Langmuir-Blodgett (LB) films of Cd arachidate and Ca arachidate with thicknesses of 1, 3, 9, and 25 layers were investigated using near edge x-ray absorption fine structure (NEXAFS spectroscopy), small angle x-ray scattering (SAXS), and reflected high energy electron diffraction (RHEED). The results from the x-ray diffraction experiments on layer thickness and interface roughness complement the structural information from NEXAFS on the average tilt angle of the alkyl chains in real space. The RHEED measurements confirm these findings and give additional information on the lateral order in these organic films. We find that the monolayer film shows a substantial degree of disorder, while for three and more LB layers, the molecular orientation is virtually identical to that of the corresponding fatty acid salts, i.e., the hydrocarbon chains are oriented perpendicular to the substrate surface in an all-trans conformation. Furthermore, a simplified and more robust analysis scheme for NEXAFS data obtained for hydrocarbon chains is presented. 7722
Background: The bone substitute NanoBone® consists of nanocrystalline hydroxyapatite embedded in a highly porous matrix of silica gel. It promotes the healing of bone defects and is degraded by osteoclasts during bone remodeling. The present study investigates the interactions of NanoBone® with bone tissue. Methods: Granules of NanoBone® were implanted in defects of critical size in the mandible of minipigs. Samples were taken after 5 and 10 weeks and demineralized. The composition of the implanted granules was analyzed by means of transmission and scanning electron microscopy and EDX. Enzymeand immunohistochemistry was used to investigate organic components of NanoBone® granules that arised after implantation in the host. Results: EDX demonstrated that 5 weeks after implantation the silica gel was degraded and replaced by an organic matrix. Ultrastructurally, the matrix appeared amorphous with only single collagen fibrillae. PAS-staining indicated the presence of carbohydrates. Immunohistochemically, the bone proteins osteopontin, osteocalcin and BMP-2 were found as constituents of the new matrix. Alkalic phosphatase activity was located in osteoblasts and newly formed bone on NanoBone® and focally in particles. Osteoclasts with ruffled borders, sealing zones, and acid phosphatase activity were situated in resorption lacunae at granule surfaces not covered by new bone. Conclusions:In vivo, the silica gel of NanoBone® is replaced by bone matrix glycoproteins with known functions in attraction, adhesion, and differentation of bone cells as osteoblasts and osteoclasts. We assume that the deposition of these molecules supports the early phase of NanoBone® degradation by osteoclasts and promotes the production of new bone tissue.
Silicified regions in the stem and leaf of the horsetail Equisetum arvensewere studied by scanning and transmission electron microscopy. The silica was present as a thin layer on the outer surface with variation in the size of this layer depending on the part investigated. There was a dense arrangement of silica spheres with some density fluctuations. A loose arrangement of silica particles with variation in their size was found beneath this dense arrangement suggesting the agglomeration of silica. An electron diffraction pattern showed the presence of amorphous silica, with the short range order being comparable to that of silica from other chemical sources. The medium range order shows the presence of silica with a high inner surface. SAXS measurements correlate with the particle size observed in TEM, and provide values for surface fractals. A new method of plasma ashing to remove the organics is also described.
An improved transform technique has been developed [Gerber (1983). Thesis, Wilhelm‐Pieck‐University Rostock, German Democratic Republic] for calculating the particle size distribution N(R) for spherical particles with radii R from small‐angle X‐ray scattering data. This method permits N(R) to be calculated from analytical expressions that were derived for point collimation and for infinitely long slit collimation. A special procedure has been introduced in order to reduce termination errors. The technique described and those developed by Schmidt [Brill, Weil & Schmidt (1968). J. Colloid Interface Sci.27, 479–492], Vonk [J. Appl. Cryst. (1976), 9, 433–440] and Glatter [J. Appl. Cryst. (1980), 13, 7–11] were used for calculating particle size distributions from theoretical scattering curves and from an experimental scattering curve of suspended SiO2 particles (Ludox). The results obtained by the different techniques were compared, and reasonable results are given by all methods employed. The accuracy of the size distributions calculated by the improved method is somewhat higher than that obtained by Schmidt's transform technique. With Glatter's procedure, the deviations from the exact distributions are comparable to those from this improved transform technique, but the use of Glatter's program requires a large computer, whereas the new method has the advantage of being suitable for a small computer. Vonk's program also requires a large computer, and the deviations obtained are larger than those produced by other methods. The experimental scattering curve of the Ludox sample was also evaluated by assuming a log‐normal distribution for the particles. The parameters μ and σ of this function were determined from a set of small‐angle X‐ray scattering structural parameters. The resulting log‐normal distribution is significantly different from the size distribution calculated by our method.
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