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Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
For the additive manufacturing of large components typically powder-based methods are used. A powder is deposited layer by layer by means of a recoater, then, the component structure is printed into each individual layer. We introduce here the new method of local laser drying, which is a suspension-based method specially developed for the manufacturing of large voluminous ceramic parts. The structure information is directly written into the freshly deposited layer of suspension by laser drying. Initially, the technology was developed for ceramic suspensions, however, first experiments with geopolymers reveal a high potential for this class of materials. Metakaolin, fly ash and lithium aluminate-based one-part geopolymers were used in first experiments. The local annealing of the geopolymer slurry results in a drying and crosslinking reaction and, thus, in a local consolidation of the material. First parts made are introduced and their properties are discussed.
The layerwise slurry deposition (LSD) has been established in the recent years as a method for the deposition of ceramic powder layers. The LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade; each layer is sequentially deposited and dried to achieve a highly packed powder layer.
The combination of binder jetting and LSD was introduced as a novel technology named LSD-print. The LSD-print takes advantage of the speed of binder jetting to print large areas, parallel to the flexibility of the LSD, which allows the deposition of highly packed powder layers with a variety of ceramic materials.
The working principle and history of the LSD technology will be shortly discussed. A theoretical background will be also discussed, highlighting advantages and drawbacks of the LSD compared to the deposition of a dry powder.
The last part of the talk will be dedicated to highlight recent results on the LSD-print of SiSiC of geometrically complex components, in collaboration between BAM and HC Starck Ceramics GmbH. Density, microstructure and mechanical properties of LSD-printed and isostatic pressed samples will be discussed and compared.
During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained.
The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution.
Many metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminium alloys, the strengthening mechanism is based on the controlled formation of nanometre-sized precipitates, which represent obstacles to dislocation movement and consequently increase the strength. Precise tuning of the material microstructure is thus crucial for optimal mechanical behaviour under service condition of a component. Therefore, analysis of the microstructure, especially the precipitates, is essential to determine the optimum parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in the first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and thereafter quantify their relevant dimensions. Often, these evaluations are still performed by manual image analysis, which is very time-consuming and to some extent also poses reproducibility problems.
Our work aims at a semantic representation of an automatable digital approach for this material specific characterization method under adaption of FAIR data practices. Based on DF-TEM images of different precipitation states of a wrought aluminium alloy, the modularizable, digital workflow of quantitative analysis of precipitate dimensions is described. The integration of this workflow into a data pipeline concept will also be discussed. Using ontologies, the raw image data, their respective contextual information, and the resulting output data of the quantitative image analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure data reproducibility. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming (SEM, TEM).
Within the European project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nano-/non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The correct identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions of the particles. For particles containing micro-pores or having a microporous coating false positive results will be produced. Furthermore, broad particle size distributions make necessary to adjust the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and to improve this good available and agglomeration tolerant method.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles. Another technology, the Gas Flow Assisted Powder Deposition, can increase the stability of the powder bed and the packing density, even in extreme conditions such as in absence of gravitational forces.
Advanced light weight applications like aircrafts and wind turbine blades are made of fibre reinforced plastics (FRP) with continuous fibre reinforcement and must withstand a high thermo-mechanical cyclic loading. The quality of the fibre matrix interface has a high impact on the fatigue life and was continuously improved over the years since the 50th. The fatigue life of glass fibre reinforced plastics (GFRP) used in aircraft industry is 10 to 100 times higher compared to glass fibre non crimp fabrics used for wind turbine blades.
To assure a constant and reliable high quality and strength of reinforcement fibres, synthetic fibre production is state of the art (CF, GF). There is a need for recycling GFRP and CFRP waste due to the upcoming use. Pyrolysis and solvolysis are more expensive than the mechanical route however enable a more sustainable recycling. Natural fibres and recycled synthetic fibres have a high scatter in quality and strength. Hence it is a challenge to optimize the production / recycling processes to get a reliable quality for any demanding (second life) application.
