Novel synthesis of superparamagnetic Ni-Co-B nanoparticles and their effect on superconductor properties of MgB2

A new procedure for the preparation of amorphous Ni-Co-B nanoparticles is reported, with a detailed investigation of their morphology by X-ray diffraction and transmission electron microscopy, as well as their magnetic properties. Many factors, such as chemical composition, anisotropy, size and shape of the particles, were controlled through chemical synthesis, resulting in the control of morphological and magnetic properties of the nanoparticles. Controlling pH values with ethylenediamine and using sodium dodecyl sulfate surfactant lowered the size of the nanoparticles to below 10 nm. Such a small structure and chemical disorder in nanocrystalline materials lead to magnetic properties that are different from those in their bulk-sized counterparts. The obtained nanoparticles can be used for different purposes, from pharmaceutical applications to implementations in different materials technology. The focus of this research is the synthesis of Ni-Co-B nanoparticles in a new way and studying the reaction of Ni-Co-B nanoparticles with Mg and B precursors and their effect on MgB2 properties. New nanostructures are formed in the reaction of Ni-Co-B nanoparticles with Mg: Mg2Ni, Co2Mg and possibly Mg2Co.

Romano-British wall-painting fragments: a spectroscopic analysis

Raman spectroscopic analyses of fragmented wall-painting specimens from a Romano-British villa dating from ca. 200 AD are reported. The predominant pigment is red haematite, to which carbon, chalk and sand have been added to produce colour variations, applied to a typical Roman limewash putty composition. Other pigment colours are identified as white chalk, yellow (goethite), grey (soot/chalk mixture) and violet. The latter pigment is ascribed to caput mortuum, a rare form of haematite, to which kaolinite (possibly from Cornwall) has been added, presumably in an effort to increase the adhesive properties of the pigment to the substratum. This is the first time that kaolinite has been reported in this context and could indicate the successful application of an ancient technology discovered by the Romano-British artists. Supporting evidence for the Raman data is provided by X-ray diffraction and SEM-EDAX analyses of the purple pigment.

Vibrational spectroscopy of intercalated kaolinites. Part I

The industrial application of kaolinite is closely related to its reactivity and surface properties. The reactivity of kaolinite can be tested by intercalation, i.e. via the insertion of low molecular weight organic compounds between the kaolinite layers resulting in the formation of a nano-layered organo-complex. Although intercalation of kaolinite is an old and ongoing research topic, there is a limited knowledge available on the reactivity of different kaolinites, the mechanism of complex formation as well as on the structure of the complexes formed. Grafting and incorporation of exfoliated kaolinite in polymer matrices and other potential applications can open new horizons in the study of kaolinite intercalation. This paper attempts to summarize (without completion) the most recent achievements in the study of kaolinite organo-complexes obtained with the most common intercalating compounds like urea, potassium acetate, dimethyl sulphoxide, formamide and hydrazine using vibrational spectroscopy combined with X-ray powder diffraction and thermal analysis.

Thermal decomposition of Bayer precipitates formed at varying temperatures

Bayer hydrotalcites prepared using the seawater neutralisation (SWN) process of Bayer liquors are characterised using X-ray diffraction and thermal analysis techniques. The Bayer hydrotalcites are synthesised at four different temperatures (0, 25, 55, 75 °C) to determine the effect on the thermal stability of the hydrotalcite structure, and to identify other precipitates that form at these temperatures. The interlayer distance increased with increasing synthesis temperature, up to 55 °C, and then decreased by 0.14 Å for Bayer hydrotalcites prepared at 75 °C. The three mineralogical phases identified in this investigation are; 1) Bayer hydrotalcite, 2), calcium carbonate species, and 3) hydromagnesite. The DTG curve can be separated into four decomposition steps; 1) the removal of adsorbed water and free interlayer water in hydrotalcite (30 – 230 °C), 2) the dehydroxylation of hydrotalcite and the decarbonation of hydrotalcite (250 – 400 °C), 3) the decarbonation of hydromagnesite (400 – 550 °C), and 4) the decarbonation of aragonite (550 – 650 °C).

Raman spectroscopy of gallium based hydrotalcites of formula Mg6Ga2(CO3)(OH)16•4H2O

Insight into the unique structure of hydrotalcites has been obtained using Raman spectroscopy. Gallium containing hydrotalcites of formula Mg4Ga2(CO3)(OH)12•4H2O (2:1 Ga-HT) to Mg8Ga2(CO3)(OH)20•4H2O (4:1 Ga-HT) have been successfully synthesised and characterized by X-ray diffraction and Raman spectroscopy. The d(003) spacing varied from 7.83 Å for the 2:1 hydrotalcite to 8.15 Å for the 3:1 gallium containing hydrotalcite. Raman spectroscopy complemented with selected infrared data has been used to characterise the synthesised gallium containing hydrotalcites of formula Mg6Ga2(CO3)(OH)16•4H2O. Raman bands observed at around 1046, 1048 and 1058 cm-1 were attributed to the symmetric stretching modes of the (CO32-) units. Multiple ν3 CO32- antisymmetric stretching modes are found at around 1346, 1378, 1446, 1464 and 1494 cm-1. The splitting of this mode indicates the carbonate anion is in a perturbed state. Raman bands observed at 710 and 717 cm-1 assigned to the ν4 (CO32-) modes support the concept of multiple carbonate species in the interlayer.

Thermogravimetric analysis-mass spectrometry (TG-MS) of selected Chinese kaolinites

Thermogravimetric analysis-mass spectrometry, X-ray diffraction and scanning electron microscopy (SEM) were used to characterize eight kaolinite samples from China. The results show that the thermal decomposition occurs in three main steps (a) desorption of water below 100 °C, (b) dehydration at about 225 °C, (c) well defined dehydroxylation at around 450 °C. It is also found that decarbonization took place at 710 °C due to the decomposition of calcite impurity in kaolin. The temperature of dehydroxylation of kaolinite is found to be influenced by the degree of disorder of the kaolinite structure and the gases evolved in the decomposition process can be various because of the different amount and kinds of impurities. It is evident by the mass spectra that the interlayer carbonate from impurity of calcite and organic carbon is released as CO2 around 225, 350 and 710 °C in the kaolinite samples.

Transition of chromium oxyhydroxide nanomaterials to chromium oxide : a hot stage Raman spectroscopic study

The transition of disc-like chromium hydroxide nanomaterials to chromium oxide nanomaterials has been studied by hot stage Raman spectroscopy. The structure and morphology of α-CrO(OH) synthesised using hydrothermal treatment was confirmed by X-ray diffraction and transmission electron microscopy. The Raman spectrum of α-CrO(OH) is characterised by two intense bands at 823 and 630 cm-1 attributed to ν1 CrIII-O symmetric stretching mode, bands at 1179 cm-1 attributed to CrIII-OH δ deformation modes. No bands are observed above 3000 cm-1. The absence of characteristic OH vibrational bands may be due to short hydrogen bonds in the α-CrO(OH) structure. Upon thermal treatment of α-CrO(OH), new Raman bands are observed at 599, 542, 513, 396, 344 and 304 cm-1, which are attributed to Cr2O3. This hot-stage Raman study shows that the transition of α-CrO(OH) to Cr2O3 occurs before 350 °C.

A solvothermal route to crystalline lithium niobate

A solvothermal route for the preparation of crystalline state lithium niobate using Li2 CO3 and Nb2 O5 is developed. Oxalic acid is employed as solvent, which coordinates with niobium oxide to stimulate the main reaction. Scanning electron microscopy images show that the as-prepared sample displays a cubic morphology. X-ray diffraction and IR spectrum of the as-prepared sample indicate that the sample is well crystalline.

Vibrational spectroscopic analysis of the mineral crandallite CaAl3(PO4)2(OH)5•(H2O) from the Jenolan Caves, Australia

The mineral crandallite CaAl3(PO4)2(OH)5•(H2O) has been identified in deposits found in the Jenolan Caves, New South Wales, Australia by using a combination of X-ray diffraction and Raman spectroscopic techniques. A comparison is made between the vibrational spectra of crandallite found in the Jenolan Caves and a standard crandallite. Raman and infrared bands are assigned to PO43- and HPO42- stretching and bending modes. The predominant features are the internal vibrations of the PO43 and HPO42- groups. A mechanism for the formation of crandallite is presented and the conditions for the formation are elucidated.

An examination of the applicability of hydrotalcite for removing oxalate anions from Bayer process solutions

Hydrotalcite and thermally activated hydrotalcites were examined for their potential as methods for the removal of oxalate anions from Bayer Process liquors. Hydrotalcite was prepared and characterised by a number of methods, including X-ray diffraction, thermogravimetric analysis, nitrogen adsorption analysis and vibrational spectroscopy. Thermally activated hydrotalcites were prepared by a low temperature method and characterised using X-ray diffraction, nitrogen adsorption analysis and vibrational spectroscopy. Oxalate intercalated hydrotalcite was prepared by two methods and analysed with X-ray diffraction and for the first time thermogravimetric analysis, Raman spectroscopy and infrared emission spectroscopy. The adsorption of oxalate anions by hydrotalcite and thermally activated hydrotalcite was tested in a range of solutions using both batch and kinetic adsorption models.

Studies on the effect of the size of polycaprolactone microspheres for the dispersion of Salbutamol Sulfate from dry powder inhaler formulations

Purpose: To study the effect of the size of the surface-coated polycaprolactone (PCL) microparticle carriers on the aerosolization and dispersion of Salbutamol Sulfate (SS) from Dry Powder Inhaler (DPI) formulations. Methods: The microparticles were fabricated using an emulsion technique in four different sizes (25, 48, 104 and 150 μm) and later coated with Magnesium stearate (MgSt) and leucine. They were characterized by laser diffraction and SEM. The Fine Particle Fraction (FPF) of SS from powder mixtures was determined by a Twin Stage Impinger (TSI). Results: As the carrier size increased from 25 μm to 150 μm, the FPF of the SS delivered by the coated PCL particles increased approximately four fold. A linear relationship was found between the FPF and Volume mean Diameter (VMD) of the particles over this range. Conclusions: The dispersion behaviour of SS from PCL carriers was dependent on the inherent size of the carriers and the increased FPF of SS with increased carrier size probably reflects the higher mechanical forces produced due to the carrier-carrier collisions or collisions between the carrier particles and the internal walls of the inhaler during aerosolization.

Dry powder inhaler formulations : effect of carrier size on the drug dispersion

Background: The size of the carrier influences drug aerosolization from a dry powder inhaler (DPI) formulation. Lactose particles with irregular shape and rough surface in a variety of sizes are additionally used as carriers; however, contradictory reports exist regarding the effect of carrier size on the dispersion of drug. We examined the influence of the spherical particle size of the biodegradable polylactide-co-glycolide (PLGA) carrier on the aerosolization of a model drug, salbutamol sulphate (SS). Methods: Four different sizes (20-150 µm) of polymer carriers were fabricated using solvent evaporation technique and the dispersion of SS from these carriers was measured by a Twin Stage Impinger (TSI). The size and morphological properties of polymer carriers were determined by laser diffraction and SEM, respectively. Results: The FPF was found to increase from 5.6% to 21.3% with increasing carrier sizeup to150 µm. Conclusions: The aerosolization of drug increased linearly with the size of polymer carriers. For a fixed mass of drug particles in a formulation, the mass of drug particles per unit area of carriers is higher in formulations containing the larger carriers, which leads to an increase in the dispersion of drug due to the increased mechanical forces occurred between the carriers and the device walls.

Ordered mixed-layer structures in the Mighei carbonaceous chondrite matrix

High resolution transmission electron microscopy of the Mighei carbonaceous chondrite matrix has revealed the presence of a new mixed layer structure material. This mixed-layer material consists of an ordered arrangement of serpentine-type (S) and brucite-type (B) layers in the sequence ... SBBSBB. ... Electron diffraction and imaging techniques show that the basal periodicity is ~ 17 Å. Discrete crystals of SBB-type material are typically curved, of small size (<1 μm) and show structural variations similar to the serpentine group minerals. Mixed-layer material also occurs in association with planar serpentine. Characteristics of SBB-type material are not consistent with known terrestrial mixed-layer clay minerals. Evidence for formation by a condensation event or by subsequent alteration of preexisting material is not yet apparent. © 1982.

Thin-film elemental analyses for precise characterization of minerals

The Analytical Electron Microscope (AEM), with which secondary X-ray emission from a thin (<150nm), electron-transparent material is measured, has rapidly become a versatile instrument for qualitative and quantitative elemental analyses of many materials, including minerals. With due regard for sources of error in experimental procedures, it is possible to obtain high spatial resolution (~20nm diameter) and precise elemental analyses (~3% to 5% relative) from many silicate minerals. In addition, by utilizing the orientational dependence of X-ray emission for certain multi-substituted crystal structures, site occupancies for individual elements within a unit cell can be determined though with lower spatial resolution. The relative ease with which many of these compositional data may be obtained depends in part on the nature of the sample, but, in general, is comparable to other solid state analytical techniques such as X-ray diffraction and electron microprobe analysis. However, the improvement in spatial resolution obtained with the AEM (up to two orders of magnitude in analysis diameter) significantly enhances interpretation of fine-grained assemblages in many terrestrial or extraterrestrial rocks.

Dry powder inhaler formulations-effect of polymer carrier size on the drug dispersion

Background The size of the carrier influences the aerosolization of drug from a dry powder inhaler (DPI) formulation. Currently, lactose monohydrate particles in a variety of sizes are preferably used in carrier based DPI formulations of various drugs; however, contradictory reports exist regarding the effect of the size of the carrier on the dispersion of drug. In this study we examined the influence of the intrinsic particle size of the polymeric carrier on the aerosolization of a model drug salbutamol sulphate (SS). Methods Four different sizes (20–150 lm) of polymer carriers were fabricated using solvent evaporation technique and the dispersion of SS particles from these carriers was measured by a Twin Stage Impinger (TSI). The size and morphological properties of polymer carriers were by laser diffraction and SEM, respectively. Results The FPF from these carriers was found to be increasing from 5.6% to 21.3% with increasing the carrier size. The FPF was found to be greater (21%) with the highest particle size of the carrier (150 lm). Conclusions The aerosolization of drug was dependent on the size of polymer carriers. The smaller size of the carrier resulted in lower FPF which was increased with increasing the carrier size. For a fixed mass of drug particles in a formulation, the mass of drug particles per unit area of carriers is higher in formulations containing the larger carriers, which leads to an increase in the dispersion of drug due to the increased mechanical forces occurred between the carriers and the device walls.