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Artificial bone replacement by individual customized three-dimensional resorbable bioactive glass has not yet been widely established in the clinical use. This is mainly due to the antagonism of sintering ability and suitable bioactivity. Competitive crystallization often prevents the generation of dense sintered bodies, especially for additive manufactured 3D structures. Previous studies of the fluoride-containing glass F3 have shown its potential to combine both sintering ability and suitable bioactivity. Furthermore, the occurring sintering blockade by surface crystallization of Na2CaSi2O6 was tunable by glass particle size.
In this study the glasses F3, F3-Cu with 1 mol% CuO added at the expense of CaO and the well-known 13-93 were chosen to determine the influence of surface crystallization on 3D printed sinter bodies. For this purpose, grain size fractions in range of smaller 32 µm to 315 µm in fraction size of 6-20 µm were sieved from jaw crushed glass frit as well as glass cubes were cut from casted blocks for all glasses. Sintering behavior of both pressed and printed powder compacts was observed via heating microscopy. Crystallization was determined by DTA and crystallization progress was monitored on fractured sinter bodies and polished cubes via electron and laser scanning microscopy as well as with diffractometry.
Depending on grain size the formation of crystalline support framework along former grain boundaries shows the capability to stabilize fully densified sinter bodies before softening. Beside of this, the generation of complex hierarchic porosity was possible as well.
Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well.
In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which could be used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions.
Laser metal deposition is described with its applications for additive manufacturing. The necessary process chain is discussed, with regard to weld bead dimensions and 3D build-up strategy. Metallurgical cross sections, x-ray and tensile tests are conducted. As demonstrative components, a gas turbine burner and a turbine blade are shown
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning.
Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, leading to potential efficiency and performance improvements. However, the rapid cooling rates associated with the process consequently leads to the generation of high magnitude residual stresses (RS). Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterization of these RS is essential for safety related engineering application and supporting the development of reliable numerical models. Diffraction-based methods for RS analysis using high energy synchrotron X-rays and neutrons enable non-destructive spatially resolved characterization of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research conducted by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys. Special focus will be given to the challenges posed by textured LPBF materials for the reliable choice of the diffraction elastic constants (DECs), which is crucial to the accurate calculation of the level of RS.
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
3D Charakterisierung wasserstoffunterstüzter Risse in Stahl mittels Synchrotron-Refraktions-CT
(2016)
Die Fehlertoleranz moderner hochfester Stähle gegenüber Prozessfehlern beim Fügen nimmt stetig ab und erfordert eine immer kritischere Beurteilung der Ergebnisse aus den vorhandenen Prüfverfahren. Deren Aussagekraft ist häufig zu gering und daher muss zum einen das wissenschaftliche Verständnis der Mikrokaltriss-Entstehung in diesen Stählen vertieft werden und zum anderen müssen die Prüfmethoden und Bewertungskriterien angepasst werden. Dies erfordert ein besseres Verständnis insbesondere der Kopplung von Eigenspannungen, Wasserstoffgehalten und der Wirkung äußerer Kräfte auf die Rissentstehung und das Risswachstum.
Erstmals soll mittels 3D-Synchrotron-Refraktions-Topographie an der BAMline am BESSY die Rissentstehung in mit Wasserstoff beladenen Zugproben charakterisiert werden. Diese Kenntnisse sollen in weiteren Untersuchungen auf Schweißnähte übertragen werden.
Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of complex structures. The quality of the feedstock material receives increasing attention, as it depicts the first part of the L-PBF process chain. The powder quality control in terms of flowability and powder bed packing density is therefore mandatory.
In this work, a workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape for three different powder batches. The polydisperse particle size distribution (PSD) was transformed into a statistically equivalent bidisperse PSD. The ratio of the small and large particles helped to understand the powder particle packing density. While the particle shape had a neglectable influence, the particle size distribution was identified as major contributor for the packing density.
Structure elucidation of complex synthetic copolymers still represents a challenge. A 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?
Is the coupling of liquid chromatographic separation techniques to mass spectrometry able to fill the gaps to a certain degree?
