Name: Forfatter Spotlight: Udvikling og anvendelse af SERS fleksible substrater ved hjælp af syntetiserede 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 er støttet af National Natural Science Foundation of China (Grant No. 61974004 and 61931018) samt National Key R&D Program of China (Grant No. 2021YFB3200100). Undersøgelsen anerkender Electron Microscopy Laboratory of Peking University for at give adgang til elektronmikroskoper. Derudover strækker forskningen sig takket være Ying Cui og School of Earth and Space Science ved Peking University for deres hjælp til Raman-målinger.

1. Syntese af nanopartikler
<ol><li>Fremstilling af sølvnitratopløsning<ol><li>Ved hjælp af en præcisionsvægt måles 0,0017 g sølvnitrat af AR-kvalitet (AgNO3, se materialetabellen) og tilsættes til 10 ml deioniseret (DI) vand. Blandingen omrøres til en 10-3 mol/lAgNO3-opløsning.</li>
	</ol></li>
	<li>Fremstilling af sølv-ammoniakkomplekset<ol><li>Tag 1 ml ammoniakvand af AR-kvalitet (NH3. H2O, se materialetabelle...

Fremstilling af fleksibelt substrat til SERS-detektion af R6G og Thiram

<ol>
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I denne undersøgelse blev der introduceret et fleksibelt SERS-substrat, som bandt AgNP'er til PDMS gennem kemisk modifikation og opnåede fremragende ydeevne. Under partikelsyntese, specifikt i sølvammoniakkomplekssyntesen (trin 1.2), spiller opløsningens farve en afgørende rolle. Tilsætning af for meget ammoniakvand dråbevis kan påvirke AgNPs syntesekvalitet negativt, hvilket potentielt kan føre til mislykkede detektionsresultater. Der skal tages hensyn til substratmodifikation (trin 2.2) under synteseprocessen;...

Surface-Enhanced Raman Scattering (SERS), som en type Raman-spredning, giver fordelene ved høj følsomhed og blide detektionsforhold og kan endda opnå enkeltmolekyledetektion 1,2,3,4. Metal nanostrukturer, såsom guld og sølv, anvendes typisk som SERS-substrater for at muliggøre stofdetektion 5,6. Forbedring af elektromagnetisk kobling på nanostrukturerede overflader spiller en væsentlig rolle i SERS-applikationer. Metalliske nanostrukturer med varierende størrelser, former, interpartikelafstande og sammensætninger kan aggregeres for at skabe adskillige "hotspots", der genererer intense elektromagnetiske felter på grund af lokaliserede overfladeplasmonresonanser 7,8. Mange undersøgelser har udviklet metal nanopartikler med forskellige morfologier som SERS substrater, hvilket viser deres effektivitet i at opnå SERS forbedring 9,10.
Fleksible SERS-substrater finder brede anvendelsesmuligheder med nanostrukturer, der er i stand til at producere SERS-effekter deponeret på fleksible substrater for at lette direkte detektion på buede overflader. Fleksible SERS-substrater anvendes til at detektere og indsamle analysander på uregelmæssige, ikke-plane eller buede overflader. Almindelige fleksible SERS-substrater inkluderer fibre, polymerfilm og grafenoxidfilm11,12,13,14. Blandt dem er polydimethylsiloxan (PDMS) et af de mest anvendte polymermaterialer og tilbyder fordele som høj gennemsigtighed, høj trækstyrke, kemisk stabilitet, ikke-toksicitet og vedhæftning15,16,17. PDMS har et lavt Raman-tværsnit, hvilket gør dets indvirkning på Raman-signalet ubetydelig18. Da PDMS-præpolymeren er i flydende form, kan den hærdes af varme eller lys, hvilket giver en høj grad af styrbarhed og bekvemmelighed. PDMS-baserede SERS-substrater er relativt almindelige fleksible SERS-substrater, der er blevet brugt i tidligere undersøgelser til at indlejre forskellige metalnanopartikler til påvisning af forskellige biokemiske stoffer med eksemplarisk ydeevne19,20.
Ved fremstillingen af SERS-substrater er fremstillingen af nanogapstrukturer afgørende. Fysisk deponeringsteknologi giver fordele som høj skalerbarhed, ensartethed og reproducerbarhed, men kræver typisk gode vakuumforhold og specialudstyr, hvilket begrænser dets praktiske anvendelser21. Derudover er fremstilling af nanostrukturer på få nanometerskalaer fortsat udfordrende med konventionelle deponeringsteknikker22. Derfor kan nanopartikler syntetiseret gennem kemiske metoder adsorberes på fleksible gennemsigtige film gennem forskellige interaktioner, hvilket letter selvmontering af metalliske strukturer på nanoskala. For at sikre vellykket adsorption kan interaktioner justeres ved fysisk eller kemisk ændring af filmoverfladen for at ændre dens overfladehydrofilicitet23. Sølvnanopartikler, sammenlignet med guldnanopartikler, udviser bedre SERS-ydeevne, men deres ustabilitet, især deres modtagelighed for oxidation i luft, resulterer i et hurtigt fald i SERS Enhancement Factor (EF), hvilket påvirker substratets ydeevne24. Derfor er det vigtigt at udvikle en stabil partikelmetode.
Tilstedeværelsen af pesticidrester har fået betydelig opmærksomhed, hvilket skaber et presserende behov for robuste metoder, der hurtigt kan detektere og identificere forskellige klasser af farlige kemikalier i fødevarer i marken25,26. Fleksible SERS-substrater giver unikke fordele i praktiske anvendelser, især inden for fødevaresikkerhed. Denne artikel introducerer en metode til fremstilling af et fleksibelt SERS-substrat ved at binde syntetiserede glucosebelagte sølvnanopartikler (AgNP'er) på et PDMS-substrat (figur 1). Tilstedeværelsen af glukose beskytter AgNP'erne og mindsker sølvoxidation i luften. Substratet demonstrerer fremragende detektionsevne, der er i stand til at detektere Rhodamin 6G (R6G) så lavt som 10-10 M og pesticidthiram så lavt som 10-8 M med god ensartethed. Desuden kan det fleksible substrat anvendes til detektion gennem binding og prøveudtagning med mange potentielle anvendelsesscenarier.

