这项工作得到了赫尔辛基大学和简和阿托斯·埃克科基金会的支持。S.H.感谢伊拉斯谟®欧盟基金的奖学金。

1. Ag-Pd/ZrO2 NP 的合成 
注:在此过程中，Ag-Pd 中的 Pd 摩尔百分比对应为 1%，ZrO2 上的 Ag-Pd 负载对应为 3 wt.%。
<ol><li>将 1 克 ZrO2 粉末放置在 250 mL 烧杯中。</li>
	<li>在室温下，在剧烈的磁搅拌（500 转/升）下，将 50 mL 的 AgNO3 （aq） （0.0059 摩尔/L） 和 K2PdCl4 （aq） （0.00031 mol/L） 溶液添加到烧杯中。</li>
	<li>添加 10 mL 的赖氨酸 （0.53 M） 液态溶液。</li>
	<li>将混合物保持在剧烈搅拌（500转pm）下20分钟。</li>
	<li>20 分钟后，使用移液器以 1 mL/min 的速度，将新制备的 NaBH4 （aq） （0.035 M） 溶液的悬架加到 10 mL 中。在整个过程中保持悬架搅拌（500 rpm）。</li>
	<li>让混合物在室温下搅拌30分钟。</li>
</ol>2. 催化剂的分离和净化
<ol><li>将悬架转移到离心管中，以 3，260 x g的离心速度将固体与混合物分离 10 分钟。</li>
	<li>用移液器小心地去除液体相，并在管子中加入 15 mL 去离子水。<ol>
<li>剧烈摇动，直到获得固体的分散。如果不能实现良好的分散，将管子放在超声波浴池中5分钟。</li>
		<li>离心分散在3，260 x g 10分钟。</li>
	</ol>
</li>
	<li>使用去离子水重复两次（2.2 到 2.2.2.），然后一次使用乙醇代替水。</li>
	<li>取出乙醇，在60°C的烤箱中干燥固体12小时。</li>
	<li>通过各种显微镜、元素和光谱技术来描述已制备的 Ag-Pd/ZrO2 NP。</li>
</ol>3. Ag/ZrO2 NPs 的合成 
注:在此过程中，ZrO2 上的 Ag 加载对应于 3 wt.%。
<ol><li>将 1 克 ZrO2 粉末放置在 250 mL 烧杯中。</li>
	<li>在室温下，在剧烈的磁搅拌（500 rpm）下，将 50 mL 的 AgNO3 （aq） （0.0059 mol/L） 溶液添加到烧杯中。</li>
	<li>添加 10 mL 的赖氨酸 （0.53 M） 液态溶液。</li>
	<li>将混合物保持在剧烈搅拌（500转pm）下20分钟。</li>
	<li>20 分钟后，使用移液器以 1 mL/min 的速度，将新制备的 NaBH4 （aq） （0.035 M） 溶液的悬架加到 10 mL 中。在整个过程中保持悬架搅拌（500 rpm）。</li>
	<li>让混合物在室温下搅拌30分钟。</li>
</ol>4. 催化剂的分离和净化
<ol><li>将悬架转移到离心管中，以 3，260 x g的离心速度将固体与混合物分离 10 分钟。</li>
	<li>用移液器小心地去除液体相，并在管子中加入 15 mL 去离子水。<ol>
<li>剧烈摇动，直到观察到固体的分散。如果不能实现良好的分散，将管子放在超声波浴池中5分钟。</li>
		<li>离心分散在3，260 x g 10分钟。</li>
	</ol>
</li>
	<li>重复洗涤步骤（4.2至4.2.2.）两次使用去离子水，然后一次使用乙醇代替水。</li>
	<li>取出乙醇，在60°C的烤箱中干燥固体12小时。</li>
