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Since the BSE signal depends on many factors, like the chemistry of the phase and the acceleration voltage, the size and position of the detector array is (slightly) different from phase to phase so that an (iterative) post-processing of the stored patterns is highly recommended. The derived BSE signal can be used for phase assignment in high resolution and high speed maps when EBSD fails and/or EDS (energy dispersive spectroscopy) needs too much time for a suitable and parallel signal acquisition.
The understanding of process-microstructure-property-performance (PMPP) relationships in additive manufacturing (AM) of metals is highly necessary to achieve wide-spread industrial application and replace conventionally manufactured parts, especially regarding safety-relevant applications. To achieve this understanding, reliable data and knowledge regarding material’s microstructure-property relationships (e.g. the role of defects) is needed, since it represents the base for future more targeted process optimizations and more reliable calculations of performance. However, producing reliable material data and assessing the AM material behaviour is not an easy task: big challenges are e.g. the actual lack of standard testing methods for AM materials and the occasional difficulties in finding one-to-one comparable material data for the conventional counterpart.
This work aims to contribute to end this lack of reliable material data and knowledge for the low cycle fatigue behaviour of the most used titanium alloy in aerospace applications (Ti-6Al-4V). For this purpose, two sets of test specimens were investigated. The first set was manufactured from cylindrical rods produced by an optimized DED-L process and the second was manufactured from a hot formed round bar. The test specimens were cyclically loaded until failure in the low-cycle-fatigue (LCF) regime. The tests were carried out according to ISO 12106 between 0.3 to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behaviour is described and compared between materials and with literature values based on cyclic deformation curves and strain-based fatigue life curves. Besides, the parameters of Manson-Coffin-Basquin relationship were calculated. The microstructures (initial and after failure) and fracture surfaces were comparative characterized. Thereby, the focus lied on understanding the role of grain morphology and defects on the failure mechanisms and fatigue lifetimes. For this latter characterization, optical microscopy (OM), scanning electron microscopy (SEM) and micro computed tomography (µCT) were used.
In Additive Manufacturing everybody is talking about Free Form, Unconventional Design, Re-thinking Components, “Think out of the box”.
However, there are a few outstanding question: a) What are the material properties ? They certainly differ from literature values for conventional materials; b) How about the microstructure? It is different from conventional materials. Does it stay so with ageing? How does it form? c) Do we properly take residual stress into account? We often blame them for our ignorance about failure scenarios. d) Do we apply tailored heat treatments? Very often, we follow conventional schedules…
This talk describes the summary of the efforts carried out within the BAM Project AGIL.
At BAM, we aimed to thoroughly investigate the microstructure and how it evolves as a function of load and temperature (service), to determine the material properties after different process and service conditions, to properly determine residual stress and the way it impacts mechanical properties and component performance, to properly quantify the impact of (unavoidable?) defects, and to determine heat treatments tailored to the process-specific material (stress relieve, microstructure homogenization etc.).
The Project AGIL was and is intimately coupled with the project ProMoAM, dealing with online monitoring of AM processes.
The roles of microalloying niobium, titanium and vanadium for controlling austenite grain growth, microstructure evolution and hardness were investigated at different simulated heat affected zones (HAZ) for high strength low alloy (HSLA) S690QL steel. High resolution FEG-SEM has been used to characterize fine bainitic ferrite, martensite and nanosized second phases at simulated coarse and fine grain HAZs. It was found that for Ti bearing steel (Ti/N ratio is 2) austenite grain had the slowest growth rate due to the presence of most stable TiN. The fine cuboidal particles promoted intragranular acicular ferrite (IGF) formation. Nb bearing steel exhibited relatively weaker grain growth retardation compared with titanium bearing steels and a mixed microstructure of bainite and martensite was present for all simulated HAZs. IGF existed at coarse grain HAZ of Ti+V bearing steel but it was totally replaced by bainite at fine grain HAZs. Hardness result was closely related to the morphology of bainitic ferrite, intragranular ferrite and second phases within ferrite. The microstructure and hardness results of different simulated HAZs were in good agreement with welded experimental results.
Avoid living dangerously: non-destructive characterization of AM parts from powder to end-of-life
(2019)
The freeform and the revolutionary design possibilities offered by additive manufacturing have skyrocketed the amount of optimization studies in the realm of engineering, and metallic additive manufactured parts are becoming a reality in industry.
Not surprisingly, this has not been paralleled by a similar enthusiastic wave in the realm of materials science, and still very little is known about AM materials properties. This has the consequence that, typically, conventional materials properties are still used in design and even in simulations.
lt is necessary to dig a lot deeper than at present, in order to understand these new materials classes, and in particular their microstructure and their intemal stresses, largely different from their cast or wrought companions.
Alkali silica reaction (ASR) is a major concrete durability problem resulting in significant maintenance and reconstruction costs for concrete infrastructures all over the world. To determine whether an aggregate is potentially reactive, accelerated concrete tests are used. Aim of this study is the chemical and microstructural characterization of ASR-products formed under the performance conditions of motorway pavements and during subsequent tests on the remaining ASR susceptibility. Samples were taken from concrete motorway pavements. Some of the samples already showed first indications for beginning damages whereas others showed deteriorations only after applying a performance testing procedure for the estimation of future risk of ASR damage. In a first step ASR-products were identified by polarized light microscopy in thin sections. The reaction products where then analyzed by Raman Spectroscopy and finally the chemical composition of the ASR-products was identified by SEM with EDX.
The results indicate that most reaction products show an increasing Ca/Si-ratio with progressive crack length. If an ASR-product develops inside an aggregate and moves through the cement paste, it has a high (Na+K)/Si-ratio at the beginning which decreases with increasing distance from its place of origin. The Raman spectra of the ASR-products are characterized by two broad bands indicating specific Q-species of different amorphous gel networks. Within the scope of the analysis distinctions in the microstructure and the chemical composition of the ASR-gels were detected relating to various conditions of accelerated testing.
Composite Facade Elements with Self-Cleaning Surface made of Ultra-High-Performance Concrete (UHPC)
(2020)
In the framework of the European project H-House various concrete façade elements were developed with the aim to ensure a long service life by combining a very durable material with self-cleaning properties. The façade elements presented are made of a shell of UHPC filled with blocks of aerated autoclaved concrete as insulating material. Self-cleaning properties were realized amongst others by imprinting a microstructure into the surface during casting. The paper focuses on selected technological aspects of the manufacturing process of prototypes which had to be performed in two concreting sections. Furthermore the challenges faced when upscaling the self-cleaning properties are addressed and the strategy to assess the self-cleaning properties by measuring the contact and the roll-off angel is presented. The results show that a successfull upscalaing process requires detailed planning and that the best results can often be achieved with a moderate work effort or material use.
Composite Facade Elements with Self-Cleaning Surface made of Ultra-High-Performance Concrete (UHPC)
(2020)
In the framework of the European project H-House various concrete façade elements were developed with the aim to ensure a long service life by combining a very durable material with self-cleaning properties. The façade elements presented are made of a shell of UHPC filled with blocks of aerated autoclaved concrete as insulating material. Self-cleaning properties were realized amongst others by imprinting a microstructure into the surface during casting. The paper focuses on selected technological aspects of the manufacturing process of prototypes which had to be performed in two concreting sections. Furthermore the challenges faced when upscaling the self-cleaning properties are addressed and the strategy to assess the self-cleaning properties by measuring the contact and the roll-off angel is presented. The results show that a successfull upscalaing process requires detailed planning and that the best results can often be achieved with a moderate work effort or material use.
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.
Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L
(2020)
A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage.