Name: Autor im Rampenlicht: Entwicklung und Anwendung von flexiblen SERS-Substraten unter Verwendung synthetisierter AgNPs
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

Die Forschung wird von der National Natural Science Foundation of China (Grant No. 61974004 und 61931018) sowie dem National Key R&D Program of China (Grant No. 2021YFB3200100) unterstützt. Die Studie würdigt das Elektronenmikroskopie-Labor der Universität Peking für den Zugang zu Elektronenmikroskopen. Darüber hinaus bedankt sich die Forschung bei Ying Cui und der School of Earth and Space Science der Peking University für ihre Unterstützung bei Raman-Messungen.

1. Synthese von Nanopartikeln
<ol><li>Herstellung von Silbernitratlösung<ol><li>Mit einer Präzisionswaage werden 0,0017 g Silbernitrat in AR-Qualität (AgNO3, siehe Materialtabelle) abgemessen und zu 10 ml deionisiertem Wasser (DI) gegeben. Rühren Sie die Mischung um, um eine 10-3 mol/LAgNO3-Lösung zu erhalten.</li>
	</ol></li>
	<li>Herstellung des Silber-Ammoniak-Komplexes<ol><li>Nehmen Sie 1 ml Ammoniakwasser in AR-Qualität (NH3. ...

Herstellung eines flexiblen Substrats für die SERS-Detektion von R6G und Thiram

<ol>
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In dieser Studie wurde ein flexibles SERS-Substrat eingeführt, das AgNPs durch chemische Modifikation an PDMS bindet und eine hervorragende Leistung erzielt. Bei der Partikelsynthese, insbesondere bei der Silber-Ammoniak-Komplexsynthese (Schritt 1.2), spielt die Farbe der Lösung eine entscheidende Rolle. Die Zugabe von zu viel Ammoniakwasser kann die Qualität der AgNP-Synthese beeinträchtigen und möglicherweise zu erfolglosen Nachweisergebnissen führen. Während des Syntheseprozesses sollte auf die Substratmodifika...

Die oberflächenverstärkte Raman-Streuung (SERS) als eine Art der Raman-Streuung bietet die Vorteile einer hohen Empfindlichkeit und schonender Detektionsbedingungen und kann sogar die Detektion einzelner Moleküle erreichen 1,2,3,4. Metallnanostrukturen, wie Gold und Silber, werden typischerweise als SERS-Substrate verwendet, um die Detektion von Substanzen zu ermöglichen 5,6. Die Verbesserung der elektromagnetischen Kopplung auf nanostrukturierten Oberflächen spielt eine wichtige Rolle in SERS-Anwendungen. Metallische Nanostrukturen mit unterschiedlichen Größen, Formen, Abständen zwischen den Partikeln und Zusammensetzungen können sich zu zahlreichen "Hotspots" zusammenschließen, die aufgrund lokalisierter Oberflächenplasmonenresonanzen intensive elektromagnetische Felder erzeugen 7,8. In vielen Studien wurden Metallnanopartikel mit unterschiedlichen Morphologien als SERS-Substrate entwickelt, was ihre Wirksamkeit bei der Erzielung einer SERS-Verbesserung belegt 9,10.
Flexible SERS-Substrate finden breite Anwendungen, wobei Nanostrukturen in der Lage sind, SERS-Effekte zu erzeugen, die auf flexiblen Substraten abgeschieden werden, um die direkte Detektion auf gekrümmten Oberflächen zu erleichtern. Flexible SERS-Substrate werden zum Detektieren und Sammeln von Analyten auf unregelmäßigen, nicht-planaren oder gekrümmten Oberflächen eingesetzt. Zu den üblichen flexiblen SERS-Substraten gehören Fasern, Polymerfilme und Graphenoxidfilme11, 12, 13, 14. Unter ihnen ist Polydimethylsiloxan (PDMS) eines der am weitesten verbreiteten Polymermaterialien und bietet Vorteile wie hohe Transparenz, hohe Zugfestigkeit, chemische Stabilität, Ungiftigkeit und Haftung15,16,17. PDMS hat einen geringen Raman-Querschnitt, so dass sein Einfluss auf das Raman-Signal vernachlässigbar ist18. Da das PDMS-Prepolymer in flüssiger Form vorliegt, kann es durch Hitze oder Licht ausgehärtet werden, was ein hohes Maß an Kontrollierbarkeit und Komfort bietet. PDMS-basierte SERS-Substrate sind relativ verbreitete flexible SERS-Substrate, die in früheren Studien verwendet wurden, um verschiedene Metallnanopartikel zum Nachweis verschiedener biochemischer Substanzen mit vorbildlicher Leistung einzubetten19,20.
Bei der Herstellung von SERS-Substraten ist die Herstellung von Nanogap-Strukturen von entscheidender Bedeutung. Die physikalische Abscheidungstechnologie bietet Vorteile wie hohe Skalierbarkeit, Gleichmäßigkeit und Reproduzierbarkeit, erfordert jedoch in der Regel gute Vakuumbedingungen und spezielle Ausrüstung, was ihre praktischen Anwendungen einschränkt21. Darüber hinaus ist die Herstellung von Nanostrukturen im Bereich von wenigen Nanometern mit herkömmlichen Abscheidungstechniken nach wie vor eine Herausforderung22. Folglich können Nanopartikel, die durch chemische Methoden synthetisiert werden, durch verschiedene Wechselwirkungen an flexiblen transparenten Filmen adsorbiert werden, was die Selbstorganisation metallischer Strukturen auf der Nanoskala erleichtert. Um eine erfolgreiche Adsorption zu gewährleisten, können Wechselwirkungen durch physikalische oder chemische Modifikation der Filmoberfläche eingestellt werden, um ihre Oberflächenhydrophiliezu verändern 23. Silbernanopartikel weisen im Vergleich zu Goldnanopartikeln eine bessere SERS-Leistung auf, aber ihre Instabilität, insbesondere ihre Anfälligkeit für Oxidation an der Luft, führt zu einer raschen Abnahme des SERS-Verstärkungsfaktors (EF), was sich auf die Substratleistung auswirkt24. Daher ist es wichtig, eine stabile Partikelmethode zu entwickeln.
Das Vorhandensein von Pestizidrückständen hat große Aufmerksamkeit erregt, was zu einem dringenden Bedarf an robusten Methoden führt, die in der Lage sind, verschiedene Klassen gefährlicher Chemikalien in Lebensmitteln vor Ort schnell zu erkennen und zu identifizieren25,26. Flexible SERS-Substrate bieten einzigartige Vorteile in der Praxis, insbesondere im Bereich der Lebensmittelsicherheit. In diesem Artikel wird eine Methode zur Herstellung eines flexiblen SERS-Substrats vorgestellt, indem synthetisierte glukosebeschichtete Silbernanopartikel (AgNPs) auf ein PDMS-Substrat geklebt werden (Abbildung 1). Das Vorhandensein von Glukose schützt die AgNPs und mildert die Silberoxidation in der Luft. Das Substrat weist eine ausgezeichnete Detektionsleistung auf und ist in der Lage, Rhodamin 6G (R6G) bis zu einer Tiefe von 10-10 M und Pestizid Thiram bis zu 10-8 M mit guter Gleichmäßigkeit zu detektieren. Darüber hinaus kann das flexible Substrat für die Detektion durch Bindung und Probenahme eingesetzt werden, mit zahlreichen potenziellen Anwendungsszenarien.

