Name: Forfatter Spotlight: Utvikling og anvendelse av SERS fleksible substrater ved bruk av syntetiserte AgNP-er
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 støttes av National Natural Science Foundation of China (Grant nr. 61974004 og 61931018), samt National Key R &D Program of China (Grant No. 2021YFB3200100). Studien anerkjenner elektronmikroskopilaboratoriet ved Peking University for å gi tilgang til elektronmikroskoper. I tillegg strekker forskningen seg takket være Ying Cui og School of Earth and Space Science ved Peking University for deres hjelp i Raman-målinger.

1. Syntese av nanopartikler
<ol><li>Fremstilling av sølvnitratoppløsning<ol><li>Bruk en presisjonsvekt til å måle 0,0017 g sølvnitrat av AR-kvalitet (AgNO3, se Materialtabell) og tilsett det til 10 ml avionisert (DI) vann. Rør blandingen for å lage en 10-3 mol / L AgNO3 løsning.</li>
	</ol></li>
	<li>Fremstilling av sølv-ammoniakkkomplekset<ol><li>Ta 1 ml ammoniakkvann av AR-kvalitet (NH3. H2O, se Materialfortegnel...

Fremstilling av fleksibelt substrat for SERS-deteksjon av R6G og Thiram

<ol>
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I denne studien ble et fleksibelt SERS-substrat introdusert, som bandt AgNPs til PDMS gjennom kjemisk modifikasjon og oppnådde utmerket ytelse. Under partikkelsyntese, spesielt i sølvammoniakkkomplekssyntesen (trinn 1.2), spiller fargen på løsningen en avgjørende rolle. Tilsetning av for mye ammoniakkvann dråpevis kan påvirke AgNPs syntesekvalitet negativt, noe som potensielt fører til mislykkede deteksjonsresultater. Det bør tas hensyn til substratmodifisering (trinn 2.2) under synteseprosessen; ellers kan AgNP...

Overflateforbedret Raman-spredning (SERS), som en type Raman-spredning, tilbyr fordelene med høy følsomhet og milde deteksjonsforhold, og kan til og med oppnå enkeltmolekyldeteksjon 1,2,3,4. Metall nanostrukturer, som gull og sølv, brukes vanligvis som SERS-substrater for å muliggjøre stoffdeteksjon 5,6. Elektromagnetisk koblingsforbedring på nanostrukturerte overflater spiller en betydelig rolle i SERS-applikasjoner. Metalliske nanostrukturer med varierende størrelser, former, interpartikkelavstander og komposisjoner kan aggregere for å skape mange "hotspots" som genererer intense elektromagnetiske felt på grunn av lokaliserte overflateplasmonresonanser 7,8. Mange studier har utviklet metall nanopartikler med forskjellige morfologier som SERS-substrater, og demonstrerer deres effektivitet i å oppnå SERS-forbedring 9,10.
Fleksible SERS-substrater finner brede applikasjoner, med nanostrukturer som er i stand til å produsere SERS-effekter avsatt på fleksible underlag for å lette direkte deteksjon på buede overflater. Fleksible SERS-substrater brukes til å oppdage og samle analytter på uregelmessige, ikke-plane eller buede overflater. Vanlige fleksible SERS-substrater inkluderer fibre, polymerfilmer og grafenoksydfilmer11,12,13,14. Blant dem er polydimetylsiloksan (PDMS) et av de mest brukte polymermaterialene og gir fordeler som høy gjennomsiktighet, høy strekkfasthet, kjemisk stabilitet, ikke-toksisitet og vedheft15,16,17. PDMS har et lavt Raman-tverrsnitt, noe som gjør innvirkningen på Raman-signalet ubetydelig18. Siden PDMS-prepolymeren er i flytende form, kan den herdes av varme eller lys, noe som gir en høy grad av kontrollerbarhet og bekvemmelighet. PDMS-baserte SERS-substrater er relativt vanlige fleksible SERS-substrater, som har blitt brukt i tidligere studier for å legge inn forskjellige metallnanopartikler for å oppdage forskjellige biokjemiske stoffer med eksemplarisk ytelse19,20.
Ved utarbeidelse av SERS-substrater er fabrikasjon av nanogapstrukturer avgjørende. Fysisk avsetningsteknologi gir fordeler som høy skalerbarhet, ensartethet og reproduserbarhet, men krever vanligvis gode vakuumforhold og spesialutstyr, noe som begrenser de praktiske bruksområdene21. I tillegg er fabrikasjon av nanostrukturer på få-nanometerskala fortsatt utfordrende med konvensjonelle avsetningsteknikker22. Følgelig kan nanopartikler syntetisert gjennom kjemiske metoder adsorberes på fleksible gjennomsiktige filmer gjennom ulike interaksjoner, noe som letter selvmontering av metalliske strukturer på nanoskala. For å sikre vellykket adsorpsjon kan interaksjoner justeres ved fysisk eller kjemisk modifisering av filmoverflaten for å endre overflatehydrofiliteten23. Sølv nanopartikler, sammenlignet med gull nanopartikler, viser bedre SERS-ytelse, men deres ustabilitet, spesielt deres følsomhet for oksidasjon i luft, resulterer i en rask reduksjon i SERS Enhancement Factor (EF), som påvirker substratets ytelse24. Derfor er det viktig å utvikle en stabil partikkelmetode.
Tilstedeværelsen av rester av plantevernmidler har fått betydelig oppmerksomhet, noe som skaper et presserende behov for robuste metoder som raskt kan oppdage og identifisere ulike klasser av farlige kjemikalier i mat i felt25,26. Fleksible SERS-substrater gir unike fordeler i praktiske applikasjoner, spesielt innen matsikkerhet. Denne artikkelen introduserer en metode for fremstilling av et fleksibelt SERS-substrat ved å binde syntetiserte glukosebelagte sølvnanopartikler (AgNPs) på et PDMS-substrat (figur 1). Tilstedeværelsen av glukose beskytter AgNPs, og reduserer sølvoksidasjon i luften. Substratet demonstrerer utmerket deteksjonsytelse, i stand til å oppdage Rhodamine 6G (R6G) så lavt som 10-10 M og plantevernmiddel Thiram så lavt som 10-8 M, med god ensartethet. Videre kan det fleksible substratet brukes til deteksjon gjennom liming og prøvetaking, med mange potensielle applikasjonsscenarier.

