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Summary
Abstract
Introduction
Protocol
Resultados
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In Situ Síntesis de nanopartículas de oro sin agregación en el espacio entre capas de Capas de titanato películas transparentes

Published: January 17, 2017
doi:
10.3791/55169
, , , , ,
1Department of Material Science and Technology, Faculty of Engineering,Niigata University

Summary

A continuación, se presenta un protocolo para la síntesis in situ de nanopartículas de oro (AuNPs) dentro del espacio de capa intermedia de películas titanato estratificado sin la agregación de AuNPs. No se observó cambio espectral incluso después de 4 meses. El material sintetizado se espera que las aplicaciones en catálisis, fotocatálisis, y el desarrollo de dispositivos plasmónicas rentables.

Abstract

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.

Introduction

Varios nanopartículas de metales nobles (MNPS) presentan colores o tonos característicos debido a su resonancia de plasmones superficiales (localizada) LSPR propiedades; Por lo tanto, MNPs pueden ser utilizados en diversas aplicaciones / fotoquímicos ópticos y o 1-4. Recientemente, combinaciones de semiconductor de óxido metálico (MOS) fotocatalizadores, tales como óxido de titanio (TiO 2) y MNPs, se han investigado a fondo como nuevos tipos de fotocatalizadores 5-14. Sin embargo, en muchos casos, cantidades muy pequeñas de MNPs existir en la superficie MOS, porque la mayoría de las partículas de MOS tienen áreas superficiales relativamente bajas. Por otro lado, en capas de semiconductores de óxido de metal (LMOSs) exhiben propiedades fotocatalíticas y tienen un área superficial grande, típicamente de varios cientos de metros cuadrados por unidad g de un OVM 15-17. Además, varios LMOSs tienen propiedades de intercalación (es decir, varias especies químicas se pueden acomodar dentro de sus espacios entre capas expandibles y grandes) 15-20. Por lo tanto, con una combinación de MNPs y LMOSs, se espera que cantidades relativamente grandes de MNPs se hibridan con los fotocatalizadores semiconductores.

Nos han informado de la primera síntesis in situ de nanopartículas de cobre (21) CuNPs dentro del espacio de capa intermedia de OVM (óxido de titanio nanosheet; TNS 16-30) películas transparentes a través de pasos muy sencillos. Sin embargo, aún no se ha informado de los detalles de los procedimientos de síntesis y la caracterización de los otros híbridos MNPs y TNS nobles. Por otra parte, los CuNPs dentro de las capas de TNS se oxidaron fácilmente y se decolora en condiciones ambientales 21. Como tal, nos centramos en las nanopartículas de oro (AuNPs), porque AuNPs son ampliamente utilizados para diversos óptica, fotoquímico, y aplicaciones catalíticas, y se espera que sean relativamente estable frente a la oxidación 3-5,7,8,10-14 , 28,31,32. Aquí, se presenta la síntesis de AuNPs dentro del espacio de capa intermedia de TNS y mostrar tha2 t-ammoniumethanethiol (2-AET +; Figura 1 recuadro) funciona efectivamente como un reactivo de protección para AuNPs dentro de la capa intermedia de TNS.

Protocol

Precaución: Siempre tenga cuidado cuando se trabaja con productos químicos y soluciones. Siga las prácticas de seguridad apropiadas y usar guantes, gafas y una bata de laboratorio en todo momento. Tenga en cuenta que los nanomateriales pueden tener riesgos adicionales en comparación con su contraparte mayor. 1. Preparación de Regentes Preparar la solución de metil viológeno acuosa mediante la disolución de 0,0012 g de dicloruro de 1,1'-dimetil-4,4'-bipiridinio (metil viológeno; MV <su…

Representative Results

Se utilizaron dos tipos de películas precursoras en este estudio (es decir, con y sin el reactivo de protección (2-AET +) dentro de la capa intermedia de TNS). En ausencia de 2-AET +, 1,1'-bipiridinio-dimetil-4,4' dicloruro de (viológeno de metilo; MV 2 +) se usó como un expansor del espacio entre capas, porque MV 2 + que contienen LMOSs haber sido se utiliza con frecuencia como intermedios en el método de intercambio de i…

Discussion

Este manuscrito proporciona un protocolo detallado para la síntesis in situ de nanopartículas de oro (AuNPs) dentro del espacio entre capas de las películas de TNS. Este es el primer informe de la síntesis in situ de AuNPs dentro del espacio entre capas de TNS. Por otra parte, se encontró que la 2-AET + funciona como un reactivo de protección eficaz para AuNPs dentro de la capa intermedia de TNS. Estos métodos se hibridan AuNPs y TNS películas transparentes. TNS películas con buena …

Declarações

The authors have nothing to disclose.

Acknowledgements

This work was partly supported by Nippon Sheet Glass Foundation for Materials Science and Engineering and JSPS KAKENHI (Grant-in-Aid for Challenging Exploratory Research, #50362281).

Materials

Methyl viologen dichloride Aldrich Chemical  Co., Inc. 1910-42-5
Tetrabutylammonium hydroxide TCI T1685
cesium carbonate Kanto Chemical Co., Inc. 07184-33
anatase titanium dixoide Ishihara Sangyo Ltd. ST-01
hydrochloric acid Junsei Chemical Co., Ltd. 20010-0350
sodium hydroxide Junsei Chemical Co., Ltd. 195-13775
Tetrachloroauric(III) acid trihydrate Kanto Chemical Co., Inc. 17044-60
sodium tetrahydroborate Junsei Chemical Co., Ltd. 39245-1210
2-ammoniumethanethiol hydrochloride TCI A0296
Ultrapure water (0.056 µS/cm) Milli-Q water purification system (Direct-Q® 3UV, Millipore)
Microscope slide (Thickness : 1.0∼1.2 mm) Matsunami glass Co., Ltd.
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Tags

Gold NanoparticlesLayered TitanateTransparent FilmsNanostructured HybridsMetal NanoparticlesRadial SemiconductorsPigmentsDyesCatalystsPhotocatalystsNanostructuresIn Situ SynthesisMethyl ViologenTetrachloroauric AcidSodium Borohydride
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Sasaki, K., Matsubara, K., Kawamura, S., Saito, K., Yagi, M., Yui, T. In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films. J. Vis. Exp. (119), e55169, doi:10.3791/55169 (2017).
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