Phase behavior in liquid crystallization for diblock copolymers consisting of rubbery amorphous and side-chain liquid crystalline components

Phase behavior in liquid crystallization was studied for a series of liquid crystalline (LC) diblock copolymers consisting of rubbery amorphous and side-chain liquid crystalline components, poly(n-butyl acrylate) (PBA) and poly[11-(4′-cyanophenyl-4″-phenoxy)undecyl acrylate] (PLC), respectively, using a time-resolved small-angle X-ray scattering (SAXS) techniques, DSC and polarized optical microscopy (POM). The block copolymers used had three kinds of copolymer compositions, 44, 20 and 15 wt% of PLC compositions (BLC44, BLC20 and BLC15, respectively). BLC44 showed a smectic liquid crystalline structure. In the process of liquid crystallization for BLC44, the SAXS peak due to the microphase separation structure existing before liquid crystallization was changed continuously to be at a smaller angular side, and at almost the same time, a new peak appeared at a further smaller angular side and developed. The former peak disappeared with the development of liquid crystallization. The behavior of these SAXS peaks suggests that the microphase separation structure was changed discretely at the transition from isotropic to smectic and that two phases coexist in the early stage of the liquid crystallization. The coexistence of two peaks in the early stage of the liquid crystallization corresponded to the POM observation. In the isotropization process, coexistence of two phases was not observed. For BLC20 exhibiting a cylindrical structure in both isotropic and liquid crystalline states, the liquid crystalline structure was not smectic but probably nematic, and the spacing was changed continuously in liquid crystallization. No liquid crystallization was observed in SAXS, POM and DSC for BLC15. The orientation of smectic layers within lamellar domains was investigated using 2D-SAXS images. The smectic layer was aligned perpendicularly to the lamellar interface.     

Simulation with an improved plasma model utilized to design a new structure of microwave plasma discharge for chemical vapor deposition of diamond crystals

A new structure of microwave plasma for chemical vapor deposition of diamond crystal is proposed. The structure is designed numerically, for which an improved model given in our previous work [H. Yamada et al., J. Appl. Phys. 101 (2007), art. no. 063302.] is utilized. The experimental observations and numerical predictions agree well with each other. It is demonstrated experimentally that the proposed structure can achieve a growth rate larger than 50 μm/h over an area 1 in. in diameter.     

Synthesis of Cubic Boron Nitride from Boron Nitride Synthesized by Pressure Pyrolysis of Borazine

Cubic BN was synthesized under high-temperature and -pressure conditions from BN powder formed by pressure pyrolysis of borazine below 700°C and 100 MPa. The conversion of BN powder to cubic BN was strongly influenced by the residual hydrogen identified by the BH/BN ratio of IR absorption band. The activation energy for cubic BN synthesis from BN powder-20 mol% AIN was 46 kJ/mol, when the starting BN was synthesized at 250°C. A mixture of BN powder and cubic BN particles was converted to cubic BN in a 100% yield by heat treatment at 1800°C and 6.5 GPa without any catalyst. The presence of cubic BN particles does enhance the conversion to cubic BN from BN powder. The energy required for the transformation of starting BN to cubic BN in the presence of cubic BN seed was 355 kJ/mol.     

Self-aligned fabrication of single crystal diamond gated field emitter array

This paper describes a self-aligned fabrication process for diamond gated field emitter array (FEA). Utilizing the non-conformal coverage sputtering conditions of silicon oxide, an interesting “sphere on cone” structure is formed on diamond nano tip array, which is the key point of gate hole opening process. This structure causes shadowing at certain regions of side-wall during Ti / Au gate metal deposition. Removal of “sphere” by wet etching leads to the successful fabrication of a single crystalline diamond gated FEA. Scanning electron microscope observations reveal the fabrication of a uniform emitter array with tip radius of curvature (20 nm) and gate hole (1.4 μm). We also confirmed that no noticeable physical damage exists on tip. In field emission characteristics of the fabricated single crystal diamond gated FEA, gate voltage control of field emission current is realized.     

Rinsing effect of alkaline electrolyzed water on nickel surfaces

The improvement in the surface cleanliness of electroplated nickel by rinsing in alkaline electrolyzed water (AEW) was determined. When the nickel plated sample was rinsed with the AEW, it was found that the amount of residual sulfate ion on the surface of a sample decreased approximately by half compared to one rinsed only with de-ionized pure water. Because nanosize hydrogen bubbles are present in the AEW, and the zeta-potential has a negative value, we then surmised that the mechanism of rinsing was as follows: The sulfate ions are selectively absorbed on the nanosize colloidal hydrogen bubbles, or substituted for anions absorbed on the hydrogen bubbles. The sulfate ions absorbed on the nickel surface then become detached. The detached sulfate ions are absorbed on the surface of the hydrogen bubbles, and negatively charge the hydrogen bubbles. It can be considered that any detached sulfate ions do not re-adhere due to the electrical repulsion force of the negatively charged nickel surface. Thus the sample is efficiently rinsed.     

