.
5A and 5B are partial perspective views illustrating features of a surface enhanced Raman scattering sensor according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings.

The embodiments of the present invention may be modified into various other forms or various embodiments may be combined, and the scope of the present invention is not limited to the embodiments described below. Further, the embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art. Accordingly, the shapes and sizes of the elements in the drawings may be exaggerated for clarity of description, and the elements denoted by the same reference numerals in the drawings are the same elements.

1 is a schematic perspective view showing a surface enhanced Raman scattering sensor according to an embodiment of the present invention.

1, a surface enhanced Raman scattering sensor 1000 according to an exemplary embodiment of the present invention includes a sensing unit 100, signal measuring units 210 and 220, and a sample preparation unit (not shown) 300). The surface enhancement Raman scattering sensor 1000 provides the analyte 10 to the sensing unit 100 through the sample preparation unit 300 and transmits the signal to the sensing unit 100 through the signal measuring units 210 and 220, By measuring the signal, the analyte 10 can be detected and analyzed.

The sensing unit 100 includes a substrate 101, metal layers 110 having a circular shape and nanoparticles 120 disposed along the edges of the metal layers 110 on the substrate 101 do.

The substrate 101 is a layer in which metal nanostructures including nanoparticles 120 are formed on the upper surface of the substrate 101, and may form a part of the sensing unit 100. The substrate 101 may be selected from a conventional semiconductor substrate such as a silicon substrate, a conductive substrate, or an insulating substrate. The surface 101S of the substrate 101, particularly the surface 101S exposed between the metal layers 110, may be a surface treated to have hydrophobic properties.

The metal layers 110 may be circularly patterned on the substrate 101 in rows and columns. However, the shape, arrangement and number of the metal layers 110 may be variously modified in the embodiments. For example, in some embodiments, only one metal layer 110 may be disposed on the substrate 101. The size of the metal layers 110 may range from a few micrometers to a few millimeters, for example, from 100 micrometers to 10 millimeters, and the thickness may be selected variously.

The metal layers 110 may be treated to have a hydrophilic surface or may be made of a material having hydrophilic properties. The metal layers 110 may include, for example, at least one of gold (Au), silver (Ag), aluminum (Al), and copper (Cu).

The nanoparticles 120 are arranged at the edges and may be arranged in a ring shape along the shape of the metal layer 110. The nanoparticles 120 may be arranged in a monolayer or multilayer at the edge of the metal layer 110 and may have the form of a nanocluster. The nanoparticles 120 may thus be arranged only on the edge of the metal layer 110 by a coffee ring effect. This will be described in more detail below with reference to FIGS. 3B and 3C.

The nanoparticles 120 may have various shapes such as a spherical shape, a cubic shape, a rod shape, and the like. The nanoparticles 120 may be made of a metal material and may include at least one of gold (Au), silver (Ag), aluminum (Al), and copper (Cu). In some embodiments, the nanoparticles 120 may be made of the same material as the metal layers 110. In some embodiments, the surface of the nanoparticles 120 may be coated with a material having a specific functional group to enhance the adsorption of the analyte 10.

Analysis can be performed by locating the analyte 10 between the nanoparticles 120 and on top of the nanoparticles 120. Hot spots may be formed in the space between the nanoparticles 120 and the space between the nanoparticles 120 and the metal layer 110 in a strong electromagnetic field to enhance the Raman signal. The surface enhanced Raman scattering sensor 1000 having high sensitivity can be realized.

The signal measuring units 210 and 220 may measure a Raman signal in the sensing unit 100 and may include a light source unit 210 and a detection unit 220. [ The signal measuring units 210 and 220 can measure the characteristic Raman scattering characteristic of the analyte 10.

The light source unit 210 may include a light source and an oscillator, and may generate a laser. The detection unit 220 can acquire an optical signal from the sensing unit 100 and convert it into an electrical signal. For example, the Raman shift by the analyte 10 can be measured. In some embodiments, the detector 220 may comprise a charge-coupled device (CCD) or a photodiode.

