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Nanotechnology at BAM
(2017)
An improved method of powder 3D printing leading to dense ceramic parts is presented. The application of powder-based binder jetting 3D printing technologies to technical ceramics is generally limited by the low packing density of the powder and by the need to use a flowable powder. With layer-wise slurry deposition, it is, however, possible to deposit powder beds with high particle packing and furthermore using submicron powders. This method was combined with the binder jetting technology to develop a novel process, named LSD-print. By means of LSD-print, a submicron Al2O3 powder could be processed to produce samples with a density comparable with that of standard pressed samples, both in the green state and after sintering.
Several Additive Manufacturing (AM) processes are based on the deposition of a powder to form a powder bed layer-by-layer, which typically has a low packing density (35-50%) and consequently hinders the ability of sintering ceramic parts to full density.
The layerwise slurry deposition (LSD) is an innovative process for the deposition of layers in AM. In the LSD, a slurry with no or small organic content is repetitively spread as thin layers on each other by means of a doctor blade. During the deposition, the ceramic particles settle to form thin layers with a high packing density (55-60%). When coupled with a printing head or with a laser, the LSD enables novel AM technologies inspired to the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder-bed.
The LSD combined with inkjet binder printing (LSD-print) was applied to a submicron Al2O3 powder to produce samples which had a comparable density to uniaxially pressed samples, both in the green and in the sintered state.
The layer-wise slurry deposition (LSD) is an innovative process for the deposition of powder layers with a high packing density for Additive Manufacturing (AM). A slurry with small organic content is repetitively spread as thin layers on top of each other by means of a doctor blade. During the deposition, the ceramic particles settle to form thin layers with a high packing density (55-60%). Each layer is then dried, resulting in the stacking of a dry powder bed with high powder packing. When coupled with a printing head or with a laser source, the LSD enables novel AM technologies inspired to the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder bed.
The LSD -3D printing, in particular, offers the potential of producing large (> 100 mm) and high quality ceramic parts, with microstructure and properties similar to traditional processing.
This presentation will give an overview of the milestones in the development of this technology, with focus on the latest results applied both to silicate and to technical ceramics.
The kinetics of the anodic dissolution of brass (CuZn42 and CuZn21Si3P) in synthetic tap water were investigated by atomic emission spectroelectrochemistry. Elemental Cu and Zn dissolution rates were measured in situ and in real time during galvanostatic dissolution. A complete mass/charge balance for the system yielded, as a function of applied current and a function of time, the quantity of Cu in the dezincification layer and the quantity of Cu and Zn in the oxide layer. In this way, a complete kinetic characterization of the fundamental chemical processes occurring during dezincification was realized for the first time. The oxide layer was composed primarily of Cu2O as indicated by grazing incidence XRD and Raman analysis. The soluble Cu oxidation product was determined to be Cu(II) by a mass/charge balance. Zn was oxidized to soluble Zn(II) leaving behind a trivial amount of solid Zn corrosion product on the surface. The kinetic analysis depicts a two-stage dissolution process of dezincification: a first stage of a rapid growth of the dezincified layer and a second stage where the growth of dezincified layer was much slower. The Cu2O layer grows continually during the exposure.
Efficient water oxidation catalysts are required for the development of water splitting technologies. Herein, the synthesis of layered hybrid NiFephenylphosphonate compounds from metal acetylacetonate precursors and phenylphosphonic acid in benzyl alcohol, and their Oxygen evolution reaction performance in alkaline medium, are reported. The hybrid particles are formed by inorganic layers of NiO6 and FeO6 distorted octahedra separated by bilayers of the organic group, and template the Formation in situ of NiFe hydroxide nanosheets of sizes between 5 and 25 nm and thicknesses between 3 and 10 nm. X-ray absorption spectroscopy measurements suggest that the hybrid also acts as a template for the local structure of the metal sites in the active catalyst, which remain distorted after the transformation. Optimum electrocatalytic activity is achieved with the hybrid compound with a Fe content of 16%. The combination of the synergistic effect between Ni and Fe with the structural properties of the hybrid results in an efficient catalyst that generates a current density of 10 mA cm−2 at an overpotential of 240 mV, and also in a stable catalyst that operates continuously at low overpotentials for 160 h.
