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Spray drying based granulation processes aim for flowable granules neither containing voids nor hard shells thus leading to a homogenous microstructure in the green and sinter bodies without strength reducing large pores. The increase of the specific surface area due to the utilization of finer powders as raw materials makes the production of granules of demanded quality more sophisticated. Innovations regarding additives as well as process engineering are therefore required.
While conventional spray granulation processes of ceramic materials are based on rotational, one stream or two stream nozzles for nebulization, the investigations in the ZIM project concentrate on the applicability of an ultra sound atomizer unit. A spray dryer comprised of the aforementioned ultra sound atomization unit implemented in a commercial spray dryer (Niro, Denmark) was used as test system. Potential advantages of the ultra sound nebulization are investigated for model systems of alumina, zirconia and a ZTA composite while focusing on solids content, yield, pressability and granule properties (size, size distribution, flowability, shape and microstructure) as well as the final sinter body properties (density, microstructure and flexural strength).
First ultra sound spray drying experiments yielded granules with excellent processability. Spray drying of identical slurries, as before tested and optimized for a two stream nozzle atomization process, resulted in a more suitable size distribution for dry pressing (less particles below 20 µm) and a higher yield. Furthermore, sinter bodies produced of ultra sound granules seem to have less large pores and a more homogenous microstructure
Trapping in T24 steel weld joints – Effects on activation energy for hydrogen diffusion during TDA
(2017)
Failure cases in the past decade exhibited severe cracking in T24 welds and showed that generally hydrogen-assisted cracking (HAC) occurring up to 200°C cannot be excluded. A basic understanding is necessary on how hydrogen diffusion is influenced by the weld process. In this regard, both weld microstructures HAZ and weld metal have particular influence on hydrogen diffusion compared to the base material. In general, hydrogen diffusion at a certain temperature is described by diffusion coefficients representing an effective value of combined lattice diffusion and effects of reversible hydrogen traps. Those traps are typically precipitates, interstitials, grain boundaries and so on. A common approach to describe the trap character and its effect on diffusion is the determination of so-called activation energy. This can be done by respective thermal desorption analysis (TDA) with linear heating. In the present study, different T24 as-welded microstructures (BM, HAZ, WM) were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by TDA with linear heating using a mass spectrometer for detection of ultra-low hydrogen amounts. The results showed that typically the as-welded HAZ had higher energy traps than the tempered base material. Nonetheless two important effects were ascertained: (1) it is strictly necessary to monitor the sample temperature due to its great impact on the hydrogen desorption peak temperature and (2) the real heating rate in the specimen vs. the applied heating rate has to be considered. Both influence the calculated activation energy, i.e. the assigned hydrogen trap character (moderate or strong trap), which changed up to a factor of two in terms of the calculated activation energy. This effect can be much more important compared to the microstructure effect itself. Hence, suitable experimental boundary conditions should be mandatory for the determination of hydrogen trap kinetics.
The present work describes the shear creep behavior of the superalloy LEK 94 at temperatures between 980 and 1050 °C and shear stresses between 50 and 140 MPa for loading on the macroscopic crystallographic shear system (MCSS) (011)[01-1]. The strain rate versus strain curves show short primary and extended secondary creep regimes. We find an apparent activation energy for creep of Qapp = 466 kJ/mol and a Norton-law stress exponent of n = 6. With scanning transmission electron microscopy, we characterize three material states that differ in temperature, applied stress, and accumulated strain/time. Rafting develops perpendicular to the maximum principal stress direction, gamma channels fill with dislocations, superdislocations cut gamma' particles, and dislocation networks form at gamma/gamma' interfaces. Our findings are in agreement with previous results for high-temperature and low-stress [001] and [110] tensile creep testing, and for shear creep testing of the superalloys CMSX-4 and CMSX-6 on the MCSSs (111)[01-1] and (001)[100]. The parameters that characterize the evolving gamma/gamma' microstructure and the evolving dislocation substructures depend on creep temperature, stress, strain, and time.
Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels.
