Name: Författare Spotlight: Utveckling och tillämpning av flexibla SERS-substrat med hjälp av syntetiserade 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

Forskningen stöds av National Natural Science Foundation of China (Grant No. 61974004 and 61931018), samt National Key R&D Program of China (Grant No. 2021YFB3200100). Studien är ett erkännande av elektronmikroskopilaboratoriet vid Pekings universitet för att ha gett tillgång till elektronmikroskop. Dessutom är forskningen tack vare Ying Cui och School of Earth and Space Science vid Pekings universitet för deras hjälp med Raman-mätningar.

1. Syntes av nanopartiklar
<ol><li>Beredning av silvernitratlösning<ol><li>Använd en precisionsvåg, mät 0,0017 g silvernitrat av AR-kvalitet (AgNO3, se materialtabell) och tillsätt det till 10 ml avjoniserat (DI) vatten. Rör om blandningen för att skapa en 10-3 mol/L AgNO3-lösning .</li>
	</ol></li>
	<li>Beredning av silver-ammoniakkomplexet<ol><li>Ta 1 ml ammoniakvatten av AR-kvalitet (NH3. H2O, se Materialförteck...

Tillverkning av flexibelt substrat för SERS-detektion av R6G och Thiram

<ol>
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I denna studie introducerades ett flexibelt SERS-substrat, som band AgNP till PDMS genom kemisk modifiering och uppnådde utmärkt prestanda. Under partikelsyntesen, särskilt i silverammoniakkomplexsyntesen (steg 1.2), spelar lösningens färg en avgörande roll. Att tillsätta för mycket ammoniakvatten droppvis kan påverka AgNPs synteskvalitet negativt, vilket kan leda till misslyckade detektionsresultat. Uppmärksamhet bör ägnas åt substratmodifiering (steg 2.2) under syntesprocessen; annars kan det hända att Ag...

Surface-Enhanced Raman Scattering (SERS), som en typ av Raman-spridning, erbjuder fördelarna med hög känslighet och skonsamma detektionsförhållanden, och kan till och med uppnå detektering av enstaka molekyler 1,2,3,4. Metallnanostrukturer, såsom guld och silver, används vanligtvis som SERS-substrat för att möjliggöra substansdetektion 5,6. Förbättring av elektromagnetisk koppling på nanostrukturerade ytor spelar en viktig roll i SERS-tillämpningar. Metalliska nanostrukturer med varierande storlek, form, interpartikelavstånd och sammansättningar kan aggregera för att skapa många "hotspots" som genererar intensiva elektromagnetiska fält på grund av lokaliserade ytplasmonresonanser 7,8. Många studier har utvecklat metallnanopartiklar med olika morfologier som SERS-substrat, vilket visar deras effektivitet när det gäller att uppnå SERS-förbättring 9,10.
Flexibla SERS-substrat har breda tillämpningar, med nanostrukturer som kan producera SERS-effekter som deponeras på flexibla substrat för att underlätta direkt detektion på krökta ytor. Flexibla SERS-substrat används för att detektera och samla in analyter på oregelbundna, icke-plana eller krökta ytor. Vanliga flexibla SERS-substrat inkluderar fibrer, polymerfilmer och grafenoxidfilmer11,12,13,14. Bland dem är polydimetylsiloxan (PDMS) ett av de mest använda polymermaterialen och erbjuder fördelar som hög transparens, hög draghållfasthet, kemisk stabilitet, giftfrihet och vidhäftning15,16,17. PDMS har ett lågt Raman-tvärsnitt, vilket gör dess inverkan på Raman-signalen försumbar18. Eftersom PDMS-prepolymeren är i flytande form kan den härdas med värme eller ljus, vilket ger en hög grad av kontrollerbarhet och bekvämlighet. PDMS-baserade SERS-substrat är relativt vanliga flexibla SERS-substrat, som har använts i tidigare studier för att bädda in olika metallnanopartiklar för att detektera olika biokemiska substanser med exemplarisk prestanda19,20.
Vid framställning av SERS-substrat är tillverkningen av nanogapstrukturer avgörande. Teknik för fysisk deponering erbjuder fördelar som hög skalbarhet, enhetlighet och reproducerbarhet, men kräver vanligtvis goda vakuumförhållanden och specialutrustning, vilket begränsar desspraktiska tillämpningar. Dessutom är det fortfarande en utmaning att tillverka nanostrukturer på några nanometernivåer med konventionella deponeringstekniker22. Följaktligen kan nanopartiklar som syntetiseras genom kemiska metoder adsorberas på flexibla transparenta filmer genom olika interaktioner, vilket underlättar självorganisering av metallstrukturer på nanoskala. För att säkerställa framgångsrik adsorption kan interaktioner justeras genom att fysiskt eller kemiskt modifiera filmytan för att ändra dess ythydrofilicitet23. Silvernanopartiklar, jämfört med guldnanopartiklar, uppvisar bättre SERS-prestanda, men deras instabilitet, särskilt deras känslighet för oxidation i luft, resulterar i en snabb minskning av SERS Enhancement Factor (EF), vilket påverkar substratprestandan24. Därför är det viktigt att utveckla en stabil partikelmetod.
Förekomsten av bekämpningsmedelsrester har fått stor uppmärksamhet, vilket skapar ett stort behov av robusta metoder som snabbt kan upptäcka och identifiera olika klasser av farliga kemikalier i livsmedel på fältet25,26. Flexibla SERS-substrat erbjuder unika fördelar i praktiska tillämpningar, särskilt när det gäller livsmedelssäkerhet. Denna artikel introducerar en metod för att framställa ett flexibelt SERS-substrat genom att binda syntetiserade glukosbelagda silvernanopartiklar (AgNP) på ett PDMS-substrat (figur 1). Närvaron av glukos skyddar AgNPs, vilket minskar silveroxidation i luften. Substratet uppvisar utmärkt detektionsprestanda och kan detektera Rhodamine 6G (R6G) så lågt som 10-10 M och bekämpningsmedel Thiram så lågt som 10-8 M, med god enhetlighet. Dessutom kan det flexibla substratet användas för detektering genom bindning och provtagning, med många potentiella applikationsscenarier.

