Name: Yazar Spotlight: Sentezlenmiş AgNP'ler Kullanılarak SERS Esnek Alt Tabakaların Geliştirilmesi ve Uygulanması
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

Araştırma, Çin Ulusal Doğa Bilimleri Vakfı (Hibe No. 61974004 ve 61931018) ve Çin Ulusal Anahtar Ar-Ge Programı (Hibe No. 2021YFB3200100) tarafından desteklenmektedir. Çalışma, elektron mikroskoplarına erişim sağladığı için Pekin Üniversitesi Elektron Mikroskobu Laboratuvarı'nı kabul ediyor. Ek olarak, araştırma, Raman ölçümlerindeki yardımları için Ying Cui'ye ve Pekin Üniversitesi Dünya ve Uzay Bilimleri Okulu'na teşekkür ediyor.

1. Nanopartiküllerin sentezi
<ol><li>Gümüş nitrat çözeltisinin hazırlanması<ol><li>Hassas bir tartım terazisi kullanarak 0,0017 g AR sınıfı gümüş nitrat ölçün (AgNO3, Malzeme Tablosuna bakın) ve 10 mL deiyonize (DI) suya ekleyin. 10-3 mol/LAgNO3 çözeltisi oluşturmak için karışımı karıştırın.</li>
	</ol></li>
	<li>Gümüş-amonyak kompleksinin hazırlanması<ol><li>1 mL AR sınıfı amonyak suyu (NH3. H2</su...

R6G ve Thiram'ın SERS Tespiti için Esnek Substrat İmalatı

<ol>
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Bu çalışmada, AgNP'leri kimyasal modifikasyon yoluyla PDMS'ye bağlayan ve mükemmel performans sağlayan esnek bir SERS substratı tanıtıldı. Partikül sentezi sırasında, özellikle gümüş amonyak kompleksi sentezinde (adım 1.2), çözeltinin rengi çok önemli bir rol oynar. Damla damla çok fazla amonyak suyu eklemek, AgNP'lerin sentez kalitesini olumsuz yönde etkileyebilir ve potansiyel olarak başarısız tespit sonuçlarına yol açabilir. Sentez işlemi sırasında substrat modifikasyonuna (adım 2.2) ...

Yüzeyde Geliştirilmiş Raman Saçılımı (SERS), bir Raman saçılımı türü olarak, yüksek hassasiyet ve hassas algılama koşullarının avantajlarını sunar ve hatta tek molekül algılaması 1,2,3,4 elde edebilir. Altın ve gümüş gibi metal nanoyapılar, madde tespitini sağlamak için tipik olarak SERS substratları olarak kullanılır 5,6. Nanoyapılı yüzeylerde elektromanyetik kuplaj geliştirme, SERS uygulamalarında önemli bir rol oynar. Farklı boyutlara, şekillere, parçacıklar arası mesafelere ve bileşimlere sahip metalik nanoyapılar, lokalize yüzey plazmon rezonansları 7,8 nedeniyle yoğun elektromanyetik alanlar üreten çok sayıda "sıcak nokta" oluşturmak için bir araya gelebilir. Birçok çalışma, SERS substratları olarak farklı morfolojilere sahip metal nanopartiküller geliştirmiş ve bunların SERS geliştirmesineulaşmadaki etkinliklerini göstermiştir 9,10.
Esnek SERS alt tabakaları, kavisli yüzeylerde doğrudan algılamayı kolaylaştırmak için esnek alt tabakalar üzerinde biriken SERS etkileri üretebilen nanoyapılar ile geniş uygulamalar bulur. Esnek SERS substratları, düzensiz, düzlemsel olmayan veya kavisli yüzeylerde analitleri tespit etmek ve toplamak için kullanılır. Yaygın esnek SERS substratları arasında lifler, polimer filmler ve grafen oksit filmler11,12,13,14 bulunur. Bunlar arasında polidimetilsiloksan (PDMS) en yaygın kullanılan polimer malzemelerden biridir ve yüksek şeffaflık, yüksek çekme mukavemeti, kimyasal stabilite, toksik olmama ve yapışma gibi avantajlar sunar15,16,17. PDMS'nin düşük bir Raman kesiti vardır, bu da Raman sinyali üzerindeki etkisini ihmal edilebilirhale getirir 18. PDMS prepolimeri sıvı formda olduğundan, ısı veya ışıkla kürlenebilir, bu da yüksek derecede kontrol edilebilirlik ve rahatlık sağlar. PDMS bazlı SERS substratları, önceki çalışmalarda örnek performansa sahip farklı biyokimyasal maddeleri tespit etmek için çeşitli metal nanopartikülleri gömmek için kullanılmış olan nispeten yaygın esnek SERS substratlarıdır19,20.
SERS substratlarının hazırlanmasında, nanogap yapılarının imalatı çok önemlidir. Fiziksel biriktirme teknolojisi, yüksek ölçeklenebilirlik, tekdüzelik ve tekrarlanabilirlik gibi avantajlar sunar, ancak tipik olarak iyi vakum koşulları ve özel ekipman gerektirir ve bu da pratik uygulamalarını sınırlar21. Ek olarak, birkaç nanometre ölçeğinde nanoyapılar üretmek, geleneksel biriktirme teknikleriyle zor olmaya devam etmektedir22. Sonuç olarak, kimyasal yöntemlerle sentezlenen nanopartiküller, çeşitli etkileşimler yoluyla esnek şeffaf filmler üzerine adsorbe edilebilir ve bu da metalik yapıların nano ölçekte kendi kendine birleşmesini kolaylaştırır. Başarılı adsorpsiyonu sağlamak için, yüzey hidrofilikliğini değiştirmek için film yüzeyi fiziksel veya kimyasal olarak değiştirilerek etkileşimler ayarlanabilir23. Gümüş nanopartiküller, altın nanopartiküllere kıyasla daha iyi SERS performansı sergiler, ancak kararsızlıkları, özellikle havadaki oksidasyona duyarlılıkları, substrat performansını etkileyen SERS Geliştirme Faktöründe (EF) hızlı bir düşüşe neden olur24. Bu nedenle, kararlı bir parçacık yöntemi geliştirmek esastır.
Pestisit kalıntılarının varlığı büyük ilgi görmüştür ve tarlada gıdalardaki çeşitli tehlikeli kimyasal sınıflarını hızlı bir şekilde tespit edebilen ve tanımlayabilen sağlam yöntemlere acil bir ihtiyaç yaratmıştır25,26. Esnek SERS substratları, pratik uygulamalarda, özellikle gıda güvenliği alanında benzersiz avantajlar sunar. Bu makale, sentezlenmiş glikoz kaplı gümüş nanopartikülleri (AgNP'ler) bir PDMS substratına bağlayarak esnek bir SERS substratı hazırlamak için bir yöntem sunmaktadır (Şekil 1). Glikozun varlığı, AgNP'leri koruyarak havadaki gümüş oksidasyonunu azaltır. Substrat, Rhodamine 6G'yi (R6G) 10-10 M kadar düşük ve pestisit Thiram'ı 10-8 M kadar düşük ve iyi bir homojenlik ile tespit edebilen mükemmel algılama performansı gösterir. Ayrıca, esnek alt tabaka, çok sayıda potansiyel uygulama senaryosu ile yapıştırma ve numune alma yoluyla tespit için kullanılabilir.