Carbon nanotube-grafted carbon fiber polymer composites: Damage characterization on the micro scale
(2017)
Multiwall carbon nanotubes (CNTs) e carbon fibers (CFs)hybrid materials were produced by directly growing CNTs on CFs by means of chemical vapor deposition. For the latter, the oxidative dehydrogenation reaction of C2H2 and CO2 was applied, which allows growing CNTs without damaging the CF surface. Uni-directional nano-engineered carbon fiber reinforced composites (nFRCs) were fabricated by impregnating these hybrid materials with epoxy. The nFRCs subjected to single fiber push-out tests revealed a decrease of the interfacial shear strength (IFSS) of about 36% compared to the carbon fiber composites without CNTs. By means of transverse three-point bending tests performed on pre-notched composite beams inside a scanning electron microscope, the fracturing behavior parallel to the fibers was studied in-situ. The nFRCs showed significantly reduced fiber/matrix debonding while CNTs pull-out, CNTs bridging as well as matrix failure occurred. These results demonstrate that the presence of CNTs in nFRCs affects the stress distribution and consequently the damage Initiation as well as the damage propagation. The presence of CNTs suppresses the stress concentration at the fiber/Matrix interface and reduces the debonding of CFs from the matrix. However, our results indicate that the stress concentration shifts towards the CNTs' ends/matrix interface and causes promoted matrix failure leading to lower IFSS.
High-strength steels are favoured materials in the industry for production of safe and sustainable structures. The main technology used for joining the components of such steel is fusion welding.
Steel alloy design concepts combined with advanced processing technologies have been extensively investigated during the development of High-Strength Low-Alloy (HSLA) steels. However, very few studies have addressed the issue of how various alloy designs, even with limited microalloy addition, can influence the properties of high-strength steel welds. In high-strength steel welding practices, the challenges regarding microstructure evolution and the resulting mechanical properties variation, are of great interest. The main focus is the debate regarding the role of microalloy elements on phase transformation and weld performance. Limited Heat Affected Zone (HAZ) softening and limited austenite grain coarsening are significant design essentials, but the primary goal is to ensure excellent toughness and tensile properties in the steel weld. To achieve this purpose, microalloy elements such as Ti, Nb, or V were intentionally added to modern high-strength steels. The focus of this work was to understand the mechanical properties of HSLA steels resulting from differences in alloy design after joining by modern welding processes.
To begin, three microalloyed S690QL steels (Nb, Ti, and Ti+V addition) were investigated. Optical microscopy confirmed that similar mixtures of tempered bainite and martensite predominated the parent microstructure in the three steels, different types of coarse microalloy precipitates were also visible. These precipitates were analysed by using a thermodynamic-based software and then identified by Transmission Electron Microscopy (TEM). Results of mechanical testing revealed that all three steels performed above the standard toughness and tensile strength values, but with varied yielding phenomena. During the welding operation, each of the three steels was joined by using the same filler material. The fused weld metal was influenced by the high dilution of microalloyed elements in the base metal, this was significantly pronounced during the modified spray arc welding technique. As a result, the Nb-containing steel exhibited sufficient amounts of alloy pick-up to transition the microstructure in the weld metal from acicular ferrite to bainite as cooling rate was increased, leading to reduced toughness. This was not observed with the other two steels.
A second focus was made on the microstructure Evolution and toughness properties of the coarse and fine grained HAZ as welding parameters changed. In order to characterise the microstructure and austenite grain growth behaviour, physical simulations were conducted. The microalloy precipitates were found to be a dominant factor restricting the austenite grain coarsening. The extent of Austenite coarsening in the HAZ is closely related to the type and volume fraction of each microalloy precipitate.
Among the three steels, the Ti-containing HAZ exhibited the smallest extent of grain growth due to the sufficient amount of stable Ti-rich precipitates. Microalloy Addition also markedly influenced the subsequent phase transformation in the HAZ. The formation of intragranular acicular ferrite was promoted by Ti-rich precipitate, acting as favourable nucleation sites of ferrite. This structure enhanced the HAZ toughness owing to fine, high-angle boundaries of ferrite plates. The synergistic effect of Nb and Mo elements was beneficial to improve the HAZ toughness at fast cooling rates by promoting fine lower bainite formation. At high heat input, large upper bainite was formed which caused reduced toughness.
