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Chemie

通过表面等离子体激发将 Pd 光沉积到胶体 Au 纳米棒上

Published: August 15, 2019
doi:
10.3791/60041
, , , , , ,
1Sensors & Electron Devices Directorate,U.S. Army Research Laboratory, 2General Technical Services

Summary

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。

Abstract

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。

Introduction

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)。

Protocol

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 …

Representative Results

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…

Discussion

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、…

Offenlegungen

The authors have nothing to disclose.

Acknowledgements

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。

Materials

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

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Tags

Keyword Extraction:PhotodepositionPdColloidal Au NanorodsSurface Plasmon ExcitationReductive Plasmonic PhotodepositionEpitaxial Metal GrowthPlatinumSilverCatalytic ApplicationsHydrochloric AcidPalladium(II) ChlorideGold NanorodCetyltrimethyl Ammonium BromideMethanolDihydrogen TetrochloropallidateTungsten-halogen Lamp

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Forcherio, G. T., Baker, D. R., Leff, A. C., Boltersdorf, J., McClure, J. P., Grew, K. N., Lundgren, C. A. Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation. J. Vis. Exp. (150), e60041, doi:10.3791/60041 (2019).
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