<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

In diesem Artikel wird eine Herstellungsmethode für ein flexibles Substrat vorgestellt, das für die oberflächenverstärkte Raman-Streuung (SERS) entwickelt wurde. Silbernanopartikel (AgNPs) wurden durch eine Komplexierungsreaktion mit Silbernitrat (AgNO3) und Ammoniak synthetisiert, gefolgt von einer Reduktion mit Glukose. Die resultierenden AgNPs wiesen eine gleichmäßige Größenverteilung von 20 nm bis 50 nm auf. Anschließend wurde 3-Aminopropyltriethoxysilan (APTES) verwendet, um ein PDMS-Substrat zu modifizieren, das mit Sauerstoffplasma oberflächenbehandelt worden war. Dieser Prozess erleichterte die Selbstorganisation von AgNPs auf dem Substrat. Eine systematische Evaluierung des Einflusses verschiedener experimenteller Bedingungen auf die Substratleistung führte zur Entwicklung eines SERS-Substrats mit exzellenter Leistung und einem Enhanced Factor (EF). Mit diesem Substrat wurden beeindruckende Nachweisgrenzen von 10-10 M für R6G (Rhodamin 6G) und 10-8 M für Thiram erreicht. Das Substrat wurde erfolgreich zum Nachweis von Pflanzenschutzmittelrückständen auf Äpfeln eingesetzt und lieferte sehr zufriedenstellende Ergebnisse. Das flexible SERS-Substrat weist ein großes Potenzial für reale Anwendungen auf, einschließlich der Detektion in komplexen Szenarien.

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 im Rampenlicht: Entwicklung und Anwendung von flexiblen SERS-Substraten unter Verwendung synthetisierter AgNPs 

Herstellung eines Polydimethylsiloxan (PDMS)-basierten flexiblen oberflächenverstärkten Raman-Streusubstrats (SERS) für die hochempfindliche Detektion

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 dieser Studie wurde ein flexibles SERS-Substrat entwickelt, das aus synthetischen AgNPs besteht, die in Glukose eingewickelt und unter Verwendung von APTES auf PDMS selbstorganisiert sind, um eine hervorragende Detektionsleistung für praktische Pestizidnachweisanwendungen zu erzielen. Die Nachweisgrenzen für R6G und Thiram wurden beide bei 10-10 M bzw. 10-8 M erreicht, mit einem Verstärkungsfaktor (EF) von 1 x 10 5. Darüber hinaus zeigte das Substrat eine Gleichmäßigkeit.
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Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

Dieses Protokoll beschreibt ein Herstellungsverfahren für ein flexibles Substrat für die oberflächenverstärkte Raman-Streuung. Diese Methode wurde beim erfolgreichen Nachweis niedriger Konzentrationen von R6G und Thiram eingesetzt.

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

Dieses Protokoll beschreibt die Herstellung flexibler SERS-Substrate und deren Anwendung auf tatsächliche Detektionsszenarien. Das von diesem Protokoll angebotene flexible SERS-Substrat ist umweltfreundlich und erzielt eine gute Detektionsleistung. Die Silbernanopartikel können leicht durch einfache Gefäße synthetisiert werden und erfordern keine komplizierten experimentellen Bedingungen und Umgebungen.In unserem Labor wollen wir uns auf die Erforschung der Silbernanopartikel konzentrieren, die durch das in dieser Studie verwendete Gefäß synthetisiert werden. Wir werden Methoden untersuchen, um ihre SERS-Detektionsfähigkeiten zu verbessern und ihre einzigartigen Eigenschaften und Eigenschaften zu nutzen, um leistungsfähigere SERS-Detektionssubstrate zu entwickeln.

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.

Forschung

Ingenieurwesen

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.