	<li>然后，制备的Ag/ZrO2 NPs可以具有各种显微镜、元素和光谱技术的特点。</li>
</ol>5. LSPR激发（光照）下对硝基苯减少的质离子催化性能调查
<ol><li>将 30 毫克催化剂与磁性搅拌棒一起放置在 25 mL 圆底烧瓶中。</li>
	<li>在异丙醇（IPA）中加入5毫升的亚硝基苯溶液（0.03摩尔/升）到反应堆中。</li>
	<li>然后，加入11.22毫克KOH粉末（0.0002摩尔）。</li>
	<li>用砷流冒泡悬架1分钟，清除反应堆。清除后立即密封烧瓶。</li>
	<li>将反应堆放在温度控制的磁搅拌器（500 rpm）上方70°C加热的油浴中。</li>
	<li>使用波长为 425 nm 的 4 个 LED 灯作为光源对管子进行辐照，光强度为 0.5 W/cm2。从灯到反应瓶的距离应该是7厘米。</li>
	<li>让反应在 70 °C 下在强磁搅拌 （500 rpm） 下进行 2.5 小时。</li>
	<li>然后，关掉灯，打开反应堆，用注射器和针头收集1mL样品。通过 0.45 μm 过滤器过滤，将催化剂颗粒去除，放入气相色谱瓶中。</li>
</ol>6. 在没有LSPR激发的情况下的反应（黑暗条件）
<ol><li>遵循 5 中描述的相同步骤，但无需光照射。用铝箔包裹反应管，防止光线暴露。</li>
</ol>7. 气相色谱（GC）分析准备
<ol><li>准备含有约 30 mmol/L 硝基苯 （NB）、30 mmol/L 苯 （AN） 和 30 mmol/L 的偶氮苯 （AB） 的 IPA 溶液。</li>
	<li>使用合适的方法对解决方案进行 GC 分析。可以通过改变柱温和气流程序来测试不同的方法。选定的方法应能够在最短的保留期内分离与 IPA、NB、AN 和 AB 对应的峰值。</li>
	<li>选择该方法后，在 IPA 中编写一组 50 mM、25 mM、10 mM、5 mM 和 2.5 mM NB 的解决方案，并在 IPA 中编写另一组浓度相同的 AN 和 AB 解决方案。</li>
	<li>对已准备的解决方案进行 GC 分析。每个色谱图应呈现 2 个峰值:较高的峰值对应 IPA，下一个对应于 NB、AN 或 AB 的峰值。对于每个色谱图，请记下所有峰值的保留时间和峰值区域。</li>
	<li>通过绘制每个样本的浓度与峰值区域来跟踪 NB、AN 和 AB 的校准曲线。</li>
</ol>8. GC 分析
<ol><li>对第 5 步收集的样本进行 GC 分析。和6.与用于步骤7.2的相同方法。和7.4。</li>
	<li>对于每个色谱图，请记下保留时间和峰值区域，并使用之前绘制的校准曲线来确定样品中 NB、AN 和 AB 的浓度。</li>
	<li>使用方程计算硝基苯转换以及苯和苯的选择性: <img alt="Equation 1" src="/files/ftp_upload/61712/61712eq1.jpg"> <img alt="Equation 2" src="/files/ftp_upload/61712/61712eq2.jpg"> <img alt="Equation 3" src="/files/ftp_upload/61712/61712eq3.jpg"> <img alt="Equation 4" src="/files/ftp_upload/61712/61712eq4.jpg">在GC分析2.5小时后，初始NB浓度（0.03摩尔/升）和CNB、C AN、C AB分别对应于NB、AN和AB浓度。</li>
</ol>

