Name: 저자 스포트라이트: Synthesized AgNPs를 사용한 SERS Flexible Substrates의 개발 및 응용.
Uploaded: 2023-11-17T14:00:00
Description: Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

이 연구는 중국 국립 자연 과학 재단(보조금 번호 61974004 및 61931018)과 중국 국가 핵심 R&D 프로그램(보조금 번호 2021YFB3200100)의 지원을 받습니다. 이 연구는 전자 현미경에 대한 접근을 제공한 북경 대학의 전자 현미경 실험실을 인정합니다. 또한 이 연구는 라만 측정에 도움을 준 Ying Cui와 베이징 대학교 지구 및 우주 과학 학교에 감사드립니다.

1. 나노 입자의 합성
<ol><li>질산은 용액의 제조<ol><li>정밀 칭량 저울을 사용하여 0.0017 g의 AR 등급 질산은(AgNO3, 재료 표 참조)을 측정하고 10 mL의 탈이온수(DI)에 첨가합니다. 혼합물을 저어 10-3 mol/LAgNO3 용액을 만듭니다.</li>
	</ol></li>
	<li>은-암모니아 복합체의 제조<ol><li>AR 등급 암모니아수 1mL(NH3. H2O, 재료표 참조)를 주?...

R6G 및 Thiram의 SERS 검출을 위한 유연한 기판 제작

<ol>
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이 연구에서는 화학적 변형을 통해 AgNP를 PDMS에 결합하고 우수한 성능을 달성한 유연한 SERS 기판을 도입했습니다. 입자 합성 중, 특히 은 암모니아 복합체 합성(1.2단계)에서 용액의 색상이 중요한 역할을 합니다. 암모니아 물을 너무 많이 적하하면 AgNP의 합성 품질에 부정적인 영향을 미쳐 검출 결과가 실패할 수 있습니다. 합성 과정에서 기판 개질(2.2단계)에 주의를 기울여야 합니다. 그렇지 않으?...

라만 산란의 일종인 표면 강화 라만 산란(SERS)은 고감도 및 부드러운 검출 조건의 이점을 제공하며 단일 분자 검출도 달성할 수 있습니다 1,2,3,4. 금 및 은과 같은 금속 나노 구조는 일반적으로 물질 검출을 가능하게 하는 SERS 기판으로 사용됩니다 5,6. 나노 구조 표면의 전자기 결합 향상은 SERS 응용 분야에서 중요한 역할을 합니다. 다양한 크기, 모양, 입자 간 거리 및 조성을 가진 금속 나노 구조는 국부적인 표면 플라즈몬 공명(7,8)으로 인해 강렬한 전자기장을 생성하는 수많은 "핫스팟"을 생성하기 위해 응집될 수 있습니다. 많은 연구에서 SERS 기판으로 형태가 다른 금속 나노 입자를 개발하여 SERS 향상 9,10을 달성하는 데 효과적임을 입증했습니다.
유연한 SERS 기판은 곡선 표면에서 직접 감지를 용이하게 하기 위해 유연한 기판에 증착된 SERS 효과를 생성할 수 있는 나노 구조를 사용하여 광범위한 응용 분야를 찾습니다. 유연한 SERS 기판은 불규칙하거나, 비평면이거나, 곡면에 있는 표면에서 분석물을 검출하고 수집하는 데 사용됩니다. 일반적인 연성 SERS 기판에는 섬유, 폴리머 필름 및 그래핀 산화막 11,12,13,14가 포함됩니다. 그 중 폴리디메틸실록산(PDMS)은 가장 널리 사용되는 고분자 재료 중 하나이며 높은 투명도, 높은 인장 강도, 화학적 안정성, 무독성 및 접착력15,16,17과 같은 이점을 제공합니다. PDMS는 라만 단면적이 낮아 라만 신호에 미치는 영향은 무시할 수 있다18. PDMS 프리폴리머는 액체 형태이기 때문에 열이나 빛에 의해 경화될 수 있어 높은 수준의 제어성과 편의성을 제공합니다. PDMS-기반 SERS 기판은 비교적 일반적인 유연한 SERS 기판으로서, 예시적인 성능(19,20)을 갖는 상이한 생화학적 물질을 검출하기 위해 다양한 금속 나노입자를 내장하기 위해 이전 연구에서 사용되어 왔다.
SERS 기판을 준비할 때 나노갭 구조의 제작이 중요합니다. 물리적 증착 기술은 높은 확장성, 균일성 및 재현성과 같은 이점을 제공하지만 일반적으로 우수한 진공 조건과 특수 장비가 필요하므로 실제 적용이 제한됩니다21. 또한, 수 나노미터 규모의 나노 구조를 제작하는 것은 기존의 증착 기술로는 여전히 어려운 과제로 남아있다 22. 결과적으로, 화학적 방법을 통해 합성된 나노 입자는 다양한 상호작용을 통해 유연한 투명 필름에 흡착될 수 있으며, 나노 스케일에서 금속 구조의 자체 조립을 용이하게 할 수 있습니다. 성공적인 흡착을 보장하기 위해, 상호 작용은 그 표면 친수성을 변경하기 위해 필름 표면을 물리적 또는 화학적으로 변형시킴으로써 조정될 수 있다(23). 은 나노 입자는 금 나노 입자에 비해 더 나은 SERS 성능을 나타내지 만 불안정성, 특히 공기 중 산화에 대한 민감성으로 인해 SERS 향상 인자 (EF)가 급격히 감소하여 기판 성능에 영향을 미친다24. 따라서 안정적인 입자 방법을 개발하는 것이 필수적입니다.
살충제 잔류물의 존재는 상당한 주목을 받아왔으며, 현장에서 식품에서 다양한 등급의 유해 화학물질을 신속하게 검출하고 식별할 수 있는 강력한 방법에 대한 긴급한 필요성을 야기하고 있다25,26. 유연한 SERS 기판은 실제 응용 분야, 특히 식품 안전 분야에서 고유한 이점을 제공합니다. 이 기사에서는 합성 포도당 코팅은 나노 입자(AgNP)를 PDMS 기판에 접착하여 유연한 SERS 기판을 제조하는 방법을 소개합니다(그림 1). 포도당의 존재는 AgNP를 보호하여 공기 중의 은 산화를 완화합니다. 이 기판은 우수한 검출 성능을 보여 10-10M의 낮은 로다 민 6G (R6G)와 10-8M의 살충제 Thiram을 우수한 균일 성으로 검출 할 수 있습니다. 또한, 유연한 기판은 다양한 잠재적 응용 시나리오와 함께 접착 및 샘플링을 통한 검출에 사용할 수 있습니다.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Ammonia (NH3.H2O, 25%)</td>
			<td>Beijing Chemical Works</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>APTES (98%)</td>
			<td>Beyotime</td>
			<td>ST1087</td>
			<td></td>
		</tr>
		<tr>
			<td>BD-20AC Laboratory Chrona Treater</td>
			<td>Electro-Technic Products Inc.</td>
			<td>12051A</td>
			<td></td>
		</tr>
		<tr>
			<td>D-glucose</td>
			<td>Beijing Chemical Works</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Environmental Scanning electron microscope (ESEM)</td>
			<td>FEI</td>
			<td>QUANTA 250</td>
			<td></td>
		</tr>
		<tr>
			<td>Raman microscope</td>
			<td>Horiba JY</td>
			<td>LabRAM HR Evolution</td>
			<td></td>
		</tr>
		<tr>
			<td>Rhodamine 6G</td>
			<td>Beijing Chemical Works</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Silicone Elastomer Base and Silicone Elastomer Curing Agent</td>
			<td>Dow Corning Corporation</td>
			<td>SYLGARD 184</td>
			<td></td>
		</tr>
		<tr>
			<td>Silver nitrate</td>
			<td>Beijing Chemical Works</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Thiram (C6H12N2S2, 99.9%)</td>
			<td>Beijing Chemical Works</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of polydimethylsiloxane (pdms)-based flexible surface-enhanced raman scattering (sers) substrate for ultrasensitive detection

이 기사에서는 SERS(Surface-Enhanced Raman Scattering)를 위해 설계된 유연한 기판의 제조 방법을 제시합니다. 은 나노 입자 (AgNP)는 질산 은(AgNO3)과 암모니아를 포함하는 착화 반응을 통해 합성 된 후 포도당을 사용하여 환원되었습니다. 그 결과 AgNP는 20nm에서 50nm 범위의 균일한 크기 분포를 나타냈습니다. 이어서, 3-아미노프로필 트리에톡시실란(APTES)을 사용하여 산소 플라즈마로 표면 처리된 PDMS 기판을 변형시켰다. 이 공정은 기판에 AgNP의 자체 조립을 용이하게 했습니다. 다양한 실험 조건이 기판 성능에 미치는 영향에 대한 체계적인 평가는 우수한 성능과 EF(Enhanced Factor)를 갖춘 SERS 기판의 개발로 이어졌습니다. 이 기판을 활용하여 R6G(로다민 6G)의 경우 10-10M , 티람의 경우 10-8M 의 인상적인 검출 한계를 달성했습니다. 이 기질은 사과의 잔류 농약을 검출하는 데 성공적으로 사용되어 매우 만족스러운 결과를 얻었습니다. 유연한 SERS 기판은 복잡한 시나리오에서의 감지를 포함하여 실제 응용 분야에 대한 큰 잠재력을 보여줍니다.

Surface-Enhanced Raman Scattering (SERS), as a type of Raman scattering, offers the advantages of high sensitivity and gentle detection conditions, and can even achieve single molecule detection1,2,3,4. Metal nanostructures, such as gold and silver, are typically used as SERS substrates to enable substance detection5,6. Electromagnetic coupling enhancement on nanostructured surfaces plays a significant role in SERS applications. Metallic nanostructures with varying sizes, shapes, interparticle distances, and compositions can aggregate to create numerous &#34;hotspots&#34; generating intense electromagnetic fields due to localized surface plasmon resonances7,8. Many studies have developed metal nanoparticles with different morphologies as SERS substrates, demonstrating their effectiveness in achieving SERS enhancement9,10.
Flexible SERS substrates find wide applications, with nanostructures capable of producing SERS effects deposited on flexible substrates to facilitate direct detection on curved surfaces. Flexible SERS substrates are employed for detecting and collecting analytes on irregular, non-planar, or curved surfaces. Common flexible SERS substrates include fibers, polymer films, and graphene oxide films11,12,13,14. Among them, polydimethylsiloxane (PDMS) is one of the most widely used polymer materials and offers advantages such as high transparency, high tensile strength, chemical stability, non-toxicity, and adhesion15,16,17. PDMS has a low Raman cross-section, making its impact on the Raman signal negligible18. Since the PDMS prepolymer is in liquid form, it can be cured by heat or light, providing a high degree of controllability and convenience. PDMS-based SERS substrates are relatively common flexible SERS substrates, having been used in previous studies to embed various metal nanoparticles for detecting different biochemical substances with exemplary performance19,20.
In the preparation of SERS substrates, the fabrication of nanogap structures is crucial. Physical deposition technology offers advantages like high scalability, uniformity, and reproducibility but typically requires good vacuum conditions and specialized equipment, limiting its practical applications21. Additionally, fabricating nanostructures at the few-nanometer scale remains challenging with conventional deposition techniques22. Consequently, nanoparticles synthesized through chemical methods can be adsorbed onto flexible transparent films through various interactions, facilitating the self-assembly of metallic structures at the nanoscale. To ensure successful adsorption, interactions can be adjusted by physically or chemically modifying the film surface to alter its surface hydrophilicity23. Silver nanoparticles, compared to gold nanoparticles, exhibit better SERS performance, but their instability, particularly their susceptibility to oxidation in air, results in a rapid decrease in the SERS Enhancement Factor (EF), affecting substrate performance24. Hence, it is essential to develop a stable particle method.
The presence of pesticide residues has garnered significant attention, creating a pressing need for robust methods capable of rapidly detecting and identifying various classes of hazardous chemicals in food in the field25,26. Flexible SERS substrates offer unique advantages in practical applications, particularly in the realm of food safety. This article introduces a method for preparing a flexible SERS substrate by bonding synthesized glucose-coated silver nanoparticles (AgNPs) onto a PDMS substrate (Figure 1). The presence of glucose protects the AgNPs, mitigating silver oxidation in the air. The substrate demonstrates excellent detection performance, capable of detecting Rhodamine 6G (R6G) as low as 10-10 M and pesticide Thiram as low as 10-8 M, with good uniformity. Moreover, the flexible substrate can be employed for detection through bonding and sampling, with numerous potential application scenarios.

저자 스포트라이트: Synthesized AgNPs를 사용한 SERS Flexible Substrates의 개발 및 응용. 

초고감도 검출을 위한 폴리디메틸실록산(PDMS) 기반 SERS(Flexible Surface-Enhanced Raman Scattering) 기판 제작

This protocol describes preparing SERS flexible substrates, applying them to actual detection scenarios. The SERS flexible substrate offered by this protocol is environmental friendly and achieves good detection performance. The silver nanoparticles can be synthesized easily by simple vessels, and do not require complicated experimental conditions and environment.In our laboratory, we plan to focus on researching the silver nanoparticles synthesized through the vessel used in this study. We'll explore methods to enhance their SERS detection capabilities, and leverage their unique properties and characteristics to design better performing SERS detection substrates.

본 연구에서는 합성 AgNP를 포도당으로 감싸고 APTES를 이용하여 PDMS에 자가 조립한 유연한 SERS 기질을 개발하여 실제 살충제 검출 응용 분야에서 우수한 검출 성능을 달성하였다. R6G 및 Thiram의 검출 한계는 각각 10-10M 및 10-8M에 도달했으며 EF(Enhancement Factor)는 1 x 10 5입니다. 또한, 기판은 균일성을 입증했다.
글루코스에 싸인 AgNP는 개선된 톨렌스 방법<sup c...

Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

이 프로토콜은 표면 강화 라만 산란을 위한 유연한 기판의 제조 방법을 설명합니다. 이 방법은 낮은 농도의 R6G 및 Thiram을 성공적으로 검출하는 데 사용되었습니다.

This article presents a fabrication method for a flexible substrate designed for Surface-Enhanced Raman Scattering (SERS). Silver nanoparticles (AgNPs) ...

이 프로토콜은 SERS 플렉시블 기판을 준비하여 실제 검출 시나리오에 적용하는 방법을 설명합니다. 이 프로토콜에서 제공하는 SERS 플렉시블 기판은 환경 친화적이며 우수한 검출 성능을 달성합니다. 은 나노 입자는 간단한 용기로 쉽게 합성 할 수 있으며 복잡한 실험 조건과 환경이 필요하지 않습니다.우리 연구실에서는 본 연구에 사용된 용기를 통해 합성된 은 나노입자 연구에 주력할 계획이다. SERS 검출 기능을 강화하고 고유한 특성과 특성을 활용하여 더 나은 성능의 SERS 검출 기판을 설계하는 방법을 살펴봅니다.

fabrication-polydimethylsiloxane-pdms-based-flexible-surface-enhanced

Research

JoVE Journal

Engineering

Fabrication of polydimethylsiloxane (PDMS)-Based Flexible Surface-Enhanced Raman Scattering (SERS) Substrate for Ultrasensitive Detection

This article presents a fabrication method for a flexible substrate designed for Surface-Enhanced Raman Scattering (SERS). Silver nanoparticles (AgNPs) were synthesized through a complexation reaction involving silver nitrate (AgNO3) and ammonia, followed by reduction using glucose. The resulting AgNPs exhibited a uniform size distribution ranging from 20 nm to 50 nm. Subsequently, 3-aminopropyl triethoxysilane (APTES) was employed to modify a PDMS substrate that had been surface-treated with oxygen plasma. This process facilitated the self-assembly of AgNPs onto the substrate. A systematic evaluation of the impact of various experimental conditions on substrate performance led to the development of a SERS substrate with excellent performance and an Enhanced Factor (EF). Utilizing this substrate, impressive detection limits of 10-10 M for R6G (Rhodamine 6G) and 10-8 M for Thiram were achieved. The substrate was successfully employed for detecting pesticide residues on apples, yielding highly satisfactory results. The flexible SERS substrate demonstrates great potential for real-world applications, including detection in complex scenarios.

This protocol describes a fabrication method for a flexible substrate for surface-enhanced Raman scattering. This method has been used in the successful detection of low concentrations of R6G and Thiram.

연구

공학

Synthesis of Silver Nanoparticles and Preparation of Flexible SERS Detection Substrate

To prepare silver nitrate solution, measure 0.0017 grams of AR grade silver nitrate on a weighing balance. Add the weighed powder to 10 milliliters of deionized water and stir the mixture. Draw one milliliter of AR grade ammonia water using a syringe and add it to the silver nitrate solution while stirring, until the solution becomes clear.To prepare 0.2 molar glucose solution, weigh 0.36 grams of glucose powder and add it to 10 milliliters of deionized water. Stir the mixture thoroughly. Next, using a pipette gun, add 30 microliters of the silver ammonia complex into the glucose solution at 30 minute intervals.To synthesize yellow colored silver nanoparticles. To synthesize the PDMS substrate, take five grams of PDMS A solution and add B solution into it, at a ratio of one to 10. Stir the mixture thoroughly.Transfer the mixed PDMS into a square Petri dish and bake it in an 80 degree Celsius oven for two hours. Once cured, use a scalpel to cut the PDMS along the dark grid of the dish, creating small cubes. Next, move the handheld plasma processor back and forth over the PDMS piece for surface plasma treatment.For APTES modification, immerse the surface modified PDMS pieces into 10%APTES solution for 10 hours. Finally, immerse the PDMS substrate into the silver nanoparticle solution for 10 hours. ESEM images showed uniformity in synthesized nanoparticles with diameters between 20 and 50 nanometers.The Surface-Enhanced Raman Scattering signals for fabricated PDMS substrates displayed excellent detection capability, reaching a limit of 10 to the negative 10th molar for R6G with notable enhancement effect. The substrate also showed Thiram detection with clear characteristic peaks, up to 10 to the minus eighth molar. The paste and peel method on the apple surface show the detection of Thiram up to 10 to the minus seventh molar, indicating the effectiveness of the substrate for identifying pesticide residues on fruit surfaces.