该研究得到了国家自然科学基金（批准号61974004和61931018）以及国家重点研发计划（批准号：2021YFB3200100）的支持。该研究感谢北京大学电子显微镜实验室提供电子显微镜。此外，这项研究还感谢崔莹和北京大学地球与空间科学学院在拉曼测量方面的帮助。

1. 纳米粒子的合成
<ol><li>硝酸银溶液的制备<ol><li>使用精密称量天平，测量 0.0017 g AR 级硝酸银（AgNO3，参见 材料表），并将其加入 10 mL 去离子 （DI） 水中。搅拌混合物以产生 10-3 mol/L AgNO3 溶液。</li>
	</ol></li>
	<li>银-氨络合物的制备<ol><li>取 1 mL AR 级氨水 （NH3.H2O，见 材料表）使用注射器，并在搅拌的同时逐滴加入硝酸银溶液中。当溶液变得透明时，停止逐滴添加。</li>
	</ol></li>
	<li>葡萄糖溶液的制备<ol><li>使用精密称量天平，测量 0.36 g AR 级葡萄糖粉（参见 材料表），并将其加入 10 mL 去离子水中。彻底搅拌混合物以产生 0.2 M 葡萄糖溶液。</li>
	</ol></li>
	<li>银纳米粒子（AgNPs）的合成<ol><li>使用移液枪以30分钟的间隔将30μL银氨复合物（在步骤1.2中制备）加入葡萄糖溶液（在步骤1.3中制备）。重复此过程 4-6 次，同时搅拌直到溶液变黄。</li>
	</ol></li>
</ol>2. 柔性基板的制备
<ol><li>PDMS衬底的制备<ol><li>为了合成PDMS底物，取约5g PDMS A溶液，并以1：10的比例加入B溶液（来自市售试剂盒，参见 材料表）。</li>
		<li>搅拌并充分混合 PDMS A 和 B 溶液。</li>
		<li>将混合的PDMS转移到方形培养皿中，然后在80°C烤箱中烘烤2小时。</li>
		<li>通过上述过程固化后，使用手术刀沿着培养皿的深色网格切割PDMS，形成尺寸约为1 cm x 1 cm的小PDMS立方体。</li>
	</ol></li>
	<li>表面改性<ol><li>对上述小PDMS片段进行等离子体处理。使用手持式等离子处理器（参见 材料表）并将其在PDMS表面上方约5-10厘米处来回移动，以进行表面等离子体处理。</li>
		<li>利用等离子体处理器对表面进行修饰，诱导在PDMS表面上形成羟基，使其亲水27。</li>
	</ol></li>
	<li>使用 APTES 进行修改<ol><li>制备10%APTES溶液（参见 材料表）。</li>
		<li>将步骤2.2中获得的表面改性PDMS浸入APTES溶液中，并静置10小时。这使得APTES能够与PDMS表面上的羟基结合。</li>
	</ol></li>
	<li>AgNP的自组装<ol><li>将步骤2.3中获得的PDMS底物浸入步骤1.4中合成的AgNPs溶液中10小时。这将AgNP自组装到PDMS衬底上，从而形成最终的柔性SERS检测衬底。</li>
	</ol></li>
</ol>

用于 R6G 和 Thiram 的 SERS 检测的柔性衬底的制备

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作者声明没有利益冲突。

本研究引入了一种柔性SERS底物，通过化学改性将AgNPs与PDMS键合，并取得了优异的性能。在颗粒合成过程中，特别是在银氨络合物合成（步骤1.2）中，溶液的颜色起着至关重要的作用。滴加过多的氨水会对AgNPs的合成质量产生不利影响，可能导致检测结果不成功。合成过程中应注意底物改性（步骤2.2）;否则，AgNP可能无法与PDMS正确结合，从而导致检测性能下降。
在实际制备中?...

表面增强拉曼散射（SERS）作为拉曼散射的一种，具有灵敏度高、检测条件温和等优点，甚至可以实现单分子检测1,2,3,4。金属纳米结构，如金和银，通常用作SERS基板，以实现物质检测5,6。纳米结构表面的电磁耦合增强在SERS应用中起着重要作用。具有不同尺寸、形状、粒子间距离和成分的金属纳米结构可以聚集起来产生许多“热点”，由于局部表面等离子体共振而产生强烈的电磁场 7,8。许多研究已经开发了具有不同形态的金属纳米颗粒作为SERS底物，证明了它们在实现SERS增强方面的有效性9,10。
柔性SERS衬底具有广泛的应用，其纳米结构能够产生SERS效应沉积在柔性衬底上，便于在曲面上直接检测。柔性SERS底物用于检测和收集不规则、非平面或曲面上的分析物。常见的柔性SERS基材包括纤维、聚合物薄膜和氧化石墨烯薄膜11,12,13,14。其中，聚二甲基硅氧烷（PDMS）是应用最广泛的高分子材料之一，具有透明度高、拉伸强度高、化学稳定性高、无毒、附着力等优点15,16,17。PDMS具有较低的拉曼截面，因此其对拉曼信号的影响可以忽略不计18。由于PDMS预聚物是液态的，因此可以通过热或光固化，从而提供了高度的可控性和便利性。基于PDMS的SERS衬底是相对常见的柔性SERS衬底，在以前的研究中已被用于嵌入各种金属纳米颗粒，用于检测具有示范性性能的不同生化物质19,20。
在SERS衬底的制备中，纳米间隙结构的制备至关重要。物理沉积技术具有高扩展性、均匀性和可重复性等优点，但通常需要良好的真空条件和专用设备，限制了其实际应用21。此外，使用传统的沉积技术在几纳米尺度上制造纳米结构仍然具有挑战性22。因此，通过化学方法合成的纳米颗粒可以通过各种相互作用吸附到柔性透明薄膜上，从而促进金属结构在纳米尺度上的自组装。为了确保成功吸附，可以通过物理或化学修饰薄膜表面来改变其表面亲水性来调整相互作用23。与金纳米颗粒相比，银纳米颗粒表现出更好的SERS性能，但它们的不稳定性，特别是它们在空气中对氧化的敏感性，导致SERS增强因子（EF）迅速降低，影响底物性能24。因此，开发一种稳定的颗粒方法至关重要。
农药残留的存在引起了人们的极大关注，因此迫切需要能够快速检测和识别现场食品中各种危险化学品的可靠方法25,26。柔性SERS基材在实际应用中具有独特的优势，特别是在食品安全领域。本文介绍了一种通过将合成的葡萄糖包被银纳米颗粒（AgNPs）键合到PDMS底物上来制备柔性SERS底物的方法（图1）。葡萄糖的存在可以保护AgNPs，减轻空气中的银氧化。该底物表现出优异的检测性能，能够检测低至10-10 M的罗丹明6G（R6G）和低至 10-8 M的农药硫兰，具有良好的均匀性。此外，柔性基板可用于通过粘接和取样进行检测，具有众多潜在的应用场景。

<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

本文介绍了一种用于表面增强拉曼散射（SERS）的柔性衬底的制备方法。通过硝酸银（AgNO3）和氨的络合反应合成了银纳米颗粒（AgNPs），然后使用葡萄糖还原。所得的AgNPs表现出均匀的尺寸分布，范围为20 nm至50 nm。随后，采用3-氨丙基三乙氧基硅烷（APTES）对已用氧等离子体表面处理的PDMS衬底进行改性。该过程有助于AgNPs在基板上的自组装。通过系统评估各种实验条件对衬底性能的影响，开发出具有优异性能和增强因子（EF）的SERS衬底。利用这种底物，R6G（罗丹明6G）的检测限为10-10 M，Thiram的检测限为10-8 M，令人印象深刻。该基质被成功用于检测苹果上的农药残留，结果非常令人满意。灵活的SERS基板在实际应用中显示出巨大的潜力，包括复杂场景中的检测。

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.

作者聚焦：使用合成的 AgNP 开发与应用 SERS 柔性底物 

基于聚二甲基硅氧烷（PDMS）的柔性表面增强拉曼散射（SERS）衬底的制备及其超灵敏检测

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.

本研究利用APTES开发了一种由葡萄糖包裹的合成AgNPs组成的柔性SERS底物，并利用APTES在PDMS上自组装，在实际农药检测应用中实现了优异的检测性能。R6G 和 Thiram 的检出限分别达到 10-10 M 和 10-8 M，增强因子 （EF） 为 1 x 10 5。此外，基材表现出均匀性。
使用改进的 Tollens 方法合成包裹在葡萄糖中的 AgNP28,29。这?...

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

该协议描述了一种用于表面增强拉曼散射的柔性基板的制造方法。该方法已成功用于检测低浓度的R6G和Thiram。

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

该协议描述了制备SERS柔性底物，并将其应用于实际检测场景。该协议提供的SERS柔性基板是环保的，并具有良好的检测性能。银纳米粒子可以很容易地通过简单的容器合成，不需要复杂的实验条件和环境。在我们的实验室中，我们计划专注于研究通过本研究中使用的容器合成的银纳米颗粒。我们将探索增强其SERS检测能力的方法，并利用其独特的特性和特性来设计性能更好的SERS检测基板。

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

1.5K 次观看.  Peking University. 该协议描述了制备SERS柔性底物，并将其应用于实际检测场景。该协议提供的SERS柔性基板是环保的，并具有良好的检测性能。银纳米粒子可以很容易地通过简单的容器合成，不需要复杂的实验条件和环境。在我们的实验室中，我们计划专注于研究通过本研究中使用的容器合成的银纳米颗粒。我们将探索增强其SERS检测能力的方法，并利用其独特的特性和特性来设计性能更?...

视频: 作者聚焦：使用合成的 AgNP 开发与应用 SERS 柔性底物 

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.

科研

工程学

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.