<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

Bu makale, Yüzeyde Geliştirilmiş Raman Saçılımı (SERS) için tasarlanmış esnek bir alt tabaka için bir üretim yöntemi sunar. Gümüş nanopartiküller (AgNP'ler), gümüş nitrat (AgNO3) ve amonyak içeren bir kompleksleşme reaksiyonu yoluyla sentezlendi, ardından glikoz kullanılarak indirgendi. Ortaya çıkan AgNP'ler, 20 nm ila 50 nm arasında değişen tek tip bir boyut dağılımı sergiledi. Daha sonra, oksijen plazması ile yüzey muamelesi görmüş bir PDMS substratını modifiye etmek için 3-aminopropil trietoksisilan (APTES) kullanıldı. Bu işlem, AgNP'lerin alt tabakaya kendi kendine montajını kolaylaştırdı. Çeşitli deneysel koşulların substrat performansı üzerindeki etkisinin sistematik bir değerlendirmesi, mükemmel performansa ve Gelişmiş Faktöre (EF) sahip bir SERS substratının geliştirilmesine yol açtı. Bu substrat kullanılarak, R6G (Rhodamine 6G) için 10-10 M ve Thiram için 10-8 M'lik etkileyici tespit limitleri elde edildi. Substrat, elmalardaki pestisit kalıntılarını tespit etmek için başarıyla kullanıldı ve oldukça tatmin edici sonuçlar verdi. Esnek SERS alt tabakası, karmaşık senaryolarda algılama da dahil olmak üzere gerçek dünya uygulamaları için büyük bir potansiyel gösterir.

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.

Yazar Spotlight: Sentezlenmiş AgNP'ler Kullanılarak SERS Esnek Alt Tabakaların Geliştirilmesi ve Uygulanması 

Ultra Hassas Algılama için Polidimetilsiloksan (PDMS) Bazlı Esnek Yüzeyle Geliştirilmiş Raman Saçılımı (SERS) Alt Tabakasının İmalatı

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.

Bu çalışmada, glikoza sarılmış ve APTES kullanılarak PDMS üzerinde kendi kendine monte edilen sentetik AgNP'lerden oluşan esnek bir SERS substratı geliştirildi ve pratik pestisit tespit uygulamaları için mükemmel tespit performansı elde edildi. R6G ve Thiram için tespit sınırlarının her ikisine de sırasıyla 10-10 M ve 10-8 M'de ulaşıldı ve 1 x 10 5'lik bir Geliştirme Faktörü (EF) ile ulaşıldı. Ayrıca, substrat tekdüzelik gösterdi.
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Watch this Scientific Journal Video about Development and Application of SERS Flexible Substrates Using Synthesized AgNPs at JoVE.com

Bu protokol, yüzeyde geliştirilmiş Raman saçılımı için esnek bir alt tabaka için bir üretim yöntemini açıklar. Bu yöntem, düşük konsantrasyonlarda R6G ve Thiram'ın başarılı bir şekilde tespit edilmesinde kullanılmıştır.

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

Bu protokol, SERS esnek alt tabakalarının hazırlanmasını ve bunların gerçek algılama senaryolarına uygulanmasını açıklar. Bu protokol tarafından sunulan SERS esnek alt tabaka çevre dostudur ve iyi algılama performansı sağlar. Gümüş nanopartiküller basit kaplar tarafından kolayca sentezlenebilir ve karmaşık deney koşulları ve ortamı gerektirmez.Laboratuvarımızda, bu çalışmada kullanılan kap aracılığıyla sentezlenen gümüş nanopartiküllerin araştırılmasına odaklanmayı planlıyoruz. SERS algılama yeteneklerini geliştirme yöntemlerini keşfedeceğiz ve daha iyi performans gösteren SERS algılama alt tabakaları tasarlamak için benzersiz özelliklerinden ve özelliklerinden yararlanacağız.

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.

Mühendislik

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.