Name: Autor destacado: Desarrollo y aplicación de sustratos flexibles SERS utilizando AgNPs sintetizadas
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La investigación cuenta con el apoyo de la Fundación Nacional de Ciencias Naturales de China (Subvención n.º 61974004 y 61931018), así como del Programa Nacional de Investigación y Desarrollo Clave de China (subvención n.º 2021YFB3200100). El estudio reconoce al Laboratorio de Microscopía Electrónica de la Universidad de Pekín por proporcionar acceso a los microscopios electrónicos. Además, la investigación se extiende gracias a Ying Cui y a la Escuela de Ciencias de la Tierra y el Espacio de la Universidad de Pekín por su ayuda en las mediciones Raman.

1. Síntesis de nanopartículas
<ol><li>Preparación de la solución de nitrato de plata<ol><li>Con una balanza de pesaje de precisión, mida 0,0017 g de nitrato de plata de grado AR (AgNO3, consulte la Tabla de materiales) y agréguelo a 10 ml de agua desionizada (DI). Revuelva la mezcla para crear una solución de AgNO 3 de 10-3 mol/L.</li>
	</ol></li>
	<li>Preparación del complejo plata-amoníaco<ol><li>Tome 1 ml de agua con amoníaco de grado AR (N...

Fabricación de sustrato flexible para la detección SERS de R6G y Thiram

<ol>
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R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Transfer+printing+for+preparing+nanostructured+PDMS+film+as+flexible+SERS+active+substrate.">Transfer printing for preparing nanostructured PDMS film as flexible SERS active substrate.</a> Composites Part B: Engineering. 84, 222-227 (2016).</li><li>West, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Searching+for+better+plasmonic+materials.">Searching for better plasmonic materials.</a> Laser &amp; Photonics Reviews. 4, 795-808 (2010).</li><li>Anastassiades, M., Lehotay, S. J., &#352;tajnbaher, d., Schenck, F. 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En este estudio, se introdujo un sustrato SERS flexible, que unió AgNPs a PDMS a través de la modificación química y logró un excelente rendimiento. Durante la síntesis de partículas, específicamente en la síntesis del complejo de plata y amoníaco (paso 1.2), el color de la solución juega un papel crucial. La adición de demasiada agua de amoníaco gota a gota puede afectar negativamente a la calidad de la síntesis de AgNPs, lo que puede dar lugar a resultados de detección infructuosos. Se debe prestar atenc...

La dispersión Raman mejorada en superficie (SERS), como un tipo de dispersión Raman, ofrece las ventajas de una alta sensibilidad y condiciones de detección suaves, e incluso puede lograr la detección de una sola molécula 1,2,3,4. Las nanoestructuras metálicas, como el oro y la plata, se utilizan normalmente como sustratos SERS para permitir la detección de sustancias 5,6. La mejora del acoplamiento electromagnético en superficies nanoestructuradas desempeña un papel importante en las aplicaciones SERS. Las nanoestructuras metálicas con diferentes tamaños, formas, distancias entre partículas y composiciones pueden agregarse para crear numerosos "puntos calientes" que generan intensos campos electromagnéticos debido a las resonancias de plasmones superficiales localizadas 7,8. Muchos estudios han desarrollado nanopartículas metálicas con diferentes morfologías como sustratos de SERS, demostrando su efectividad para lograr el aumento de SERS 9,10.
Los sustratos SERS flexibles encuentran amplias aplicaciones, con nanoestructuras capaces de producir efectos SERS depositadas sobre sustratos flexibles para facilitar la detección directa en superficies curvas. Los sustratos flexibles SERS se emplean para detectar y recolectar analitos en superficies irregulares, no planas o curvas. Los sustratos SERS flexibles comunes incluyen fibras, películas de polímero y películas de óxido de grafeno11,12,13,14. Entre ellos, el polidimetilsiloxano (PDMS) es uno de los materiales poliméricos más utilizados y ofrece ventajas como alta transparencia, alta resistencia a la tracción, estabilidad química, no toxicidad y adhesión15,16,17. El PDMS tiene una sección transversal Raman baja, lo que hace que su impacto en la señal Raman sea insignificante18. Dado que el prepolímero PDMS está en forma líquida, se puede curar con calor o luz, lo que proporciona un alto grado de controlabilidad y comodidad. Los sustratos SERS basados en PDMS son sustratos SERS flexibles relativamente comunes, habiéndose utilizado en estudios previos para incrustar varias nanopartículas metálicas para detectar diferentes sustancias bioquímicas con un rendimiento ejemplar19,20.
En la preparación de sustratos SERS, la fabricación de estructuras nanogap es crucial. La tecnología de deposición física ofrece ventajas como alta escalabilidad, uniformidad y reproducibilidad, pero normalmente requiere buenas condiciones de vacío y equipos especializados, lo que limita sus aplicaciones prácticas21. Además, la fabricación de nanoestructuras a escala de unos pocos nanómetros sigue siendo un reto con las técnicas convencionales de deposición22. En consecuencia, las nanopartículas sintetizadas a través de métodos químicos pueden adsorberse en películas transparentes flexibles a través de diversas interacciones, lo que facilita el autoensamblaje de estructuras metálicas a nanoescala. Para garantizar una adsorción exitosa, las interacciones se pueden ajustar modificando física o químicamente la superficie de la película para alterar su hidrofilicidadsuperficial 23. Las nanopartículas de plata, en comparación con las nanopartículas de oro, exhiben un mejor rendimiento del SERS, pero su inestabilidad, en particular su susceptibilidad a la oxidación en el aire, da como resultado una rápida disminución del factor de mejora (FE) del SERS, lo que afecta el rendimiento del sustrato24. Por lo tanto, es esencial desarrollar un método de partículas estables.
La presencia de residuos de plaguicidas ha atraído una atención significativa, creando una necesidad apremiante de métodos robustos capaces de detectar e identificar rápidamente varias clases de productos químicos peligrosos en los alimentos en el campo25,26. Los sustratos flexibles SERS ofrecen ventajas únicas en aplicaciones prácticas, especialmente en el ámbito de la seguridad alimentaria. Este artículo presenta un método para preparar un sustrato SERS flexible mediante la unión de nanopartículas de plata recubiertas de glucosa sintetizadas (AgNPs) en un sustrato de PDMS (Figura 1). La presencia de glucosa protege las AgNPs, mitigando la oxidación de la plata en el aire. El sustrato demuestra un excelente rendimiento de detección, capaz de detectar rodamina 6G (R6G) a una velocidad tan baja como 10-10 M y el pesticida Thiram a una velocidad tan baja como 10-8 M, con buena uniformidad. Además, el sustrato flexible se puede emplear para la detección a través de la unión y el muestreo, con numerosos escenarios de aplicación potenciales.

