Karen Pantleon

In situ investigation of the microstructure evolution in nanocrystalline copper electrodeposits at room temperature

The microstructure evolution in copper electrodeposits at room temperature (self-annealing) was investigated by means of x-ray diffraction analysis and simultaneous measurements of the electrical resistivity as a function of time. In situ studies were started immediately after deposition of the various thick layers and continued with a unique time resolution until stabilization of the recorded data occurred. Independent of the copper layer thickness, the as-deposited microstructure consisted of nanocrystalline grains with orientation dependent crystallite sizes. Orientation dependent grain growth, crystallographic texture changes by multiple twinning, and a decrease of the electrical resistivity occurred as a function of time at room temperature. The kinetics of self-annealing is strongly affected by the layer thickness: the thinner the layer, the slower the microstructure evolution is, and self-annealing is suppressed completely for a thin layer with 0.4μm. The preferred crystallographic orientation of t...

Induction surface hardening of hard coated steels

Abstract The properties of hard coatings deposited using CVD processes are usually excellent. However, high deposition temperatures negatively influence the substrate properties, especially in the case of low alloyed steels. Therefore, a subsequent heat treatment is necessary to restore the properties of steel substrates. Here, induction surface hardening is used as a method of heat treatment after the deposition of TiN hard coatings on AISI 4140 (DIN42CrMo4) substrates. The influences of the heat treatment on both the coating and the substrate properties are discussed in relation to the parameters of induction heating. Thereby, the heating time, heating atmosphere and the power input into the coating–substrate compounds are varied. As a result of induction surface hardening, the properties of the substrates are improved without losing good coating properties. High hardness values in the substrate near the interface allow the AISI 4140 substrates to support TiN hard coatings very well. Consequently, higher critical loads are measured in scratch tests after the heat treatment. Also, compressive residual stresses in the substrate are generated. In addition, only a very low distortion appears.

Dislocation density and Burgers vector population in fiber-textured Ni thin films determined by high- resolution X-ray line profile analysis

Nanocrystalline Ni thin films have been produced by direct current electrodeposition with different additives and current density in order to obtain 〈100〉, 〈111〉 and 〈211〉 major fiber textures. The dislocation density, the Burgers vector population and the coherently scattering domain size distribution are determined by high-resolution X-ray diffraction line profile analysis. The substructure parameters are correlated with the strength of the films by using the combined Taylor and Hall–Petch relations. The convolutional multiple whole profile method is used to obtain the substructure parameters in the different coexisting texture components. A strong variation of the dislocation density is observed as a function of the deposition conditions.

Interpretation of Quantitative Crystallographic Texture in Copper Electrodeposits on Amorphous Substrates

Crystallographic texture and morphology in Cu electrodeposits was studied in relation to the current density and the content of the organic levelling additive 3-mercapto-1-propanesulfonate. The substrate onto which Cu was electrodeposited consisted of amorphous Ni-P in order to allow substrate-unbiased texture development in the electrodeposit. Comprehensive X-ray diffraction studies of the crystallographic texture, including calculations of the three-dimensional orientation distribution function, were performed and accompanied by investigations of the deposit morphology by means of light optical microscopy. Electrodeposits with totally different microstructures having the same main crystallographic orientation of grains were observed. For interpretation of the results, not only the original growth behavior in direct dependence on the applied process parameters, but also process dependent self-annealing effects ~recrystallization! of the as-deposited layers were considered.

Thermally activated growth of lath martensite in Fe-Cr-Ni-Al stainless steel

Abstract The austenite to martensite transformation in a semi-austenitic stainless steel containing 17 wt-%Cr, 7 wt-%Ni and 1 wt-%Al was investigated with vibrating sample magnetometry and electron backscatter diffraction. Magnetometry demonstrated that, within experimental accuracy, martensite formation can be suppressed on fast cooling to 77 K as well as on subsequent fast heating to 373 K. Surprisingly, martensite formation was observed during moderate heating from 77 K, instead. Electron backscatter diffraction demonstrated that the morphology of martensite is lath type. The kinetics of the transformation is interpreted in terms of athermal nucleation of lath martensite followed by thermally activated growth. It is anticipated that substantial autocatalytic martensite formation occurs during thermally activated growth. The observation of a retardation of the transformation followed by a new acceleration during slow isochronal (i.e. at constant rate) cooling is interpreted in terms of the combined effect of the strain energy introduced in the system during martensite formation, which thermodynamically and/or mechanically stabilises austenite, and autocatalytic nucleation of martensite.

