Properties of Injectable Apatite-Forming Premixed Cements

Previous studies reported premixed calcium phosphate cements (CPCs) that were stable in the package and form hydroxyapatite (HA) as the product after exposure to an aqueous environment. These cements had setting times of greater than 60 min, which are too long to be useful for some clinical applications. The present study investigated properties of fast-setting HA-forming premixed CPCs that initially consisted of two separate premixed pastes: (1) finely ground (1.0 μm in median size) dicalcium phosphate anhydrous (DCPA) mixed with an aqueous NaH(2)PO(4) solution, 1.5 mol/L or 3.0 mol/L in concentration, and (2) tetracalcium phosphate consisting of combinations of particles of two different size distributions, 5 μm (TTCP5) and 17 μm (TTCP17) in median size, mixed with glycerin. Equal volume of Pastes 1 and 2 were injected with the use of atwo-barrel syringe fitted with a static mixer into sample molds. The molar Ca/P ratio of combined paste was approximately 1.5. Cements were characterized in terms of setting time (Gilmore needle), diametral tensile strength (DTS), and phase composition (powder x-ray diffraction, XRD). Setting times were found to range from (4.3 ± 0.6 to 68 ± 3) min (mean ± sd; n = 3), and 1-d and 7-d DTS values were from (0.89 ± 0.08 to 2.44 ± 0.16) MPa (mean ± sd; n = 5). Both the NaH(2)PO(4) concentration and TTCP particle size distribution had significant (p < 0.01) effects on setting time and DTS. Powder XRD analysis showed that low crystallinity HA and unreacted DCPA were present in the 1-day specimens, and the extent of HA formation increased with increasing amount of TTCP5 in the TTCP paste. CONCLUSION: Injectable HA-forming premixed CPCs with setting times from 4 to 70 min can be prepared by using DCPA and TTCP as the ingredients. Compared to the conventional powder liquid cements, these premixed CPCs have the advantages of being easy to use and having a range of hardening times.     

Profile structure of magnetic flux lines in type-II superconductor from a rectangular electron hologram

Profile magnetic configuration of a quantized flux line and flux-line lattice penetrating a type-II superconductor thin foil, niobium, was observed by electron holography and Lorentz microscopy using a 300 kV field-emission electron microscope. Each single flux line was distributed periodically as lattice structure in the mixed state just below its critical temperature of 8.5 K, while at low temperature of 5 K the flux lines were weakly bound as bundles. In order to observe the flux-line distribution over a wide area, discrete Fourier transform reconstruction in the holography was extended for a rectangular area without loss of information and data precision.     

Electron microscope studies of nano-domain structures in Ru-based magneto-superconductors: RuSr(2)Gd(1.5)Ce(0.5)Cu(2)O(10-delta) (Ru-1222) and RuSr(2)GdCu(2)O(8) (Ru-1212)

Microstructures of the RuSr(2)Gd(1.5)Ce(0.5)Cu(2)O(10-delta) (Ru-1222) and RuSr(2)GdCu(2)O(8) (Ru-1212) magneto-superconductors have been investigated by using selected-area electron diffraction, convergent-beam electron diffraction, dark-field electron microscopy and high-resolution electron microscopy at room temperature. Both Ru-1212 and Ru-1222 consist of nm-size domains stacked along the [Formula: see text] direction, where the domains are formed by two types of superstructures due to ordering of rotated RuO(6) octahedra about the c-axis. In Ru-1212, both primitive-and body-centered tetragonal superstructures (the possible space groups: P4/mbm and I4/mcm) are derived to form the corresponding nm-domains. It is of great interest that Ru-1212 consists of domains of two crystallographically different superstructures, while the similar domains observed in Ru-1222 have crystallographically identical superstructure with an orthorhombic symmetry (possible space group: Aeam), related by 90 degrees rotation around the c-axis (Yokosawa et al., 2003, submitted for publication).     

β-phase transformation and thermoelectric power in FeSi2 and Fe2Si5 based alloys containing small amounts of Cu

The effects of Cu addition on the β phase formation rate and the thermoelectric power in various FeSi₂ and Fe₂Si₅ based alloys was examined. The peritectoid reaction (a+→β) in FeSi₂ alloys was initially enhanced by the addition of Cu but it became slower for longer annealing times. The retained metallic ε was harmful for the thermoelectric power. The inherent thermoelectric properties of (FeSi₂)_99−XMn₁Cu_X (X=0–1.O at.%), (FeSi₂)_99−X Co₁Cu_X (X=0–1.0 at.%) alloys were attained after the elimination of ε. In the case of eutectoid reaction (→β+Si). Differential thermal analysis, X-ray diffraction and microscopic observation clearly confirmed that the eutectoid reaction rate was drastically enhanced by the addition of a small amount of Cu and its rate decreased with decreasing Cu content. The rate also depends on the annealing temperature and reached a maximum at about 1073 K for most alloys. The addition of only 0.1 at.% Cu was still very effective even in Mn or Co doped alloys. The thermoelectric power of these alloys increased very quickly with annealing time. Their final values decreased with Cu content and saturated at 0.2 at.% Cu. The value of the 0.1 at.% Cu added alloy was higher than that of both the conventional p- and a-type FeSi₂ based alloys. These results suggest that the Fe₂Si₅ alloys with a small amount of Cu may be attractive as new thermoelectric materials.     

Postbuckling behaviour of stainless steel (SUS304) columns under loading-unloading cycles

Based on the equilibrium configuration paths, this study investigates the postbuckling behaviour, including the shape recovery capability, of stainless steel (SUS304) columns after a complete loading-unloading cycle. Experiments were conducted and later numerical simulation was carried out in order to analyze the observed buckling and postbuckling behaviour. Large deflection analysis is necessary for slender columns. Moreover, comparison of the experimental critical load with analytical predictions verifies the fact that physical nonlinearity should be taken into account to analyze the column’s buckling behaviour comprehensively. Thus, based on large deflection theory as well as the nonlinear stress-strain relations, the load-deformation curves of the columns during a complete loading-unloading cycle have been predicted by using the finite element modelling (FEM) code ANSYS.Precise and quantitative analyses of the results verify the fact that the material’s stress-strain properties, both in tension and compression, attribute to the column’s buckling behaviour.     

Grafting of poly(ethylene oxide) onto C60 fullerene using macroazo initiators

In order to improve the solubility of C₆₀ fullerene in conventional solvents, grafting of hydrophilic poly(ethylene oxide) (PEO) by utilizing the radical-trapping nature of C₆₀ fullerene was investigated. Macroazo initiators containing a poly(ethylene oxide) unit, known as Azo-PEO, were prepared at various molecular weights by the reaction of 4,4′-azobis(4-cyanopentanoyl chloride) with poly(ethylene glycol) methyl ether. PEO radicals formed by thermal decomposition of Azo-PEO were successfully trapped by C₆₀ fullerene to give PEO-grafted C₆₀ fullerene. Their structures were confirmed by FT-IR spectroscopy, size exclusion chromatography, UV-vis spectroscopy, and differential scanning calorimetry. When Azo-PEO with low-molecular weight was reacted with C₆₀ fullerene, a bis-adduct, C₆₀-(PEO)₂, and a tetrakis-adduct, C₆₀-(PEO)₄, were formed. In contrast, in reactions with Azo-PEO of higher molecular weight, only the bis-adduct was formed, and no formation of the tetrakis-adduct was observed. The structure of bis-adduct was found to be 1,4-type. The solubility of C₆₀ fullerene in water, THF, methanol, and other conventional organic solvents was remarkably improved by grafting of PEO. In addition, the thermal stability of PEO was dramatically increased by grafting onto C₆₀ fullerene.     

Phospholipid polymer hydrogel formed by the photodimerization of cinnamoyl groups in the polymer side chain

We synthesized new polymers with both photocrosslinkability and biocompatibility by a random copolymerization of 4‐(4‐methoxycinnamoyl)phenyl methacrylate and 2‐methacryloyloxyethyl phosphorylcholine. These polymers were used as prepolymers to make a hydrogel by photoirradiation. Gelation began with 5 s of photoirradiation and reached an equilibrium state after 360 s of photoirradiation. The absorption maximum at 347 nm, attributed to the cinnamoyl group, disappeared with the photoirradiation time. That is, dimerization between cinnamoyl groups in the polymer proceeded and formed a hydrogel. The equilibrium water concentration of the hydrogels was more than 90%. Moreover, we succeeded in making a microshape hydrogel on glass by photoirradiation through a photomask. The window shape of the photomask was transferred to the hydrogel that was formed. We concluded that these photocrosslinkable polymers could be useful in preparing microfluidic devices for separating or immobilizing biomolecules and cells. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 44–50, 2007     

Observation of polymer film drawing by use of thermography. An introductory investigation on the thermodynamics

The local heat generation that accompanied tensile drawing of polymer films was successfully observed by infrared thermography as a series of temperature distribution images. These images showed that the high temperature part where rearrangements of molecular orientation and microcrystallines occurred was located mainly at the end of the necked part for the polymers that exhibited necking or appeared uniformly throughout films for the polymers that did not exhibit necking. The generated heat could be roughly estimated, and the relation between the estimated heat and mechanical work led to the thermodynamic investigation. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2895–2900, 2006     

Separation of crude palm oil components by semipreparative supercritical fluid chromatography

Successful separation of triglycerides, diglycerides, free fatty acids, carotenes, tocopherol, and tocotrienols from crude palm oil has been achieved by supercritical fluid chromatography (SFC) with a combination of a C18 and a silica gel column. The separation was carried out by the programmed extraction elution method. Free fatty acids were separated into five components by gas-liquid chromatography; tocopherol and tocotrienols were also separated into four components by SFC analysis, and the pure fractionated carotenes were obtained by preparative SFC. Thus, by using supercritical fluid chromatography, crude palm oil components can be separated and fractionated, based on differences in their functional groups.     

Main‐chain smectic liquid crystalline polymer exhibiting unusually high thermal conductivity in an isotropic composite

The thermal conductivity (TC) of an isotropic composite comprising of a main‐chain smectic liquid crystalline PB‐10 polyester and 50‐μm‐sized roughly spherical magnesium oxide (MgO) particles is investigated. The increase in the composite TC with higher MgO fractions is steeper than that expected by Bruggeman's theory for the TC of a polydomain PB‐10 polyester (0.52 W m^?1 K^?1). When the filler content is larger than 30 vol %, the composite TC approaches a value that can be explained only if the polyester functions as a matrix with 1.0 W m^?1 K^?1, which is five times as high as those of isotropic common polymers (0.2 W m^?1 K^?1). Such an unusually high TC for a polymer matrix is attributed to some polymer lamellae that lie parallel to the particle surface and are stacked toward neighboring particles, thus creating effective heat paths between the particles and a continuous thermal network in a composite. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2014 , 131, 39896.