Name: Auteur in de schijnwerpers: Ontwikkeling en toepassing van flexibele SER-substraten met behulp van gesynthetiseerde AgNP's
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

Het onderzoek wordt ondersteund door de National Natural Science Foundation of China (Grant No. 61974004 and 61931018), evenals het National Key R&D Program of China (Grant No. 2021YFB3200100). De studie erkent het Electron Microscopy Laboratory van de Universiteit van Peking voor het bieden van toegang tot elektronenmicroscopen. Bovendien strekt het onderzoek zich uit dankzij Ying Cui en de School of Earth and Space Science van de Universiteit van Peking voor hun hulp bij Raman-metingen.

1. Synthese van nanodeeltjes
<ol><li>Bereiding van zilvernitraatoplossing<ol><li>Meet met een precisieweegschaal 0,0017 g zilvernitraat van AR-kwaliteit (AgNO3, zie materiaaltabel) af en voeg dit toe aan 10 ml gedeïoniseerd (DI) water. Roer het mengsel tot een 10-3 mol/L AgNO3-oplossing .</li>
	</ol></li>
	<li>Bereiding van het zilver-ammoniakcomplex<ol><li>Neem 1 ml ammoniakwater van AR-kwaliteit (NH3. H2O, zie Materiaalt...

Fabricage van flexibel substraat voor SER-detectie van R6G en thiram

<ol>
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In deze studie werd een flexibel SERS-substraat geïntroduceerd, dat AgNP's door middel van chemische modificatie aan PDMS bond en uitstekende prestaties bereikte. Tijdens de deeltjessynthese, met name in de synthese van het zilverammoniakcomplex (stap 1.2), speelt de kleur van de oplossing een cruciale rol. Het druppelsgewijs toevoegen van ammoniakwater kan de synthesekwaliteit van AgNP's nadelig beïnvloeden, wat mogelijk kan leiden tot mislukte detectieresultaten. Tijdens het syntheseproces moet aandacht worden bestee...

Surface-Enhanced Raman Scattering (SERS), als een type Raman-verstrooiing, biedt de voordelen van hoge gevoeligheid en zachte detectieomstandigheden, en kan zelfs detectie van één molecuul bereiken 1,2,3,4. Metalen nanostructuren, zoals goud en zilver, worden meestal gebruikt als SERS-substraten om stofdetectie mogelijk te maken 5,6. Verbetering van elektromagnetische koppeling op nanogestructureerde oppervlakken speelt een belangrijke rol in SERS-toepassingen. Metallische nanostructuren met verschillende groottes, vormen, afstanden tussen deeltjes en samenstellingen kunnen samenklonteren om talrijke "hotspots" te creëren die intense elektromagnetische velden genereren als gevolg van gelokaliseerde oppervlakteplasmonresonanties 7,8. Veel studies hebben metalen nanodeeltjes ontwikkeld met verschillende morfologieën als SERS-substraten, wat hun effectiviteit aantoont bij het bereiken van SER-verbetering 9,10.
Flexibele SERS-substraten vinden brede toepassingen, met nanostructuren die SERS-effecten kunnen produceren die op flexibele substraten worden afgezet om directe detectie op gebogen oppervlakken te vergemakkelijken. Flexibele SERS-substraten worden gebruikt voor het detecteren en verzamelen van analyten op onregelmatige, niet-vlakke of gebogen oppervlakken. Veel voorkomende flexibele SERS-substraten zijn vezels, polymeerfilms en grafeenoxidefilms11,12,13,14. Onder hen is polydimethylsiloxaan (PDMS) een van de meest gebruikte polymeermaterialen en biedt het voordelen zoals hoge transparantie, hoge treksterkte, chemische stabiliteit, niet-toxiciteit en hechting15,16,17. PDMS heeft een lage Raman-doorsnede, waardoor de impact op het Raman-signaal verwaarloosbaar is18. Omdat het PDMS-prepolymeer in vloeibare vorm is, kan het worden uitgehard door warmte of licht, wat een hoge mate van controleerbaarheid en gemak biedt. PDMS-gebaseerde SER-substraten zijn relatief veel voorkomende flexibele SERS-substraten, die in eerdere studies zijn gebruikt om verschillende metalen nanodeeltjes in te bedden voor het detecteren van verschillende biochemische stoffen met voorbeeldige prestaties19,20.
Bij de bereiding van SERS-substraten is de fabricage van nanogap-structuren cruciaal. Fysische depositietechnologie biedt voordelen zoals hoge schaalbaarheid, uniformiteit en reproduceerbaarheid, maar vereist doorgaans goede vacuümomstandigheden en gespecialiseerde apparatuur, waardoor de praktische toepassingen ervan worden beperkt21. Bovendien blijft het vervaardigen van nanostructuren op een schaal van enkele nanometers een uitdaging met conventionele depositietechnieken22. Bijgevolg kunnen nanodeeltjes die door middel van chemische methoden worden gesynthetiseerd, door verschillende interacties worden geadsorbeerd aan flexibele transparante films, waardoor de zelfassemblage van metalen structuren op nanoschaal wordt vergemakkelijkt. Om een succesvolle adsorptie te garanderen, kunnen interacties worden aangepast door het filmoppervlak fysisch of chemisch te wijzigen om de hydrofiliciteit van het oppervlak te veranderen23. Zilveren nanodeeltjes vertonen in vergelijking met gouden nanodeeltjes betere SERS-prestaties, maar hun instabiliteit, met name hun gevoeligheid voor oxidatie in lucht, resulteert in een snelle afname van de SERS Enhancement Factor (EF), wat de prestaties van het substraat beïnvloedt24. Daarom is het essentieel om een stabiele deeltjesmethode te ontwikkelen.
De aanwezigheid van residuen van bestrijdingsmiddelen heeft veel aandacht gekregen, waardoor er een dringende behoefte is ontstaan aan robuuste methoden die in staat zijn om snel verschillende klassen gevaarlijke chemische stoffen in voedsel in het veld te detecteren en te identificeren25,26. Flexibele SERS-substraten bieden unieke voordelen in praktische toepassingen, met name op het gebied van voedselveiligheid. Dit artikel introduceert een methode voor het bereiden van een flexibel SERS-substraat door gesynthetiseerde glucose-gecoate zilveren nanodeeltjes (AgNP's) te binden aan een PDMS-substraat (Figuur 1). De aanwezigheid van glucose beschermt de AgNP's en vermindert de zilveroxidatie in de lucht. Het substraat vertoont uitstekende detectieprestaties, in staat om Rhodamine 6G (R6G) zo laag als 10-10 M en pesticide Thiram zo laag als 10-8 M te detecteren, met een goede uniformiteit. Bovendien kan het flexibele substraat worden gebruikt voor detectie door middel van verlijming en bemonstering, met tal van mogelijke toepassingsscenario's.