<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 artikel præsenterer en fremstillingsmetode til et fleksibelt substrat designet til overfladeforbedret Ramanspredning (SERS). Sølvnanopartikler (AgNP'er) blev syntetiseret gennem en kompleksationsreaktion, der involverede sølvnitrat (AgNO3) og ammoniak, efterfulgt af reduktion ved anvendelse af glucose. De resulterende AgNP'er udviste en ensartet størrelsesfordeling fra 20 nm til 50 nm. Efterfølgende blev 3-aminopropyltriethoxysilan (APTES) anvendt til at modificere et PDMS-substrat, der var blevet overfladebehandlet med oxygenplasma. Denne proces lettede selvmontering af AgNP'er på substratet. En systematisk evaluering af virkningen af forskellige eksperimentelle betingelser på substratets ydeevne førte til udviklingen af et SERS-substrat med fremragende ydeevne og en forbedret faktor (EF). Ved hjælp af dette substrat blev der opnået imponerende detektionsgrænser på 10-10 M for R6G (Rhodamin 6G) og 10-8 M for Thiram. Substratet blev med succes anvendt til påvisning af pesticidrester på æbler, hvilket gav meget tilfredsstillende resultater. Det fleksible SERS-substrat demonstrerer et stort potentiale for applikationer i den virkelige verden, herunder detektion 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: Udvikling og anvendelse af SERS fleksible substrater ved hjælp af syntetiserede AgNP'er 

Fremstilling af polydimethylsiloxan (PDMS)-baseret fleksibelt overfladeforstærket Ramanspredningssubstrat (SERS) til ultrafølsom 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 denne undersøgelse blev der udviklet et fleksibelt SERS-substrat sammensat af syntetiske AgNP'er pakket ind i glukose og selvmonteret på PDMS ved hjælp af APTES, hvilket opnåede fremragende detektionsydelse til praktiske pesticiddetekteringsapplikationer. Detektionsgrænserne for R6G og Thiram blev begge nået ved henholdsvis 10-10 M og 10-8 M med en forbedringsfaktor (EF) på 1 x 10 5. Desuden viste substratet ensartethed.
AgNP'erne indpakket i glukose b...

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

Denne protokol beskriver en fabrikationsmetode for et fleksibelt substrat til overfladeforstærket Raman-spredning. Denne metode er blevet anvendt til vellykket påvisning af lave koncentrationer af R6G og Thiram.

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

Denne protokol beskriver forberedelse af SERS fleksible substrater og anvender dem på faktiske detektionsscenarier. Det fleksible SERS-substrat, der tilbydes af denne protokol, er miljøvenligt og opnår god detektionsydelse. Sølvnanopartiklerne kan let syntetiseres af enkle beholdere og kræver ikke komplicerede eksperimentelle forhold og miljø.I vores laboratorium planlægger vi at fokusere på at undersøge sølvnanopartiklerne syntetiseret gennem beholderen, der anvendes i denne undersøgelse. Vi vil undersøge metoder til at forbedre deres SERS-detektionsfunktioner og udnytte deres unikke egenskaber og egenskaber til at designe SERS-detektionssubstrater med bedre ydeevne.

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.