KR101532881B1 - Method of producinig gold structure with platium frame located inside and chemical/bio sensor comprising gold structure with platium frame located inside - Google Patents
Method of producinig gold structure with platium frame located inside and chemical/bio sensor comprising gold structure with platium frame located inside Download PDFInfo
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- KR101532881B1 KR101532881B1 KR1020140103246A KR20140103246A KR101532881B1 KR 101532881 B1 KR101532881 B1 KR 101532881B1 KR 1020140103246 A KR1020140103246 A KR 1020140103246A KR 20140103246 A KR20140103246 A KR 20140103246A KR 101532881 B1 KR101532881 B1 KR 101532881B1
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Abstract
According to the method for synthesizing a gold structure in which the platinum frame of the present invention is located, a platinum frame is contained in the gold structure, thereby preventing agglomeration of gold nanoparticles. Therefore, it can be used for a long time when used in a biosensor, Even when exposed to solution or air, it does not affect the analytical results, thus enabling reliable sensing.
In addition, according to the method for synthesizing the gold structure in which the platinum frame of the present invention is disposed, since the etchant (etchant) is also used as a metal precursor, the gold nanoparticles can be etched by adding a reducing agent, The re-growth process can be easily switched.
According to the present invention, by providing a gold structure having a platinum frame inside a two-dimensional or three-dimensional shape, the surface area is widened to effectively interact with light outside and inside the structure to interact with the electromagnetic field of the nanorail It can be utilized more efficiently in biosensing.
Description
The present invention relates to a method of synthesizing a gold structure in which a platinum frame is disposed. The present invention also relates to a biosensor including a gold structure in which a platinum frame is disposed.
In the case of biosensors, molecular detection, identification, and analysis are possible using surface plasmon resonance of gold particles. For reliability of surface plasmon resonance, it is very important to prevent agglomeration of gold nanoparticles used.
In the case of gold nanoparticles, when agglomeration occurs, biosensing affects the analysis results and thus fails to provide stable measurement. Therefore, it is very important to prevent the surface agglomeration of these gold nanoparticles. For this purpose, various methods of synthesizing gold nanoparticles are being carried out.
In general, lithography using a polymer particle such as polystyrene as a mold and sputtering is mainly used. However, this method has a disadvantage in that it can be synthesized only on a limited surface of a two-dimensional substrate, and it is difficult to separate it from a substrate.
In addition, there is a method of synthesizing silver nanoparticles by using galvanic substitution reaction with gold ions. However, the nanoparticles synthesized by this method have a limitation in controlling the thickness, and they sometimes aggregate to show structural instability .
The present invention provides a manufacturing method for preventing agglomeration of gold nanoparticles in which coagulation phenomenon occurs in the prior art, and provides a biosensor including the gold nanoparticle structure manufactured thereby.
In addition, it is also possible to provide a two-dimensional or three-dimensional structure in which gold nanoparticles are coated on the outside with a platinum frame in the inside, and a ring structure in the case of a two- By interacting with light, it is expected to be used more effectively in biosensing through interaction with the electromagnetic field of the nanorail.
According to another aspect of the present invention, there is provided a method of fabricating a gold structure having a platinum frame disposed therein, the method comprising: preparing a gold structure having platinum grown on the gold structure; Etching the gold structure having the platinum around it in an aqueous solution to etch all of the gold therein to leave only the platinum frame; And a reducing agent in an aqueous solution to reduce gold particles on the surface of the platinum frame to regrow.
In this case, the gold structure is etched in an aqueous solution by a solution providing gold trivalent ions. The solution providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution.
In addition, the solution providing the trivalent ions is used as a gold precursor in the step of reducing gold particles on the surface of the platinum frame and regrowing them.
The gold structure has a three-dimensional shape, and the gold structure in which the platinum is grown is platinum grown along the periphery, edge, and vertex of the gold structure.
According to a further embodiment of the present invention, there is provided a method of synthesizing a gold structure in which a platinum frame is disposed, comprising: preparing a gold structure; Growing platinum along the perimeter, corners and vertices of the gold structure; Etching the gold structure having the platinum around it in an aqueous solution to etch all of the gold therein to leave only the platinum frame; And a reducing agent in an aqueous solution to reduce gold particles on the surface of the platinum frame to regrow.
A biosensor according to an embodiment of the present invention includes a platinum frame of a three-dimensional shape; And gold particles covering the surface of the platinum frame.
