Name: photodeposition of pd onto colloidal au nanorods by surface plasmon excitation
Uploaded: 2019-08-15T14:45:00
Description: Watch this Scientific Journal Video about Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation at JoVE.com

这项工作由陆军研究实验室赞助,根据美国陆军实验室的合作协议号W911NF_17_2_0057授予G.T.F.本文件所载的观点和结论是作者的观点和结论,不应被解释为代表陆军研究实验室或美国政府的明示或暗示的官方政策。美国政府有权复制和分发用于政府目的的重印,尽管此处有版权说明。

1. Au 纳米棒的分配
注:乙酰甲基溴二铵(CTAB)覆盖的AuNR可由湿化学(步骤1.1)合成,或根据读者喜好进行商业采购(步骤1.2),每种结果均有类似结果。这项工作的结果是基于商业来源的AuNR与五角双晶结构。AuNR种子晶体结构(即单晶与五角双)对次生金属壳最终形态的影响在质质光沉积范围内仍不清楚,但两者一直备受关注。15和类似的光化学<sup ...

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使用透射UV-vis光谱监测光学吸收的变化有助于评估光催化反应的状态,特别注意H2 PdCl4的LMCT特性。在步骤 2.3.1 中注入 H2PdCl4后 LMCT 功能的波长最大值(图 1中从纯黑色到纯蓝色)提供了对 [PdCl4+2 分子1 (例如,与N+ CTAB头组进行静电协调,然后输送到AuNR表面1和/或相应的水解和/或氧化31、32、...

通过从共振外部场生成的质子热载体引导金属沉积到质子基板上,可以支持在环境条件下两步形成异质金属等向性纳米结构,具有新的自由度1 ,2,3.传统的氧化还原化学、气相沉积和/或电镀方法不适合大批量处理。这主要是由于过量/牺牲试剂废物、低通量 5+ 步光刻工艺以及能源密集型环境(0.01-10 Torr 和/或 400-1000 °C 温度),很少或根本没有直接控制由此产生的材料特性.将质子基质(例如Au纳米粒子/种子)浸入前体环境(例如,水性Pd盐溶液)的照明下,在局部表面质质共振(SPR)下启动外部可调(即场极化和强度)前体通过质子热电子和/或光热梯度3、4的光化学沉积。例如,Au、Cu、Pb 和 Ti 有机金属和 Ge hydrides 在纳米结构 Ag 和 Au 基板上的质子驱动光热分解的协议参数/要求已详细到5、6、 7,8,9.然而,利用飞度质子热电子在金属溶液界面上直接光减金属盐,在很大程度上仍未开发,没有采用丁酸盐或聚(乙烯基)配体作为中间电荷的工艺用于直接成核/生长的次级金属2、10、11、12。最近报道了在纵向SPR (LSPR) 激发下Au纳米棒(AuNR)的各向异性Pt装饰,其中Pt分布与偶极极性重合(即,假定的空间分布)热载体)。
本文扩展了近期的Pt-AuNR工作,包括Pd,并突出显示了可实时观测的关键合成指标,表明还原质质光沉积技术适用于其他金属卤化物盐(Ag、Ni、Ir等)。

<table>
	<tbody>
		<tr>
			<td>Aspheric Condenser Lens w/ Diffuser</td>
			<td>Thorlabs</td>
			<td>ACL5040U-DG15</td>
			<td>f=40 mm, NA=0.60, 1500 grit, uncoated</td>
		</tr>
		<tr>
			<td>Deuterium + Tungsten-Halogen Lightsource</td>
			<td>StellarNet</td>
			<td>SL5</td>
			<td></td>
		</tr>
		<tr>
			<td>Gold Nanorods, AuNR</td>
			<td>NanoPartz</td>
			<td>A12-40-808-CTAB</td>
			<td>CTAB surfactant, 808 nm LSPR, 40 nm diameter</td>
		</tr>
		<tr>
			<td>Ground Glass Diffuser</td>
			<td>Thorlabs</td>
			<td>DG20-1500</td>
			<td>1500 grit, N-BK7</td>
		</tr>
		<tr>
			<td>Hydrochloric acid, HCl</td>
			<td>J.T. Baker</td>
			<td>9539-03</td>
			<td>concentrated, 37%</td>
		</tr>
		<tr>
			<td>Low Profile Magnetic Stirrer</td>
			<td>VWR</td>
			<td>10153-690</td>
			<td></td>
		</tr>
		<tr>
			<td>Macro Disposable Cuvettes, UV Plastic</td>
			<td>FireFlySci</td>
			<td>1PUV</td>
			<td>10 mm path length</td>
		</tr>
		<tr>
			<td>Methanol, MeOH</td>
			<td>J.T. Baker</td>
			<td>9073-05</td>
			<td>&#8805;99.9%</td>
		</tr>
		<tr>
			<td>Palladium (II) chloride, PdCl2</td>
			<td>Sigma Aldrich</td>
			<td>520659</td>
			<td>&#8805;99.9%</td>
		</tr>
		<tr>
			<td>Plano-Convex Lens</td>
			<td>Thorlabs</td>
			<td>LA1145</td>
			<td>f=75 mm, N-BK7, uncoated</td>
		</tr>
		<tr>
			<td>Quartz Tungsten-Halogen Lamp</td>
			<td>Thorlabs</td>
			<td>QTH10</td>
			<td></td>
		</tr>
		<tr>
			<td>UV-vis Spectrometer</td>
			<td>Avantes</td>
			<td>ULS2048L-USB2-UA-RS</td>
			<td>AvaSpec-ULS2048L</td>
		</tr>
	</tbody>
</table>