<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

Este artículo presenta un método de fabricación para un sustrato flexible diseñado para la dispersión Raman mejorada en superficie (SERS). Las nanopartículas de plata (AgNPs) se sintetizaron a través de una reacción de complejación en la que intervinieron nitrato de plata (AgNO3) y amoníaco, seguida de una reducción con glucosa. Las AgNPs resultantes exhibieron una distribución de tamaño uniforme que osciló entre 20 nm y 50 nm. Posteriormente, se empleó 3-aminopropiltrietoxisilano (APTES) para modificar un sustrato de PDMS que había sido tratado superficialmente con plasma de oxígeno. Este proceso facilitó el autoensamblaje de AgNPs sobre el sustrato. Una evaluación sistemática del impacto de diversas condiciones experimentales en el rendimiento del sustrato condujo al desarrollo de un sustrato SERS con excelente rendimiento y un factor mejorado (FE). Utilizando este sustrato, se lograron impresionantes límites de detección de 10-10 M para R6G (Rhodamine 6G) y 10-8 M para Thiram. El sustrato se empleó con éxito para la detección de residuos de plaguicidas en manzanas, obteniendo resultados altamente satisfactorios. El sustrato flexible de SERS demuestra un gran potencial para aplicaciones del mundo real, incluida la detección en escenarios complejos.

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.

Autor destacado: Desarrollo y aplicación de sustratos flexibles SERS utilizando AgNPs sintetizadas 

Fabricación de sustrato de dispersión Raman mejorada en superficie flexible (SERS) basado en polidimetilsiloxano (PDMS) para detección ultrasensible

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.

En este estudio, se desarrolló un sustrato SERS flexible compuesto por AgNPs sintéticos envueltos en glucosa y autoensamblados en PDMS utilizando APTES, logrando un excelente rendimiento de detección para aplicaciones prácticas de detección de plaguicidas. Los límites de detección para R6G y Thiram se alcanzaron a 10-10 M y 10-8 M, respectivamente, con un factor de mejora (FE) de 1 x 10 5. Además, el sustrato demostró uniformidad.
Las AgNPs envueltas e...

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

Este protocolo describe un método de fabricación de un sustrato flexible para la dispersión Raman mejorada en superficie. Este método se ha utilizado en la detección exitosa de bajas concentraciones de R6G y Thiram.

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

Este protocolo describe la preparación de sustratos flexibles SERS, aplicándolos a escenarios de detección reales. El sustrato flexible SERS que ofrece este protocolo es respetuoso con el medio ambiente y logra un buen rendimiento de detección. Las nanopartículas de plata se pueden sintetizar fácilmente mediante recipientes simples y no requieren condiciones experimentales y ambientales complicadas.En nuestro laboratorio, planeamos centrarnos en la investigación de las nanopartículas de plata sintetizadas a través del recipiente utilizado en este estudio. Exploraremos métodos para mejorar sus capacidades de detección de SERS y aprovecharemos sus propiedades y características únicas para diseñar sustratos de detección de SERS de mejor rendimiento.

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.

Investigación

Ingeniería

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.