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.     

Structural,Thermal and Magnetic Properties of Thin Metal Films and Adsorbate–Substrate Systems Studied by XAFS and XMCD

Thin metal films often exhibit interesting properties that are essentially different from the bulk ones. XAFS (X-ray absorption fine structure) and XMCD (X-ray magnetic circular dichroism) techniques are quite suitable to investigate structural, thermal and magnetic properties of thin metal films. In this proceeding, we will present following two topics concerning structural and magnetic properties of adsorbates on thin metal films. The first one is the adsorption geometry of SO₂ on a 1-monolayer (ML) Pd thin film grown on a Ni(111) single crystal. It was found by S K-edge XAFS that SO₂ is lying flat on 1-ML Pd/Ni(111). This result is not similar to the bulk Pd surface but to the bulk Ni one. This finding indicates significant modification of the electronic structure of the 1-ML Pd film compared to the bulk one. The second topic is the magnetic moment induced on CO adsorbed on Ni epitaxial films grown on Cu(001). The O K-edge XMCD results revealed that in the perpendicularly magnetized 10-ML Ni film the orbital moment of CO is parallel to the substrate Ni magnetization, while it is antiparallel in the in-planar magnetized 6-ML and thick (>100 ML) films. The origin of the induced orbital moment at CO is discussed.     

Dietary conjugated linolenic acid in relation to CLA differently modifies body fat mass and serum and liver lipid levels in rats

The present study compared the effect of dietary conjugated linolenic acid (CLNA) on body fat and serum and liver lipid levels with that of CLA in rats. FFA rich in linoleic acid, α-linolenic acid, CLA, or CLNA were used as experimental fats. Male Sprague-Dawley rats (4 wk old) were fed purified diets containing 1% of one of these experimental fats. After 4 wk of feeding, adipose tissue weights, serum and liver lipid concentrations, serum tumor necrosis factor (TNF)-α and leptin levels, and hepatic β-oxidation activities were measured. Compared with linoleic acid, CLA and, more potently, CLNA were found to reduce perirenal adipose tissue weight. The same trend was observed in the weight of epididymal adipose tissue. CLNA, but not CLA, was found to significantly increase serum and liver IG concentrations. Serum FFA concentration was also increased in the CLNA group more than in the other groups. The activity of β-oxidation in liver mitochondria and peroxisomes was significantly higher in the CLNA group than in the other groups. Thus, the amount of liver TG exceeded the ability of hepatic β-oxidation. Significant positive correlation was found between the adipose tissue weights and serum leptin levels in all animals (vs. perirenal: r=0.557, P<0.001; vs. epididymal: r=0.405, P<0.05). A less significant correlation was found between adipose tissue weights and serum TNF-α level (vs. perirenal: r=0.069, P<0.1; vs. epididymal: r=0.382, P<0.05). Although the mechanism for the specific effect of CLNA is not clear at present, these findings indicate that in rats CLNA modulated the body fat and TG metabolism differently from CLA.     

New class of cellulose fiber spun from the novel solution of cellulose by wet spinning method

A novel cellulose solution, prepared by dissolving an alkali-soluble cellulose, which was obtained by the steam explosion treatment on almost pure natural cellulose (soft wood pulp), into the aqueous sodium hydroxide solution with specific concentration (9.1 wt %) was employed for the first time to prepare a new class of multifilament-type cellulose fiber. For this purpose a wet spinning system with acid coagulation bath was applied. The mechanical properties and structural characteristics of the resulting cellulose fibers were compared with those of regenerated cellulose fibers such as viscose rayon and cuprammonium rayon commercially available. X-ray analysis shows that the new cellulose fiber is crystallographically cellulose II, and its crystallinity is higher but its crystalline orientation is slightly lower than those of other commercial regenerated fibers. The degree of breakdown of intramolecular hydrogen bond at C₃[X_am(C₃)] of the cellulose fiber, as determined by solid-state cross-polarization magic-angle sample spinning (CP/MAS) ¹³C NMR, is much lower than other, and the NMR spectra of its dry and wet state were significantly different from each other, indicating that cellulose molecules in the new cellulose fiber are quite mobile when wet. This phenomenon has not been reported for so-called regenerated cellulose fibers.     