<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

Dit artikel presenteert een fabricagemethode voor een flexibel substraat dat is ontworpen voor Surface-Enhanced Raman Scattering (SERS). Zilveren nanodeeltjes (AgNP's) werden gesynthetiseerd door middel van een complexatiereactie met zilvernitraat (AgNO3) en ammoniak, gevolgd door reductie met behulp van glucose. De resulterende AgNP's vertoonden een uniforme grootteverdeling variërend van 20 nm tot 50 nm. Vervolgens werd 3-aminopropyltriethoxysilaan (APTES) gebruikt om een PDMS-substraat te modificeren dat aan het oppervlak was behandeld met zuurstofplasma. Dit proces vergemakkelijkte de zelfassemblage van AgNP's op het substraat. Een systematische evaluatie van de impact van verschillende experimentele omstandigheden op de prestaties van het substraat leidde tot de ontwikkeling van een SERS-substraat met uitstekende prestaties en een Enhanced Factor (EF). Door gebruik te maken van dit substraat werden indrukwekkende detectielimieten van 10-10 M voor R6G (Rhodamine 6G) en 10-8 M voor Thiram bereikt. Het substraat werd met succes gebruikt voor het detecteren van residuen van bestrijdingsmiddelen op appels, wat zeer bevredigende resultaten opleverde. Het flexibele SERS-substraat heeft een groot potentieel voor toepassingen in de echte wereld, waaronder detectie in complexe scenario's.

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.

Auteur in de schijnwerpers: Ontwikkeling en toepassing van flexibele SER-substraten met behulp van gesynthetiseerde AgNP's 

Fabricage van op polydimethylsiloxaan (PDMS) gebaseerd flexibel oppervlakteversterkt Raman-verstrooiingssubstraat (SERS) voor ultragevoelige detectie

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 deze studie werd een flexibel SERS-substraat ontwikkeld dat bestaat uit synthetische AgNP's gewikkeld in glucose en zelf geassembleerd op PDMS met behulp van APTES, waardoor uitstekende detectieprestaties worden behaald voor praktische toepassingen voor de detectie van pesticiden. De detectielimieten voor R6G en Thiram werden beide bereikt op respectievelijk 10-10 M en 10-8 M, met een Enhancement Factor (EF) van 1 x 10 5. Bovendien vertoonde de ondergrond uniformiteit.
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Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

Dit protocol beschrijft een fabricagemethode voor een flexibel substraat voor oppervlakteversterkte Raman-verstrooiing. Deze methode is gebruikt bij de succesvolle detectie van lage concentraties R6G en Thiram.

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

Dit protocol beschrijft het voorbereiden van flexibele SER-substraten en het toepassen ervan op daadwerkelijke detectiescenario's. Het flexibele SERS-substraat dat door dit protocol wordt aangeboden, is milieuvriendelijk en behaalt goede detectieprestaties. De zilveren nanodeeltjes kunnen gemakkelijk worden gesynthetiseerd door eenvoudige vaten, en vereisen geen ingewikkelde experimentele omstandigheden en omgeving.In ons laboratorium zijn we van plan ons te concentreren op het onderzoeken van de zilveren nanodeeltjes die worden gesynthetiseerd via het vat dat in deze studie wordt gebruikt. We zullen methoden onderzoeken om hun SER-detectiemogelijkheden te verbeteren en hun unieke eigenschappen en kenmerken te benutten om beter presterende SER-detectiesubstraten te ontwerpen.

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.

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.