Structure and thermal properties of yttrium alumino-phosphate glasses

The structure and thermal properties of yttrium alumino-phosphate glasses, of nominal composition (Y2O3)(0.31-z)(Al2O3)(z)(P2O5)(0.69) with 0 less than or similar to z less than or similar to 0.31, were studied by using a combination of neutron diffraction, Al-27 and P-31 magic angle spinning nuclear magnetic resonance, differential scanning calorimetry and thermal gravimetric analysis methods. The Vickers hardness of the glasses was also measured. The data are compared to those obtained for pseudo-binary Al2O3-P2O5 glasses and the structure of all these materials is rationalized in terms of a generic model for vitreous phosphate materials in which Y3+ and Al3+ act as modifying cations that bind only to the terminal (non-bridging) oxygen atoms of PO4 tetrahedra. The results are used to help elucidate the phenomenon of rare-earth clustering in phosphate glasses which can be reduced by substituting Al3+ ions for rare-earth R3+ ions at fixed modifier content.

The effect of bioglass addition on mechanical and physical properties of photoactive UDMA-TEGDMA resin composites

Light curable dimethacrylate resin composites undergo free radical photopolymerisation in response to blue light (wavelength 450-500 nm) and may offer superior handling and setting characteristics for novel hard tissue repair materials. The current investigation aims to determine the optimum formulation of bisphenol-A glycidyl methacrylate and triethyleneglycoldimethacrylate (bisGMA/TEGDMA) or urethane dimethacrylate (UDMA)/TEGDMA resin mixtures and the effect of Bioglass incorporation on the rate of polymerisation (RP), degree of conversion (DC) and flexural strength (FS) of light-curable filled resin composites (FRCs). Experimental photoactive resins containing a range of bisGMA, UDMA and TEGDMA ratios and/or filled with non-silanised irregular or spherical 45S5-Bioglass (50 μm; 5-40 wt%) and/or silanised silicate glass filler particulates (0.7 μm; 50-70 wt%) were tested. RP and DC were analysed in real-time using nearinfrared spectroscopy. FS of resins and FRCs were determined using three-point flexural strength tests. UDMA/TEGDMA resins exhibited increased DC compared with bisGMA/TEGDMA resins (p<0.05). The addition of spherical particles of Bioglass had a detrimental effect on the FS (p>0.05), whereas they increased DC of UDMA/TEGDMA resins (p<0.05). Addition of irregular shaped Bioglass particles increased the FS of UDMA/TEGDMA resins up to 20 wt% Bioglass (p<0.05). The flexibility and strength conferred by the urethane group in UDMA may result in enhanced physical and mechanical properties compared with conventional resins containing bulky (bisGMA) molecules. Addition of 45S5-Bioglass with specific filler content, size and morphology resulted in enhanced mechanical and physical properties of UDMA/TEGDMA composites. © (2014) Trans Tech Publications, Switzerland.

Grewia gum 1:some mechanical and swelling properties of compact and film

Purpose: To study the mechanical and dynamic swelling properties of grewia gum, evaluate its compression behaviour and determine the effect of drying methods on its properties. Methods: Compacts (500 mg) of both freeze-dried and air-dried grewia gum were separately prepared by compression on a potassium bromide (KBr) press at different pressures and subjected to Heckel analysis. Swelling studies were performed using 200 mg compacts of the gum (freeze-dried or air-dried) compressed on a KBr press. The mechanical properties of the films of the gum prepared by casting 1 % dispersions of the gum were evaluated using Hounsfield tensiometer. The mechanical properties of grewia gum films were compared with films of pullulan and guar gum which were similarly prepared. The effect of temperature on the water uptake of the compacts was studied and the data subjected to Schott's analysis. Results: Drying conditions had no effect on the yield pressure of the gum compacts as both air-dried and freeze-dried fractions had a yield pressure of 322.6 MPa. The plots based on Schott's equation for the grewia gum samples showed that both samples (freeze-dried and air-dried) exhibited long swelling times. Grewia gum film had a tensile strength of 19.22±3.61 MPa which was similar to that of pullulan films (p > 0.05). It had an elastic modulus of 2.13±0.12 N/mm2 which was significantly lower (p < 0.05) than those of pullulan and guar gum with elastic moduli of 3.33±0.00 and 2.86±0.00 N/mm2, respectively. Conclusion: The type of drying method used does not have any effect on the degree of plasticity of grewia gum compacts. Grewia gum obtained by either drying method exhibited extended swelling duration. Matrix tablet formulations of the gum will likely swell slowly and promote sustained release of drug. © Pharmacotherapy Group, Faculty of Pharmacy, University of Benin, Benin City.

