KR101331088B1 - Chemical Sensor by using the Metal Nano Particle and Method of Manufacturing the same - Google Patents
Chemical Sensor by using the Metal Nano Particle and Method of Manufacturing the same Download PDFInfo
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Abstract
A chemical sensor using metal nanoparticles and a method of manufacturing a chemical sensor using metal nanoparticles are provided. Chemical sensor using a metal nanoparticle according to an embodiment of the present invention is formed on the metal nanoparticles, the ligand organic monomolecules bonded using the metal nanoparticles and the metal bonding functional group, the metal nanoparticles and the ligand organic monomolecules formed A substrate bonding function, a substrate, an electrode having an IDT (interdigitate) structure formed on the substrate, and a substrate functional group formed on the substrate and positioned between the electrodes, wherein the substrate bonding function and the substrate functional group may be covalently bonded. have. Accordingly, it is possible to provide a chemical sensor that compensates for the disadvantages while maintaining the advantages of the existing metal nanoparticle sensor. In addition, the chemical sensor is very easy to manufacture, the sensing characteristics can be designed very precisely, and the size can also be manufactured very small. In particular, in the sensing characteristics, the detection of polar and non-polar components is also very good, the response speed is fast, and the sensing performance and characteristics persist without changing for a long time, thereby making it possible to manufacture a sensor having excellent durability and reliability.
Description
The present invention relates to a chemical sensor using metal nanoparticles and a method of manufacturing a chemical sensor using metal nanoparticles, and more particularly, to a chemical sensor using metal nanoparticles having excellent sensing characteristics and durability, and a chemical sensor using metal nanoparticles. It relates to a method for producing.
Conventional representative chemical sensors are metal oxide sensors, which are detected at a high temperature (200 ° C. to 400 ° C.), and are detected by a redox reaction with a molecule to be detected as the metal oxide on the surface is activated at a high temperature. Because redox reactions occur irreversibly, the surface activity decreases with time of use and eventually loses detection.
Therefore, there is a long service life and a correction function for the detection characteristic change is entered even during the service life. Despite these drawbacks, metal oxides account for most of the commercial sensors due to the robustness of detection performance and the recent development of chemical sensors based on metal oxides.
As a sensor to overcome the inconvenience of high temperature sensing, a sensor using a polymer sensing film has been developed. A polymer is present on the electrode as a sensing film. Sensing is performed by the polymer membrane absorbing the analyte in the atmosphere and affecting the mechanical or electrical properties of the polymer depending on the amount of the substance being absorbed.
Such sensing can occur at room temperature, allowing the sensing to proceed at room temperature. And the sensing reaction time depends on the dynamic equilibrium of the molecules to be detected on the polymer surface. In general, the dynamic equilibrium on the polymer surface takes a long time.
There is an example in which gold nanoparticles surrounded by octanethiol are present in a thin film form on an electrode substrate and used as a chemical sensor. At this time, the sensitivity of 1 ppm to toluene was excellent and the reaction time was also within a few seconds.
However, the octanethiol gold nanoparticle sensor showed excellent sensitivity to nonpolar molecules, but very low sensitivity to alcohol or water, which is the polarity sensing object.
A gold nanoparticle sensor surrounded by phenol was synthesized to form a chemical sensor in the form of a thin film on an electrode substrate, showing excellent sensitivity to polar molecules. In particular, branches were also found in the tens ppm level.
However, even after several minutes at 100 ppm, saturation did not occur and the reaction continued to occur. In this case, the sensitivity to the polar molecules is excellent, but it does not overcome the problem of long reaction time.
In addition, chemical sensors using polymers and metal nanoparticles may change morphology of the sensor thin film over time. In particular, due to the interaction between the gas molecules and the sensor thin film while reacting to various types of vapor, the physical structure previously maintained by the sensor thin film may change, and thus the sensing characteristics may change.
Unlike a metal oxide sensor, it is not a chemical irreversible reaction, so the sensing performance does not degrade with time, but as mentioned above, the sensing characteristic is changed due to the change in the physical and structural properties of the sensor thin film. There is a risk of deterioration.
An object of the present invention is to provide a chemical sensor using metal nanoparticles excellent in detection characteristics and durability.
Another object of the present invention is to provide a method of manufacturing a chemical sensor using metal nanoparticles having excellent sensing characteristics and durability.
Chemical sensor using a metal nanoparticle for achieving the above object of the present invention is a metal nanoparticle; Ligand organic monomolecules bonded using the metal nanoparticles and the metal bonding functional groups; A functional group for bonding the substrate formed on the bonded metal nanoparticle and the ligand organic monomolecule; Board; An electrode having an IDT structure formed on the substrate; And a substrate functional group formed on the substrate and positioned between the electrodes. The substrate bonding function and the substrate functional group may be covalently coupled.
Here, the bonded metal nanoparticles and ligand organic monomolecules may be formed as a mono layer on the substrate.
Here, the metal nanoparticles may be gold (Au).
Here, the ligand organic single molecule may be composed of the bottom and the body.
Here, the bottom of the ligand organic single molecule may be formed of any one of an amine and a thiol.
Here, the body of the ligand organic single molecule may be formed of any one of-(CH 2) n-and-(CH 2 CH 2 O) n-.
Here, the body of the ligand organic monomolecule may be formed of any one structure of an aromatic ring and an aliphatic ring.
Here, the functional group for bonding the substrate may be formed of any one of amine, -COOH and benzyl halogen.
Here, the substrate may be formed of any one of silicon and glass.
Here, the substrate functional group may be formed of any one of -OH, -NH 2 and -COOH.
Method for producing a chemical sensor using a metal nanoparticle for achieving the above another object of the present invention comprises the steps of combining the metal nanoparticles and ligand organic monomolecules using a metal bonding functional group; Forming a functional group for bonding the substrate to the bonded metal nanoparticle and the ligand organic monomolecule; Forming an electrode having an interdigitate (IDT) structure on the substrate; Forming a substrate functional group between the electrodes formed on the substrate; And covalently coupling the substrate functional group and the substrate functional group.
Here, the step of coupling the metal nanoparticles with the ligand organic monomolecule using the metal bonding functional group may be a two-phase method.
Here, the step of forming a functional group for bonding the substrate to the bonded metal nanoparticles and ligand organic monomolecules may be to use a ligand exchange reaction (Ligand Exchange Reaction).
Here, the step of forming an electrode having an IDT structure on the substrate may be using a lithography method.
Here, the ligand organic monomolecules bonded to the metal nanoparticles may be formed as a mono layer on the substrate by using the substrate bonding function and the substrate functional group covalently bonding.
According to the manufacturing method of the chemical sensor using the metal nanoparticles and the metal nanoparticles as described above, it is possible to provide a chemical sensor that compensates for the disadvantages while maintaining the advantages of the conventional metal nanoparticle sensor.
In addition, the chemical sensor is very easy to manufacture, the sensing characteristics can be designed very precisely, and the size can also be manufactured very small.
In particular, in the sensing characteristics, the detection of polar and non-polar components is also very good, the response speed is fast, and the sensing performance and characteristics persist without changing for a long time, thereby making it possible to manufacture a sensor having excellent durability and reliability.
As a result, it is possible to provide a chemical sensor having three main properties of sensitivity, sensitivity, and speed.
1 is a structural diagram illustrating a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
2 is a structural diagram illustrating a metal nanoparticle and a ligand organic monomolecule bonded in a chemical sensor using metal nanoparticles according to an exemplary embodiment of the present invention.
3 is a plan view illustrating a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
4 is a graph illustrating the performance of a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
5 is a flowchart illustrating a method of manufacturing a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail.
It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
The terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component. And / or < / RTI > includes any combination of a plurality of related listed items or any of a plurality of related listed items.
When a component is referred to as being "connected" or "connected" to another component, it may be directly connected to or connected to that other component, but it may be understood that other components may be present in between. Should be. On the other hand, when an element is referred to as being "directly connected" or "directly connected" to another element, it should be understood that there are no other elements in between.
The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this application, the terms "comprise" or "have" are intended to indicate that there is a feature, number, step, operation, component, part, or combination thereof described in the specification, and one or more other features. It is to be understood that the present invention does not exclude the possibility of the presence or the addition of numbers, steps, operations, components, components, or a combination thereof.
Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be interpreted in an ideal or overly formal sense unless explicitly defined in the present application Do not.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In order to facilitate the understanding of the present invention, the same reference numerals are used for the same constituent elements in the drawings and redundant explanations for the same constituent elements are omitted.
1 is a structural diagram illustrating a chemical sensor using metal nanoparticles according to an embodiment of the present invention. 2 is a structural diagram illustrating a metal nanoparticle and a ligand organic monomolecule bonded in a chemical sensor using metal nanoparticles according to an exemplary embodiment of the present invention.
1 and 2 in parallel, the
In particular, in the
Since it is formed as a single layer on the substrate as described above, the resistance can be adjusted by changing the size of the metal nanoparticles and the size of the ligand organic monomolecules, and at the same time the resistance between the electrodes by changing the distance from several hundred nm to several tens of um level Can be adjusted.
First, the
Next, the ligand
Here, the bottom of the ligand organic
In addition, the body of the ligand organic
Next, the
Meanwhile, the
In addition, the
3 is a plan view illustrating a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
Referring to Figure 3, it can be seen the structure of the chemical sensor using the metal nanoparticles according to an embodiment of the present invention. That is, the
When the gas to be detected in the above structure is introduced, a change is generated between the electrodes by the interaction between the gas and the combination of the metal nanoparticle and the ligand organic monomolecule, and the change of the electrode is detected to detect the presence or absence of a specific gas. And concentration can be determined.
4 is a graph illustrating the performance of a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
Referring to FIG. 4, FIG. 4 is a potential of an electrode according to a specific gas (NH 3) concentration on a time axis (horizontal axis) when sensing using a chemical sensor using metal nanoparticles according to an embodiment of the present invention. It can be seen that there is a change.
That is, it can be seen that as the concentration of the specific gas NH3 gradually increases, the potential change of the electrode also increases. Although the time for detecting the specific gas NH3 is slightly different, it is understood that a long time is not required. Can be.
As a result, it can be seen that the chemical sensor using the metal nanoparticles according to an embodiment of the present invention has excellent detection sensitivity for a specific gas and a fast response speed, and a substrate, a metal nanoparticle, and a ligand organic single molecule. It will be seen that the binder is also excellent in durability because it is bonded to each other by covalent bonds.
5 is a flowchart illustrating a method of manufacturing a chemical sensor using metal nanoparticles according to an embodiment of the present invention.
5, the method of manufacturing a chemical sensor using a metal nanoparticles according to an embodiment of the present invention comprises the steps of binding the metal nanoparticles and ligand organic monomolecules using a metal bonding functional group (step 510); Forming a functional group for bonding a substrate to the bonded metal nanoparticle and the ligand organic monomolecule (step 520); Forming an electrode having an interdigitate (IDT) structure on the substrate (step 530); Forming a substrate functional group between the electrodes formed on the substrate (step 540); And covalently coupling the substrate functional group and the substrate functional group (step 550).
First, the step of binding the metal nanoparticle and the ligand organic single molecule using the metal bonding functional group (step 510) may be to use a two-phase method.
Next, forming a functional group for bonding the substrate to the bonded metal nanoparticle and the ligand organic monomolecule (step 520) may be to use a Ligand Exchange Reaction.
Next, forming an electrode having an IDT (interdigitate) structure on the substrate (step 530) may be by using a lithography method.
Next, the step of covalently bonding the substrate functional group and the substrate functional group (step 550) may be a bond between the substrate, the metal nanoparticles and the conjugate of the ligand organic monomolecule, Using the step of covalently binding the substrate functional group (step 550), the ligand organic monomolecules bound to the metal nanoparticles may be formed as a mono layer on the substrate.
Preparation Example 01: Bonding of Metal Nanoparticles with Ligand Organic Single Molecules (When Thiol Is Formed at the Bottom of Ligand Organic Single Molecules)
Dissolve 20.0 g of tetraoctylammonium bromide in 800 ml of toluene, mix HAuCl4 (3.5 g, 8.9 mol) in this solution with 300 ml of water and stir for several minutes.
4-methylbenzenethiol (1.08 g, 8.7 mol) and sodiumborohydride (3.8 g) dissolved in water (250 ml) were added to the mixed solution, followed by stirring for 3 hours, and the organic layer was separated.
The organic solvent is evaporated and suspended in ethanol and placed in the refrigerator to induce precipitation.
The precipitated product is washed with ethanol and dried to obtain 4-methylbenzenethiol gold nanoparticles (4-MB-AuNP).
Preparation Example 02: Bonding of Metal Nanoparticles with Ligand Organic Single Molecules (When Amine Was Formed at the Bottom of Ligand Organic Single Molecules)
Dissolve tetraoctylammonium bromide in toluene, mix HAuCl4 in 300 ml of water in this solution and stir for several minutes.
Diaminobenzene and sodiumborohydride dissolved in water are added to the mixed solution, stirred for 3 hours, and the organic layer is separated.
The organic solvent is evaporated, suspended in ethanol and placed in the refrigerator to induce precipitation.
The precipitated product is washed with ethanol and dried to obtain diaminobenzene gold nanoparticles.
Preparation Example 03: Bonding of Metal Nanoparticles with Ligand Organic Single Molecules
Dissolve tetraoctylammonium bromide in toluene, mix HAuCl4 in 300 ml of water in this solution and stir for several minutes.
n-alkylthiol and sodiumborohydride dissolved in water are added to the mixed solution, stirred for 3 hours, and the organic layer is separated.
The organic solvent is evaporated, suspended in ethanol and placed in the refrigerator to induce precipitation.
The precipitated product is washed with ethanol and dried to obtain n-alkylthiol gold nanoparticles.
Preparation Example 4 Bonding of Metal Nanoparticles with Ligand Organic Single Molecules
Dissolve tetraoctylammonium bromide in toluene, mix HAuCl4 in 300 ml of water in this solution, and stir for several minutes.
SH (CH2CH2O) n-HS and sodiumborohydride dissolved in water are added to the mixed solution, stirred for 3 hours, and the organic layer is separated.
The organic solvent is evaporated, suspended in ethanol and placed in the refrigerator to induce precipitation.
The precipitated product is washed with ethanol and dried to obtain SH (CH2CH2O) n-HS gold nanoparticles.
Preparation Example 05 Formation of Substrate Bonding Functional Group on Bonded Metal Nanoparticles and Ligand Organic Monomers
4-methylbenzenethiol gold nanoparticles (4-MB-AuNP, 100 mg), which is a metal nanoparticle and a ligand organic monomolecular complex, is mixed with a large amount of 4-hydroxybenzenethiol (14 mg), and then stirred for 5 days.
The final product is suspended in a solvent, filtered, washed with a solvent, and the solvent is evaporated under reduced pressure to form a functional group for joining the substrate to the bound metal nanoparticles and ligand organic monomolecules.
Preparation Example 06: Formation of substrate bonding functional groups on the bonded metal nanoparticles and ligand organic monomolecules (when Amine is used as the substrate bonding functionality)
4-methylbenzenethiol gold nanoparticles (4-MB-AuNP, 100 mg), which is a metal nanoparticle and a ligand organic monomolecular complex, is mixed with a large amount of 4-aminobenzenethiol, dissolved in a solvent, and stirred for 5 days.
The final product is suspended in a solvent, filtered, washed with a solvent, and the solvent is evaporated under reduced pressure to form a functional group for joining the substrate to the bound metal nanoparticles and ligand organic monomolecules.
Preparative Example 07: Forming a functional group for bonding the substrate to the bonded metal nanoparticles and the ligand organic monomolecule (when COOH is used as the functional group bonding
4-methylbenzenethiol gold nanoparticles (4-MB-AuNP, 100 mg), which is a metal nanoparticle and a ligand organic monomolecular complex, is mixed with a large amount of carboxylicbenzenethiol, dissolved in a solvent, and stirred for 5 days.
The final product is suspended in a solvent, filtered, washed with a solvent, and the solvent is evaporated under reduced pressure to form a functional group for joining the substrate to the bound metal nanoparticles and ligand organic monomolecules.
Preparation Example 08: Forming a functional group for bonding the substrate on the bonded metal nanoparticles and ligand organic monomolecules (when Benzyl halogen is used as the substrate bonding function)
4-methylbenzenethiol gold nanoparticles (4-MB-AuNP, 100 mg), which is a metal nanoparticle and a ligand organic monomolecular conjugate, is mixed with a large amount of bromobenzenethiol and chlorobenzenethiol, dissolved in a solvent, and stirred for 5 days.
The final product is suspended in a solvent, filtered, washed with a solvent, and the solvent is evaporated under reduced pressure to form a functional group for joining the substrate to the bound metal nanoparticles and ligand organic monomolecules.
Preparation Example 09 An electrode having an IDT (interdigitate) structure was formed on a substrate
The
The mask is painted with IDT electrodes, is aligned with the substrate using a stepper or contactor, exposed, then developed to form a PR pattern.
Here, both intaglio and embossed patterns can be used, and the PR used can be changed in some cases.
A metal film is deposited on the substrate on which the PR pattern is formed by using E-beam or sputtering, and the PR is removed to complete the substrate on which the IDT is formed.
Preparation Example 10 Formation of Substrate Functional Group Between Electrodes Formed on Substrate (When -OH is Used as Substrate Functionality)
Since OH group exists on a glass substrate, it may be used as it is.
In the case of a silicon substrate, an OH function is introduced by depositing an oxide layer on the surface with a thickness of tens to hundreds of nm.
Preparation Example 11 Formation of Substrate Functional Group Between Electrodes Formed on Substrate (When -NH2 Is Used as Substrate Functionality)
One of the glass substrate and the silicon substrate on which the oxide film is loaded is sequentially washed with deionized water, ethanol, THF, and deionized (DI) water and then dried.
One of 2% 3-aminopropyl trimethoxysilane and 3-aminopropyltriethoxysilane is prepared, and -OH substrate is dipped in this solution for 4 hours, and then dried at 100 ° C for one hour.
Preparation Example 12: Forming a Substrate Functional Group Between the Electrodes formed on the Substrate (When Using -COOH as the Substrate Functionality)
Prepare a 10% solution of either COOH-C6H6-COOH and COOH- (CH) 4-COOH.
DI water, THF and ethanol are used as a solvent.
An amine substrate was deposited on the solution under an acid or base catalyst to install COOH groups on the surface.
Preparation Example 13: Covalent Bonding of a Substrate Bonding Functionality and the Substrate Functionality
Before the gold nanoparticles are placed between the electrodes of the fabricated substrate, the electrodes are soaked in piranha solution (H2SO4 / H2O2 = 3: 1), sonicated for 1 minute and washed with methanol and acetone.
After dissolving gold nanoparticles in a solvent, dip-coating the substrate electrode to form a covalent bond between the substrate bonding function and the substrate functional group.
It will be understood by 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 in the appended claims. It will be possible.
