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Organisationseinheit der BAM
Data and prediction for the mass burning rate of a tert-butyl-peroxy-benzoat (TBPB) pool fire (pool diameter = 3 m) is presented. The mass burning rates of TBPB fires are up to six times higher and less dependent on pool diameter compared to hydrocarbon pool fires caused by an additional heat release rate due to exothermic decomposition reaction in the liquid phase. This heat release rate is calculated using a 1st order reaction kinetic obtained from micro calorimetric measurements. A new model is derived considering the heat release rate due to the decomposition reaction which is shown to be 100 % of the heat release rate radiated to the pool surface. With the presented model, including also physical quantities, especially the limiting fuel concentration for upward flame propagation, it is possible to predict the mass burning rates of large TBPB pool fires. The predicted values are in very good agreement with the experiments.
A kinetic model of smouldering of pine wood is determined by thermo-gravimetric analysis (TGA), describing the reactions of wood pyrolysis, wood oxidation and char oxidation. Thermo-gravimetric experiments were conducted with constant heating rates ranging from 2.5 to 10 K/min in atmospheres of pure nitrogen and mixtures of nitrogen and oxygen (with 20.5%, 8.2% and 4.3% O2). At first wood pyrolysis and char oxidation experiments are carried out in an independent way. Then smouldering experiments are conducted, which combine the two previous reactions with wood oxidation. Finally, the heats of the reactions are determined by differential scanning calorimetry (DSC). The results are discussed, compared with the literature and the derived kinetic model is presented, which includes five components: three pseudo-components of wood – representing roughly cellulose, hemi-cellulose and lignin – as well as char and ashes.
Calcium alkaline phosphate scaffolds for bone regeneration 3D-fabricated by additive manufacturing
(2012)
Calcium alkaline phosphate granulates can be used for substitution of several bone defects but for the reconstruction of large skeletal parts in the maxillofacial and orthopaedic fields fitted scaffolds are preferable. Within the additive manufacturing methods, the 3D printing process offers exciting opportunities to generate defined porous scaffolds. We used a R1 printer from ProMetal Company, USA, for producing scaffolds directly from a ceramic powder. For this direct free form fabrication technology the powder has to possess a lot of specific properties both for the generation of a stable green body and also for the subsequent sintering preparation. For this printing process we prepared different granules in a fluidized bed process containing Ca2KNa(PO4)2 as main crystalline phase. Granules were characterized by different methods and several sieve fractions were used for preparing disc like and cylindrical parts. The suitability of granules for this printing process was determined by porosity and strength of produced bodies. Next to granules' performance both of these properties can be directly influenced by 3D printing process parameters. With knowledge of suitable process parameters scaffolds with different porosity in a respective desired design can be created. In this study, cylindrical scaffolds with graded porosity were produced for bone regeneration of segmental defects in maxillofacial surgery and dental implantology by tissue engineering.
Ideally, bioactive ceramics for use in alveolar ridge augmentation should possess the ability to activate bone formation and, thus, cause the differentiation of osteoprogenitor cells into osteoblasts at their surfaces. Therefore, in order to evaluate the osteogenic potential of novel bone substitute materials, it is important to examine their effect on osteoblastic differentiation. This study examines the effect of rapidly resorbable calcium-alkali-orthophosphates on osteoblastic phenotype expression and compares this behavior to that of β-tricalcium phosphate (TCP) and bioactive glass 45S5. Test materials were three materials (denominated GB14, GB9, GB9/25) with a crystalline phase Ca2KNa(PO4)2 and with a small amorphous portion containing either magnesium potassium phosphate (GB14) or silica phosphate (GB9 and GB9/25, which also contains Ca2P2O7); and a material with a novel crystalline phase Ca10[K/Na](PO4)7 (material denominated 352i). SaOS-2 human bone cells were grown on the substrata for 3, 7, 14, and 21 days, counted, and probed for an array of osteogenic markers. GB9 had the greatest stimulatory effect on osteoblastic proliferation and differentiation, suggesting that this material possesses the highest potency to enhance osteogenesis. GB14 and 352i supported osteoblast differentiation to the same or a higher degree than TCP, whereas, similar to bioactive glass 45S5, GB9/25 displayed a greater stimulatory effect on osteoblastic phenotype expression, indicating that GB9/25 is also an excellent material for promoting osteogenesis.
Bioactive ceramics used as coating materials combine the conductive properties of a bioceramic with the mechanical stability of the metal implant. We studied a calcium zirconium phosphate-containing coating material, FA-CZP [Ca5(PO4)3F, CaZr4(PO4)6], that is relatively insoluble in the biological milieu. The reaction of bone to this material was investigated histologically and histomorphometrically in an animal trial. Cylindrical Ti6Al4V specimens that had been coated with FA-CZP by plasma spraying were implanted in the femoral condyles of rabbits. The implants were left in place for 2, 4, 6, 12, and 14 weeks. FA-CZP led to impaired mineralization of the newly formed bone at the interface. Noncalcified osteoid was found throughout the whole study period. The layer seemed to become thicker with time. The mineralization disorder is evidently caused by zirconium ions. The presence of zirconium in the osteoid in contact with the implant was demonstrated by means of two different staining methods.
We performed spatially resolved synchrotron-induced x-ray fluorescence analyses (SY-XRF) of five silverpoint drawings from the famous `Karlsruhe sketchbook´ and a silverpoint, which is assumed to be an original one used by the Renaissance artist Hans Baldung Grien (1484-1545) himself. The silverpoint, one out of a very small number of ancient styli conserved nowadays, is fixed on the so-called `Karlsruhe sketchbook´. Measurements were executed at the FLUO-TOPO beamline at the electron storage ring ANKA. It has been shown, that SY-XRF at this beamline is nondestructive and sensitive enough for the analysis of minor and major elements in the silver strokes. This study provides new insights into this graphical technique and ancient drawing instruments: results are that three drawings have been created with a common type of silverpoint containing about (10.4 ± 0.7) wt% of Cu. In all the cases, Hg at a 10% level by weight was identified in the strokes. Presence of Hg is not due to the original silver alloy, but is a result of a general alteration phenomenon of silverpoint drawings. This fact is confirmed by the analysis of the original silverpoint, which contains only small traces of Hg. The result for the copper content of the silverpoint (10.4 ± 1.7) wt% is in good agreement with that of these three drawings. It is supposable that the silverpoint found attached today served for the creation of the corresponding drawings. Moreover, the graphical technique of Baldung is found to be continual over three decades. Only one very late drawing dated to 1543 was probably realized with another silverpoint, containing about 3 wt% of Cu. This difference in the chemical composition of drawings from the late period might be used as a more precise dating indicator of Baldung drawings that are not clearly attributed to a certain period.
One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an Approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The
mass deposition is converted into film density by division of measured film thickness.
Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the
porosity is demonstrated on thin templated mesoporous TiO₂
films, dip-coated on silicon
wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed
in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films.