ARCOR,a new photolithography technique with antireflective coating on resist

The multiple interference effect is one of the major causes of the fluctuation in critical dimension control (CD) and in mark detection for alignment. Suppressing this effect is critical for future photolithography. We propose a new photolithography technique called anti reflective coating on resist (ARCOR), which improves linewidth accuracy and overlay accuracy by suppressing multiple interference. ARCOR consists of relatively simple processes: A clear antireflective film is spun onto the resist prior to the mark detecting for alignment and exposure. The film is subsequently removed and the resist developed in the conventional way. ARCOR differs from ARC, which suppresses the reflection at the resist/substrate interface. ARCOR suppresses the reflection at the air/resist interface. ARCOR allows mark detection and exposure without light intensity-loss and multiple interference. The experiments mainly examine polysiloxane and perfluoroalkylpolyether as ARCOR materials. It is shown that linewidth accuracy can be improved from 0.3 to 0.03 μm. The signal-to-noise ratio of the alignment signal is drastically improved, and the overlay error is about half that of the conventional method. ARCOR is also effective for directly measuring the reflectivity at the resist/substrate interface, which is a key parameter of the multiple interference effect and the halation. Using ARCOR and a thin resist film, the measured ratio of reflected light to incident light indicates the reflectivity at the resist/substrate interface. Because, the probe light does not reflect off the resist surface and the intensity-loss at the resist surface is suppressed. With perfluoroalkylpolyether film, the measurement error is ～ 1.5%.     

Automated Synthesis of (rac)‐, (R)‐, and (S)‐[18F]Epifluorohydrin and Their Application for Developing PET Radiotracers Containing a 3‐[18F]Fluoro‐2‐hydroxypropyl Moiety

To introduce the 3‐[¹⁸F]fluoro‐2‐hydroxypropyl moiety into positron emission tomography (PET) radiotracers, we performed automated synthesis of (rac)‐, (R)‐, and (S)‐[¹⁸F]epifluorohydrin ([¹⁸F] 1 ) by nucleophilic displacement of (rac)‐, (R)‐, or (S)‐glycidyl tosylate with ¹⁸F^? and purification by distillation. The ring‐opening reaction of (R)‐ or (S)‐[¹⁸F] 1 with phenol precursors gave enantioenriched [¹⁸F]fluoroalkylated products without racemisation. We then synthesised (rac)‐, (R)‐, and (S)‐ 2‐{5‐[4‐(3‐[¹⁸F]fluoro‐2‐hydroxypropoxy)phenyl]‐2‐oxobenzo[d]oxazol‐3(2H)‐yl}‐N‐methyl‐N‐phenylacetamide ([¹⁸F] 6 ) as novel radiotracers for the PET imaging of translocator protein (18 kDa) and showed that (R)‐ and (S)‐[¹⁸F] 6 had different radioactivity uptake in mouse bone and liver. Thus, (rac)‐, (R)‐, and (S)‐[¹⁸F] 1 are effective radiolabelling reagents and can be used to develop PET radiotracers by examining the effects of chirality on their in vitro binding affinities and in vivo behaviour.     

Thermodynamic Properties of Ionic Semiclathrate Hydrate Formed with Tetrabutylammonium Propionate

The phase equilibrium temperature and dissociation heat of tetrabutylammonium propionate (TBAPr) hydrate are reported. TBAPr hydrate is a type of ionic semiclathrate hydrates and also could potentially be used as thermal energy storage material. The temperature‐composition phase diagram of the TBAPr hydrate was determined in a defined range of mass fractions. Considering the dissociation heat of differential scanning calorimetry (DSC) measurements, multiple peaks of heat flow were observed in the TBAPr‐water system at the TBAPr mass fraction lower than 0.35, and there was a single peak at the mass fraction higher than 0.37.     

Effects of compressive strain on the evolution of interfacial strength of steel/nickel solid-state bonding at low temperature

Solid-state bonding between ultralow-carbon steel and pure nickel was conducted by hot pressing with various compressive strain ranging from 5 to 15% and subsequent isothermal holding at 923?K. It was found that the interfacial strength of contact area is accounted for by the evolution of the intrinsic strength of the interface and the amount of plastic energy dissipation at the crack tip during interface fracture. The compression induces severe deformation around the interface and consequently inhibits the plastic energy dissipation during interface fracture. In the first stage of isothermal holding, the residual strain around the interface on the steel side is reduced by recovery process, which concurrently decreases in the yield stress of the area adjacent to the interface. This promotes plastic energy dissipation of the area, leading to a significant increase in interfacial strength in the first stage.     

High-efficiency finishing process for metal mold by large-area electron beam irradiation

A new finishing process for metal molds by large-area electron beam (EB) irradiation is proposed in this study. In the large-area EB irradiation equipment used here, an EB with high-energy density is irradiated without focusing the beam, and so the EB with a maximum diameter of 60 mm can be used for melting or evaporating metal surface instantly. Experimental results show that the surface roughness decreases from 6 μmRz to less than 1 μmRz in just a few minutes under proper machining conditions. The corrosion resistance of metal mold surface also could be greatly improved by large-area EB irradiation. Furthermore, the surface roughness of tilting surface close to 90° could be well improved. Therefore, large-area EB irradiation method has a possibility to become a high-efficiency finishing process for metal molds.