100: chemical sensor using metal nanoparticles
110: metal nanoparticles
120: functional group for metal bonding
130: ligand organic single molecule
140: functional group for board bonding
150: substrate
160: electrode
170: substrate functional group
Claims (15)
Ligand organic monomolecules bonded using the metal nanoparticles and the metal bonding functional groups;
A functional group for bonding the substrate formed on the bonded metal nanoparticle and the ligand organic monomolecule;
Board;
An electrode having an IDT structure formed on the substrate; And
And a substrate functional group formed on the substrate and positioned between the electrodes.
The substrate bonding group and the substrate functional group is a chemical sensor characterized in that the covalent coupling.
The combined metal nanoparticles and ligand organic monomolecules are formed as a mono layer on the substrate.
The metal nanoparticles are gold (Au) chemical sensor, characterized in that.
The ligand organic monomolecule is a chemical sensor, characterized in that consisting of the bottom and the body.
The bottom of the ligand organic monomolecule is a chemical sensor, characterized in that formed with any one of the amine (amine) and thiol (thiol).
The body of the ligand organic monomolecule is formed of any one of-(CH2) n- and-(CH2CH2O) n- chemical sensor.
The body of the ligand organic monomolecule is a chemical sensor, characterized in that formed in the structure of any one of the aromatic ring (aromatic ring) and aliphatic ring (aliphatic ring).
The substrate bonding functional group is a chemical sensor, characterized in that formed with any one of amine, -COOH and benzyl halogen.
And the substrate is formed of any one of silicon and glass.
The substrate functional group is a chemical sensor, characterized in that formed with any one of -OH, -NH2 and -COOH.
Forming a functional group for bonding the substrate to the bonded metal nanoparticle and the ligand organic monomolecule;
Forming an electrode having an interdigitate (IDT) structure on the substrate;
Forming a substrate functional group between the electrodes formed on the substrate; And
And a step of covalently coupling the substrate functional group and the functional group for bonding the substrate.
The bonding of the metal nanoparticles and the ligand organic monomolecules using the functional group for metal bonding may use a two-phase method.
Forming a functional group for bonding the substrate to the bonded metal nanoparticles and the ligand organic monomolecule is a method of manufacturing a chemical sensor, characterized in that using a Ligand Exchange Reaction.
Forming an electrode having an IDT structure on the substrate using a lithography method.
Preparation of a chemical sensor, characterized in that the ligand organic monomolecules bonded to the metal nanoparticles are formed as a mono layer on the substrate by using the substrate bonding function and the substrate functional group covalently bonded Way.
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| US12/946,852 US8398921B2 (en) | 2009-12-18 | 2010-11-15 | Chemical sensor using metal nano-particles and method for manufacturing chemical sensor using metal nano-particles |
| US13/765,889 US9034275B2 (en) | 2009-12-18 | 2013-02-13 | Chemical sensor using metal nano-particles and method for manufacturing chemical sensor using metal nano-particles |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020046960A (en) * | 2000-12-12 | 2002-06-21 | 소니 인터내셔널(유로파) 게엠베하 | Selective chemical sensors based on interlinked nanoparticle assemblies |
| US7347974B1 (en) * | 1998-05-04 | 2008-03-25 | The United States Of America As Represented By The Secretary Of The Navy | Materials, method and apparatus for detection and monitoring of chemical species |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7347974B1 (en) * | 1998-05-04 | 2008-03-25 | The United States Of America As Represented By The Secretary Of The Navy | Materials, method and apparatus for detection and monitoring of chemical species |
| KR20020046960A (en) * | 2000-12-12 | 2002-06-21 | 소니 인터내셔널(유로파) 게엠베하 | Selective chemical sensors based on interlinked nanoparticle assemblies |
Non-Patent Citations (1)
| Title |
|---|
| BURKHARD RAGUSE et al. "Gold Nanoparticle Chemiresistor Sensors: Direct Sensing of Organics in Aqueous Electrolyte Solution", Analytical Chemistry, Vol. 79, No. 19, pp. 7333-7339, 2007.10.01. * |
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