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G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+Plasmon+Resonance+in+Bimetallic+Core-Shell+Nanoparticles.">Surface Plasmon Resonance in Bimetallic Core-Shell Nanoparticles.</a> Journal of Physical Chemistry C. 119 (29), 16836-16845 (2015).</li><li>Liu, Z., Huang, Y., Xiao, Q., Zhu, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+reduction+of+nitroaromatics+to+azoxy+compounds+on+supported+Ag-Cu+alloy+nanoparticles+through+visible+light+irradiation.">Selective reduction of nitroaromatics to azoxy compounds on supported Ag-Cu alloy nanoparticles through visible light irradiation.</a> Green Chemistry. 18 (3), 817-825 (2016).</li><li>Chaiseeda, K., Nishimura, S., Ebitani, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gold+nanoparticles+supported+on+alumina+as+a+catalyst+for+surface+plasmon-enhanced+selective+reductions+of+nitrobenzene.">Gold nanoparticles supported on alumina as a catalyst for surface plasmon-enhanced selective reductions of nitrobenzene.</a> ACS Omega. 2 (10), 7066-7070 (2017).</li><li>Peiris, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Metal+nanoparticle+photocatalysts:+emerging+processes+for+green+organic+synthesis.">Metal nanoparticle photocatalysts: emerging processes for green organic synthesis.</a> Catalysis Science and Technology. 6 (2), 320-338 (2016).</li><li>Garc&#237;a-Garc&#237;a, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Silver-Based+Plasmonic+Catalysts+for+Carbon+Dioxide+Reduction.">Silver-Based Plasmonic Catalysts for Carbon Dioxide Reduction.</a> ACS Sustainable Chemistry and Engineering. 8 (4), 1879-1887 (2020).</li><li>Agrawal, A., Johns, R. W., Milliron, D. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Control+of+Localized+Surface+Plasmon+Resonances+in+Metal+Oxide+Nanocrystals.">Control of Localized Surface Plasmon Resonances in Metal Oxide Nanocrystals.</a> Annual Review of Materials Research. 47 (1), 1-31 (2017).</li><li>Lounis, S. D., Runnerstrom, E. L., Llord&#233;s, A., Milliron, D. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Defect+chemistry+and+Plasmon+physics+of+colloidal+metal+oxide+Nanocrystals.">Defect chemistry and Plasmon physics of colloidal metal oxide Nanocrystals.</a> Journal of Physical Chemistry Letters. 5 (9), 1564-1574 (2014).</li><li>Rej, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determining+Plasmonic+Hot+Electrons+and+Photothermal+Effects+during+H2+Evolution+with+TiN-Pt+Nanohybrids.">Determining Plasmonic Hot Electrons and Photothermal Effects during H2 Evolution with TiN-Pt Nanohybrids.</a> ACS Catalysis. 10 (9), 5261-5271 (2020).</li><li>Barragan, A. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Photochemistry+of+Plasmonic+Titanium+Nitride+Nanocrystals.">Photochemistry of Plasmonic Titanium Nitride Nanocrystals.</a> The Journal of Physical Chemistry C. 123 (35), 21796-21804 (2019).</li></ol>