The platinum frame is formed by etching a gold structure in which platinum is grown to etch the gold structure in an aqueous solution to etch all of the gold. The etching is performed by a solution which provides gold trivalent ions. The solution for providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution.
According to the method for synthesizing a gold structure in which the platinum frame of the present invention is located, a platinum frame is contained in the gold structure, thereby preventing agglomeration of gold nanoparticles. Therefore, it can be used for a long time when used in a biosensor, Even when exposed to solution or air, it does not affect the analytical results, thus enabling reliable sensing.
In addition, according to the method for synthesizing the gold structure in which the platinum frame of the present invention is disposed, since the etchant (etchant) is also used as a metal precursor, the gold nanoparticles can be etched by adding a reducing agent, The re-growth process can be easily switched.
According to the present invention, by providing a gold structure having a platinum frame inside a two-dimensional or three-dimensional shape, the surface area is widened to effectively interact with light outside and inside the structure to interact with the electromagnetic field of the nanorail It can be utilized more efficiently in biosensing.
FIG. 1 shows a flowchart of a method of synthesizing a gold structure in which a platinum frame is disposed according to an embodiment of the present invention.
FIG. 2 is a schematic view of a method of synthesizing a gold structure in which a platinum frame is disposed according to an embodiment of the present invention.
FIG. 3 is a photograph of a gold structure in which a platinum frame manufactured according to an embodiment of the present invention is located.
FIG. 4 shows UV-vis absorption spectra of a gold structure in which a platinum frame fabricated according to an embodiment of the present invention is located.
FIG. 5 is a view showing the control of the thickness of the gold structure by increasing the amount of the etching solution to increase the Au 3+ ion.
FIG. 6 is a photograph showing a stepwise view of a three-dimensional gold structure in which a platinum frame manufactured according to an embodiment of the present invention is located.
FIG. 7 is a graph showing sensitivity of chemical sensing by a gold structure in which a platinum frame according to an embodiment of the present invention is located.
Figure 8 shows a flow diagram of a method of synthesizing a gold structure in which a platinum frame is located, according to a further embodiment of the present invention.
Various embodiments are now described with reference to the drawings, wherein like reference numerals are used throughout the drawings to refer to like elements. For purposes of explanation, various descriptions are set forth herein to provide an understanding of the present invention. It is evident, however, that such embodiments may be practiced without these specific details. In other instances, well-known structures and devices are shown in block diagram form in order to facilitate describing the embodiments.
The following description provides a simplified description of one or more embodiments in order to provide a basic understanding of embodiments of the invention. This section is not a comprehensive overview of all possible embodiments and is not intended to identify key elements or to cover the scope of all embodiments of all elements. Its sole purpose is to present the concept of one or more embodiments in a simplified form as a prelude to the more detailed description that is presented later.
FIG. 1 is a flow chart of a method of synthesizing a gold structure in which a platinum frame is disposed according to an embodiment of the present invention. FIG. 2 is a view illustrating a method of synthesizing a gold structure in which a platinum frame is disposed according to an embodiment of the present invention Fig.
Referring to FIG. 1, a method of synthesizing a gold structure in which a platinum frame is disposed according to an embodiment of the present invention includes the steps of: (S110) preparing a gold structure in which platinum is grown; A step (S 120) in which an inner gold layer is etched to leave only a platinum frame by etching a gold structure having platinum around it; And adding a reducing agent into the aqueous solution to regenerate the gold particles on the surface of the platinum frame (S 130).
In step S 110, a gold structure having platinum grown around it is prepared. This step is disclosed in the paper entitled " Site-specific growth of a Pt shell on Au nanoplates: tailoring their surface plasmonic behavior "(Nanoscale, 2014, 6. 7339) published by the present inventors in June 2014, The paper is alleged to be an exception claim for the novelty loss of the present application. The step of preparing the gold structure in which the platinum is grown in step S 110 can be prepared according to the disclosure of the relevant paper.
FIG. 2 is a schematic view of a method of synthesizing a gold structure having a platinum frame according to an embodiment of the present invention. Referring to FIG. 2, a disk-shaped Au nano disk is prepared, One example is a nano disk in which a Pt shell is grown on a nano disk. Step S 110 is a step of preparing a nanodisk in which a Pt shell is grown on an Au nanodisk in FIG.
In step S 120, the gold structure in which the platinum is grown is etched in an aqueous solution to etch all of the gold, leaving only the platinum frame. This is a view of the etching process in FIG. 2. As shown in the schematic diagram of FIG. 2, Au in the center of Au nanodices is etched and only the Pt nano-frame remains.
In order to etch gold, an etching solution is required. In this case, an etching solution capable of providing gold trivalent ions (Au 3+ ) is required. These gold trivalent ions have a strong oxidizing power, and thus the central gold component can be etched in the gold structure where the platinum is grown around.
The solution providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution. HAuCl 4 · nH 2 O is a solution state of AuCl 3 that provides gold trivalent ions.
According to the method of the present invention, the etching solution for providing such a trivalent ion is also used as a gold precursor in the step of reducing and regrowing gold particles in step S 130.
In step S 130, the reducing agent is added to the aqueous solution, and the gold particles are reduced on the surface of the platinum frame to grow again. This is a regrowth step in FIG. 2, in which gold particles are reduced on the surface of the platinum frame and re-grown.
In this case, a reducing agent is used to reduce ionic gold ions. In the embodiment shown in FIG. 2, ascorbic acid is used as a reducing agent.
According to a method for synthesizing a gold structure in which a platinum frame according to an embodiment of the present invention is disposed, as shown in FIG. 2, a platinum frame is present as a final structure, and a gold nanoparticle- Loses.
Although FIG. 2 exemplarily shows a ring shape, the present invention is not limited thereto, and a polygon or a circle having an empty interior such as a ring can be formed, and a three-dimensional shape is also possible. .
Platinum is grown along the perimeter, corners, and vertices of the gold structure where platinum is grown around it. Referring to FIGS. 5 and 6, platinum is grown along the perimeter, corners, and vertices of the gold structure in the step of preparing the gold structure in which the platinum is grown in the step S 110.
Therefore, if the gold is etched in step S 120, only the frame of the platinum is left, and then the gold is regrowthed in step S 130, the structure of the present invention is obtained.
Referring to FIG. 6, a gold structure is prepared in step A, and a gold structure in which platinum is grown along the vertex and corner of the gold structure in step B, and platinum is grown around the gold structure. After that, only the platinum frame is left as in the step C by the etching, and the gold nanoparticles are regrown on the surface of the platinum frame in the step D by the regrowth step to obtain the final structure. FIG. 6 is a photograph showing a stepwise view of a three-dimensional gold structure in which a platinum frame manufactured according to an embodiment of the present invention is located.
According to a further embodiment of the present invention, a method of synthesizing a gold structure in which a platinum frame is disposed comprises the steps of: preparing a gold plate; Growing platinum along the perimeter, corners and vertices of the gold plate; Etching the gold structure having the platinum around it in an aqueous solution to etch all of the gold therein to leave only the platinum frame; And adding a reducing agent into the aqueous solution to reduce gold particles on the surface of the platinum frame to regrow.
This is shown in the flowchart of FIG. 8, and each step corresponds to steps 710 to 740 as shown in FIG. The important point in step S720 of FIG. 8 is that it is very important to deposit silver thinly on the surface of the gold plate using silver ions and a reducing agent. This is because platinum grows along the perimeter / corners / vertices of the gold plate in step S720.
A gold structure in which a platinum frame according to an embodiment of the present invention is disposed can be used as a material for a biosensor. The biosensor includes a gold structure in which a platinum frame according to an embodiment of the present invention is disposed.
A biosensor according to an embodiment of the present invention includes: a platinum frame having at least one of a circular shape, a polygonal shape, and a three-dimensional shape; And gold particles covering the surface of the platinum frame. As can be seen in FIG. 2, it can be seen that the gold particles cover the Pt frame located inside and such a frame. This structure is described in more detail in the following embodiments with reference to FIGS. 3-6.
The Pt frame is obtained by etching all internal gold through a process of etching a gold structure grown on the periphery of the platinum, as described above, in an aqueous solution, and this etching is carried out by a solution providing gold trivalent ions. The solution providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution.
The present invention provides a gold structure in which a platinum frame is disposed. As shown in FIGS. 2-6, the structure has a void space in the inside of the structure (meaning an internal space formed by a structure other than the inside of the structure itself) The surface area of the structure is increased. With this structure, it is possible to effectively interact with light to the inside as well as the outside, and thus, a clean signal can be obtained when used as a biosensor.
In addition, since the platinum frame is present inside, it is possible to suppress the aggregation of the gold nanoparticles as mentioned in the prior art, and thus the shape of the gold nanoparticles can be maintained, thereby enabling reliable measurement of the biosensor .
A gold structure in which a platinum frame according to an embodiment of the present invention is disposed is used as a chemical / biosensor. A gold structure with a platinum frame inside can be used as a biosensor because it can be used for sensing chemical substances. FIG. 7 is a graph showing sensitivity of chemical sensing by a gold structure in which a platinum frame according to an embodiment of the present invention is located. Referring to FIG. 7, in the case of A, the absorption spectrum of the gold nano ring structure is shifted to a long wavelength by changing the refractive index (1.33-1.48) of the solvent. B shows again the change of the peak position with respect to the refractive index in the preceding spectrum, indicating that the chemical sensing of the present nanoparticles is sensitive.
Hereinafter, the contents of the present invention will be further described with reference to specific embodiments.
* Example
All experiments were carried out through aqueous liquid phase reaction and ultraviolet - visible spectrophotometry was used to determine the degree of reaction.
The inventors of the present invention synthesized on the basis of a paper "Site-specific growth of a Pt shell on Au nanoplates: tailoring their surface plasmonic behavior" (Nanoscale, 2014, 6. 7339) published in June 2014, Pt was grown along the perimeter of the disk to prepare a nano disk on which a Pt shell was grown on an Au nano disk dispersed in 5 ml of distilled water.
Then, 2 ml of 0.05 M cetyltrimethylammonium bromide (CTAB) aqueous solution was added as a metal nanoparticle stabilizer and 100 μl of 2 mM HAuCl 4 aqueous solution as a gold precursor was added. To this aqueous solution, a Pt shell was grown on Au nanodisc dispersed in 5 ml of distilled water prepared above After 300 μl of the nanodisk was added, etching was performed at a temperature of 50 ° C for 30 minutes.
After the completion of the etching, the temperature of the reaction solution dropped to room temperature. After that, 250 μl of 5.3 mM ascorbic acid was added for regeneration. After about 4 hours, regeneration was terminated.
The reagent information used is as follows.
Hydrogen tetrachloroaurate (III) hydrate (HAuCl 4 · nH 2 O, 99%, Kojima), L-ascorbic acid (C 6 H 8 O 6, 99.5%, Sigma Aldrich), cetyl trimethyl ammonium bromide (CTAB, C 19 H 42 BrN, 95%, Fluka), distilled water (18.2 M OMEGA, Milli-Q)
FIG. 3 is a photograph of a gold structure in which a platinum frame manufactured according to an embodiment of the present invention is located. As shown in FIG. 3, a nano disk having a Pt shell grown on an Au nanodisk was prepared in step A, gold was etched in step B, and a final structure was obtained by regrowth in step C. As shown in the photograph of step C, a ring-shaped structure is obtained, and it can be seen that these structures are obtained uniformly as a whole as shown in the E photograph. F is an enlarged image of the structure, and it can be seen that gold particles cover the surface of the platinum frame as seen in G.
FIG. 4 shows UV-vis absorption spectra of a gold structure in which a platinum frame fabricated according to an embodiment of the present invention is located. A shows the UV-vis absorption spectrum in the etching process. As a result, it can be confirmed that the peak of gold has disappeared due to the etching of gold. B shows the UV-vis absorption spectrum of the regrowth process. As the gold nanoparticles regrow on the surface of the platinum frame by regrowth, it is confirmed that a peak for gold appears.
Since the experimental method according to the present invention is synthesized through an aqueous liquid phase reaction, the thickness of the gold structure can be easily controlled by adjusting the addition amount of the aqueous etching solution (HAuCl 4 aqueous solution). FIG. 5 is a view showing the control of the thickness of the gold structure by increasing the amount of the etching solution to increase the Au 3+ ion. In the case of Fig. 5, the structure of the annular embodiment described in the above embodiment is made. In FIG. 5, a is a circle, b is a triangle, and c is a polygon. The amount of the etching solution was increased from the left to the right, and the final thickness of the gold structure was increased. This is because the etching solution is also used as a metal precursor in the present invention.
According to the method of the present invention, the thickness of the gold structure can be controlled very easily by controlling the amount of the etching solution, and the peak position of the optical spectrum can be controlled by adjusting the thickness. In addition, the use of thiols, which are known to be well adhered to gold because the surface is made of gold, is capable of surface modification such as attaching bio materials.