The configuration of the signal measuring units 210 and 220 may be variously changed in the embodiments. For example, in some embodiments, the signal measuring units 210 and 220 may further include a separate monitoring unit, such as an optical microscope, to observe changes in the analyte 10. For example,

The sample preparation unit 300 may provide a solution SL containing the analyte 10 on the metal layers 110. The analyte 10 may include, for example, metal ions or biomolecules such as DNA, proteins, and the like.

The sample preparation unit 300 may supply the solution SL on the metal layers 110 to correspond to the sizes of the metal layers 110. [ The sample preparation unit 300 may be, for example, a micropipette, a syringe, or the like, and may be selected as a mechanism for providing the solution SL with a size corresponding to the size of the metal layer 110. However, the shape and arrangement of the sample preparation part 300 are not limited to those shown in the drawings, and can be variously changed.

The solution SL provided by the sample preparation unit 300 can form a droplet on the metal layers 110 having hydrophilicity even if the solution SL is provided larger than the size of the metal layer 110 . This can be induced by a difference in hydrophilicity degree between the surface 101S of the substrate 101 and the surface of the metal layers 110. [

2 is a flowchart illustrating a measurement method using a surface enhanced Raman scattering sensor according to an embodiment of the present invention.

FIGS. 3A to 3C are cross-sectional views illustrating major steps of a method of manufacturing a surface enhanced Raman scattering sensor according to an embodiment of the present invention. Figures 3A-3C show cross-sections taken along the line I-I 'of Figure 1.

Referring to FIG. 2, a step S110 of forming a substrate having at least one metal layer having a circular shape and nanoparticles disposed along the edges of the metal layer may be performed. That is, the surface enhanced Raman scattering sensor 1000 shown in FIG. 1 can be provided.

Referring to FIG. 3A, metal layers 110 may be formed on a substrate 101 by patterning.

Before forming the metal layers 110, the surface 101S of the substrate 101 may be treated to have hydrophobicity. For example, when the substrate 101 is a silicon substrate, a hydrophobic surface 101S can be formed by a hydrofluoric acid (HF) treatment. In some embodiments, such a surface treatment process may be performed after formation of the metal layers 110.

The metal layers 110 may be formed by depositing a metal material on the entire surface of the substrate 110 and then performing photolithography using a separate mask layer or by using a nanoimprint process. By forming the metal layers 110 having a relatively large size, the visibility of the sensing region can be improved, and an electromagnetic field is also formed between the metal layers 110 and the nanoparticles 120 formed in the subsequent steps, Can be further enhanced.

Referring to FIG. 3B, a solution SL 'containing nanoparticles 120 may be provided on the metal layers 110.

As shown in the figure, the nanoparticles 120 may be provided using a mechanism such as a pipette (PT), but are not limited thereto. For example, in some embodiments, the nanoparticles 120 may be provided by spin coating, dip coating, or the like. In this case, by appropriately selecting the solvent of the solution SL 'containing the nanoparticles 120, the solution SL' can be wetted only on the surface of the metal layers 110 having hydrophilicity.

The solution SL 'containing the nanoparticles 120 on the metal layers 110 can form one droplet DP'. This can be controlled by adjusting the size of the metal layers 110 or by appropriately selecting the pipette PT so that the sizes of the liquid droplets DP 'provided by the metal layers 110 and the pipette PTs correspond to each other .

Referring to FIG. 3C, the solvent of the solution SL 'containing the nanoparticles 120 may be evaporated to form a layer of the nanoparticles 120 on the metal layers 110.

As the solvent evaporates, the nanoparticles 120 may be annularly disposed along the edges of the metal layers 110 by a coffee-ring effect. The coffee-ring effect is a phenomenon in which the density distribution of particles becomes uneven due to the movement of colloidal particles to the edge by hydrodynamic action. Due to such a coffee-ring effect, the nanoparticles 120 can be arranged in a strip shape along the edges of the metal layers 110, and the nanoparticles 120 in the solution SL ' May be arranged in a single layer or multiple layers depending on the density of the substrate 120. The evaporation time of the solvent can be controlled so that the nanoparticles 120 can be arranged by the coffee-ring effect, for example, the type of solvent, ambient humidity and temperature, etc. can be controlled.