Chemical routes for using renewables resources and recycling, is going to be a good approach especially for polymer-matrix systems to get 100% quality (back) compared to the state of the art.
Finally, a proper design, life-time extension and repair is preferable to recycling to keep the carbon footprint as low as possible.
The EU recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. Within the European Project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nanomaterial or non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nanomaterial or non-nanomaterial. The correct identification of a nanomaterial by VSSA method (positive test) is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape. For particles containing micro-pores or having a microporous coating, false positive results will be produced.
Furthermore, broad particle size distributions – as typically for ceramic materials – as well as multi-modal size distributions make necessary to adjust the threshold.
Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and
improve the method.
Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies.
The mechanical strength of wrought high-strength aluminum alloys is essentially based on precipitation hardening, possibly in combination with prior forming, e. g. by stretching. Important parameters for achieving an optimum combination of hardness, strength, ductility, toughness, and further properties such as corrosion resistance are age-hardening temperature and time.
During thermal (mechanical) treatment, nucleation and growth of precipitates takes place, leading to the desired degree of hardening. In aluminum alloys, precipitation sequences are usually passed through, i. e. a sequence of metastable precipitates is formed before the stable phase can precipitate. The optimum combination of properties is therefore based on a certain (optimum) microstructure, which can, however, change during the use of a component, since the microstructure is not stable. This happens in particular when the operating temperatures are close to the aging temperature and/or the operating times are sufficiently long. An external mechanical load may accelerate the processes. The presentation gives some examples for this.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices.
Low melting Li2O-PbO-B2O3, Me2O-ZnO-B2O3, Me = Li, Na, K, Rb and CaO-ZnO-B2O3 glasses were studied with Raman and infrared spectroscopies to advance the structural understanding of zinc borate glasses as potential candidates for substitution of lead containing glasses. Although the effect of type of alkali ions on the number (N4) of fourfold coordinated boron (B4) in the glasses is small, the alkali ions direct the type of borate groups, i.e., pentaborate in lithium, sodium, and calcium zinc borate glasses, as well as diborate in potassium and rubidium containing ones. Both groups were simultaneously found in Li2O-PbO-B2O3. Alkali ions are mainly responsible for the formation of B4-units and metaborate. Zinc ions favorably compensate non-bridging oxygen and partially form ZnO4. With decreasing N4 and field strength of the alkali ions the atomic packing density, glass transition temper ature and Young’s Modulus also decrease. The coefficient of thermal expansion increases with decreasing N4.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced. Finally, the extended research data management in this project is highlighted and its advantages for sustainable use in material science and engineering applications are shown.
The high operating temperatures of radial compressor wheels in exhaust gas turbochargers lead to abchange in the original microstructure of the heat-resistant aluminum alloy EN AW-2618A (overaging). This is caused by thermal loads that are close to the age hardening temperature and can even exceed it for a short time. The aging mechanisms have been investigated together with low cycle fatigue (LCF), thermomechanical fatigue (TMF) and creep up to max. 190 °C in previous research projects. The behavior of the alloy under high cycle fatigue (HCF) and the influence of load spectra have hardly been investigated. Since the operating temperatures of centrifugal compressors are expected to increase in the future, this research project investigated the HCF behavior at 230 °C, a test temperature significantly higher than the age hardening temperature. The objectives of the project were to establish a suitable experimental database, to understand the relevant microstructural processes, and to further develop and adapt suitable models and evaluation methods. In addition to a basic characterization of the HCF behavior in the initial condition T61, the experimental investigation program included targeted mechanical tests to isolate the influencing factors of mean stress (𝑅 = −1, 𝑅 = 0.1), material overaging (T61, 10 h/230 °C, 1000 h/230 °C), test temperature (20 °C, 230 °C), test frequency (0.2 Hz, 20 Hz) as well as variable amplitudes. On this basis, the models and evaluation methods developed in the previous projects were adapted and further developed to reflect thermal and mechanical loads in the lifetime assessment.