作者没有什么可透露的。

该方法描述的结果表明，Pd（或其他催化但非质子金属）的内在催化活性可以通过双金属合金NPs35中的可见光照射通过LSPR激发显著增强。在这种情况下，Ag（或其他质离子金属）能够通过LSPR激发从可见光照射中获取能量。LSPR激发导致热电荷载体（热电子和孔）的形成和局部加热5，14，15，16，17，18，19。</s...

在金属纳米粒子（NPs）的几种应用中，催化值得特别关注。催化在可持续的未来发挥着核心作用，有助于减少能源消耗，更好地利用原材料，并使反应条件更清洁1，2，3，4。因此，催化的进展可以为提高化学过程的原子效率提供工具，使它们更清洁、更经济、更环保。金属NP包括银（Ag）、金（Au）或铜（Cu），可以通过局部表面质子共振（LSPR）激发5、6、7、8在纳米尺度上与光相互作用的独特方式，在可见范围内显示有趣的光学特性。在这些NP中，称为质子NP，LSPR包括事件光子（来自来袭电磁波）与电子5、6、7、8的集体运动的共振相互作用。这种现象发生在一个典型的频率，这取决于大小，形状，组成，和介电常数的环境9，10，11。例如，对于Ag、Au和Cu，这些频率的范围从可见到近红外，为利用太阳能激发其LSPR 5、6、7、8、12、13提供了可能性。
最近，人们已经证明，质子核动力学中的LSPR激发有助于加快速率，控制分子转换5，14，15，16，17，18，19的选择性。这催生了一个叫做质子催化的领域，它专注于利用光的能量来加速、驱动和/或控制化学转化5、14、15、16、17、18、19。在此背景下，已确定质离子NP中的LSPR激发可导致高能热电子和孔的形成，称为LSPR激发热载体。这些载体可以通过电子或振动激活15，16与吸附物种相互作用。除了提高反应率外，该过程还可以提供传统热化学驱动过程无法进入的替代反应途径，为控制反应选择性20、21、22、23、24、25开辟了新的途径。重要的是，值得注意的是，质粒衰变也会导致热消散，导致NP附近的温度上升，这也有助于加快反应速率15，16。
由于这些有趣的特点，质子催化已成功地应用于各种分子转换18。然而，一个重要的挑战依然存在。虽然 Ag 和 Au 等质离子 NP 在可见和近红外范围内具有出色的光学特性，但其催化性能在转化范围方面是有限的。换句话说，它们对于几个转换没有表现出良好的催化性能。此外，在催化中很重要的金属，如铂金（Pd）和铂金（Pt），不支持可见或近高射能范围内的LSPR激发。为了弥补这一差距，含有质离子和催化金属的双金属NP代表一个有效的策略20，26，27，28，29。在这些系统中，质离子金属可以用作天线，通过LSPR从光激发中获取能量，然后用于驱动、加速和控制催化金属的分子转换。因此，这种策略使我们能够超越传统的质离子金属NPs20，26，27，28，29的质离子催化。
该协议描述了 ZrO 2（Ag-Pd/ZrO2）上支持的双金属银铂（Ag-Pd）合金 NP 的简单合成，可作为质离子催化的质子催化系统。Ag-Pd/ZrO2 NP 由 ZrO2支持上的相应金属前体共同浸渍而制备，然后同时减少30个。这种方法导致在 ZrO2支座表面直接形成大小约为 10 nm 的双金属 NP。NP 由 1 摩尔% 的 Pd 组成，以最大限度地减少催化金属的利用，同时最大限度地提高由此产生的 Ag-Pd NP 的光学特性。演示了在质离子催化中应用Ag-Pd/ZrO2 NPs的议定书，用于减少硝基苯。我们使用425 nm LED照明为LSPR激发。进行气相色谱检查，以监测在暗光照射条件下减少反应的转换和选择性。LSPR 激发导致与纯热驱动条件相比，Ag-Pd/ZrO2 NP 的催化性能增强，并控制选择性。此协议中描述的方法基于简单的光催化反应设置，加上气相色谱，可适应广泛的分子转换和 NP 组成。因此，这种方法使得光催化活性的描述成为可能，在转换和反应选择性方面，不同的NP和无数的液相转换。我们相信这篇文章将为新来者和更有经验的科学家提供重要的指导方针和见解。

<table><tbody><tr><td>2-Propanol (anhydrous, 99.5%)</td><td>Sigma-Aldrich</td><td>278475</td><td>CAS Number 67-63-0</td></tr><tr><td>Aniline (for synthesis)</td><td>Sigma-Aldrich</td><td>8.22256</td><td>CAS Number 62-53-3</td></tr><tr><td>Azobenzene (98%)</td><td>Sigma-Aldrich</td><td>424633</td><td>CAS Number 103-33-3</td></tr><tr><td>Ethanol</td><td>Honeywell</td><td>32221</td><td>CAS Number 64-17-5</td></tr><tr><td>Hydrochloric acid (37%)</td><td>VWR</td><td>PRLSMC310066</td><td>CAS Number 7647-01-0</td></tr><tr><td>L-Lysine (crystallized, &amp;ge;98.0% (NT))</td><td>Sigma-Aldrich</td><td>62840</td><td>CAS Number 56-87-1</td></tr><tr><td>Nitric acid (65%)</td><td>Merck</td><td>100456</td><td>CAS Number 7697-37-2</td></tr><tr><td>Nitrobenzene</td><td>Sigma-Aldrich</td><td>8.06770</td><td>CAS Number 98-95-3</td></tr><tr><td>Potassium hydroxide</td><td>Fisher</td><td>10448990</td><td>CAS Number 1310-58-3</td></tr><tr><td>Potassium tetrachloropalladate (II) (98%)</td><td>Sigma-Aldrich</td><td>205796</td><td>CAS Number 10025-98-6</td></tr><tr><td>Silver nitrate (ACS reagent, &amp;ge;99.0%)</td><td>Sigma-Aldrich</td><td>209139</td><td>CAS Number 7761-88-8</td></tr><tr><td>Sodium borohydride (fine granular for synthesis)</td><td>Sigma-Aldrich</td><td>8.06373</td><td>CAS Number 16940-66-2</td></tr><tr><td>Zirconium (IV) oxide (nanopowder, &amp;lt;100 nm particle size (TEM))</td><td>Sigma-Aldrich</td><td>544760</td><td>CAS Number 1314-23-4</td></tr></tbody></table>

preparation of silver-palladium alloyed nanoparticles for plasmonic catalysis under visible-light illumination