After the layer of nanoparticles 120 is formed, a cleaning process to remove organic and / or inorganic materials remaining in the layer of nanoparticles 120 may be further performed. The organic and / or inorganic material may be, for example, a material for dispersing the surfactant or nanoparticles 120 covering the nanoparticles 120 in the solvent. The cleaning process can be performed using, for example, UV-ozone (O 3 ) or Piranha solution. The surface enhancement Raman scattering sensor 1000 can perform such a cleaning process after arranging the nanoparticles 120 before providing a sample for measurement, so that the sensitivity of the sensor can be further improved.

Thus, the surface enhanced Raman scattering sensor 1000 according to an embodiment of the present invention can be provided.

FIGS. 4A to 4C are cross-sectional views schematically showing major steps of a measurement method using a surface enhanced Raman scattering sensor according to an embodiment of the present invention. 4A to 4C are enlarged views of the area 'A' in FIG. 3C.

Referring to FIG. 4A, a metal layer 110 is illustrated in which the nanoparticles 120 described with reference to FIG. 3C are arranged.

Referring to FIGS. 2 and 4B, step S120 of supplying a solution SL (see FIG. 1) containing the analyte 10 onto the metal layers 110 on which the nanoparticles 120 are arranged .

This step may be performed similarly to the formation of the nanoparticles 120 described above with reference to FIG. 3B. The solution SL containing the analyte 10 may be provided using the sample preparation unit 300 as shown in FIG. 1, but the present invention is not limited thereto. For example, in some embodiments, the analyte 10 may be provided by spin coating, dip coating, or the like. In this case, by appropriately selecting the solvent of the solution SL containing the analyte 10, the solution SL containing the analyte 10 can be wetted only on the surface of the metal layers 110 having hydrophilicity .

The solution SL containing the analyte 10 on the metal layers 110 can form one droplet DP. This can be controlled by adjusting the size of the metal layers 110 or appropriately selecting the pipette (PT) so that the sizes of the liquid droplets DP provided by the pipette (PT) and the metal layers 110 correspond to each other.

2 and 4C, step S130 of evaporating the solvent of the solution SL containing the analyte 10 so that the analyte 10 remains may be performed.

As the solvent evaporates, the analyte 10 can be annularly disposed on the nanoparticles 120 along the edges of the metal layers 110 by a coffee-ring effect. The analyte 10 may be disposed between the nanoparticles 120 and above the nanoparticles 120. Since the hot spot is formed between the nanoparticles 120, the Raman signal can be further enhanced by the analyte 10 disposed between the nanoparticles 120. [

In the figure, the size and shape of the analysis object 10 are simplified for the sake of illustration and may have various shapes such as the shape of the polymer depending on the type of the analysis object 10.

Next, referring to FIG. 2, measuring a Raman signal from the analyte 10 (S140) may be performed.

The optical signals from the analyte 10 can be measured using the signal measuring units 210 and 220 shown in Fig. The optical signal may be a Raman scattering shift, but is not limited thereto. By analyzing the optical signal, it is possible to detect presence, type, and change of the analyte 10.

5A and 5B are partial perspective views illustrating features of a surface enhanced Raman scattering sensor according to an embodiment of the present invention.

Referring to FIG. 5A, the nanoparticles 120 may be disposed along the edges by a coffee-ring effect on the metal layer 110 to form a first coffee ring. Referring to FIG. 5B, the analyte 10 may be disposed along the edge by a coffee-ring effect on the metal layer 110 to form a second coffee ring.

That is, the surface enhanced Raman scattering sensor of the present invention comprises nanoparticles 120 arranged by spontaneously formed first coffee ring. Such a sensor can be provided in a portable form. Also, at the time of measurement using the sensor, a second coffee ring spontaneously formed by the analyte 10 on the nanoparticles 120 may be formed by overlapping with the nanoparticles 120. The analyte 10 forms a second coffee ring and naturally reaches the hot spot between the nanoparticles 120 and can be arranged at a high concentration, so that the sensitivity of the sensor can be improved.

The present invention is not limited to the above-described embodiment and the accompanying drawings, but is intended to be limited by the appended claims. It will be apparent to those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. something to do.

