Name: Autore in primo piano: Sviluppo e applicazione di substrati flessibili SERS utilizzando AgNP sintetizzati
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

La ricerca è sostenuta dalla National Natural Science Foundation of China (Grant n. 61974004 e 61931018), nonché dal National Key R&D Program of China (Grant n. 2021YFB3200100). Lo studio riconosce al Laboratorio di Microscopia Elettronica dell'Università di Pechino l'accesso ai microscopi elettronici. Inoltre, la ricerca si estende grazie a Ying Cui e alla Scuola di Scienze della Terra e dello Spazio dell'Università di Pechino per la loro assistenza nelle misurazioni Raman.

1. Sintesi di nanoparticelle
<ol><li>Preparazione della soluzione di nitrato d'argento<ol><li>Utilizzando una bilancia di precisione, misurare 0,0017 g di nitrato d'argento di grado AR (AgNO3, vedere la tabella dei materiali) e aggiungerlo a 10 mL di acqua deionizzata (DI). Mescolare la miscela per creare una soluzione di AgNO 3 10-3 mol/L.</li>
	</ol></li>
	<li>Preparazione del complesso argento-ammoniaca<ol><li>Assumere 1 mL di acqua ammoniacale di gr...

Fabbricazione di substrato flessibile per la rilevazione SERS di R6G e Thiram

<ol>
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In questo studio, è stato introdotto un substrato SERS flessibile, che ha legato le AgNP al PDMS attraverso la modifica chimica e ha ottenuto prestazioni eccellenti. Durante la sintesi delle particelle, in particolare nella sintesi del complesso dell'ammoniaca d'argento (fase 1.2), il colore della soluzione gioca un ruolo cruciale. L'aggiunta di troppa acqua ammoniacale goccia a goccia può influire negativamente sulla qualità della sintesi delle AgNP, portando potenzialmente a risultati di rilevamento non riusciti. Pr...

Il Surface-Enhanced Raman Scattering (SERS), come tipo di scattering Raman, offre i vantaggi di un'elevata sensibilità e di condizioni di rilevamento delicate e può persino ottenere il rilevamento di una singola molecola 1,2,3,4. Le nanostrutture metalliche, come l'oro e l'argento, sono tipicamente utilizzate come substrati SERS per consentire il rilevamento di sostanze 5,6. Il miglioramento dell'accoppiamento elettromagnetico su superfici nanostrutturate svolge un ruolo significativo nelle applicazioni SERS. Le nanostrutture metalliche con dimensioni, forme, distanze interparticellari e composizioni variabili possono aggregarsi per creare numerosi "hotspot" che generano intensi campi elettromagnetici a causa di risonanze plasmoniche superficiali localizzate 7,8. Molti studi hanno sviluppato nanoparticelle metalliche con diverse morfologie come substrati SERS, dimostrando la loro efficacia nel raggiungimento del potenziamento SERS 9,10.
I substrati flessibili di SERS trovano ampie applicazioni, con nanostrutture in grado di produrre effetti SERS depositati su substrati flessibili per facilitare il rilevamento diretto su superfici curve. I substrati flessibili SERS sono impiegati per la rilevazione e la raccolta di analiti su superfici irregolari, non planari o curve. I substrati SERS flessibili comuni includono fibre, film polimerici e film di ossido di grafene11,12,13,14. Tra questi, il polidimetilsilossano (PDMS) è uno dei materiali polimerici più utilizzati e offre vantaggi come elevata trasparenza, elevata resistenza alla trazione, stabilità chimica, non tossicità e adesione15,16,17. Il PDMS ha una bassa sezione d'urto Raman, rendendo trascurabile il suo impatto sul segnale Raman18. Poiché il prepolimero PDMS è in forma liquida, può essere polimerizzato con il calore o la luce, fornendo un elevato grado di controllabilità e praticità. I substrati SERS basati su PDMS sono substrati SERS flessibili relativamente comuni, essendo stati utilizzati in studi precedenti per incorporare varie nanoparticelle metalliche per la rilevazione di diverse sostanze biochimiche con prestazioni esemplari19,20.
Nella preparazione dei substrati SERS, la fabbricazione di strutture nanogap è cruciale. La tecnologia di deposizione fisica offre vantaggi come un'elevata scalabilità, uniformità e riproducibilità, ma in genere richiede buone condizioni di vuoto e attrezzature specializzate, limitandone le applicazioni pratiche21. Inoltre, la fabbricazione di nanostrutture su scala di pochi nanometri rimane impegnativa con le tecniche di deposizione convenzionali22. Di conseguenza, le nanoparticelle sintetizzate attraverso metodi chimici possono essere adsorbite su film trasparenti flessibili attraverso varie interazioni, facilitando l'autoassemblaggio di strutture metalliche su scala nanometrica. Per garantire il successo dell'adsorbimento, le interazioni possono essere regolate modificando fisicamente o chimicamente la superficie del film per alterarne l'idrofilia superficiale23. Le nanoparticelle d'argento, rispetto alle nanoparticelle d'oro, mostrano migliori prestazioni SERS, ma la loro instabilità, in particolare la loro suscettibilità all'ossidazione nell'aria, si traduce in una rapida diminuzione del fattore di potenziamento SERS (EF), influenzando le prestazioni del substrato24. Quindi, è essenziale sviluppare un metodo a particelle stabili.
La presenza di residui di pesticidi ha attirato un'attenzione significativa, creando una pressante necessità di metodi robusti in grado di rilevare e identificare rapidamente varie classi di sostanze chimiche pericolose negli alimentisul campo 25,26. I substrati flessibili SERS offrono vantaggi unici nelle applicazioni pratiche, in particolare nel campo della sicurezza alimentare. Questo articolo presenta un metodo per preparare un substrato SERS flessibile legando nanoparticelle d'argento rivestite di glucosio (AgNP) sintetizzate su un substrato PDMS (Figura 1). La presenza di glucosio protegge le AgNP, mitigando l'ossidazione dell'argento nell'aria. Il substrato dimostra eccellenti prestazioni di rilevamento, in grado di rilevare la Rhodamine 6G (R6G) fino a 10-10 M e il pesticida Thiram fino a 10-8 M, con una buona uniformità. Inoltre, il substrato flessibile può essere impiegato per il rilevamento tramite incollaggio e campionamento, con numerosi potenziali scenari applicativi.

