Hydrothermal synthesis and in situ surface modification of boehmite nanoparticles in supercritical water

In situ surface modification of boehmite (AlOOH) nanoparticles during hydrothermal synthesis in supercritical water was examined by adding CH₃(CH₂)₄CHO and CH₃(CH₂)₅NH₂ as modifier reagents to the reactants. Changes in surface properties of the nanoparticles by surface modification was observed by FTIR, dispersion in solvents and TEM analyses, which demonstrated that reagents chemically binded onto the surface of the AlOOH nanoparticles. The results of SEM and TEM pictures show that the surface modification affects crystal growth and reduces the particle size and changes the morphology of the particles.     

Supercritical hydrothermal synthesis of organic-inorganic hybrid nanoparticles

We have developed supercritical hydrothermal synthesis method of metal oxide nanoparticles where metal salt aqueous solution is mixed with high temperature water to rapidly increase the temperature of the metal salt solution and thus reduce the reactions and crystallizations during the heating up period. By using this method, we succeeded in the continuous and rapid production of metal oxide nanocrystals. A new method proposes to synthesize organic-inorganic fused materials based on the methods of supercritical hydrothermal synthesis. By introducing organic materials in a reaction atmosphere of supercritical hydrothermal synthesis, we successfully synthesized metal oxide nanoparticles whose surface was modified with organic materials. In supercritical state, water and organic materials form a homogeneous phase, which provides an excellent reaction atmosphere for the organic modification of nanoparticles. Modification with bio-materials including amino acids was also possible. By changing organic modifiers, particle morphology and crystal structure were changed. This organic surface modification provides a various unique characteristics for the nanoparticles: Dispersion of nanoparticles in aqueous solutions, organic solvents or in liquid polymers can be controlled by selecting hydrophilic or hydrophobic modifiers.     

Synthesis of iron nanoparticle: Challenge to determine the limit of hydrogen reduction in supercritical water

Supercritical hydrothermal syntheses of metal nanoparticles were investigated. Organic metal salt and hydrogen gas produced by water catalyzed decomposition of formic acid was employed as metal sources and reduction agent, respectively. The formation of iron was verified by measuring the magnetic property of the products by superconducting quantum interference device (SQUID) magnetometer as well as crystallographic analysis by X-ray diffraction (XRD). As predicted by the free energy calculation of reduction of metal oxides by hydrogen molecule, silver, palladium, copper, nickel and cobalt nanoparticles were synthesized without using surface modifier, whereas, iron could be synthesized at small yield. The main product was iron oxides (mainly magnetite). In order to increase the yield of iron, hexanoic acid was employed as an in situ surface modifier of the synthesis. The surface modification lessened the size of the synthesized nanoparticles and increased the yield of iron. The optimum condition for iron synthesis was also investigated, as a result, 7.6% yield of iron was achieved.     

Hydrothermal synthesis of surface-modified iron oxide nanoparticles

We synthesized surface-modified iron oxide nanoparticles in aqueous phase by heating an aqueous solution of iron sulfate (FeSO₄) at 473 K with a small amount of either n-decanoic acid (C₉H₁₉COOH) or n-decylamine (C₁₀H₂₁NH₂), which is not miscible with water at room temperature. Transmission electron microscopy showed that the addition of n-decanoic acid or decylamine changed the shape of the obtained nanoparticles. X-ray diffraction spectra revealed that the synthesized nanoparticles were in α-Fe₂O₃ or Fe₃O₄ phase while Fourier transform infrared spectroscopy and thermogravimetry indicated the existence of an organic layer on the surface of the nanoparticles. In the synthetic condition, decreased dielectric constant of water at higher temperature increased the solubility of n-decanoic acid or n-decylamine in water to promote the reaction between the surface of iron oxide nanoparticles and the organic reagents. After the synthesis, the used organic modifiers separated from the aqueous phase at room temperature, which may help the environmentally benign synthesis of surface-modified metal oxide nanoparticles.     

On the heat removal characteristics and the analytical model of a thermal energy storage capsule using gelled Glauber's salt as the PCM

An analytical and experimental investigation was performed on a heat removal process of the thermal energy storage (TES) capsule, using gelled Glauber's salt. Transient heat flux at the capsule wall was measured for various cooling conditions. In cases where the initial temperature was lower than the saturation temperature of the phase change material (PCM), numerical analyses were performed, approximating the process by a relaxation phenomenon where crystals grew around crystal nuclei. The results of the numerical solution agreed very well with the experimental results.     

Temperature control for the expansion of artificial DNA motif

The DNA, which forms a double helical conformation by the highly selective base-pairing rule with the width of 2 nm, is one of the polymers utilized as a template for nanoparticle assembly. Then, holiday junction structure, where two different DNA double strands intersect and replace each complement strand, is an important artificial motif for forming two-dimensional mesh-like DNA morphology. In this study, the two-dimensional sheet with the mesh-like conformation is formed and the growth of the DNA morphology is controlled by changing the temperature in the formation process. The influence of the cooling procedure on the formation process of the two-dimensional DNA sheet is observed by atomic force microscope, and the formation of double strands in the process is traced by absorption spectra. The spectroscopic results demonstrate that the two-dimensional DNA sheet is strongly dependent on the correlation between the applied cooling process and the melting temperature of double helical conformation, and that the growth of the two-dimensional DNA sheet can be manipulated by the cooling procedure. Further, we will show the size control of the DNA sheet by mixing the designed DNA which inhibits the growth of the DNA sheet.