10: Analyte
100: sensing part
101: substrate
110: metal layer
120: nanoparticles
210:
220:
300: Sample preparation
1000: Surface enhanced Raman scattering sensor

Claims (12)

At least one metal layer disposed on the substrate and having a circular shape;
Nanoparticles disposed along an edge of the metal layer; And
And a sample providing unit for providing a solution containing an analyte corresponding to the size of the metal layer on the metal layer on which the nanoparticles are arranged.
The method according to claim 1,
Wherein the nanoparticles are arranged in a ring shape along the shape of the metal layer.
The method according to claim 1,
And a signal measuring unit for measuring a Raman signal from the analyte after the solvent of the solution provided by the sample preparation is evaporated.
The method according to claim 1,
Wherein the metal layer has a hydrophilic surface and the substrate has a hydrophobic surface.
The method according to claim 1,
Wherein the metal layer and the nanoparticles are made of the same material.
The method according to claim 1,
Wherein the plurality of metal layers are arranged in rows and columns on the substrate.
Forming at least one metal layer having a circular shape on a substrate;
Providing a solution comprising nanoparticles on the metal layer; And
And evaporating the solvent of the solution so that the nanoparticles remain,
Wherein the nanoparticles are arranged in a ring shape along the edges of the metal layer spontaneously by a coffee-ring effect.
8. The method of claim 7,
After the step of evaporating the solvent,
And cleaning the surface of the nanoparticles arranged on the metal layer. ≪ RTI ID = 0.0 > 21. < / RTI >
8. The method of claim 7,
The upper surface of the substrate exposed around the metal layer is treated to have hydrophobicity,
Wherein the surface of the metal layer is formed to have hydrophilicity.
Providing a substrate on which at least one metal layer having a circular shape and nanoparticles disposed along an edge of the metal layer are formed;
Providing a solution containing the analyte on the metal layer on which the nanoparticles are disposed, the analyte corresponding to the size of the metal layer;
Evaporating the solvent of the solution so that the analyte remains; And
And measuring the Raman signal from the analyte using a surface enhanced Raman scattering sensor.
11. The method of claim 10,
Wherein the analyte is spontaneously located between the nanoparticles along the edge of the metal layer by a coffee-ring effect and by a surface enhanced Raman scattering sensor.
11. The method of claim 10,
Wherein the metal layer has a hydrophilic surface and the substrate is provided with a hydrophobic surface such that the solution forms a defined droplet on the metal layer.
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Cited By (3)

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KR102202509B1 (en) * 2019-12-16 2021-01-13 인하대학교 산학협력단 Hydrophobic Paper-based SERS Substrate Using Gold nanoparticle Decorated on Graphene Oxide Flakes And Manufacturing Method Thereof
WO2022182125A1 (en) * 2021-02-23 2022-09-01 모던밸류 주식회사 Heat controller-integrated, turn-off-type droplet loading cartridge for measuring optical signal
KR20230082715A (en) * 2021-12-01 2023-06-09 성균관대학교산학협력단 Triple or quadruple nanoring structure and method of manufacturing the same

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CN109164085A (en) * 2018-08-27 2019-01-08 嘉兴长维新材料科技有限公司 A method of methamphetamine class drugs are detected based on Surface enhanced Raman scattering technology
KR102271473B1 (en) * 2020-04-27 2021-07-02 경희대학교 산학협력단 Hydrogel-based array substrate manufacturing method for surface-enhanced raman scattering analysis and analysis method using the same

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
KR102202509B1 (en) * 2019-12-16 2021-01-13 인하대학교 산학협력단 Hydrophobic Paper-based SERS Substrate Using Gold nanoparticle Decorated on Graphene Oxide Flakes And Manufacturing Method Thereof
WO2022182125A1 (en) * 2021-02-23 2022-09-01 모던밸류 주식회사 Heat controller-integrated, turn-off-type droplet loading cartridge for measuring optical signal
KR20230082715A (en) * 2021-12-01 2023-06-09 성균관대학교산학협력단 Triple or quadruple nanoring structure and method of manufacturing the same

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