Name: in situ synthesis of gold nanoparticles without aggregation in the interlayer space of layered titanate transparent films
Uploaded: 2017-01-17T14:00:00
Description: Watch this Scientific Journal Video about In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films at JoVE.com

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).

Caution: Always use caution when working with chemicals and solutions. Follow the appropriate safety practices and wear gloves, glasses, and a lab coat at all times. Be aware that nanomaterials may have additional hazards as compared to their bulk counterpart.
1. Preparation of Regents
<ol>
	<li>Prepare the methyl viologen aqueous solution by dissolving 0.0012 g of 1,1&#39;-dimethyl-4,4&#39;-bipyridinium dichloride (methyl viologen; MV2+) in 20 ml of water to give 0.2 mM MV2+.</li>
	<li>Pre...

This manuscript provides a detailed protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of TNS films. This is the first report of the in situ synthesis of AuNPs within the interlayer space of TNS. Moreover, we found that the 2-AET+ works as an effective protective reagent for AuNPs within the interlayer of TNS. These methods hybridized AuNPs and TNS transparent films. TNS films with good optical transparency21 were synthesized through sinter...

Various noble metal nanoparticles (MNPs) exhibit characteristic colors or tones due to their localized surface plasmon resonance (LSPR) properties; thus, MNPs can be used in various optical and/or photochemical applications1-4. Recently, combinations of metal oxide semiconductor (MOS) photocatalysts, such as titanium oxide (TiO2) and MNPs, have been thoroughly investigated as new types of photocatalysts5-14. However, in many cases, very small amounts of MNPs exist on the MOS surface, because most MOS particles have relatively low surface areas. On the other hand, layered metal oxide semiconductors (LMOSs) exhibit photocatalytic properties and have a large surface area, typically several hundred square meters per unit g of an LMOS15-17. In addition, various LMOSs have intercalation properties (i.e., various chemical species can be accommodated within their expandable and large interlayer spaces)15-20. Thus, with a combination of MNPs and LMOSs, it is expected that relatively large amounts of MNPs are hybridized with the semiconductor photocatalysts.
We have reported the first in situ synthesis of copper nanoparticles (CuNPs)21 within the interlayer space of LMOS (titania nanosheet; TNS16-30) transparent films through very simple steps. However, the details of the synthetic procedures and the characterization of the other noble MNPs and TNS hybrids have not yet been reported. Moreover, the CuNPs within the TNS layers were easily oxidized and decolorized under ambient conditions21. As such, we focused on gold nanoparticles (AuNPs), because AuNPs are widely used for various optical, photochemical, and catalytic applications, and it is expected that they will be relatively stable against oxidation3-5,7,8,10-14,28,31,32. Here, we report the synthesis of AuNPs within the interlayer space of TNS and show that 2-ammoniumethanethiol (2-AET+; Figure 1 inset) works effectively as a protective reagent for AuNPs within the interlayer of TNS.

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		<tr height="22">
			<td height="22" style="height:22px;width:295px;">Methyl viologen dichloride</td>
			<td style="width:173px;">Aldrich Chemical&#160; Co., Inc.</td>
			<td style="width:124px;">1910-42-5</td>
			<td style="width:388px;"></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">Tetrabutylammonium hydroxide</td>
			<td>TCI</td>
			<td>T1685</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">cesium carbonate</td>
			<td>Kanto Chemical Co., Inc.</td>
			<td>07184-33</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">anatase titanium dixoide</td>
			<td>Ishihara Sangyo Ltd.</td>
			<td>ST-01</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">hydrochloric acid</td>
			<td>Junsei Chemical Co., Ltd.</td>
			<td>20010-0350</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">sodium hydroxide</td>
			<td>Junsei Chemical Co., Ltd.</td>
			<td>195-13775</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">Tetrachloroauric(III) acid trihydrate</td>
			<td>Kanto Chemical Co., Inc.</td>
			<td>17044-60</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">sodium tetrahydroborate</td>
			<td>Junsei Chemical Co., Ltd.</td>
			<td>39245-1210</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;">2-ammoniumethanethiol hydrochloride</td>
			<td>TCI</td>
			<td>A0296</td>
			<td></td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;">Ultrapure water (0.056 &#181;S/cm)</td>
			<td></td>
			<td></td>
			<td>Milli-Q water purification system (Direct-Q&#174; 3UV, Millipore)</td>
		</tr>
		<tr height="22">
			<td>Microscope slide (Thickness : 1.0&#8764;1.2 mm)</td>
			<td>Matsunami glass Co., Ltd.</td>
			<td></td>
			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
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</table>

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.

Two types of precursor films were used in this study (i.e., with and without the protective reagent (2-AET+) within the interlayer of TNS). In the absence of 2-AET+, 1,1&#39;-dimethyl-4,4&#39;-bipyridinium dichloride (methyl viologen; MV2+) was used as an expander of the interlayer space, because MV2+-containing LMOSs have been frequently used as intermediates in the guest exchange method for preparing LMOSs16,17,21,33-36.</p...

Watch this Scientific Journal Video about In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films at JoVE.com

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.

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 ...

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