质离子纳米粒子（NPs）中的局部表面质子共振（LSPR）可以加速和控制各种分子转换的选择性。当支持这些范围内LSPR激发的质粒纳米粒子被用作催化剂时，这为使用可见光或近射光作为驱动和控制反应的可持续输入开辟了可能性。不幸的是，对于几种催化金属（如铂（Pd）来说，情况并非如此。克服这一限制的一个策略是采用含有质离子和催化金属的双金属NP。在这种情况下，质离子金属中的LSPR激发有助于加速和控制催化组件驱动的转化。本文报告的方法侧重于在ZrO 2（Ag-Pd/ZrO2）上支持的双金属银-铂（Ag-Pd）NPs的合成，该点作为质粒催化系统。NP 的编制是通过在 ZrO2支持上共同浸渍相应的金属前体，然后同时减少导致直接在 ZrO2支持上形成双金属 NP。然后，Ag-Pd/ZrO2 NP 被用作质离子催化剂，用于通过 LED 灯在 425 nm 照明下减少硝基苯。使用气相色谱（GC），可以监测暗光照射条件下减少反应的转换和选择性，证明在将非质子Pd与质离子金属Ag合金后，LSPR激发下的催化性能和对选择性的控制增强。该技术可适应广泛的分子转化和NPs成分，有助于描述不同类型催化在转化和选择性方面的质离子催化活性。

图 1A 显示了含有纯 ZrO2 氧化物（左）和 Ag-Pd/ZrO2 NP（右）的固体样品的数码照片。这种颜色从白色（ZrO2）到棕色（Ag-Pd/ZrO2）的变化为Ag-Pd NP在ZrO2 表面的沉积提供了初步的定性证据。 图 1B 显示了来自 Ag-Pd/ZrO2 NP（蓝色跟踪）以及 ZrO2（ 黑色跟踪）和 Ag/ZrO2 NP（红色跟踪）的紫外线可见吸...

Watch this Scientific Journal Video about Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination at JoVE.com

Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

这里介绍了在 ZrO 2 （Ag-Pd/ZrO2）上支持的银铂 （Ag-Pd） 合金纳米粒子 （NPs） 合成的协议。该系统允许从可见光照射中获取能量，以加速和控制分子转化。在Ag-Pd/ZrO2 NPs催化的光照射下，硝基苯的减少就说明了这一点。

在可见光照射下为质子催化准备银-铂合金纳米粒子

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular ...

preparation-silver-palladium-alloyed-nanoparticles-for-plasmonic

Research

JoVE Journal

Chemistry

5.4K 次观看.  University of Helsinki. 这里介绍了在 ZrO 2 （Ag-Pd/ZrO2）上支持的银铂 （Ag-Pd） 合金纳米粒子 （NPs） 合成的协议。该系统允许从可见光照射中获取能量，以加速和控制分子转化。在Ag-Pd/ZrO2 NPs催化的光照射下，硝基苯的减少就说明了这一点。

视频: Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Gyroid镍纳米结构的嵌段共聚物超分子

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

科研

化学

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

合成，表征和混合金/硫化镉和Au / ZnS核/壳纳米颗粒功能化

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to neutral gold Au(0) by reducing agents, such as sodium citrate or sodium borohydride. The extension of this method to decorate iron oxide or similar nanoparticles with gold nanoparticles to create multifunctional hybrid Fe2O3-Au nanoparticles is straightforward. This approach yields fairly good control over Au nanoparticle dimensions and loading onto Fe2O3. Additionally, the Au metal size, shape, and loading can easily be tuned by changing experimental parameters (e.g., reactant concentrations, reducing agents, surfactants, etc.). An advantage of this procedure is that the reaction can be done in air or water, and, in principle, is amenable to scaling up. The use of such optically tunable Fe2O3-Au nanoparticles for hyperthermia studies is an attractive option as it capitalizes on plasmonic heating of gold nanoparticles tuned to absorb light strongly in the VIS-NIR region. In addition to its plasmonic effects, nanoscale Au provides a unique surface for interesting chemistries and catalysis. The Fe2O3 material provides additional functionality due to its magnetic property. For example, an external magnetic field could be used to collect and recycle the hybrid Fe2O3-Au nanoparticles after a catalytic experiment, or alternatively, the magnetic Fe2O3 can be used for hyperthermia studies through magnetic heat induction. The photothermal experiment described in this report measures bulk temperature change and nanoparticle solution mass loss as functions of time using infrared thermocouples and a balance, respectively. The ease of sample preparation and the use of readily available equipment are distinct advantages of this technique. A caveat is that these photothermal measurements assess the bulk solution temperature and not the surface of the nanoparticle where the heat is transduced and the temperature is likely to be higher.