The final set of experimental work was concentrated on understanding the HAZ softening mechanisms that influenced variations in the tensile properties of the welded joints. The tensile failure in the softened HAZ or base material depended on the welding parameters and the type of steel being joined. In Ti-containing steel, increased heat Input extended the softened zone width, which caused a significant decrease in hardness and then resulted in failure in this area. Therefore, limited heat Input was used to shift failure position to base material. But this was not observed in the other two steels.
Hence, small differences in microalloy addition exhibited large variation in tensile properties. Among the three steels, Ti-containing welds were found to have the most pronounced softening, followed by Ti+V-containing welds and finally Nb-containing welds. This varied softening phenomenon was related to two significant processes supported by the results of additional dilatometry simulation: phase transformation and tempering behaviour. In the Ti-containing steel, the phase Transformation product ferrite was large-sized, as a consequence of initial large austenite grains. This led to the decreased corresponding hardness of the Ti-containing steel. Furthermore, lower tempering resistance in Ti-containing steel as compared to Nb-containing steel, resulted in additional softening effect in the softened HAZ. Therefore, steel alloy identification and heat Input during welding were critical, proven by the experimentation within the same S690QL steel grade.
This work emphasised the influence of microalloy elements on weld microstructure and mechanical properties in welded joints. Knowledge of this delicate balance between steel alloy design and appropriate welding parameters is critical for the end product. Thus, this work provides specific recommendations and results to ensure proper welding practice and steel design of microalloyed high-strength steels.
If fracture mechanics shall be applied to the total lifetime respectively the fatigue limit of components (within the meaning of the S-N curve approach) it has to address four challenges:
(a) It has to adequately describe so-called short crack propagation, which cannot be based on the common long crack concepts for principle reasons. Since the crack size is in the order of the plastic zone size, the modelling of short crack propagation cannot be based on the common linear elastic Delta K concept. Instead, an elastic-plastic parameter such as the cyclic J integral has to be applied. A second point is that the crack closure concept has to be modified in that the crack opening stress is not a constant, crack size- independent parameter but shows a transient behaviour with increasing short crack size.
(b) It has to provide a meaningful definition of the initial crack dimensions as the starting point for an S-N curve relevant (residual) lifetime analysis. This can be based either on the (statistical) size of material defects which can be treated as cracks or by the size of the crack which would arrest subsequent to early crack propagation, whatever is larger.
(c) It has to cope with the problem of multiple cracks for load levels higher than the fatigue limit such as it occurs in many applications in the absence of very large initial defects.
(d) This requires consequent statistical treatment taking into account variations in the local geometry of the area where crack initiation has to be expected as well as the scatter in the initial crack size and in the material data used for the analyses.
If fracture mechanics shall be applied to the total lifetime respectively the fatigue limit of components (within the meaning of the S-N curve approach) it has to address four challenges:
(a) It has to adequately describe so-called short crack propagation, which cannot be based on the common long crack concepts for principle reasons. Since the crack size is in the order of the plastic zone size, the modelling of short crack propagation cannot be based on the common linear elastic Delta K concept. Instead, an elastic-plastic parameter such as the cyclic J integral has to be applied. A second point is that the crack closure concept has to be modified in that the crack opening stress is not a constant, crack size- independent parameter but shows a transient behaviour with increasing short crack size.
(b) It has to provide a meaningful definition of the initial crack dimensions as the starting point for an S-N curve relevant (residual) lifetime analysis. This can be based either on the (statistical) size of material defects which can be treated as cracks or by the size of the crack which would arrest subsequent to early crack propagation, whatever is larger.
(c) It has to cope with the problem of multiple cracks for load levels higher than the fatigue limit such as it occurs in many applications in the absence of very large initial defects.
(d) This requires consequent statistical treatment taking into account variations in the local geometry of the area where crack initiation has to be expected as well as the scatter in the initial crack size and in the material data used for the analyses.