TY - CONF A1 - Abram, Sarah-Luise A1 - Mrkwitschka, Paul A1 - Prinz, Carsten A1 - Rühle, Bastian A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan A1 - Resch-Genger, Ute T1 - Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements N2 - In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles. The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum. 1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties. 2. Iron oxide nanoparticles are under development as new candidate reference material at BAM. 3. Narrow particle size distribution confirmed by light scattering and electron microscopy. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Electron microscopy KW - Nanoplattform PY - 2020 AN - OPUS4-52774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides N2 - Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced. Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant. T2 - Virtual Conference on Thermoelectrics (VCT) CY - Online meeting DA - 21.07.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives KW - Calcium manganate KW - Calcium cobaltite PY - 2020 AN - OPUS4-51070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Improved thermoelectric properties of CaMnO3 and Ca3Co4O9 by increasing the driving force for sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties. The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives. All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower. T2 - Electroceramics XVII CY - Online meeting DA - 24.08.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives PY - 2020 AN - OPUS4-51163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite JF - Journal of the American Ceramic Society N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinellato, Fabio A1 - Wilbig, Janka A1 - Al-Sabbagh, Dominik A1 - Colombo, P. A1 - Günster, Jens T1 - Gas flow assisted powder deposition for enhanced flowability of fine powders: 3D printing of alpha-tricalcium phosphate JF - Open Ceramics N2 - The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts. KW - Additive Manufacturing KW - Binder Jetting KW - Gas flow assisted powder deposition KW - Alpha-tricalcium phosphate KW - Scaffold PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510138 DO - https://doi.org/10.1016/j.oceram.2020.100003 SN - 2666-5395 VL - 1 SP - 100003 PB - Elsevier Ltd. AN - OPUS4-51013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Melo Bernardino, Raphael A1 - Valentino, S. A1 - Franchin, G. A1 - Günster, Jens A1 - Zocca, Andrea T1 - Manufacturing of ceramic components with internal channels by a novel additive/subtractive hybridizazion process JF - Open Ceramics N2 - A new approach for fabrication of ceramic components with inner channels is proposed, as a result of the combination of two additive and one subtractive manufacturing processes. In this project, porcelain parts are manufactured by the Layerwise Slurry Deposition (LSD) process, meanwhile end milling and Direct Ink Writing (DIW) are applied to create channels on the surface of the deposited ceramic. Unique to the LSD process is the Formation of a freestanding powder bed with a mechanical strength comparable to conventional slip casted ceramic green bodies. Combining these three processes allows the manufacturing of ceramic objects containing an internal path of ink, which in this case was a graphite-based ink that can be further eliminated by heat treatment to obtain a porcelain object embedded with channels. The results show the capabilities of this method and its potential to fabricate not only parts with inner channels, but also multi-material and multi-functional components (such as integrated electronic circuits). KW - Additive Manufacturing KW - Layerwise Slurry Deposition KW - Hybrid Manufacturing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510012 UR - https://www.sciencedirect.com/science/article/pii/S2666539520300109?via%3Dihub DO - https://doi.org/10.1016/j.oceram.2020.100010 VL - 2 SP - 100010 PB - Elsevier Ltd. AN - OPUS4-51001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gibson, N. A1 - Kuchenbecker, Petra A1 - Rasmussen, K. A1 - Hodoroaba, Vasile-Dan A1 - Rauscher, H. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A.G. T1 - Volume-specific surface area by gas adsorption analysis with the BET method T2 - Characterization of nanoparticles - Measurement processes for nanoparticles N2 - This chapter first gives an introduction to the concepts of SSA and volume-specific surface area (VSSA) and an outline of the BET method. It continues with a discussion of the relationship between particle size, shape, and the VSSA, followed by an overview of instrumentation, experimental methods, and standards. Finally, sections on the use of the VSSA as a tool to identify nanomaterials and non-nanomaterials and its role in a regulatory context provide some insight on the importance of VSSA in the current Regulation of nanomaterials. KW - Nanomaterials KW - Volume specific surface area PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00017-1 SP - 265 EP - 293 PB - Elsevier CY - Amsterdam AN - OPUS4-49572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Gojani, Ardian A1 - Völker, Tobias A1 - Günther, Tobias A1 - Gornushkin, Igor B. A1 - Wilsch, Gerd A1 - Günster, Jens T1 - Investigation of grain sizes in cement-based materials and their influence on laser-induced plasmas by shadowgraphy and plasma imaging JF - Spectrochimica Acta Part B: Atomic Spectroscopy N2 - The effect of particle grain sizes in different cement-based mixtures on the laser-induced plasma evolution is studied using two experimental methods: (i) temporal and spatial evolution of the laser-induced shock wave is investigated using shadowgraphy and two-dimensional plasma imaging, and (ii) temporal and spatial distribution of elements in the plasma is investigated using two-dimensional spectral imaging. This study is motivated by the interest in applying laser-induced breakdown spectroscopy (LIBS) for chemical analysis of concrete, and subsequently obtain information related to damage assessment of structures like bridges and parking decks. The distribution of grain sizes is of major interest in civil engineering as for making concrete different aggregate grain sizes defined by a sieving curve (64mm to 0.125 mm) are needed. Aggregates up to a size of 180 μm can be excluded from the data set, therefore only the amount of small aggregates with a grain size below 180 μm must be considered with LIBS. All components of the concrete with a grain size smaller than 0.125mm are related to the flour grain content. Tested samples consisted of dry and hardened cement paste (water-cement ratio w/z=0.5), which served as a reference. Aggregate mixtures were made by adding flour grains (size 40 μm) and silica fume (size 0.1 μm) in different ratios to cement: 10%, 30%, 50% and 60%, all combined to the remaining percentage of dry or hydrated cement. The visualization results show that a dependance in the evolution of the plasma as a function of sample grain size can be detected only in the initial stages of the plasma formation, that is, at the initial 3 μs of the plasma life. Spectral information reveals the elemental distribution of the silicon and calcium in plasma, in both neutral and ionized form. Here also, a significant effect is observed in the first 1 μs of the plasma lifetime. KW - LIBS KW - Cement-based materials KW - Particle size KW - Shadowgraphy KW - Plasma imaging PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105772 VL - 165 SP - 105772 PB - Elsevier B.V. AN - OPUS4-50319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates JF - Journal of Alloys and Compounds N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization JF - International Journal of Applied Ceramic Technology N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -