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>Prepare the gold(III) chloride aqueous solution by dissolving 0.1050 g of gold(III) tetrachloride trihydrate (HAuCl4&#8226; 3H2O) in 10 ml of water to give 25 mM HAuCl4.</li>
	<li>Prepare the sodium borohydride aqueous solution by dissolving 0.03844 g of sodium tetrahydroborate (NaBH4) in 10 ml of water to give 100 mM NaBH4.</li>
	<li>Prepare the 2-ammoniumethanethiol aqueous solution by dissolving 0.2985 g of 2-ammoniumethanethiol chloride salt (2-AET+) in 25 ml of water to give 100 mM 2-AET+.</li>
</ol>
2. Synthesis of TNS Colloidal Suspensions
NOTE: Titania nanosheets (TNS; Ti0.91O2) were prepared according to the well-established procedure reported previously22,23,30.
<ol>
	<li>Prepare the starting material of layered cesium titanate Cs0.7Ti1.825O4 by calcining a stoichiometric mixture of Cs2CO3 (0.4040 g) and TiO2 (ST-01; 0.5000 g) at 800 &#176;C for 20 hr22. Repeat this twice.</li>
	<li>Prepare the protonated layered titanate (H0.7Ti1.825O4&#183;H2O) by repeatedly treating 0.8142 g of cesium titanate with an HCl (100 mM, 81.42 ml) aqueous solution by using a shaker (300 Hz) for 12 hr.</li>
	<li>Prepare the exfoliated layered titanate (TNS) colloidal suspensions by stirring the protonated titanate powder (0.0998 g) vigorously (500 rpm) with 25 ml of a 17 mM tetrabutylammonium hydroxide (TBA+ OH&#8722;) aqueous solution for about 2 weeks at ambient temperature under dark conditions. The resulting opalescent suspension contains exfoliated titania nanosheets (TNS; 1.4 g/L, pH = 11~12).</li>
</ol>
3. Synthesis of TNS Films21
<ol>
	<li>Preparation of TNS cast films (c-TNS)
	<ol>
		<li>Pre-clean glass substrates (~20 x 20 mm2) through ultrasonic treatments using an ultrasonic cleaner (27 kHz) in 1 M aqueous sodium hydroxide (NaOH) for 30 min.</li>
		<li>Rinse the substrates with 5-10 mL of ultrapure water (&#60;0.056 &#181;S cm-1).</li>
		<li>Dip a glass substrate in a 0.1 M aqueous hydrochloric acid (HCl) for 3 min and rinse with 5-10 ml of ultrapure water.</li>
		<li>Clean the substrates through ultrasonic treatments (27 kHz) in pure water for 1 hr, and then rinse with pure water. Dry with a hairdryer for 2-3 min (until dry).</li>
		<li>Cast the colloidal suspension of TNS on the glass substrate in 300 &#181;l aliquots.</li>
		<li>Dry at 60 &#176;C for 2 hr using a dry oven to give the c-TNS film.</li>
	</ol>
	</li>
	<li>Preparation of Sintered TNS Film (s-TNS)
	<ol>
		<li>To achieve thermal fixation of the TNS components on the glass substrate (s-TNS film), sinter the obtained c-TNS film in air at 500 &#176;C for 3 hr (heating from 25 to 500 &#176;C at a rate of 6.8 &#176;C/min) using the oven.</li>
		<li>Repeat the sintering process twice.</li>
	</ol>
	</li>
	<li>Preparation of Films
	<ol>
		<li>When the s-TNS films are immersed in solution, position the deposited s-TNS film so that it faces the top for all experimental procedures.</li>
		<li>Carry out all experiments under dark conditions by covering the setup with aluminum foil to avoid the photoreaction of TNS.</li>
	</ol>
	</li>
	<li>Preparation of Methyl Viologen (MV2+) Intercalated TNS Films (TNS/MV2+)
	<ol>
		<li>Immerse an s-TNS film in an aqueous solution of MV2+ dichloride salt (0.2 mM, 3 ml) in a Petri dish for 7 h at room temperature (RT) under dark conditions.</li>
		<li>Rinse the obtained samples with ultrapure water (5-10 ml) and dry in air at 60 &#176;C using an oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Preparation of Au(III) Intercalated TNS Films (TNS/Au(III))
	<ol>
		<li>Immerse a TNS/MV2+ film in an aqueous solution of HAuCl4 (25 mM, 3 ml) in a Petri dish for 3 hr at RT under dark conditions.</li>
		<li>Rinse the obtained samples with ultrapure water (5-10 ml) and dry in air at 60 &#176;C using an oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Synthesis of AuNP within the Interlayer Space of TNS Films (TNS/AuNP)
	<ol>
		<li>Immerse a TNS/Au(III) film in an aqueous solution of NaBH4 (0.1 M, 5 ml) in a Petri dish for 0.5 hr at RT under dark conditions.</li>
		<li>Dry the obtained films in air at 60 &#176;C using an oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Preparation of 2-AET+ Intercalated TNS Films (TNS/2-AET+)
	<ol>
		<li>Immerse an s-TNS film in an aqueous solution of 2-AET+ Cl&#8722; (0.1 M, 3 ml) in a Petri dish for 24 hr at RT.</li>
		<li>Rinse obtained films with ultrapure water (5-10 ml) and dry in air at 60 &#176;C using an oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Au(III) and 2-AET+ Co-Intercalated TNS Films (TNS/2-AET+/Au(III)).
	<ol>
		<li>Immerse a TNS/2-AET+ film in an aqueous solution of HAuCl4 (25 mM, 3 ml) for 3 h at RT.</li>
		<li>Rinse the obtained films with ultrapure water (5-10 ml) and dry in air at 60 &#176;C using an oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Synthesis of AuNP within the Interlayer Space of TNS/2-AET+ Films (TNS/2-AET+/AuNP).
	<ol>
		<li>Immerse a TNS/2-AET+/Au(III) film in an aqueous solution of NaBH4 (0.1 M, 5 ml) in a Petri dish for 0.5 hr at RT under dark conditions.</li>
		<li>Rinse the obtained films with ultrapure water (5-10 ml) and dry in air at 60 &#176;C using oven in the dark for ~1 hr.</li>
	</ol>
	</li>
	<li>Characterizations
	<ol>
		<li>Carry out X-ray diffraction (XRD) analyses21 using a desktop X-ray diffractometer with monochromatized Cu-K&#945; radiation (&#955; = 0.15405 nm), operated at 30 kV and 15 mA.</li>
		<li>Take energy dispersive X-ray spectrometry (EDS) spectra21.</li>
		<li>Employ a multichannel photodetector or steady-state ultraviolet-visible (UV-Vis) absorption spectrophotometer to record UV-Vis absorption spectra for the prepared samples using transmittance mode21.</li>
	</ol>
	</li>
</ol>

We have nothing to disclose.

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.

<table border="0" cellpadding="0" cellspacing="0" width="979">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<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>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</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 ...

in-situ-synthesis-gold-nanoparticles-without-aggregation-interlayer

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

8.0K Views.  Niigata University. 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.

Video: In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Synthesis and Functionalization of Nitrogen-doped Carbon Nanotube Cups with Gold Nanoparticles as Cork Stoppers

Nitrogen-doped carbon nanotubes consist of many cup-shaped graphitic compartments termed as nitrogen-doped carbon nanotube cups (NCNCs). These as-synthesized graphitic nanocups from chemical vapor deposition (CVD) method were stacked in a head-to-tail fashion held only through noncovalent interactions. Individual NCNCs can be isolated out of their stacking structure through a series of chemical and physical separation processes. First, as-synthesized NCNCs were oxidized in a mixture of strong acids to introduce oxygen-containing defects on the graphitic walls. The oxidized NCNCs were then processed using high-intensity probe-tip sonication which effectively separated the stacked NCNCs into individual graphitic nanocups. Owing to their abundant oxygen and nitrogen surface functionalities, the resulted individual NCNCs are highly hydrophilic and can be effectively functionalized with gold nanoparticles (GNPs), which preferentially fit in the opening of the cups as cork stoppers. These graphitic nanocups corked with GNPs may find promising applications as nanoscale containers and drug carriers.

We discussed the synthesis of individual graphitic nanocups using a series of techniques including chemical vapor deposition, acid oxidation and probe-tip sonication. By citrate reduction of HAuCl4, the graphitic nanocups were effectively corked with gold nanoparticles due to the chemically reactive edges of the cups.

Nitrogen-doped carbon  nanotubes consist of many cup-shaped graphitic compartments termed as  nitrogen-doped carbon nanotube cups (NCNCs).  These ...

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Fabrication and Characterization of Superconducting Resonators

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors (MKIDs) for the detection of faint astrophysical signatures, as well as for quantum computing applications and materials characterization. In this paper, procedures are presented for the fabrication and characterization of thin-film superconducting microwave resonators. The fabrication methodology allows for the realization of superconducting transmission-line resonators with features on both sides of an atomically smooth single-crystal silicon dielectric. This work describes the procedure for the installation of resonator devices into a cryogenic microwave testbed and for cool-down below the superconducting transition temperature. The set-up of the cryogenic microwave testbed allows one to do careful measurements of the complex microwave transmission of these resonator devices, enabling the extraction of the properties of the superconducting lines and dielectric substrate (e.g., internal quality factors, loss and kinetic inductance fractions), which are important for device design and performance.

Superconducting microwave resonators are of interest for detection of light, quantum computing applications and materials characterization. This work presents a detailed procedure for fabrication and characterization of superconducting microwave resonator scattering parameters.

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors ...

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two chalcogenide compositions are demonstrated: Ge23Sb7S70 and As40S60, which have both been studied extensively for planar mid-infrared (mid-IR) microphotonic devices. In this approach, uniform thickness films are fabricated through the use of computer numerical controlled (CNC) motion. Chalcogenide glass (ChG) is written over the substrate by a single nozzle along a serpentine path. Films were subjected to a series of heat treatments between 100 &#176;C and 200 &#176;C under vacuum to drive off residual solvent and densify the films. Based on transmission Fourier transform infrared (FTIR) spectroscopy and surface roughness measurements, both compositions were found to be suitable for the fabrication of planar devices operating in the mid-IR region. Residual solvent removal was found to be much quicker for the As40S60 film as compared to Ge23Sb7S70. Based on the advantages of electrospray, direct printing of a gradient refractive index (GRIN) mid-IR transparent coating is envisioned, given the difference in refractive index of the two compositions in this study.

