Sulfur Concentration in Nanoporous Alumina Membrane

Nanoporous alumina membrane prepared by anodic oxidation using sulfuric acid electrolyte was subjected to TG-DTA and X-ray Photoelectron Spectroscopy (XPS or ESCA) to further study the distribution of sulfur. In XPS study, Ar⁺ ion bombardment was performed on the sample to etch the surface at a rate of 3 nm min^-1. As a result, sulfur was found to be concentrated within a depth of 3nm from the surface. The S content of the surface was found to be 2.7±0.5 wt%, and that at a depth of ca. 3 nm and ca. 10 nm was found to be as low as about 0.6±0.11 wt% (5.37±1.0 wt%→ 1.26±0.2wt% SO₂). In TG-DTA, the mass loss of 7.3% was in fair agreement with that calculated on XPS results (7.1±1.2%). This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermoanalytical characterization of carbon/carbon hybrid material, Apple Woodceramics

Woodceramics, a carbon/carbon composite of plant-originated carbon reinforced by glassy carbon from phenolic resin, was prepared from apple pomace at carbonizing temperatures of 1073 K (AWC800) and 1473 K (AWC1200), and characterized by thermoanalytical methods and X-ray diffraction (XRD). Simultaneous differential scanning calorimetry (DSC) and thermogravimetric (TG) showed complicated overlapping reactions similar to those of coal. The initial temperature of pyrolysis was obtained by fitting logistic functions to observed TG data. The results suggested that AWC1200 contained more volatile matter than AWC800. In an inert atmosphere, complicated devolatilization takes place. In an oxidizing atmosphere, thermal change occurs roughly in four steps: desorption of physically adsorbed matter; pyrolysis into aliphatic and aromatic fragments; ignition; combustion of char. The oxidation resistance of AWC1200 was superior to AWC800.     

Evolution of water vapor from indium-tin-oxide transparent conducting films fabricated by dip coating process

Tin-doped indium oxide In₂O₃ (indium-tin-oxide) transparent conducting films were fabricated on silicon substrates by a dip coating process. The thermal analysis of the ITO films was executed by temperature-programmed desorption (TPD) or thermal desorption spectroscopy (TDS) in high vacuum. Gas evolution from the ITO film mainly consisted of water vapor. The total amount of evolved water vapor increased on increasing the film thickness from approx. 25 to 250 nm and decreased by increasing the preparation temperature from 365 to 600°C and by annealing at the same temperature for extra 10 h. The evolution occurred via two steps; the peak temperatures for 250 nm thick films were approx. 100-120 and 205-215°C. The 25 nm thick films evolved water vapor at much higher temperatures; a shoulder at approx. 150-165°C and a peak at approx. 242°C were observed. The evolution temperatures increased by increasing the preparation and the annealing temperatures except in case of the second peak of the 25 nm thick films. The evolution of water vapor at high temperature was tentatively attributed to thermal decomposition of indium hydroxide, In(OH)₃, formed on the surface of the nm-sized ITO particles. This revised version was published online in August 2006 with corrections to the Cover Date.     

Thermal change of Alq3, tris(8-hydroxyquinolinato) aluminum(III) studied by TG and XRD-DSC

The thermal change of the tris(8-hydroxyquinolinato)aluminum (Alq₃) is currently investigated by XRD-DSC and TG. The phase transition of Alq₃ from α-phase to γ-phase takes place at 643–669 K. A very sharp peak with the peak temperature at approx. 709 K is ascribed to the melting of the Alq₃. The decomposition of the Alq₃ was observed accompanied with the melting and evaporation at >703K. The effect of the atmospheres on the mass loss procedure was studied by TG. It was found that thermal process of Alq₃ was strongly influenced by the partial pressure of water vapor in the atmosphere instead of oxygen.     