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

We describe the synthesis and properties of multifunctional Fe2O3-Au nanoparticles produced by a wet chemical approach and investigate their photothermal properties using laser irradiation. The composite Fe2O3-Au nanoparticles retain the properties of both materials, creating a multifunctional structure with excellent magnetic and plasmonic properties.

多功能混合铁<sub&gt; 2</sub&gt; 0<sub&gt; 3</sub&gt; -Au纳米粒子高效的电浆暖气

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to ...

工程学

Colloidal Synthesis of Nanopatch Antennas for Applications in Plasmonics and Nanophotonics

We present a method for colloidal synthesis of silver nanocubes and the use of these in combination with a smooth gold film, to fabricate plasmonic nanoscale patch antennas. This includes a detailed procedure for the fabrication of thin films with a well-controlled thickness over macroscopic areas using layer-by-layer deposition of polyelectrolyte polymers, namely poly(allylamine) hydrochloride (PAH) and polystyrene sulfonate (PSS). These polyelectrolyte spacer layers serve as a dielectric gap in between silver nanocubes and a gold film. By controlling the size of the nanocubes or the gap thickness, the plasmon resonance can be tuned from about 500 nm to 700 nm. Next, we demonstrate how to incorporate organic sulfo-cyanine5 carboxylic acid (Cy5) dye molecules into the dielectric polymer gap region of the nanopatch antennas. Finally, we show greatly enhanced fluorescence of the Cy5 dyes by spectrally matching the plasmon resonance with the excitation energy and the Cy5 absorption peak. The method presented here enables the fabrication of plasmonic nanopatch antennas with well-controlled dimensions utilizing colloidal synthesis and a layer-by-layer dip-coating process with the potential for low cost and large-scale production. These nanopatch antennas hold great promise for practical applications, for example in sensing, ultrafast optoelectronic devices and for high-efficiency photodetectors.

A protocol for the colloidal synthesis of silver nanocubes and fabrication of plasmonic nanoscale patch antennas with sub-10 nm gaps is presented.

在等离子体激元和纳米光子学应用Nanopatch天线的合成胶体

We present a method for colloidal synthesis of silver nanocubes and the use of these in combination with a smooth gold film, to fabricate plasmonic ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

在没有聚集的层状钛酸盐薄膜透明的层间金纳米粒子的原位合成

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

Ligand-Mediated Nucleation and Growth of Palladium Metal Nanoparticles

The size, size distribution and stability of colloidal nanoparticles are greatly affected by the presence of capping ligands. Despite the key contribution of capping ligands during the synthesis reaction, their role in regulating the nucleation and growth rates of colloidal nanoparticles is not well understood. In this work, we demonstrate a mechanistic investigation of the role of trioctylphosphine (TOP) in Pd nanoparticles in different solvents (toluene and pyridine) using in situ SAXS and ligand-based kinetic modeling. Our results under different synthetic conditions reveal the overlap of nucleation and growth of Pd nanoparticles during the reaction, which contradicts the LaMer-type nucleation and growth model. The model accounts for the kinetics of Pd-TOP binding for both, the precursor and the particle surface, which is essential to capture the size evolution as well as the concentration of particles in situ. In addition, we illustrate the predictive power of our ligand-based model through designing the synthetic conditions to obtain nanoparticles with desired sizes. The proposed methodology can be applied to other synthesis systems and therefore serves as an effective strategy for predictive synthesis of colloidal nanoparticles.

The main goal of this work is to elucidate the role of capping agents in regulating the size of palladium nanoparticles by combining in situ small angle x-ray scattering (SAXS) and ligand-based kinetic modeling.

配体介导成核与钯金属纳米粒子的生长

The size, size distribution and stability of colloidal nanoparticles are greatly affected by the presence of capping ligands. Despite the key contribution ...