Synthesis of Ba2NaNb5O15 Powders and Thin Films Using Metal Alkoxides

Transparent and highly oriented Ba₂NaNb₅O₁₅ (BNN) thin films have been prepared by using metal alkoxides. A homogeneous precursor solution was prepared by the controlled reaction of NaOC₂H₅, Nb(OC₂H₅)₅, and barium metal. The BNN precursor included a molecular-level mixture of NaNb(OC₂H₅)₆ and Ba[Nb(OC₂H₅)₆]₂ in ethanol. The alkoxy-derived powder crystallized to a low-temperature phase, and then transformed to orthorhombic BNN (tungsten bronze) at 600°C. BNN precursor films on substrates crystallized to orthorhombic BNN at 800°C via the low-temperature phase. Highly (002) oriented BNN films of tungsten bronze structure were successfully prepared on MgO (100) substrates at 700°C by using BNN underlayer.     

Synthesis and Magneto-mechanical Properties of Ce-TZP/La M-Type Hexaferrite Composite

An in situ composite composed of ceria-stabilized tetragonal zirconia polycrystals (Ce-TZP) and La{Co_0.5Fe_0.5(Fe_0.9Al_0.1)₁₁}O₁₉ was synthesized from a powder mixture of Ce-TZP, La(Fe_0.9Al_0.1)O₃, Fe₂O₃, Al₂O₃, and CoO. The dense Ce-TZP dispersed with platelike La{Co_0.5Fe_0.5(Fe_0.9Al_0.1)₁₁}O₁₉ crystals as a second phase were formed after sintering from 1250° to 1350°C. The saturation magnetization of the in situ composite Ce-TZP/La{Co_0.5Fe_0.5(Fe_0.9Al_0.1)₁₁}O₁₉ was proportional to the mass fraction of the hexaferrite second phase in Ce-TZP. The coercivity of the composite with a 20 mass% of second phase decreased from 9.14 to 2.52 kOe (from 728 to 201 kA/m) after the pulverization of the composite. The susceptibility (χ) increased by 15%–25% under uniaxial stress on the composite. The change of the susceptibility (Δχ/χ) value increased with decreasing the mass fraction of the second phase in the composite. The Δχ was found to increase linearly with applied stress and abruptly change on cracking, which is expected for the application in fracture sensing of the composite.     

Synthesis of High Density and Transparent Forsterite Ceramics Using Nano-Sized Precursors and Their Dielectric Properties

Forsterite (Mg₂SiO₄) ceramics were prepared using Mg(OH)₂ and SiO₂ as precursors, and the effect of powder characteristics of Mg(OH)₂ on calcination and sintering was investigated. The use of highly dispersed Mg(OH)₂ powder (HD powder) resulted in a lower calcination temperature. Forsterite powder of high homogeneity and small particle size prepared from the HD powder enabled synthesis of high-density forsterite ceramics by ordinary sintering without applying external pressure. Moreover, transparent forsterite ceramics were successfully synthesized through addition of excess Mg to the precursors to compensate for Mg evaporated during the sintering process. Subsequent dielectric measurements revealed that the transparent forsterite ceramics had a very low dielectric loss (tan δ<10⁻⁴).     

高质量密度储氢材料-氨基化合物的合成

采用真空蒸发法制备了氨基化锂LiNH2(+2·LiH)薄膜,即首先将Li真空镀膜到金属基板上,然后经氮化、氢化处理合成LiNH2薄膜.此外,真空蒸发法也用于Mg部分置换Li后薄膜的制备.实验结果证明,与传统的粉末状试样相比,薄膜状试样能够在更低的温度下释放出氢气.研究表明采用包括真空蒸发法等非传统方法合成金属络合物储氢材料对进一步提高其储放氢特性具有良好的效果.     

High temperature superconductor micro-superconducting-quantum-interference-device magnetometer for magnetization measurement of a microscale magnet

We have developed a high temperature superconductor (HTS) micrometer-sized dc superconducting quantum interference device (SQUID) magnetometer for high field and high temperature operation. It was fabricated from YBa2Cu3O7-delta of 92 nm in thickness with photolithography techniques to have a hole of 4x9 microm2 and 2 microm wide grain boundary Josephson junctions. Combined with a three dimensional magnetic field coil system, the modulation patterns of critical current Ic were observed for three different field directions. They were successfully used to measure the magnetic properties of a molecular ferrimagnetic microcrystal (23x17x13 microm3), [Mn2(H2O)2(CH3COO)][W(CN)8]2H2O. The magnetization curve was obtained in magnetic field up to 0.12 T between 30 and 70 K. This is the first to measure the anisotropy of hysteresis curve in the field above 0.1 T with an accuracy of 10(-12) J T(-1) (10(-9) emu) with a HTS micro-SQUID magnetometer.