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.
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.
The lecture will provide a series of examples where LC-MS has been applied to evaluate complex macromolecules and mixtures of these.
On- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed.
Das DVS-Vorhaben 01.3211 „Herstellung beanspruchungsgerechter Oberflächen durch Kombination innovativer additiver und abtragender Fertigungsschritte an hochbelasteten Komponenten“ ist ein Kooperationsprojekt der Bundesanstalt für Materialforschung und -prüfung (BAM) und dem Institut für Schweißtechnik und Trennende Fertigungsverfahren (ISAF) der Technischen Universität Clausthal. Das Übergeordnete Projektziel ist das Erlangen von Erkenntnissen für eine sichere und wirtschaftliche, kombinierte additive und abtragende Fertigung aus kostenintensiven Werkstoffen hochbelasteter Komponenten insbesondere für KMU. Dabei stehe die beiden Werkstoffe CoCr26Ni9Mo5W (2.4681) und FeNi36 (1.3912) im Fokus. Mittels Modifikation der Schweißzusätze sind homogen und isotrop ausgeprägte Werkstoffeigenschaften und eine Erhöhung der Prozessstabilität und Fertigungsfreiheitsgrade bei der additiven Fertigung erzielbar. Darüber hinaus wird der Einfluss nachfolgender abtragender Bearbeitungsschritte des ultraschallunterstützen und des konventionellen Fräsprozesses untersucht. Im Laufe der Sitzung des projektbegleitenden Ausschusses (PbA) wurde der aktuelle Bearbeitungsstand sowie der Zeitplan vorgestellt. Darüber hinaus wurde mit dem PbA über die bereits erzielten Ergebnisse diskutiert. Abschließend wurde ein kurzer Ausblick über die zeitnah beginnenden Arbeiten beider Forschungseinrichtungen sowie ein Überblick über die vorhabenbezogenen Aufwendungen der Wirtschaft und des Ergebnistransfers in die Wirtschaft gegeben.
The slip-rolling 2Disk tribometer from Optimol Instruments represented the technological evolution in tribotesting of the well-known AMSLER-type tribometer marketed in 1922. Both use two discs with the same outer diameter rolling against each other on their circumference. In the AMSLER, the lower disc dips into an oil reservoir, whereas in the 2Disk the oil is injected into the contact. The oil supply of the 2Disk is controlled by pump and temperature by a heat exchanger.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
Actions from the meeting in April 2016: 1. Four SAC test methods are in place and were revised: SH/T 0721 (Grease, coefficient of friction and wear), SH/T 0784 (Grease, pass load/O.K. load), SH/T 0847 (Oil, coefficient of friction and wear) and SH/T 0882 released by 11-2014 (Oil, pass load/O.K. load). 2. New test method to evaluate anti-fretting properties of greases based was approved by SAC TC280 and will be released. 3. SAC TC280 accepted the project “Simulation of synchronizer by using SRV”. Draft text to be submitted by 03-2017. Discussions on a parallel ASTM test method. 4. A procedure for “Wear Volume” is under development for SAC TC280.
Tribological profile of hydraulic oils by using SRV. The determination of a set of critical, tribological by using different SRV-based test methods. The SRV-based concept of tribological profile generates the wear volumes on two triboelements (specimen), the extreme pressure properties and friction under different contact pressures.
Thus, the benchmark and validation of hydraulic oils bear on a wider range of tribological properties.
The RR2016 extends with six hydraulic oils to other base oil types including biodegradable fluids, which were all tested according to ASTM D7043 in order to consolidate the correlation between SRV and V104C.
The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed.
In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies!
(Pre)Standardisation and Metrology in Microbeam Analysis – Ongoing Activities and Opportunities
(2023)
The presentation addresses the current ongoing projects as well as the gaps and opportunities in microbeam analysis within ISO/TC 202 Microbeam Analysis standardisation body and in-liaison Technical Working Areas (TWAs) at the pre-standardization platform of VAMAS (Versailles Project on Advanced Materials and Standards).