Electrochemically deposited nickel membranes; process–microstructure–property relationships

Abstract This paper reports on the manufacturing, surface morphology, internal structure and mechanical properties of Ni-foils used as membranes in reference-microphones. Two types of foils, referred to as S-type and 0-type foils, were electrochemically deposited from a Watts-type electrolyte, with (S-type) or without (0-type) the use of the sulfur-containing additive sodium saccharin. Both types of Ni-foils appeared perfectly smooth when investigated with scanning electron microscopy (SEM), while atomic force microscopy (AFM) and transmission electron microscopy (TEM) revealed differences in the surface morphologies and a smaller grain-size in the S-type foils. X-Ray diffraction showed a 〈311〉 texture component in both types of Ni-foils, most pronounced for 0-type foils. A minor 〈111〉 texture component observed in both foil types was strongest in the S-type foils. Mechanically 0-type foils proved more ductile than S-type foils during thin film tensile testing, due to microstructural defects caused by sodium saccharin during deposition. Tensile strengths in the order of 700–1000 MPa were observed—highest for the more ductile 0-type foils. A hardness in the order of 6 GPa (590 HV) was found by nanoindentation.

The complementary use of electron backscatter diffraction and ion channelling imaging for the characterization of nanotwins

On the example of electrodeposited nickel films, it is shown that unique information on twins with dimensions on the nanoscale can be obtained by suitable combination of ion channelling imaging and electron backscatter diffraction analysis, whereas both (routine) single techniques cannot meet the requirements for analysis of these films. High‐resolution electron backscatter diffraction is inadequate for full characterization of nanotwins, but image quality maps obtained from electron backscatter diffraction at least yield a qualitative estimation of the location and number of nanotwins. Complementing this information with ion channelling imaging provides more representative insights into the microstructure, because it supplements the quantitative investigation of the number and width of twin lamellae with additional crystallographic orientation analysis provided by EBSD. To this end, two methods for adjusting EBSD data based on ion channelling images are proposed. Thorough selection of the complementary techniques opens future perspectives for the investigation of other challenging samples with nanoscale features in the microstructure.

High temperature corrosion during biomass firing: improved understanding by depth resolved characterisation of corrosion products

Abstract The high temperature corrosion of an austenitic stainless steel (TP 347H FG), widely utilised as a superheater tube material in Danish power stations, was investigated to verify the corrosion mechanisms related to biomass firing. KCl coated samples were exposed isothermally to 560°C, for one week, under conditions simulating straw-firing. Thorough characterisation of the exposed samples was conducted by the analysis of sample cross-sections applying microscopy and spectroscopy based techniques. Cross-section analysis revealed the microstructure, as well as chemical and morphological changes within the near surface region (covering both the deposit and the steel surface). Such cross-section analysis was further complemented by plan view investigations (additionally involving X-ray diffraction) combined with removal of the corrosion products. Improved insights into the nature of the corrosion products as a function of distance from the deposit surface were revealed through this comprehensive characterisation. Corrosion attack during simulated straw-firing conditions was observed to occur through both active oxidation and sulphidation mechanisms.

Phase Identification and Internal Stress Analysis of Steamside Oxides on Plant Exposed Superheater Tubes

During long-term, high-temperature exposure of superheater tubes in thermal power plants, various oxides are formed on the inner side (steamside) of the tubes, and oxide spallation is a serious problem for the power plant industry. Most often, oxidation in a steam atmosphere is investigated in laboratory experiments just mimicking the actual conditions in the power plant for simplified samples. On real plant-exposed superheater tubes, the steamside oxides are solely investigated microscopically. The feasibility of X-ray diffraction for the characterization of steamside oxidation on real plant-exposed superheater tubes was proven in the current work; the challenges for depth-resolved phase analysis and phase-specific residual stress analysis at the inner side of the tubes with concave surface curvature are discussed. Essential differences between the steamside oxides formed on two different steels typically applied for superheaters, ferritic-martensitic X20CrMoV12-1 and lean austenitic stainless steel TP347H, respectively, are revealed by X-ray diffraction.

Columns formed by multiple twinning in nickel layers—An approach of grain boundary engineering by electrodeposition

Complementary microscopic and diffraction based methods revealed a peculiar microstructure of electrodeposited nickel. For the as-deposited layer, thus, without any additional treatment, multiple twinning yields a high population of Σ3n boundaries, which interrupts the network of normal high angle grain boundaries. A peculiar arrangement of Σ3 boundaries forming five-fold junctions is observed. The resulting microstructure meets the requirements for grain boundary engineering. Twinning induced effects on the crystallographic orientation of grains result in one major texture component being a ⟨210⟩ fiber axis and additional minor orientations originating from first and second generation twins of ⟨210⟩, i.e., ⟨542⟩ and ⟨20 2 1⟩.