The high operating temperatures of radial compressor wheels in exhaust gas turbochargers lead to a change in the original microstructure of the heat-resistant aluminum alloy EN AW-2618A (overaging). This is caused by thermal loads that are close to the age hardening temperature and can even exceed it for a short time. The aging mechanisms have been investigated together with low cycle fatigue (LCF), thermomechanical fatigue (TMF) and creep up to max. 190 °C in previous research projects. The be-havior of the alloy under high cycle fatigue (HCF) and the influence of load spectra have hardly been investigated. Since the operating temperatures of centrifugal compressors are expected to increase in the future, this research project investigated the HCF behavior at 230 °C, a test temperature significantly higher than the age hardening temperature. The objectives of the project were to establish a suitable experimental database, to understand the relevant microstructural processes, and to further develop and adapt suitable models and evaluation methods.
In addition to a basic characterization of the HCF behavior in the initial condition T61, the experimental investigation program included targeted mechanical tests to isolate the influencing factors of mean stress (𝑅=−1, 𝑅=0.1), material overaging (T61, 10 h/230 °C, 1000 h/230 °C), test temperature (20 °C, 230 °C), test frequency (0.2 Hz, 20 Hz) as well as variable amplitudes. On this basis, the models and evaluation methods developed in the previous projects were adapted and further developed to reflect thermal and mechanical loads in the lifetime assessment.
Due to the increasing scarcity of critical raw materials current high-temperature materials are sought to be replaced by alloys based on more abundant metals. One possibility within the class of intermetallics are iron aluminides, which combine sustainability and cost-efficiency with the prospect of mass savings. Iron aluminides show competitive specific strength up to 700 °C and excellent creep and wet corrosion resistance by small additions of Mo, Ti and B. Nevertheless, a Mo content of above 2 at.% which is needed for optimum corrosion resistance results in enhanced brittleness, especially at room temperature. This is why alloys with these Mo fractions were only mechanically tested under compressive loading so far. Still, testing of static and creep properties under tensile loading is required for reliable component design. Besides high standards for crack-free processing, data acquisition for tensile loads is especially complicated by environmental embrittling effects for iron aluminides. To cope with these challenges, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated. The main goal is to collect standardised data on ambient and high-temperature tensile properties and creep properties. Samples with a nominal composition of Fe-26Al-4Mo-0.5Ti-1B [at.%] were manufactured via centrifugal casting in ceramic shell moulds followed by machining. Heat treatment for homogenisation and final polishing were carried out where appropriate. A summary of the achieved tensile and creep properties such as yield and tensile strength, maximum elongation, secondary creep rate and stress exponents will be given. Results will be also discussed regarding the influence of temperature, stress level and microstructure on the damage mechanisms. Furthermore, the effect of different alloy concentrations on the mechanical response at different temperatures will be outlined within a small experimental series.
Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. 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 residual stress distribution in the bulk of IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-build condition (on a build plate) and after removal from the build plate.
The absolute values of all stress components decreased after removal from the build plate. Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component depending on the thermal gradient in the respective direction.
Having been introduced almost two decades ago, Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. 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 residual stress distribution in IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron (bulk) and laboratory X-ray (surface) diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-build condition (on a build plate) and after removal from the build plate.
The absolute values of all stress components decreased after removal from the build plate. Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component depending on the thermal gradient in the respective direction.
Having been introduced almost two decades ago, Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. 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 residual stress distribution in IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron (bulk) and laboratory X-ray (surface) diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-build condition (on a build plate) and after removal from the build plate.
The absolute values of all stress components decreased after removal from the build plate. Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component depending on the thermal gradient in the respective direction.
The full-notch creep test (FNCT) is a common method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD) container materials . The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of specimens mechanically loaded in a well-defined liquid environment. Since the craze-crack damage mechanism underlying the ESC process is associated with brittle failure, the occurrence of globally brittle fracture surfaces is a prerequisite to consider an FNCT measurement as representative for ESC . Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. Due to the experimental setup, an inevitable increase of the true mechanical stress and the associated appearance of small ductile parts on fracture surfaces is induced in any case. Hence, an FNCT experiment is considered as 'valid', if the corresponding fracture surface is predominantly brittle . Based on laser scanning microscopy (LSM) height data of FNCT fracture surfaces , a universal and easy-to-use phenomenological criterion was developed to assess the validity of distinct FNCT experiments. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing.