Morphological and structural change of nano-pored alumina membrane above 1200 K

The transition and the change in pore morphology of a porous alumina membrane prepared by anodically oxidizing aluminum in sulfuric acid were studied mainly by TG-DTA, TMA, dilatometry and TEM. At ca. 1243 K, TMA showed an expansion followed by contraction; the CO₂ and SO₂ gases were quickly discharged, and the pore morphology of the as-prepared porous membrane (ca 150 mm-t, with pores ca 25 nm in diameter and containing ca 11% by mass of SO₂) showed an abrupt change, but the pores were retained to ca. 1573 K. Sulfur incorporated in the membrane was lost in two stages, i.e., at ca 1243 K and in a range up to 1373 K. Isothermal measurements revealed the complex crystallization of the amorphous phase into polycrystalline phase. This revised version was published online in August 2006 with corrections to the Cover Date.     

Transient DSC,a Novel and Rapid Method for Assessing Pharmaceutical Powder Compacts

The previously described method involving the use of transient DSC was applied to pharmaceutical powder compacts and to ceramic powder compacts. The samples were prepared by compressing powders of pentaerythritol tetraacetate and two kinds of alumina powder (differing in particle size distribution) up to a pressure of 20 MPa by using a jig. For pentaerythritol tetraacetate, a linear relationship was obtained between the parameter obtained by DSC and the compaction pressure. This revised version was published online in August 2006 with corrections to the Cover Date.     

Inhibitory study of two cephalosporins on <Emphasis Type="Italic">E. coli</Emphasis> by microcalorimetry

The microcalorimetric method has been used to study the effects of cefpiramide and ceftizoxime sodium on the E. coli growth. The results revealed that these two cephalosporins may alter the metabolic way of the E. coli. Moreover, the lethal doses of cefpiramide and ceftizoxime sodium are 2.000 and 0.2000 μg mL⁻¹, respectively. Combining with the relationships between growth rate constant (k), the maximum power output (P _m ), the time corresponding to the maximum power output (t _m ) and cephalosporins concentration (C), one can draw the conclusion that the ceftizoxime sodium has a stronger inhibition effects on the growth of E. coli than that of cefpiramide and they both have the possibility to induce the drug fever.     

Crystallization of Anodic Alumina Membranes Studied by Simultaneous TG-DTA/FTIR

The thermal change of anodic alumina (AA), particularly the exothermic peak followed by the endothermic peak at ca 950°C was studied in detail by mainly using simultaneous TG-DTA/FTIR. The gradual loss of mass up to ca 910°C is attributed to dehydration. When heated at a constant rate by using TG-DTA, an exothermic peak with subsequent endothermic peak is observed at ca 950°C, but the exothermic peak becomes less distinct with decreasing heating rate. It has been found that gaseous SO₂ accompanying a small amount of CO₂ is mainly discharged at this stage. The reaction in this stage can be considered roughly in two schemes. The first scheme can be said collectively as crystallization, in which the migration of S or C trapped inside the crystal lattice of the polycrystalline phase (γ-, δ-, and θ-Al₂O₃, which presumably accompanies a large amount of amorphous or disordered phase) occurs. In the second scheme, the initial polycrystalline (+amorphous) phase crystallizes into a quasi-crystallineγ-Al₂O₃-like metastable phase after amorphization. Conclusively,after the distinct exo- and endothermic reactions, the amorphous phase crystallizes intoγ-Al₂O₃, presumably accompanying small amount of δ-Al₂O₃. It is also found that, when maintained isothermally, the metastable phases undergo transformation into the stable α-Al₂O₃ at 912°C. This revised version was published online in July 2006 with corrections to the Cover Date.     

DSC of etched aluminum foils for use in electrolytic capacitors

A DSC method for evaluating the surface area of etched Al foils for use in high performance electrolytic capacitors is presented. A linear relationship between the etching degree (effective surface area) and the thermal resistance of the sample is obtained by means of DSC, based on the transient phenomenon. This method using the transient state in DSC measurement is not only novel, but also rapid and simple in evaluating the surface area of an etched aluminum foil. The method is effective even when the Al foil has a naturally oxidized surface.The authors wish to thank to Mr. Adachi and Mr. Koike of ELNA Co., Ltd. for supplying us with etched aluminum foils. This work is partially supported by the Research Fund of North Shore College of SONY Institute. R. O. whishes to express her gratitude to the support.