M. Björkqvist

Studies of Thermally‐Carbonized Porous Silicon Surfaces

Thermally-carbonized porous silicon films have been prepared by exploiting the dissociation of acetylene. Thermoanalytical methods have been used to study the oxidation behavior of these films in different oxidizing ambients. The results have been compared to other stabilization methods. Due to enhanced adsorption and only slightly reduced specific surface area, the carbonization of porous silicon was found to be an attractive treatment for sensing applications. The possible post-treatments are also discussed.

Studies on hysteresis reduction in thermally carbonized porous silicon humidity sensor

Different ways to reduce hysteresis in a capacitive-type thermally carbonized porous silicon (TC-PS) humidity sensor are studied and compared. Modification of the contact angle of the dielectric surface, enlargement of the pore size of dielectric, and operating the sensor at elevated temperature proved all to be possible ways to reduce hysteresis in a TC-PS humidity sensor. By variation of the carbonization temperature, we produced TC-PS surfaces of different contact angles. Although the hydrophobic surface prevents hysteresis, it also decreases considerably the sensitivity of the sensor. Enlargement of the pore size reduces and tunes the hysteresis loop into the higher relative humidity (RH) values. Also operation of the sensor only few degrees above room temperature was found to be a workable method to prevent hysteresis. However, a constant temperature is crucial for exact humidity measurement using a TC-PS sensor

Intraorally fast-dissolving particles of a poorly soluble drug: Preparation and in vitro characterization

In this study, the dissolution rate of a poorly soluble drug, perphenazine (PPZ) was improved by a solid dispersion technique to permit its usage in intraoral formulations. Dissolution of PPZ (4 mg) in a small liquid volume (3 ml, pH 6.8) within one minute was set as the objective. PVP K30 and PEG 8000 were selected for carriers according to the solubility parameter approach and their 5/1, 1/5 and 1/20 mixtures with PPZ (PPZ/polymer w/w) were prepared by freeze-drying from 0.1 N HCl solutions. The dissolution rate of PPZ was improved with all drug/polymer mixture ratios compared to crystalline or micronized PPZ. A major dissolution rate improvement was seen with 1/5 PPZ/PEG formulation, i.e. PPZ was dissolved completely within one minute. SAXS, DSC and XRPD measurements indicated that solid solutions of amorphous PPZ in amorphous PVP or in partly amorphous PEG were formed. DSC and FTIR studies suggested that PPZ dihydrochloride salt was formed and hydrogen bonding was occurred between PPZ and the polymers. It was concluded that molecular mixing together with salt formation promoted the dissolution of PPZ, especially in the case of the 1/5 PPZ/PEG dispersion, making it a promising candidate for use in intraoral formulations.

Perphenazine solid dispersions for orally fast-disintegrating tablets: physical stability and formulation

Aim: The aim of this study was to prepare an orally fast-disintegrating tablet (FDT) by direct compression, containing a poorly soluble drug (perphenazine, PPZ) formulated as a stable solid dispersion. Methods: The stability studies of the fast dissolving 5/1, 1/5, 1/20 (w/w), PPZ/polyvinylpyrrolidone K30 (PVP) or polyethylene glycol 8000 (PEG)) solid dispersions, and amorphous PPZ were conducted with differential scanning calorimetry, X-ray powder diffraction, Fourier-transform infrared spectroscopy, small-angle X-ray scattering, and dissolution rate studies. Results and discussion: It was found that 1/5 PPZ/PEG was the most stable dispersion under elevated temperature and/or humidity. FDTs containing 60% of mannitol, 15% of calcium silicate, 15% of crospovidone, and 10% of 1/5 PPZ/PEG solid dispersion exhibited fast disintegration times (37 ± 3), sufficient hardness (1.28 ± 0.06 MPa), and fast onset of drug dissolution (34% of PPZ dissolved in 4 minutes), and these properties were found to be retained with storage. Thus, by optimizing the drug/excipient ratio of the solid dispersion and tablet composition, it was possible to produce FDTs that possessed fast disintegration and satisfactory drug dissolution in addition to adequate tensile strength, so that they can be handled and packed normally.

A role of illumination during etching to porous silicon oxidation

The oxidation behavior of porous silicon (PS) has been found to be related to illumination during etching. The autocatalytic oxidation behavior at room temperature arises from the unrelaxed surface induced by the preparation under illumination and can be removed using thermal treatment in a nitrogen atmosphere. The effect is absent in the case of degenerate PS and smaller in p type than in n-type PS. The correlation between the oxidation behavior and the microstructural dimensions is also discussed.

Compatibility of chewing gum excipients with the amino acid L-cysteine and stability of the active substance in directly compressed chewing gum formulation.

Using l‐cysteine chewing gum to eliminate carcinogenic acetaldehyde in the mouth during smoking has recently been introduced. Besides its efficacy, optimal properties of the gum include stability of the formulation. However, only a limited number of studies exist on the compatibility of chewing gum excipients and stability of gum formulations. In this study we used the solid‐state stability method, Fourier transform infrared spectroscopy and isothermal microcalorimetry to investigate the interactions between l‐cysteine (as a free base or as a salt) and excipients commonly used in gum. These excipients include xylitol, sorbitol, magnesium stearate, Pharmagum S, Every T Toco and Smily 2 Toco. The influence of temperature and relative humidity during a three‐month storage period on gum formulation was also studied. Cysteine alone was stable at 25°C/60% RH and 45°C/75% RH whether stored in open or closed glass ambers. As a component of binary mixtures, cysteine base remained stable at lower temperature and humidity but the salt form was incompatible with all the studied excipients. The results obtained with the different methods corresponded with each other. At high temperature and humidity, excipient incompatibility with both forms of cysteine was obvious. Such sensitivity to heat and humidity during storage was also seen in studies on gum formulations. It was also found that cysteine is sensitive to high pressure and increase in temperature induced by compression. The results suggest that the final product should be well protected from temperature and humidity and, for example, cooling process before compression should be considered.

Comparison of different methods in microstructural characterization of porous silicon

Results obtained using the Brunauer-Emmett-Teller method, small-angle x-ray scattering and wide angle x-ray diffraction in the study of porous silicon are compared. The BET method seems to fail when the porosity of samples is smaller than 50%, giving unrealistically large values for the specific surface area, but giving results similar to SAXS when the porosity is larger than 50%. In the comparison of the WAXD and SAXS data quite large differences between the average particle size and chord length were observed in low-porosity samples. The possible origin of the differences is discussed.

Small-angle X-ray scattering studies on oxide layer thickness at the porous silicon interface

We have determined the thickness of an oxide layer at the p+-type porous silicon interface as a function of oxidation time, by using a small angle X-ray scattering (SAXS). The scattering experiments were carried out using a Kratky camera with a step-scanning device. Oxidation was achieved by storing the porous silicon samples in various temperatures under high relative humidity. The negative deviations from Porods law were observed from the scattering curves of oxidized samples. The oxide layer thickness was determined from the scattering curve using a sigmoidal-gradient approximation for the diffuse boundary. The oxide layer thickness values as a function of oxidation time, obtained using SAXS are compared to measured weight increase values, caused by the oxidation.