The presentation will start with an overview of ceramic additive manufacturing (AM) technologies and will discuss the potential of AM in the field of bioceramics.
The presentation will then focus on two possible use cases of binder jetting technologies.
In the first example, standard powder-based binder jetting is used to manufacture a porous implant design for large scale bone defects. The related challenges in the process chain will be discussed, from powder synthesis to sintering and characterization of the printed part.
In the second example, the LSD-print slurry-based binder jetting technology is presented as a possibility to adapt powder-bed AM to produce dense ceramic parts. The use case will focus on an application in the field of dental ceramics, specifically for the manufacturing of patient individualized single tooth restorations (veneers, crowns) with a high throughput process chain.
Low melting zinc borate glasses awake interest to replace lead borate glasses in the silver metallization pastes for solar cells or microelectronics. In the current study, characteristic properties of alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) were compared to an earth alkali zinc borate glass (CaO-ZnO-B2O3). Additionally, zinc oxide is partially substituted by lead oxide or cooper oxide in the borate glasses (Li2O-PbO-B2O3, Na2O ZnO CuO-B2O3). The alkali zinc borate glasses indicate less differences in Raman spectra, and thus in structural properties, in comparison to the Ca and Pb ions influence. LPbB (Tg = 401 °C) has a lower viscosity than LZB (Tg = 468 °C) and CaZB has the highest glass transition temperature (Tg = 580 °C). The Angell plot for the alkali zinc borate glasses shows a high fragility m = 80. Besides Tg, the density measured by means of the Archimedean principle, molar volume, and coefficient of thermal expansion (CTE) of the glasses were investigated. Trends could be found according to alkali ions or intermediate oxides. The density increases with decreasing alkali ion size from KZB (2.632 g/cm3) to LZB (2.829 g/cm3) and increases from LZB to LPbB (3.764 g/cm3). CTE ranges between 7.09 10-6 K-1 for CaZB and 11.5 10 6 K 1 for KZB and RZB. The differential thermal analysis (DTA) and X ray diffraction (XRD) indicate crystallization of various crystalline phases during heating with 5 K/min in most cases.
The presence, fate and effects of microplastics (MP) in terrestrial systems are largely unknown. The few existing studies investigated either agricultural or industrial sites. Several techniques were used for analysis, primarly spectroscopic methods such as FTIR or Raman. Sample pretreatments like density separations are common to reduce matrix. A lack of harmonised and standardised sampling instructions for microplastic investigations in the terrestrial area was identified as particular critical, because different studies are barely comparable.
The aim of the project is to develop a proposal for a harmonized procedure for sampling, sample preparation and the detection of microplastics in terrestrial matrices for total content determination. By detecting specific degradation products the thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) allows a direct determination of mass content of MP in environmental samples.
Due to their excellent combination of ductility, strength and corrosive resistance, austenitic stainless steels (ASS) are widely used in many industrial applications. Thus, these steel grades can be found as structural components in the (petro-)chemical industry, in offshore applications and more recent for storage and transport of hydrogen fuel. Steels employed for these applications are exposed to aggressive environments and hydrogen containing media. The ingress and accumulation of hydrogen into the microstructure is commonly observed during service leading to a phenomenon called “hydrogen embrittlement”. A loss in ductility and strength, the formation of cracks and phase transformations are typical features of this hydrogen-induced degradation of mechanical properties.
Although, great efforts are made to understanding hydrogen embrittlement, there is an ongoing debate of the underlying mechanisms. This knowledge is crucial for the safe use and durability of components on the one side and the development of new materials on the other.