<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

Den här artikeln presenterar en tillverkningsmetod för ett flexibelt substrat designat för Surface-Enhanced Raman Scattering (SERS). Silvernanopartiklar (AgNPs) syntetiserades genom en komplexbildningsreaktion som involverade silvernitrat (AgNO3) och ammoniak, följt av reduktion med hjälp av glukos. De resulterande AgNP uppvisade en enhetlig storleksfördelning som sträckte sig från 20 nm till 50 nm. Därefter användes 3-aminopropyltrietoxisilan (APTES) för att modifiera ett PDMS-substrat som hade ytbehandlats med syreplasma. Denna process underlättade självorganiseringen av AgNP på substratet. En systematisk utvärdering av effekten av olika experimentella förhållanden på substratprestanda ledde till utvecklingen av ett SERS-substrat med utmärkt prestanda och en Enhanced Factor (EF). Med hjälp av detta substrat uppnåddes imponerande detektionsgränser på 10-10 M för R6G (Rhodamine 6G) och 10-8 M för Thiram. Substratet användes framgångsrikt för att detektera rester av bekämpningsmedel på äpplen, vilket gav mycket tillfredsställande resultat. Det flexibla SERS-substratet visar stor potential för verkliga tillämpningar, inklusive detektering i komplexa scenarier.

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.

Författare Spotlight: Utveckling och tillämpning av flexibla SERS-substrat med hjälp av syntetiserade AgNPs 

Tillverkning av polydimetylsiloxan (PDMS)-baserat flexibelt ytförstärkt Raman-spridningssubstrat (SERS) för ultrakänslig 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.

I denna studie utvecklades ett flexibelt SERS-substrat bestående av syntetiska AgNP insvepta i glukos och självorganiserat på PDMS med hjälp av APTES, vilket uppnådde utmärkt detektionsprestanda för praktiska bekämpningsmedelsdetektionsapplikationer. Detektionsgränserna för R6G och tiram uppnåddes båda vid 10-10 M respektive 10-8 M, med en förstärkningsfaktor (EF) på 1 x 10 5. Dessutom uppvisade substratet enhetlighet.
AgNP insvepta i glukos synt...

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

Detta protokoll beskriver en tillverkningsmetod för ett flexibelt substrat för ytförstärkt Raman-spridning. Denna metod har använts för framgångsrik detektion av låga koncentrationer av R6G och Thiram.

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

Detta protokoll beskriver förberedelse av flexibla SERS-substrat och tillämpar dem på faktiska detektionsscenarier. Det flexibla SERS-substratet som erbjuds av detta protokoll är miljövänligt och uppnår god detektionsprestanda. Silvernanopartiklarna kan enkelt syntetiseras av enkla kärl och kräver inte komplicerade experimentella förhållanden och miljö.I vårt laboratorium planerar vi att fokusera på att undersöka de silvernanopartiklar som syntetiseras genom kärlet som används i denna studie. Vi kommer att utforska metoder för att förbättra deras SERS-detektionsförmåga och utnyttja deras unika egenskaper och egenskaper för att designa bättre presterande SERS-detektionssubstrat.

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.