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

A method of uniform thickness solution-derived chalcogenide glass film deposition is demonstrated using computer numerical controlled motion of a single-nozzle electrospray.

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two ...

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Controllable Nucleation of Cavitation from Plasmonic Gold Nanoparticles for Enhancing High Intensity Focused Ultrasound Applications

In this study, plasmonic gold nanoparticles were simultaneously exposed to pulsed near-infrared laser light and high intensity focused ultrasound (HIFU) for the controllable nucleation of cavitation in tissue-mimicking gel phantoms. This in vitro protocol was developed to demonstrate the feasibility of this approach, for both enhancement of imaging and therapeutic applications for cancer. The same apparatus can be used for both imaging and therapeutic applications by varying the exposure duration of the HIFU system. For short duration exposures (10 &#181;s), broadband acoustic emissions were generated through the controlled nucleation of inertial cavitation around the gold nanoparticles. These emissions provide direct localization of nanoparticles. For future applications, these particles may be functionalized with molecular-targeting antibodies (e.g. anti-HER2 for breast cancer) and can provide precise localization of cancerous regions, complementing routine diagnostic ultrasound imaging. For continuous wave (CW) exposures, the cavitation activity was used to increase the localized heating from the HIFU exposures resulting in larger thermal damage in the gel phantoms. The acoustic emissions generated from inertial cavitation activity during these CW exposures was monitored using a passive cavitation detection (PCD) system to provide feedback of cavitation activity. Increased localized heating was only achieved through the unique combination of nanoparticles, laser light and HIFU. Further validation of this technique in pre-clinical models of cancer is necessary.

This protocol demonstrates the controllable nucleation of cavitation in gel phantoms, through simultaneous exposure to both near-infrared pulsed laser light and high intensity focused ultrasound (HIFU). The cavitation activity can then be used for enhancing imaging and/or therapeutic uses of HIFU.

In this study, plasmonic gold nanoparticles were simultaneously exposed to pulsed near-infrared laser light and high intensity focused ultrasound (HIFU) ...

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 (STO) Single-crystal Substrates

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF) magnetron sputtering. LSMO nanoparticles were deposited with diameters from 10 to 20 nm and heights between 20 and 50 nm. At the same time, (Gd) Ba2Cu3O7&#8722;&#948; ((Gd) BCO) films were fabricated on both undecorated and LSMO nanoparticle decorated STO substrates using RF magnetron sputtering. This report also describes the properties of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 quasi-bilayer films structures (e.g., crystalline phase, morphology, chemical composition); magnetization, magneto-transport, and superconducting transport properties were also evaluated.

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7ÃƒÆ’Ã‚Â¢Ãƒâ€¹Ã¢â‚¬Â 'ÃƒÆ’Ã…Â½ Â´/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 STO Single-crystal Substrates

Here, we present a protocol to grow LSMO nanoparticles and (Gd) BCO films on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF)-sputtering.

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio ...

An Efficient Method for Selective Desalination of Radioactive Iodine Anions by Using Gold Nanoparticles-Embedded Membrane Filter

Here, we demonstrate a detail protocol for the preparation of nanomaterials-embedded composite membranes and its application to the efficient and ion-selective removal of radioactive iodines. By using citrate-stabilized gold nanoparticles (mean diameter: 13 nm) and cellulose acetate membranes, gold nanoparticle-embedded cellulose acetate membranes (Au-CAM) have easily been fabricated. The nano-adsorbents on Au-CAM were highly stable in the presence of high concentration of inorganic salts and organic molecules. The iodide ions in aqueous solutions could rapidly be captured by this engineered membrane. Through a filtration process using an Au-CAM containing filter unit, excellent removal efficiency (&gt;99%) as well as ion-selective desalination result was achieved in a short time. Moreover, Au-CAM provided good reusability without significant decrease of its performances. These results suggested that the present technology using the engineered hybrid membrane will be a promising process for the large-scale decontamination of radioactive iodine from liquid wastes.

An efficient method for the rapid and ion-selective desalination of radioactive iodine in several aqueous solutions is described by using gold nanoparticles-immobilized cellulose acetate membrane filters.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

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Electrospray Deposition of Uniform Thickness Ge₂₃Sb₇S₇₀ and As₄₀S₆₀ Chalcogenide Glass Films

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Controllable Nucleation of Cavitation from Plasmonic Gold Nanoparticles for Enhancing High Intensity Focused Ultrasound Applications

Radio Frequency Magnetron Sputtering of GdBa₂Cu₃O₇₋_δ/ La_0.67Sr_0.33MnO₃ Quasi-bilayer Films on SrTiO₃ (STO) Single-crystal Substrates

An Efficient Method for Selective Desalination of Radioactive Iodine Anions by Using Gold Nanoparticles-Embedded Membrane Filter