Additive Manufacturing (AM) by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts in comparison to the traditional subtractive manufacturing strategies. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
The current study reports on the effect of the sintering temperature and secondary carbide (VC, Mo2C and TiC) additions on the microstructure and concommitant Vickers hardness (HV30) and fracture toughness of Ni-bonded NbC cermets. All cermets were prepared by pressureless sintering in vacuum. Detailed microstructural investigation was performed by electron probe microanalysis (EPMA) and X-ray diffraction (XRD) analysis. Sintering results indicated that both the sintering temperature and secondary carbide additions had a significant effect on the properties of NbC-Ni cermets. Nickel pools and residual pores were observed in the cermets sintered at temperatures ≤ 1340 °C. Increasing of the sintering temperature up to 1420 or 1480 °C resulted in fully densified NbC-Ni based cermets composed of homogeneous contrast cubic NbC grains for the single carbide (VC or Mo2C) modyfied system, whereas core-rim structured NbC grains were observed with the additon of TiC + VC or TiC+Mo2C. The secondary carbide doped cermets with 5–10 vol.% VC/Mo2C and 10 vol.% TiC showed a significantly improved hardness and fracture toughness, as compared to the plain NbC-Ni cermets.
Magnesium (Mg) alloys have attracted much attention due to their merits of meeting requirements of lightweight, energy-efficient and environmental friendly engineering. In this study, a modified refill friction stir spot welding (refill-FSSW) method is proposed to weid AMSO Mg alloy, in which pin and sleeve rotate at different states. Effects of process parameters on the microstructure, material flow, and mechanical properties of welds were studied. Results showed that, the modified refill-FSSW technology could enhance the intennixing of material by changing the flow state. Lap shear strength of welds could be significantly improved with changed failure modes. The modified refill FSSW technology is a competitive welding method for Mg alloy.
The aluminum alloy 2618A is an Al-Cu-Mg alloy with additions of Fe and Ni, which was designed for long-term operation at elevated temperature in transportation and aerospace industries. Typical applications include aircraft parts and structures (sheet material) or engine components such as turbo charger centrifugal compressor wheels (forged material). Such components are subjected to prolonged aging during service, (e.g. 50 000 h) at temperatures which are close to their age hardening temperature (ca. 190 °C).
The microstructural evolution during creep exposure is studied.
The aluminum alloy 2618A is an Al-Cu-Mg alloy with additions of Fe and Ni, which was designed for long-term operation at elevated temperature in transportation and aerospace industries. Typical applications include aircraft parts and structures (sheet material) or engine components such as turbo charger centrifugal compressor wheels (forged material). Such components are subjected to prolonged aging during service, (e.g. 50 000 h) at temperatures which are close to their age hardening temperature (ca. 190 °C). The microstructural evolution was investigated.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2017)
Additive Manufacturing (AM) by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts in comparison to the traditional subtractive manufacturing strategies. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
In general, hydrogen assisted cracking is a result of a critical combination of local microstructure, mechanical load and hydrogen concentration. In that connection, welded microstructures of low-alloyed creep-resistant steels can show different hydrogen trapping kinetics. That influences the adsorbed hydrogen concentration as well as the diffusion itself in terms of moderate or strong trapping. A common approach to describe trapping is by the activation energy that is necessary to release hydrogen from a specific trap site. In the present study, T24 base material and weld metal were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis(TDA) with linear heating using a mass spectrometer. The results showed a microstructure effect on hydrogen trapping kinetics at elevated temperatures. Additionally, it is necessary to monitor the specimen temperature. A comparison between idealized temperature profile and real specimen temperature showed that the calculated activation energy varied up to a factor of two. Thus, the assigned trap character(moderate or strong) changed. In case of high temperature peaks, this effect could be more important compared to the microstructure effect itself.
Evaluation of high spatial resolution imaging of magnetic stray fields for early damage detection
(2017)
The paper discusses the evaluation of elastic and plastic strain states in two low-carbon steels of the same steel group with high spatial resolution GMR (giant magneto resistance) sensors. The residual stress distributions of tungsten inert gas welded plates were determined by means of neutron diffraction as a reference. The normal component of local residual magnetic stray fields arise in the vicinity of the positions of maximum stress. The experiments performed on flat tensile specimen indicate that the boundaries of plastic deformations are a source of stray fields. The spatial variations of magnetic stray fields for both the weld and the tensile samples are in the order of the earths magnetic field.
Additive Manufacturing by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts as compared to the traditional subtractive manufacturing strategies. However, the residual stresses (RS) developed during the processing can reduce the load bearing capacity as well as induce unwanted distortion, limiting the application of SLM parts. In the present work, residual stresses in additivly manufactured IN718 part were analised by means of neutron diffraction and synchrotron X-ray diffraction.
Copolymer structure elucidation by multidimensional techniques with focus on UPLC x ESI-TOF-MS
(2017)
Structure elucidation of complex synthetic copolymers still represents a challenge. An one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Herein a new approach is demonstrated to provide evidence of different functionalities and short block sequences in statistical EO-PO copolymers. Furthermore silsesquioxane mixtures and Polyglycerols are investigated concerning occurring topology effects.