The composite structure according to an exemplary embodiment of the present invention has structural stability because the surface of the composite structure is made of gold and has an optical activity and a platinum framework therein. These structures were able to observe the surface plasmon resonance phenomenon due to the optical activity, and it was possible to clearly observe the in-plane mode and the in-plane mode due to the anisotropy. In general, anisotropic nanoparticles are characterized by their high surface area relative to their volume, allowing them to interact more efficiently with electromagnetic fields. In addition, since the inner space is open, the inner surface of the nanorring can be chemically modified, and electromagnetic field interaction in the inner space is enabled, so that the surface of the particle can be efficiently utilized. By utilizing these advantages, biomaterials can be attached through surface modification and applied as a biosensing material.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features presented herein.
Claims (11)
Etching the gold structure having the platinum around it in an aqueous solution to etch all of the gold therein to leave only the platinum frame; And
And adding a reducing agent into the aqueous solution to reduce the gold particles on the surface of the platinum frame to grow again.
A method of synthesizing a gold structure in which a platinum frame is located.
Characterized in that said gold structure is etched in an aqueous solution by a solution which provides gold trivalent ions.
A method of synthesizing a gold structure in which a platinum frame is located.
Wherein the solution providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution.
A method of synthesizing a gold structure in which a platinum frame is located.
The solution in which the gold trivalent ions are provided,
Wherein the gold particles are used as a gold precursor in the step of reducing and regrowing gold particles on the surface of the platinum frame.
A method of synthesizing a gold structure in which a platinum frame is located.
Wherein the gold structure is in a three-dimensional form.
A method of synthesizing a gold structure in which a platinum frame is located.
Wherein the platinum is grown around the gold structure, the platinum being grown along the circumference, edge, and vertex of the gold structure.
A method of synthesizing a gold structure in which a platinum frame is located.
Growing platinum along the perimeter, corners and vertices of the gold structure;
Etching the gold structure having the platinum around it in an aqueous solution to etch all of the gold therein to leave only the platinum frame; And
And adding a reducing agent into the aqueous solution to reduce the gold particles on the surface of the platinum frame to grow again.
A method of synthesizing a gold structure in which a platinum frame is located.
And gold particles covering the surface of the platinum frame.
Wherein the platinum frame is formed by etching a gold structure in which platinum is grown around the gold structure in an aqueous solution to etch all of the gold therein.
Wherein the etching is performed by a solution providing gold trivalent ions.
Wherein the solution providing the gold trivalent ions is HAuCl 4 .nH 2 O or HAuCl 4 solution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102260209B1 (en) * | 2020-01-28 | 2021-06-02 | 성균관대학교산학협력단 | Single or double frame nanoparticle synthesis method, and single or double frame nanoparticles produced thereby |
| KR102497161B1 (en) * | 2021-09-06 | 2023-02-08 | 성균관대학교산학협력단 | Synthesis method of frame nanoparticles having porous structure and surface-enhanced raman scattering analysis method using the same |
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| WO2023244068A1 (en) * | 2022-06-17 | 2023-12-21 | 성균관대학교산학협력단 | Triple frame nanoparticles and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102260209B1 (en) * | 2020-01-28 | 2021-06-02 | 성균관대학교산학협력단 | Single or double frame nanoparticle synthesis method, and single or double frame nanoparticles produced thereby |
| US11796476B2 (en) | 2020-01-28 | 2023-10-24 | Research & Business Foundation Sungkyunkwan University | Single or double frame nanoparticle synthesis method, and single or double frame nanoparticle produced thereby |
| KR102497161B1 (en) * | 2021-09-06 | 2023-02-08 | 성균관대학교산학협력단 | Synthesis method of frame nanoparticles having porous structure and surface-enhanced raman scattering analysis method using the same |
| KR20230082715A (en) * | 2021-12-01 | 2023-06-09 | 성균관대학교산학협력단 | Triple or quadruple nanoring structure and method of manufacturing the same |
| KR102628030B1 (en) | 2021-12-01 | 2024-01-24 | 성균관대학교산학협력단 | Triple or quadruple nanoring structure and method of manufacturing the same |
| WO2023244068A1 (en) * | 2022-06-17 | 2023-12-21 | 성균관대학교산학협력단 | Triple frame nanoparticles and preparation method therefor |
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