photodeposition of pd onto colloidal au nanorods by surface plasmon excitation

描述了一种使用表面质子共振(SPR)将Pd沉积光引导到Au纳米棒(AuNR)上的方案。激发质子热电子在SPR辐照驱动还原沉积Pd在胶体AuNR的存在[PdCl4]2-。在目标位置,由质子驱动还原二次金属电位,亚波长沉积与利用外部场(如激光)的质子基板的电场"热点"发生。本文所述过程详细介绍了催化活性贵金属(Pd)从过渡金属卤化盐(H2PdCl 4)到水悬浮各向异性质质结构(AuNR)的溶液相沉积。溶液相过程适用于制造其他双金属结构。对光化学反应的透射紫外线监测,加上原位XPS和统计TEM分析,提供即时的实验反馈,以评估双金属结构在光催化反应。在 [PdCl4+2 -存在]时,AuNR的共振质质照射可产生一个薄的共价边界Pd0壳,在此代表性的实验/批次中对其质子行为没有任何显著的阻尼作用。总体而言,质子光沉积为具有5nm以下特征的光电子材料(例如异金属光催化剂或光电互连)的高容量、经济性合成提供了另一种途径。

在黑暗和共振辐照下,在H2PdCl4存在/不存在的情况下,为CTAB覆盖的AuNR采集了透外光谱、X射线光电子光谱(XPS)数据和传输电子显微镜(TEM)图像在其纵向SPR(LSPR)中催化Pd的成核/生长。图1和图2中的透射UV-vis光谱根据以下变化提供了对反应动力学的见解:(a)前体配体-金属电荷转移(LMCT)特征强度和波长以及 (b) 纳米棒 SPR 强度、最大半宽 (FWHM) 和波长...

Watch this Scientific Journal Video about Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation at JoVE.com

Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation

通过表面等离子体激发将 Pd 光沉积到胶体 Au 纳米棒上

提出了一种通过局部表面质子激发将Pd各向异性光沉积到水悬浮Au纳米棒上的协议。

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

还原质感光沉积协议可有效引导五纳米以下共价金属组装在目标位置，在环境处理条件下具有最佳的相面特性。该技术的主要优点是能够使用外部场（如激光）来控制外延金属生长的厚度和位置。我们已经演示了金属铂金和银的质光沉积，并有信心将这种方法推广到许多其他催化应用。演示这个程序的将是我和我和乔纳森·博尔特斯多夫，美国陆军研究实验室的化学家。为了开始这一程序，将830微升的库存盐酸与水稀释至100毫升，以获得0.1摩尔盐酸溶液。将该溶液的4毫升水稀释至20毫升，形成20毫升盐酸溶液。移液10毫升这种20毫升盐酸溶液成适当的玻璃器皿。接下来，在盐酸中加入0.0177克氯化铝，通过声波混合，直到所有氯化铝溶解。由此产生的二氢化四氯酸酯溶液的浓度应为10毫摩尔，并应表现出深橙色。然后，移液器2.5毫升水悬浮金纳米棒溶液与1至10毫升乙酰甲基溴化铵表面活性剂成1厘米的路径长度宏体积，用磁搅拌棒。将蛋黄酱放在搅拌盘上。在轻轻搅拌时，将甲醇脱气到蛋黄酱中的移液器 475 微升。继续搅拌约 15 到 20 分钟，同时根据需要轻轻敲击玻璃盒底部，以压在刚性表面上，定期去除任何气泡。在此之后，移液器5微升的库存浓缩盐酸到蛋黄酱，让它混合15分钟。接下来，将25微升的10毫摩尔二氢二氢二氯棕榈酸盐注入反应混合物中，使铂与黄金的原子比为1至5。让溶液在黑暗中复杂一小时，同时搅拌。然后用无极化715纳米的经过过滤的钨卤素灯照射反应混合物，强度为35毫瓦/厘米平方，24小时。第二天，将残留的化学物质和试剂从金纳米棒中洗涤，以9000倍G.使用移液器去除上流液，并在水中重新悬浮颗粒。将小瓶浸入沐浴声波器中一至两分钟，以分散纳米棒并完成洗涤。重复整个洗涤过程。在这项研究中，UV对吸水光谱进行时间记录，以阐明添加每个成分，包括从金纳米棒开始的反应混合物时的变化。甲醇和盐酸的加入通过稀释降低吸光量。二氢原四氯层酸盐的加入导致紫外线滞后和金属电荷转移特征的出现。在黑暗中平衡了一个小时后，铂分子在247和310纳米上表现出电荷转移带。在金纳米棒纵向表面表面磁共振时，电荷转移带迅速蓝移到230纳米和277纳米。由于质子热电子对吸收的铂金（ii）的光还原，主导电荷转移峰值的吸收量在24小时内从1.7减至约0.47。然后分析两种SPR模式在振振辐照之前和之后。纵向SPR红移从807纳米到816纳米。随着 7 纳米线宽的扩展，横向 SPR 保持不变。XPS 通过以 335 和 340 电子伏特的绑定能量出现铂金-3D 线来证实金属铂的存在。TEM揭示了金纳米棒与二氢质三氯生物在黑暗中和在共鸣照射后混合的形态。和振照明产生具有粗糙径向界面的尖尖纳米棒。这种特征在黑暗中是无法观察到的。纳米棒长度的分布表明平均长度从127纳米增长到129纳米。这是因为在杆的末端存在照片的铂金，这在 EDS 地图中得到了确认。在库存金纳米棒溶液中，CTAB 浓度不得超过 1 至 10 毫摩尔，这一点很重要。否则，前体运输到黄金表面将被禁止。该程序可以很容易地适应光还原其他催化金属，如铂金或虹膜到质的活性种子结构，以合成广泛的光催化剂。我们现在有一个架构，其中质电能可以直接传递到催化表面，没有任何相面屏障，使我们能够更有效地研究质光催化。盐酸是一种腐蚀性强酸，应在防烟罩中处理，并配有适当的个人防护设备，如护目镜和手套。

Research

JoVE Journal

Chemistry

Exploring the Radical Nature of a Carbon Surface by Electron Paramagnetic Resonance and a Calibrated Gas Flow

通过电子顺磁共振和校准气体流量探索碳表面的激进性质

While the first Electron Paramagnetic Resonance (EPR) studies regarding the effects of oxidation on the structure and stability of carbon radicals date ...

科研

化学

Quantitative and Qualitative Examination of Particle-particle Interactions Using Colloidal Probe Nanoscopy

粒子粒子相互作用采用胶体探针纳米显微定量和定性检查

Colloidal Probe Nanoscopy (CPN), the study of the nano-scale interactive forces between a specifically prepared colloidal probe and any chosen substrate ...

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

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 ...

Synthesis and Exfoliation of Discotic Zirconium Phosphates to Obtain Colloidal Liquid Crystals

合成与盘状磷酸盐锆剥落获取胶体液晶

Due to their abundance in natural clay and potential applications in advanced materials, discotic nanoparticles are of interest to scientists and ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

铱氧化物纳米颗粒对硒化镉硫化镉@纳米棒光化学氧化增长

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

Hydroquinone Based Synthesis of Gold Nanorods

金纳米棒基于对苯二酚合成

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

毛细管电泳监视肽接枝壳聚糖膜实时

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

形状-各向异性胶体镉硫纳米结构的 Facet-to-facet 连接

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

通过活性表面生长机制合成基片束缚金纳米线

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

直接溶液还原法快速合成金、钯、铂气凝胶的研究

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...