Browsing by Author "Hoeche, Daniel"

Due to the present shortage of He-3 and the associated tremendous increase of its price, the supply of large neutron detection systems with He-3 becomes unaffordable. Alternative neutron detection concepts, therefore, have been invented based on solid B-10 converters. These concepts require development in thin film deposition technique regarding high adhesion, thickness uniformity and chemical purity of the converter coating on large area substrates. We report on the sputter deposition of highly uniform large-area (B4C)-B-10 coatings of up to 2 mu m thickness with a thickness deviation below 4% using the Helmholtz-Zentrum Geesthacht large area sputtering system. The (B4C)-B-10 coatings are x-ray amorphous and highly adhesive to the substrate. Material analysis by means of X-ray-Photoelectron Spectroscopy, Secondary-Ion-Mass-Spectrometry, and Rutherford-Back-Scattering (RBS) revealed low impurities concentration in the coatings. The isotope composition determined by Secondary-Ion-Mass-Spectrometry, RBS, and inelastic nuclear reaction analysis of the converter coatings evidences almost identical B-10 isotope contents in the sputter target and in the deposited coating. Neutron conversion and detection test measurements with variable irradiation geometry of the converter coating demonstrate an average relative quantum efficiency ranging from 65% to 90% for cold neutrons as compared to a black He-3-monitor. Thus, these converter coatings contribute to the development of He-3-free prototype detectors based on neutron grazing incidence. Transferring the developed coating process to an industrial scale sputtering system can make alternative He-3-free converter elements available for large area neutron detection systems. (C) 2015 AIP Publishing LLC.

Samples of pure titanium were laser nitrided by continuous wave CO(2) laser irradiation in mixtures of nitrogen and argon gas with different ratios. In all cases, TiN formed in the surface. The properties and the characteristics of the processed samples were evaluated using a nanoindentation technique, optical microscopy, surface roughness measurements, x-ray diffraction and wear resistance measurements. It was found that the nitrogen content in the gas atmosphere has a massive effect on the microstructure and the mechanical properties of the laser nitrided samples. For all treated samples, the mechanical properties improve with the nitrogen content in the gas atmosphere. Moreover, the thickest TiN layers with high values of the microhardness and good wear resistance were obtained for the titanium sample that was treated in 80% N(2) and 20% Ar. In addition, the strain and the grain size of the coatings formed at the surface of the laser nitrided titanium samples were determined from x-ray data.

Titanium sheets were irradiated by free electron laser radiation in cw mode in pure nitrogen. Due to the interaction, nitrogen diffusion occurs and titanium nitride was synthesized in the tracks. Overlapping tracks have been utilized to create coatings in order to improve the tribological properties of the sheets. Caused by the local heating and the spatial dimension of the melt pool, convection effects were observed and related to the track properties. Stress, hardness, and nitrogen content were investigated with x-ray diffraction, nanoindention, and resonant nuclear reaction analysis. The measured results were correlated with the scan parameters, especially to the lateral track shift. Cross section micrographs were prepared and investigated by means of scanning electron microscopy. They show the solidification behavior, phase formation, and the nitrogen distribution. The experiments give an insight into the possibilities of materials processing using such a unique heat source.

Laser nitriding of materials is based on the interaction of short pulsed laser radiation with the treated material and the hitherto formed laser plasma. The process is very promising for the fast formation of surface coatings with superior properties. Due to the short interaction times and the thin surface films an experimental observation of the underlying processes is very difficult. In order to access the basic mechanism, finite element method simulations of laser heating, evaporation, plasma formation and expansion, plasma composition and interaction with the materials surface have been performed. As a result, evaporation and expansion velocities, pressure balances and dissociation degrees have been derived. The results give a better insight into the physical processes and dependencies of the coating formation, in this case for the titanium-nitrogen system. This finally allows an optimization of the coating synthesis. (c) 2007 Elsevier B.V. All rights reserved.

Titanium was laser nitrided by means of free-electron laser irradiation in pure nitrogen atmosphere. The variation of pulse frequency and macropulse duration of the free electron laser resulted in delta-TiNx coatings with different thickness and different micro- and macroscopic morphologies. The coatings revealed, characteristic values for hardness, roughness and crystallographic texture, which originate from the growth mechanism, the solid-liquid interface energy and the strain. Further investigations showed that the dendritic growth is beginning at the surface and that the alignment of dendrites is normal to the surface. A correlation of the texture with the time structure of the laser pulses was found. Numerical simulations were performed and compared with the experimental results. The simulations can explain the experimental results. (c) 2007 Elsevier B.V. All rights reserved.

Embedding ceramic particles with a negative thermal expansion coefficient into a metallic corrosion resistant coating can establish a reversible thermal activation of a defined surface microstructure with the aim of having a shark-skin at high temperatures (in use) and self-cleaning at low temperatures (out of use). For that, CoNiCrAlY alloy is intermixed with yttrium and tungsten oxide as powder and then laser cladded onto a substrate. This coating is implanted with energetic ions in order to incubate the formation of Y(2)W(3)O(12) which is a ceramic with strong negative thermal expansion. Such prepared coatings are then exposed to high temperature and the effects are investigated in detail. Results of phase formation, surface micro-morphology, microstructure and properties of the coatings are presented. (C) 2008 Elsevier B.V. All rights reserved.

Nitriding is a well known technique to improve properties of materials. The process utilizing laser contains many different processes like heat transport and melting effects, diffusion and convection, which partially determine the synthesized coatings. This review concludes the research on titanium nitride synthesis in reactive ambient and draws conclusions for the general handling of the method. Afterwards, it becomes clear which and why, transport processes limit the coating properties.

Titanium was laser nitrided by means of free electron laser ( FEL) irradiation in pure nitrogen atmosphere. The variation of macropulse frequency and duration of the FEL micropulse trains resulted in the formation of delta-TiNx coatings with different thicknesses and different micro- and macroscopic morphologies. The coatings revealed characteristic values for hardness, roughness and crystallographic texture, which originate from the growth mechanism, the solid - liquid interface energy and the strain. Further investigations showed that the dendritic growth begins at the surface and the alignment of the dendrites is normal to the surface. A correlation of the texture with the time structure of the laser pulses was found. Combined numerical simulations of temperature evolution and nitrogen diffusion were performed and the results were compared with the experimental findings. The simulations can explain the experimental results to a great extent.

Pure titanium was treated by free electron laser (FEL) radiation in a nitrogen atmosphere. As a result, nitrogen diffusion occurs and a TiN coating was synthesized. Local gradients of interfacial tension due to the local heating lead to a Marangoni convection, which determines the track properties. Because of the experimental inaccessibility of time-dependent occurrences, finite element calculations were performed, to determine the physical processes such as heat transfer, melt flow, and mass transport. In order to calculate the surface deformation of the gas-liquid interface, the level set approach was used. The equations were modified and coupled with heat-transfer and diffusion equations. The process was characterized by dimensionless numbers such as the Reynolds, Peclet, and capillary numbers, to obtain more information about the acting forces and the coating development. Moreover, the nitrogen distribution was calculated using the corresponding transport equation. The simulations were compared with cross-sectional micrographs of the treated titanium sheets and checked for their validity. Finally, the process presented is discussed and compared with similar laser treatments.

Pure titanium was irradiated by pulsed Nd:YAG laser irradiation in nitrogen atmosphere. As a result, nitrogen uptake and diffusion occurred and a TiN layer was synthesized at the titanium surface. These TiN coatings were analyzed by X-ray diffraction and the diffraction patterns were investigated in detail, in order to obtain more information about the physical processes during the coating formation. The diffraction peaks were fitted by Pearson VII profiles and the grain size and the microstrain were determined by the analysis of line broadening and peak shifts, using the Williamson-Hall and the Warren-Averbach formalisms. Additional single-line analyses were performed by means of the method of Langford and Keijser to obtain information about the preferred grain orientation and the texture development. The maximum grain size was about 100 nm and a corresponding average lattice strain of 0.002 was found. A relation between the treatment parameters and the coating properties, such as grain size and microstrain, can be shown. Thus, it was possible to determine optimal scan parameters for material processing and to establish the physical limits of the coating properties.

Titanium was treated by pulsed Nd:YAG laser irradiation in nitrogen atmosphere, which led to nitrogen in-diffusion and TiN coating formation. The thickness of the TiN films was about 1.2 mu m and the coatings had a universal hardness of about 11 GPa. The layers were investigated by X-ray diffraction at grazing incidence and resonant nuclear reaction analysis for nitrogen depth profiling. Fitting of the experimental depth profiles gave information about the physical processes (diffusion time and depth) with respect to the achieved hardness. The microscopic properties like lattice constants and the variation of the nitrogen content were evaluated. A relationship between laser scan parameters and coating properties could be revealed. Thus, it was possible to determine the physical limits such as film thickness, nitrogen content, and hardness of this direct laser synthesis.