<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

Questo articolo presenta un metodo di fabbricazione per un substrato flessibile progettato per lo scattering Raman potenziato dalla superficie (SERS). Le nanoparticelle d'argento (AgNP) sono state sintetizzate attraverso una reazione di complessazione che coinvolge nitrato d'argento (AgNO3) e ammoniaca, seguita da una riduzione mediante glucosio. Le AgNP risultanti hanno mostrato una distribuzione dimensionale uniforme compresa tra 20 nm e 50 nm. Successivamente, il 3-amminopropiltrietossisilano (APTES) è stato impiegato per modificare un substrato PDMS che era stato trattato in superficie con plasma di ossigeno. Questo processo ha facilitato l'auto-assemblaggio delle AgNP sul substrato. Una valutazione sistematica dell'impatto di varie condizioni sperimentali sulle prestazioni del substrato ha portato allo sviluppo di un substrato SERS con prestazioni eccellenti e un fattore avanzato (EF). Utilizzando questo substrato, sono stati raggiunti impressionanti limiti di rilevamento di 10-10 M per R6G (Rhodamine 6G) e 10-8 M per Thiram. Il substrato è stato impiegato con successo per rilevare residui di pesticidi sulle mele, ottenendo risultati molto soddisfacenti. Il substrato flessibile SERS dimostra un grande potenziale per le applicazioni del mondo reale, incluso il rilevamento in scenari complessi.

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.

Autore in primo piano: Sviluppo e applicazione di substrati flessibili SERS utilizzando AgNP sintetizzati 

Fabbricazione di substrato SERS (Flexible Surface-Enhanced Raman Scattering) a base di polidimetilsilossano (PDMS) per la rilevazione ultrasensibile

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.

In questo studio, è stato sviluppato un substrato SERS flessibile composto da AgNP sintetiche avvolte nel glucosio e autoassemblate su PDMS utilizzando APTES, ottenendo eccellenti prestazioni di rilevamento per applicazioni pratiche di rilevamento di pesticidi. I limiti di rilevamento per R6G e Thiram sono stati entrambi raggiunti rispettivamente a 10-10 M e 10-8 M, con un fattore di miglioramento (EF) di 1 x 10 5. Inoltre, il substrato ha dimostrato uniformità.
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Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

Questo protocollo descrive un metodo di fabbricazione per un substrato flessibile per lo scattering Raman potenziato dalla superficie. Questo metodo è stato utilizzato per rilevare con successo basse concentrazioni di R6G e Thiram.

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

Questo protocollo descrive la preparazione dei substrati flessibili SERS, applicandoli a scenari di rilevamento reali. Il substrato flessibile SERS offerto da questo protocollo è rispettoso dell'ambiente e raggiunge buone prestazioni di rilevamento. Le nanoparticelle d'argento possono essere sintetizzate facilmente da semplici recipienti e non richiedono complicate condizioni sperimentali e ambientali.Nel nostro laboratorio, abbiamo in programma di concentrarci sulla ricerca delle nanoparticelle d'argento sintetizzate attraverso il recipiente utilizzato in questo studio. Esploreremo i metodi per migliorare le loro capacità di rilevamento SERS e sfrutteremo le loro proprietà e caratteristiche uniche per progettare substrati di rilevamento SERS più performanti.

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.

Ricerca

Ingegneria

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.