<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

Denne artikkelen presenterer en fabrikasjonsmetode for et fleksibelt substrat designet for overflateforbedret Raman-spredning (SERS). Sølv nanopartikler (AgNPs) ble syntetisert gjennom en komplekseringsreaksjon som involverer sølvnitrat (AgNO3) og ammoniakk, etterfulgt av reduksjon ved bruk av glukose. De resulterende AgNPene viste en jevn størrelsesfordeling fra 20 nm til 50 nm. Deretter ble 3-aminopropyltrietoksysilan (APTES) brukt til å modifisere et PDMS-substrat som hadde blitt overflatebehandlet med oksygenplasma. Denne prosessen lettet selvmontering av AgNPs på underlaget. En systematisk evaluering av virkningen av ulike eksperimentelle forhold på substratytelsen førte til utviklingen av et SERS-substrat med utmerket ytelse og en forbedret faktor (EF). Ved hjelp av dette substratet ble imponerende deteksjonsgrenser på 10-10 M for R6G (Rhodamine 6G) og 10-8 M for Thiram oppnådd. Substratet ble vellykket brukt til å oppdage plantevernmiddelrester på epler, noe som ga svært tilfredsstillende resultater. Det fleksible SERS-substratet demonstrerer stort potensial for virkelige applikasjoner, inkludert deteksjon i komplekse 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.

Forfatter Spotlight: Utvikling og anvendelse av SERS fleksible substrater ved bruk av syntetiserte AgNP-er 

Fabrikasjon av polydimetylsiloksan (PDMS)-basert fleksibelt overflateforbedret Raman-spredning (SERS) substrat for ultrasensitiv deteksjon

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 denne studien ble det utviklet et fleksibelt SERS-substrat sammensatt av syntetiske AgNP-er innpakket i glukose og selvmontert på PDMS ved hjelp av APTES, og oppnådde utmerket deteksjonsytelse for praktiske plantevernmiddeldeteksjonsapplikasjoner. Deteksjonsgrensene for R6G og Thiram ble begge nådd ved henholdsvis 10-10 M og 10-8 M, med en forbedringsfaktor (EF) på 1 x 10 5. Videre viste substratet ensartethet.
AgNPene innpakket i glukose ble syntetisert ...

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

Denne protokollen beskriver en fabrikasjonsmetode for et fleksibelt substrat for overflateforbedret Raman-spredning. Denne metoden har blitt brukt i vellykket påvisning av lave konsentrasjoner av R6G og Thiram.

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

Denne protokollen beskriver klargjøring av fleksible SERS-substrater, og bruker dem på faktiske deteksjonsscenarier. SERS fleksible substrat som tilbys av denne protokollen er miljøvennlig og oppnår god deteksjonsytelse. Sølvnanopartiklene kan syntetiseres enkelt ved enkle fartøy, og krever ikke kompliserte eksperimentelle forhold og miljø.I vårt laboratorium planlegger vi å fokusere på å undersøke sølvnanopartikler syntetisert gjennom fartøyet som brukes i denne studien. Vi vil utforske metoder for å forbedre deres SERS-deteksjonsfunksjoner, og utnytte deres unike egenskaper og egenskaper for å designe SERS-deteksjonssubstrater med bedre ytelse.

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.