Comparative physical, mechanical and crystallographic properties of a series of gemfibrozil salts

Objectives Understanding the impact of the counterion on the properties of an acidic or basic drug may influence the choice of salt form, especially for less potent drugs with a high drug load per unit dose. The aim of this work was to determine the influence of the hydrogen bonding potential of the counterion on the crystal structure of salts of the poorly soluble, poorly compressible, acidic drug gemfibrozil and to correlate these with mechanical properties. Methods Compacts of the parent drug and the salts were used to determine Young's modulus of elasticity using beam bending tests. Crystal structures were determined previously from X-ray powder diffraction data. Key findings The free acid, tert-butylamine, 2-amino-2-methylpropan-1-ol and 2-amino-2-methylpropan-1, 3-diol salts had a common crystal packing motif of infinite hydrogen-bonded chains with cross-linking between pairs of adjacent chains. The tromethamine (trsi) salt, with different mechanical properties, had a two-dimensional sheet-like network of hydrogen bonds, with slip planes, forming a stiffer compact. Conclusions The type of counter ion is important in determining mechanical properties and could be selected to afford slip and plastic deformation. © 2010 Royal Pharmaceutical Society of Great Britain.

Preparation, optimisation and characterisation of lyophilised rapid disintegrating tablets based on gelatin and saccharide

Despite recent success, rapidly disintegrating lyophilized tablets still face problems of low mechanical strength and higher disintegration times resulting in poor patient compliance. The aim of the current work was to carry out a systematic study to understand the factors controlling mechanical properties of these formulations. The work investigated the influence of two bloom strengths of gelatin: low (60 bloom) and high (225 bloom) at different stock solution concentrations (2, 5, 7.5, and 10 %w/w). This was followed by investigation of addition of five saccharides (xylitol, glucose, trehalose, maltotriose and mannitol) at varied concentration range (10-80 %w/w) to decipher their influence on disintegration time, mechanical and thermal properties of the formulation. The results indicated that the disintegration time of the tablets dramatically decreased by decreasing the concentration and bloom strength of gelatin in the stock solution. However the mechanical properties of the tablets were mainly influenced by the concentration of gelatin rather than the bloom strength. The addition of saccharides resulted in enhancement of tablet properties and was concentration dependent. All the saccharides improved the fractubility of the tablets significantly at high concentration (equal or higher than 40% w/w). However, only high concentration (equal or higher than 40% w/w) of trehalose, maltotriose and mannitol significantly enhanced the hardness. Additionally, mannitol crytallised during freeze drying and consequently produced elegant tablets, whilst the other saccarides exhibited lyoprotectant activity as they were able to retain amorphous status. Based on the above findings, an optimized formulation was also successfully developed and characterized to deliver 100 microg dose of Clonidine HCl.

Design of films for oral dosage formulations

A novel method for tablet coating was studied where a thin polymer film was cast (pre-formed film), dried and applied as a coating hence eliminating the need for using any solvent during the actual coating process. A pre-formed film is initially heating to a temperature where it becomes flexible, a vacuum is applied and the film is then pulled around the tablet. The proposed films (gelatine or cellulose-based) were characterised in terms of their dissolution, swelling, mechanical and thermal properties prior to using them in the novel coating process; selected films were then coated onto tablets containing paracetamol or ibuprofen and the effect of the film on the subsequent dissolution was evaluated. It was found that the pre-formed films could be designed to be fast dissolving and mechanically strong to withstand the stress from the coating process. Also metoclopramide was incorporated in a gelatine film-coating formulation which was then successfully coated on paracetamol-containing core. Gelatin-based films were found to be successful in the novel coating process therefore to be suitable as finished coatings for immediate release dosage forms. Orally disintegrating dosage forms have been identified as a favourable dosage form due to the following reasons: fast onset of drug release, easy to use, not painful and possible increase of amount absorbed to systemic circulation. Selected films formulated for coating studies were also successfully formulated to contain active ingredient suitable for orally disintegrating dosage form; cellulose-based naratriptan-films were studied as orally disintegrating dosage forms of where the effect of formulation on the film properties was studied. It was found that strength of the film can affect the dissolution of the film but it may be the inclusion of specific excipients in the formulation which affect the penetration of the drug through mucosa.

Fiber Bragg grating structures inscribed using 800nm femtosecond laser in single- and multi-core mid-IR glass fibers with their spectral, thermal and strain properties

Single- and multi-core passive and active germanate and tellurite glass fibers represent a new class of fiber host for in-fiber photonics devices and applications in mid-IR wavelength range, which are in increasing demand. Fiber Bragg grating (FBG) structures have been proven as one of the most functional in-fiber devices and have been mass-produced in silicate fibers by UV-inscription for almost countless laser and sensor applications. However, because of the strong UV absorption in germanate and tellurite fibers, FBG structures cannot be produced by UVinscription. In recent years femtosecond (fs) lasers have been developed for laser machining and microstructuring in a variety of glass fibers and planar substrates. A number of papers have been reported on fabrication of FBGs and long-period gratings in optical fibers and also on the photosensitivity mechanism using 800nm fs lasers. In this paper, we demonstrate for the first time the fabrication of FBG structures created in passive and active single- and three-core germanate and tellurite glass fibers by using 800nm fs-inscription and phase mask technique. With a fs peak power intensity in the order of 1011W/cm2, the FBG spectra with 2nd and 3rd order resonances at 1540nm and 1033nm in a single-core germanate glass fiber and 2nd order resonances between ~1694nm and ~1677nm with strengths up to 14dB in all three cores of three-core passive and active tellurite fibers were observed. Thermal and strain properties of the FBGs made in these mid-IR glass fibers were characterized, showing an average temperature responsivity of ~20pm/°C and a strain sensitivity of 1.219±0.003pm/µe.

Fiber Bragg grating structures inscribed using 800nm femtosecond laser in single- and multi-core mid-IR glass fibers with their spectral, thermal and strain properties

Single- and multi-core passive and active germanate and tellurite glass fibers represent a new class of fiber host for in-fiber photonics devices and applications in mid-IR wavelength range, which are in increasing demand. Fiber Bragg grating (FBG) structures have been proven as one of the most functional in-fiber devices and have been mass-produced in silicate fibers by UV-inscription for almost countless laser and sensor applications. However, because of the strong UV absorption in germanate and tellurite fibers, FBG structures cannot be produced by UVinscription. In recent years femtosecond (fs) lasers have been developed for laser machining and microstructuring in a variety of glass fibers and planar substrates. A number of papers have been reported on fabrication of FBGs and long-period gratings in optical fibers and also on the photosensitivity mechanism using 800nm fs lasers. In this paper, we demonstrate for the first time the fabrication of FBG structures created in passive and active single- and three-core germanate and tellurite glass fibers by using 800nm fs-inscription and phase mask technique. With a fs peak power intensity in the order of 1011W/cm2, the FBG spectra with 2nd and 3rd order resonances at 1540nm and 1033nm in a single-core germanate glass fiber and 2nd order resonances between ~1694nm and ~1677nm with strengths up to 14dB in all three cores of three-core passive and active tellurite fibers were observed. Thermal and strain properties of the FBGs made in these mid-IR glass fibers were characterized, showing an average temperature responsivity of ~20pm/°C and a strain sensitivity of 1.219±0.003pm/µe.

Thermal properties of fibre Bragg gratings inscribed point-by-point by infrared femtosecond laser

Direct, point-by-point inscription of fibre Bragg gratings by an infrared femtosecond laser has been reported recently. Response of these gratings to annealing at temperatures in the range 500 to 1050°C is studied for the first time. Gratings inscribed by infrared femtosecond lasers were thermally stable at temperatures up to 900°C, representing a significant improvement in comparison with the 'common', UV-inscribed, gratings. Annealing at temperatures up to 700°C increased grating reflectivity. © IEE 2005.

A study of the electrical and optical properties of unhydrogenated neon-sputtered amorphous silicon

Films of amorphous silicon (a-Si) were prepared by r.f. sputtering in a Ne plasma without the addition of hydrogen or a halogen. The d.c. dark electrical conductivity, he optical gap and the photoconductivity of the films were investigated for a range of preparation conditions, the sputtering gas pressure, P, the target-substrate spacing, d, the self-bias voltage, Vsb, on the target and the substrate temperature, Ts. The dependence of the electrical and optical properties on these conditions showed that various combinations of P, d and Vsb, at a constant Ts, giving the same product (Pd/V sb) result in films with similar properties, provided that P, d and Vsb remain vithin a certain range. Variation of Pd/Vsb between about 0.2 and 0.8 rrTorr.cm!V varied the dark conductivity over about 4 orders of magnitude, the optical gap by 0.5 eV and the photoconductivity over 4-5 orders of magnitude. This is attributed to controlling the density-of-states distribution in the mobility gap. The temperature-dependence of photoconductivity and the photoresponse of undoped films are in support of this conclusion. Films prepared at relatively high (Pd/Vsb) values and Ts=300 ºc: exhibited low dark-conductivity and high thermal activation energy, optical gap and photoresponse, characteristic properties of a 'low density-of-states material. P-type doping with group-Ill elements (Al, B and Ga) by sputtering from a composite target or from a predoped target (B-.doped) was investigated. The systematic variation of room-temperature conductivity over many orders of magnitude and a Fermi-level shift of about 0.7 eV towards the valence-band edge suggest that substitutional doping had taken place. The effects of preparation conditions on doping efficiency were also investigated. The post-deposition annealing of undoped and doped films were studied for a temperature range from 250 ºC to 470 ºC. It was shown that annealing enhanced the doping efficiency considerably, although it had little effect on the basic material (a-Si) prepared at the optimum conditions (Pd/Vsb=0.8 mTorr.cm/V and Ts=300 $ºC). Preliminary experiments on devices imply potential applications of the present material, such as p-n and MS junctions.

The mechanical and wear behaviour of B(SiC) fibre-reinforced composite materials

The mechanical properties and wear behaviour of B(SiC) fibre-reinforced metal matrix composites (MMCs) and aluminium alloy (2014) produced by metal infiltration technique were determined. Tensile tests were peliormed at different conditions on both the alloy matrix and its composite, and the tensile fracture surfaces were also examined by Scanning Electron Microscopy (SEM). Dry wear of the composite materials sliding on hardened steel was studied using a pin-on-disc type machine. The effect of fibre orientation on wear rate was studied to provide wear resistance engineering data on the MMCs. Tests were carried out with the wear surface sliding direction set normal, parallel and anti-parallel to the fibre axis. Experiments were perfonned for sliding speeds of 0.6, 1.0 and 1.6 m/s for a load range from 12 N to 60 N. A number of sensitive techniques were used to examine worn surface and debris, i.e: Scanning Electron Microscopy (SEM), Backscattered Electron Microscopy (BSEM) and X-ray Photoelectron Spectroscopy (XPS). Finally, the effect of fibre orientation on the wear rate of the Borsic-reinforced plastic matrix composites (PMCs) produced by hot pressing technique was also investigated under identical test conditions. It was found that the composite had a markedly increased tensile strength compared with the matrix. The wear results also showed that the composite exhibited extremely low wear rates compared to the matrix material and the wear rate increased with increasing sliding speed and normal load. The effect of fibre orientation was marked, the lowest wear rates were obtained by arranging the fibre perpendicular to the sliding surface, while the highest wear was obtained for the parallel orientation. The coefficient of friction was found to be lowest in the parallel orientation than the others. Wear of PMCs were influenced to the greatest extent by these test parameters although similar findings were obtained for both composites. Based on the results of analyses using SEM, BSED and XPS, possible wear mechanisms are suggested to explain the wear of these materials.

Assessment of physical and hydrological properties of biological soil crusts using x-ray microtomography and modelling

Biological soil crusts (BSCs) are formed by aggregates of soil particles and communities of microbial organisms and are common in all drylands. The role of BSCs on infiltration remains uncertain due to the lack of data on their role in affecting soil physical properties such as porosity and structure. Quantitative assessment of these properties is primarily hindered by the fragile nature of the crusts. Here we show how the use of a combination of non-destructive imaging X-ray microtomography (XMT) and Lattice Boltzmann method (LBM) enables quantification of key soil physical parameters and the modeling of water flow through BSCs samples from Kalahari Sands, Botswana. We quantify porosity and flow changes as a result of mechanical disturbance of such a fragile cyanobacteria-dominated crust. Results show significant variations in porosity between different types of crusts and how they affect the flow and that disturbance of a cyanobacteria-dominated crust results in the breakdown of larger pore spaces and reduces flow rates through the surface layer. We conclude that the XMT–LBM approach is well suited for study of fragile surface crust samples where physical and hydraulic properties cannot be easily quantified using conventional methods.

Thermal stability of sputter-deposited 330 austenitic stainless-steel thin films with nanoscale growth twins

We have explored the thermal stability of nanoscale growth twins in sputter-deposited 330 stainless-steel (SS) films by vacuum annealing up to 500 °C. In spite of an average twin spacing of only 4 nm in the as-deposited films, no detectable variation in the twin spacing or orientation of twin interfaces was observed after annealing. An increase in the average columnar grain size was observed after annealing. The hardness of 330 SS films increases after annealing, from 7 GPa for as-deposited films to around 8 GPa for annealed films, while the electrical resistivity decreases slightly after annealing. The changes in mechanical and electrical properties after annealing are interpreted in terms of the corresponding changes in the residual stress and microstructure of the films. © 2005 American Institute of Physics.

Hydrogen-terminated detonation nanodiamond:impedance spectroscopy and thermal stability studies

In this paper, we investigated the effect of hydrogen termination on the electrical properties and impedance spectra of detonation nanodiamond. The impedance spectra revealed that the hydrogen-termination process increases the electrical conductivity by four orders of magnitude at room temperature. An equivalent circuit has been proposed to correlate with the conduction mechanism. Arrhenius plot showed that there were two different activation energy levels located at 0.089 eV and 0.63 eV between 50 °C and 400 °C. The possible physical mechanism corresponding to these activation energy levels has been discussed. Hydrogen-terminated detonation nanodiamond has been further annealed at different temperatures prior to FTIR and XPS measurements in order to understand their thermal stability. The results demonstrated that the surface oxidization occurred between 100 °C and 150 °C. However, the C-H bonds could partially survive when the temperature reaches 400 °C in air. © 2013 American Institute of Physics.

One- and two-step spin-crossover behavior of [Fe(II)(isoxazole)6]2+ and the structure and magnetic properties of triangular [Fe(III)3O(OAc)6(isoxazole)3][ClO4)]

The structure and spin-crossover magnetic behavior of [FeII16][BF4]2 (1 = isoxazole) and [FeII16][ClO4]2 have been studied. [FeII16][BF4]2 undergoes two reversible spin-crossover transitions at 91 and 192 K, and is the first two-step spin transition to undergo a simultaneous crystallographic phase transition, but does not exhibit thermal hysteresis. The single-crystal structure determinations at 260 [space group P3̄, a = 17.4387(4) Å, c = 7.6847(2) Å] and at 130 K [space group P1̄, a = 17.0901(2) Å, b = 16.7481(2) Å, c = 7.5413(1) Å, α = 90.5309(6)°, β = 91.5231(6)°, γ = 117.8195(8)°] reveal two different iron sites, Fe1 and Fe2, in a 1:2 ratio. The room-temperature magnetic moment of 5.0 μB is consistent with high-spin Fe(II). A plateau in μ(T) having a moment of 3.3 μB centered at 130 K suggests a mixed spin system of some high-spin and some low-spin Fe(II) molecules. On the basis of the Fe−N bond distances at the two temperatures, and the molar fraction of high-spin molecules at the transition plateau, Fe1 and Fe2 can be assigned to the 91 and 192 K transitions, respectively. [FeII16][ClO4]2 [space group P3̄, a = 17.5829(3) Å, c = 7.8043(2) Å, β = 109.820 (3)°, T = 295 K] also possesses Fe1:Fe2 in a 1:2 ratio, and magnetic measurements show a single spin transition at 213 K, indicating that both Fe1 and Fe2 undergo a simultaneous spin transition. [FeII16][ClO4]2 slowly decomposes in solutions containing acetic anhydride to form [FeIII3O(OAc)613][ClO4] [space group I2, a = 10.1547(7) Å, b = 16.5497(11) Å, c = 10.3205(9) Å, β = 109.820 (3)°, T = 200 K]. The isosceles Fe3 unit contains two Fe···Fe distances of 3.2844(1) Å and a third Fe···Fe distance of 3.2857(1) Å. The magnetic data can be fit to a trinuclear model with ℋ = −2J(S1·S2 + S2·S3) − 2J13(S1·S3), where J = −27.1 and J13 = −32.5 cm-1.