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a powerful tool for depicting the distribution of the hydrogen isotope deuterium in the microstructure of austenitic and duplex steels. The combination with imaging techniques such as electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM), delivering structural and morphological information, creates a comprehensive picture of the hydrogen/deuterium-induced effects in the materials. All the gathered data is treated with principal component analysis (PCA) and data fusion to enhance the depth of information.
The mobility of hydrogen and deuterium in a steel microstructure is affected by external mechanical stress. To investigate the behaviour of deuterium in a strained microstructure, a new in situ experimental approach was developed. This gives the possibility of analysing samples in the SIMS instrument simultaneously to four-point-bending-tests.
Specimens made from ASS AISI 304L were electrochemically charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and hydrogen existing in the pristine material or adsorbed from the rest gas in the analysis chamber. Nonetheless, similar diffusion, permeation and solubility data allow to draw qualitative conclusions from the experiments, which are relevant for the application addressed.
Ceramic multilayer technology is an attractive approach for the cost-effective fabrication of thermoelectric generators. Therefore, efforts are being made to co-sinter two promising thermoelectric oxides, namely calcium cobaltite and calcium manganate. In this study, calcium cobaltite, calcium manganate and release tapes were pressure assisted sintered. A major challenge here is the cracking of calcium manganate during cooling. A relationship between the properties of the release tape used in pressure-assisted sintering and the cracking behavior was observed experimentally.
To understand the origin of failure, formed reaction layers in the multilayer were analyzed by EDX and grazing incident XRD. Based on this analysis, bulk samples were prepared, and thermal expansion and Young's modulus and were determined thereon, if they were not known from the literature. The biaxial strength of the thermoelectric oxides was determined by the ball on three ball method.
The thermal stresses during cooling of different multilayer designs were estimated by finite element simulations. The stresses caused by the reaction layers turned out to be negligible. The FEM study indicated further, and a validation experiment proved, that the thickness of the release tape has the main effect on thermal stresses during cooling in single material. For best performance, the design of a thermoelectric multilayer generator needs to consider thermoelectric performance and thermal stresses during cooling.
High-performance composites, including glass-fiber reinforced plastic (GFRP) materials, are favored as a construction material for wind turbine rotor blades due to their high specific strength and stiffness properties. During the manufacturing process, however, imperfections are often introduced, then further propagated due to harsh environmental conditions and a variety of loads. This leads to failure significantly before their projected 20-year lifespan. As replacement of entire blades can be a costly potential outcome, localized repair of the damaged region to restore structural integrity and thus lengthen its lifespan has become an important issue in recent years. Rotor blades are often repaired using a common technique for composite laminates: adhesively bonded structural repair patches. These methods involve replacing the lost load path with a new material that is joined to the parent structure, and include scarf or plug repairs. However, there currently do not exist any standardized repair procedures for wind turbine rotor blades, as comparisons of blade properties repaired with the existing methods have not been studied in depth. Namely, there is a lack of understanding about the effects of various repair methods on the fatigue life of the shells of rotor blades. This study therefore aims to begin to fill this knowledge gap by testing the influence of different repair patches on the blades’ mechanical properties. Manufactured with the vacuum-assisted resin infusion process, the test specimens are produced as a curved structure with GFRP sandwiching a polyvinyl chloride foam core to best represent a portion of a rotor blade shell. Scarf repairs are then introduced with varying layup techniques, and material properties are examined with cyclical fatigue tests. Crack growth and development is monitored during fatigue testing by various non-destructive testing methods, including passive thermography with an infrared camera system, and a 3D deformation analysis system with ARAMIS. Large deformation fields and detection of in- and out-of-plane deformations is thus possible in-situ. The mechanical behavior and development of defects in the various repaired specimens is compared to each other as well as to reference test specimens with no repair patches. In-situ test data is combined with further non-destructive testing methods, including laminography, and active thermography, to develop a robust understanding of the effects of repair concepts.
Gypsum (CaSO4∙2H2O), bassanite (CaSO4∙0.5H2O), and anhydrite (CaSO4) are essential evaporite minerals for the evolution of hyper-arid surface environments on Earth and Mars (Voigt et al. 2019; Vaniman et al. 2018). The formation mechanism of especially anhydrite has been a matter of scientific debate for more than a century (van’t Hoff et al. 1903). To date, there exists no model that can reliably predict anhydrite formation at earth’s surface conditions. While thermodynamics favor its formation, it is hardly achieved on laboratory time scales at conditions fitting either the Atacama Desert on Earth, or the surface of Mars (Wehmann et al. 2023). In light of most recent developments (e.g. Stawski et al. 2016), that advocate for a complex, non-classical nucleation mechanism for all calcium sulphates, we present an analysis of natural samples from the Atacama Desert to identify key features that promote the nucleation and growth of anhydrite under planetary surface conditions. Our analyses reveal at least three distinct anhydrite facies, with differing mineralogy and micro- to nano-structures. The facies are (1) aeolian deposits with sub-μm grain sizes, (2) (sub-)surface nodules that formed from aeolian deposits and (3) selenites with secondary anhydrite rims. Possible mechanisms of their formation will be discussed.
Our research focused on Inconel 625 weld overlays on 16Mo3 steel boiler pipes. The Investigation focused on the characterization of changes in the microstructure and chemical composition after annealing. The annealing was performed for ten hours at temperatures from 600 to 1000°C. Changes in the microstructure were observed with a scanning and transmission electron microscope (SEM and TEM). The investigation was supplemented by hardness measurements.
Recent advances in Deep Learning (DL) have significantly impacted the field of materials modelling. DL tools have been recently considered as promising tools to address the complex relationships among processing, microstructure and property of materials. The thermal stability of polycrystalline materials is a highly interesting and complex problem that could be addressed using DL techniques. The Multi-Phase-Field (MPF) method has emerged as a powerful tool for addressing grain growth phenomena from multiple perspectives. Unlike sharp-interface based methods, the MPF approach bypasses the need for detailed information on individual grains. In this work, we use DL to address issues related to MPF simulations of grain growth including numerical efficiency, computing speed, and resource consumption. This presents specific challenges for high-performance computing (HPC) due to the large datasets and complex computations required by both MPF and DL methods. We study various 3D microstructure settings with the goal of accelerating the simulation process while exploring different physical effects. In particular, the impact of grain boundary and triple junction energies on grain growth are to be investigated. The results will be presented in terms of the evolving size and shape distribution of the grains.
Corrosion Science Meets X-Rays, Neutrons and Electrons. The presentation gives an overview on current research activities applying in-situ X-ray diffraction and spectroscopy for a better understanding of fundamental mechanisms of high temperature corrosion. Additionally the knowledge gain by applying neutron powder diffraction and EBSD analysis is presented.
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.
The elastic properties (Young's modulus, shear modulus) of austenitic stainless steel AISI 316L were investigated between room temperature and 900 °C in an additively manufactured variant (laser powder bed fusion, PBF‑LB/M) and from a conventional process route (hot rolled sheet). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
The elastic properties (Young's modulus, shear modulus) of Ni-based alloy Inconel IN718 were investigated between room temperature and 800 °C in an additively manufactured variant (laser powder bed fusion, PBF‑LB/M) and from a conventional process route (hot rolled bar). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
The elastic properties (Young's modulus, shear modulus) of titanium alloy Ti-6Al-4V were investigated between room temperature and 400 °C in an additively manufactured variant (laser-based directed energy deposition with powder as feedstock, DED-LB/M) and from a conventional process route (hot rolled bar). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, microstructure, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
The Binder Jetting BJ process is one of the most versatile additive manufacturing technologies in use. In this process a binder is locally jetted into a powder bed for the consolidation of a 3D structure, layer by layer. Basically, all materials which can be provided as a flowable powder and, thus, spreadable to a thin layer, can be processed. Metals, ceramics and polymers are processable, but also materials from nature, such as sand, wood sawdust and insect frass. Moreover, the BJ technology is adapted to large building volumes of some cubic meters easily. Besides these striking advantages, the manufacture of ceramic parts by BJ is still challenging, as the packing density of the powder bed is generally too low and the particle size of a flowable powder too large for a successful densification of printed parts in a subsequent sintering step to an advanced ceramic product. After an introduction of binder jetting in general and highlighting some examples, strategies for obtaining dense ceramic parts by BJ will be introduced.
Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductivity/osteoinductivity. Nowadays, hydroxyapatite (HA) and tricalcium phosphate (TCP) are the most widespread ceramics for bone grafting at the market, however, their resorption is reported, in some cases, to be not enough. This is why the search for more soluble ceramics compared to HA and TCP looks rather viable.
A possible way to increase ceramics solubility leads to partial substitution of Ca2+-ions in Ca3(PO4)2 by alkali castions, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy, but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making study of sintering of aforementioned ceramics highly important.
Brinell test ontology (BTO)
(2024)
Brinell Test Ontology (BTO) has developed for representing the Brinell testing process, testing equipment requirements, test pieces charactristics, and related testing parameters and their measurement procedure according to DIN EN ISO 6506-1 standard.
Versions info:
V2 developed using BFO+CCO top-level ontologies.
V3 developed using EMMO+CHAMEO top-level ontologies.
V4 developed using PROVO+PMDco top-level ontologies.
V5 developed using BFO+IOF top-level ontologies.
Repositories:
GitLab: https://gitlab.com/kupferdigital/process-graphs/brinell-hardness-test
GitHub: https://github.com/HosseinBeygiNasrabadi/Brinell-Test-Ontology-BTO-
MatPortal: https://matportal.org/ontologies/BTO
IndustryPortal: https://industryportal.enit.fr/ontologies/BTO
Additive manufacturing (AM) processes are opening new design possibilities for large scale electrical devices such as power generators. Conventional manufacturing methods use copper rods which are wrapped, vacuum impregnated, bend and welded. These processes are labor-intensive and time-consuming. The introduction of AM methods for manufacturing the copper conductor and electrical insulation can reduce the size of the generator head, the most complex part of the generator.
In this study, the electrical and dielectrical properties of additively deposited ceramic layers are investigated and compared with the properties of conventionally fabricated bulk ceramics. The ceramic layers are thermally deposited by atmospheric plasma spraying of a commercially available alumina powder. Bulk ceramics are fabricated by dry pressing and sintering of the same powder. Microstructure and porosity were analyzed by scanning electron microscopy (SEM). Electrical and dielectrical properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards.
The microstructures of sprayed and sintered alumina show significant differences with respect to grain form and porosity. The density of the bulk ceramic is lower than the density of the sprayed layer due to the coarse particle size (d50 = 33 μm). Therefore, data from dense samples of the same chemical composition but lower particle size alumina powder were used for comparison.
CALM is software for determining the Bravais lattice type and the resulting lattice parameters from a single Kikuchi pattern. It requires the definition of 4 bands and a single bandwidth from which all other band positions as well as bandwidths are derived. For band detection, it uses the Funk transform, which allows detection of twice as many bands as usual. CALM works for any symmetry and requires low-noise patterns of at least 320x240 pixels. The resulting errors are <2% even for such small patterns, assuming good quality. The relative errors are <0.5%. However, this requires a projection centre position best derived from a sample of a cubic phase in CALM. However, this must have been recorded under identical conditions. Hundreds of Kikuchi patterns of phases with different symmetries were examined.
Engineering grain boundaries demands a quantitative description of both their segregation and specific phase behavior. Recently I have proposed a density-based model for grain boundary thermodynamics that enables CALPHAD integrated derivation of grain boundary phase diagrams, broadly applied now in studying various alloys. Combining this model with experimental investigations, in this talk, new aspects of interfacial segregation and phase transformation revealed in polycrystalline alloys are discussed. The effect of elastic interaction on grain boundary phase behavior is incorporated. We consider Al alloys and novel high-entropy alloys and discuss a general strategy for grain boundary engineering.