A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic nanoparticles is developed. Guidelines for the replication of the reactor and its operation are provided in detail. Three different composite systems (Pt/graphene, Pt/TiO2, and Au/TiO2) with monodisperse and uniformly distributed particles are produced by this reactor, and the photodeposition mechanism, as well as the synthesis optimization strategy, are discussed. The synthesis methods and their technical aspects are described comprehensively. The role of the ultraviolet (UV) dose (in each excitation pulse) on the photodeposition process is investigated and the optimum values for each composite system are provided.

For a continuous and scalable synthesis of noble-metal-based nanocomposites, a novel photocatalytic reactor is developed and its structure, operation principles, and product quality optimization strategies are described.

一种用于金属纳米粒子精确控制沉积的连续流动光催化反应器

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic ...

Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation

A protocol is described to photocatalytically guide Pd deposition onto Au nanorods (AuNR) using surface plasmon resonance (SPR). Excited plasmonic hot electrons upon SPR irradiation drive reductive deposition of Pd on colloidal AuNR in the presence of [PdCl4]2-. Plasmon-driven reduction of secondary metals potentiates covalent, sub-wavelength deposition at targeted locations coinciding with electric field &#8220;hot-spots&#8221; of the plasmonic substrate using an external field (e.g., laser). The process described herein details a solution-phase deposition of a catalytically-active noble metal (Pd) from a transition metal halide salt (H2PdCl4) onto aqueously-suspended, anisotropic plasmonic structures (AuNR). The solution-phase process is amenable to making other bimetallic architectures. Transmission UV-vis monitoring of the photochemical reaction, coupled with ex situ XPS and statistical TEM analysis, provide immediate experimental feedback to evaluate properties of the bimetallic structures as they evolve during the photocatalytic reaction. Resonant plasmon irradiation of AuNR in the presence of [PdCl4]2- creates a thin, covalently-bound Pd0 shell without any significant dampening effect on its plasmonic behavior in this representative experiment/batch. Overall, plasmonic photodeposition offers an alternative route for high-volume, economical synthesis of optoelectronic materials with sub-5 nm features (e.g., heterometallic photocatalysts or optoelectronic interconnects).

A protocol for anisotropic photodeposition of Pd onto aqueously-suspended Au nanorods via localized surface plasmon excitation is presented.

通过表面等离子体激发将 Pd 光沉积到胶体 Au 纳米棒上

A protocol is described to photocatalytically guide Pd deposition onto Au nanorods (AuNR) using surface plasmon resonance (SPR). Excited plasmonic hot ...

等离子体金锡合金纳米颗粒的水合成

Aqueous Synthesis of Plasmonic Gold-Tin Alloy Nanoparticles

This protocol describes the synthesis of Au nanoparticle seeds and the subsequent formation of Au-Sn bimetallic nanoparticles. These nanoparticles have potential applications in catalysis, optoelectronics, imaging, and drug delivery. Previously, methods for producing alloy nanoparticles have been time-consuming, require complex reaction conditions, and can have inconsistent results. The outlined protocol first describes the synthesis of approximately 13 nm Au nanoparticle seeds using the Turkevich method. The protocol next describes the reduction of Sn and its incorporation into the Au seeds to generate Au-Sn alloy nanoparticles. The optical and structural characterization of these nanoparticles is described. Optically, prominent localized surface plasmon resonances (LSPRs) are apparent using UV-visible spectroscopy. Structurally, powder X-ray diffraction (XRD) reflects all particles to be less than 20 nm and shows patterns for Au, Sn, and multiple Au-Sn intermetallic phases. Spherical morphology and size distribution are obtained from transmission electron microscopy (TEM) imaging. TEM reveals that after Sn incorporation, the nanoparticles grow to approximately 15 nm in diameter.

作者聚焦：设计可持续的纳米材料以促进合成和元素混合

Here, the synthesis of gold (Au) seeds is described using the Turkevich method. These seeds are then used to synthesize gold-tin alloy (Au-Sn) nanoparticles with tunable plasmonic properties.

This protocol describes the synthesis of Au nanoparticle seeds and the subsequent formation of Au-Sn bimetallic nanoparticles. These nanoparticles have ...