JoVE Journal > Engineering
Summary
Abstract
Introduction
Protocol
Results
Discussion
Disclosures
Acknowledgements
Materials
References
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Engineering

In Situ Synthese van Gold Nanodeeltjes zonder Aggregation in de tussenlaag ruimte van Layered Titanate Transparent Films

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

Summary

Hier presenteren we een protocol voor de in situ synthese van goud nanodeeltjes (AuNPs) binnen de tussenlaag ruimte van gelaagd titanaat films zonder de aggregatie van AuNPs. Geen spectrale verandering werd waargenomen, zelfs na 4 maanden. De gesynthetiseerde materiaal heeft toepassingen in de katalyse, foto-katalyse, en de ontwikkeling van kosteneffectieve plasmonische apparaten verwacht.

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

Diverse edelmetaal nanodeeltjes (MNP) karakteristieke kleuren en tinten als gevolg van hun lokale surface plasmon resonance (LSPR) eigenschappen vertonen; dus kunnen MNP worden gebruikt in verschillende optische en / of fotochemische toepassingen 1-4. Onlangs van metaal- oxide halfgeleider (MOS) fotokatalysatoren, zoals titaanoxide (TiO 2) en MNP's, zijn grondig onderzocht als nieuwe soorten fotokatalysatoren 5-14. In veel gevallen, zeer kleine hoeveelheden MNP's bestaan ​​op de MOS oppervlak, omdat de meeste MOS deeltjes betrekkelijk lage specifieke oppervlakken. Anderzijds, gelaagd metaaloxide halfgeleiders (LMOSs) vertonen fotokatalytische eigenschappen en hebben een groot oppervlak, gewoonlijk enkele honderden vierkante meters per eenheid g van een VLO 15-17. Daarnaast zijn er diverse LMOSs hebben intercalatie eigenschappen (dat wil zeggen, kan verschillende chemische stoffen worden ondergebracht in hun uitbreidbaar en grote tussenlaag spaties) 15-20. Dus, met een combinatie van MNP's en LMOSs wordt verwacht dat betrekkelijk grote hoeveelheden MNP's worden gehybridiseerd met de halfgeleider fotokatalysatoren.

We hebben gemeld de eerste in situ synthese van koper nanodeeltjes (CuNPs) 21 binnen de tussenlaag ruimte van VLO (titania nanosheet; TNS 16-30) transparante films door middel van eenvoudige stappen. De gegevens van de synthetische procedures en karakterisering van de andere edele MNP's en TNS hybriden nog niet gemeld. Bovendien waren de CuNPs binnen de TNS lagen gemakkelijk geoxideerd en ontkleurd onder omgevingsomstandigheden 21. Daarom hebben we ons gericht op gouden nanodeeltjes (AuNPs), omdat AuNPs schaal worden gebruikt voor verschillende optische, fotochemische en katalytische toepassingen, en verwacht wordt dat zij relatief stabiel tegen oxidatie 3-5,7,8,10-14 zal , 28,31,32. Hier melden wij de synthese van AuNPs binnen de tussenlaag ruimte van TNS en show-that 2-ammoniumethanethiol (2-AET + Figuur 1 inzet) werkt effectief als een beschermende reagens voor AuNPs binnen de tussenlaag van TNS.

Protocol

Let op: Wees altijd voorzichtig bij het werken met chemicaliën en oplossingen. Volg de veiligheidsvoorschriften en draag handschoenen, bril en een laboratoriumjas te allen tijde. Wees ervan bewust dat nanomaterialen bijkomende gevaren kunnen hebben in vergelijking met hun bulk tegenhanger. 1. Voorbereiding van Regenten Bereid de methylviologeen waterige oplossing door het oplossen van 0,0012 g 1,1'-dimethyl-4,4'-bipyridiniumdichloride (methylviologeen; MV 2+) in 20 ml water 0,2 mM …

Representative Results

Twee types precursor films werden gebruikt in deze studie (dat wil zeggen met en zonder de beschermende reagens (2-AET +) in de tussenlaag van TNS). Aangezien 2-AET +, 1,1'-dimethyl-4,4'-bipyridiniumdichloride (methylviologeen; MV 2+) werd gebruikt als een uitbreiding van de tussenlaag ruimte, omdat MV 2+ bevattende LMOSs geweest vaak gebruikt als tussenproducten bij de gast ruil werkwijze voor het bereiden LMOSs 16,17,21,…

Discussion

Het manuscript geeft een gedetailleerd protocol voor de in situ synthese van gouden nanodeeltjes (AuNPs) in de tussenlaag ruimte van TNS films. Dit is het eerste verslag van de in situ synthese van AuNPs binnen de tussenlaag ruimte van TNS. Bovendien vonden we dat de 2-AET + werkt als een effectieve beschermende reagens voor AuNPs in de tussenlaag van TNS. Deze methoden gehybridiseerd AuNPs en TNS transparante films. TNS films met goede optische transparantie 21 werden gesynthetis…

Disclosures

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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