TY - CONF A1 - Mieller, Björn T1 - Numerical study of electric field distribution in breakdown strength testing of ceramics N2 - Dielectric breakdown of insulators is a combined electrical, thermal, and mechanical failure. The exact breakdown mechanism in ceramics and the formulation of useful models are still subject of investigation. Recent studies highlighted that several experimental aspects of dielectric breakdown strength testing affect the test results, and thus impede the recognition of fundamental principles. Excess field strength near the electrode can lead to premature breakdown in the insulating liquid. This would cause superficial damage to the test specimen and thus falsify the measurement results. The field strength distribution is influenced by the ratio of permittivity of the sample and the surrounding insulating liquid. Premature breakdown depends on the breakdown strength of the liquid and the actual test voltage. The test voltage again depends on the specimen thickness. To systematically investigate these relations, a numerical simulation study (FEM) of the electric field distribution in a typical testing rig with cylindrical electrodes was performed. The permittivity of the sample and the insulating liquid was parameterized, as well as the sample thickness. The electric field distribution was calculated for increasing test voltage. Field strength maxima are compared to experimental breakdown strength of typical insulating liquids and experimental breakdown locations on alumina. Strategies are discussed to adjust the insulation liquid and the sample thickness to reduce the influence of the testing setup on the dielectric breakdown strength results. T2 - Ceramics in Europe 2022 CY - Krakow, Poland DA - 10.07.2022 KW - Ceramics KW - Dielectric breakdown strength KW - Electric field distribution KW - Alumina PY - 2022 AN - OPUS4-55325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Widjaja, Martinus Putra A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Multi-energy high dynamic range synchrotron X-ray computed tomography N2 - Synchrotron X-ray computed tomography (SXCT) is regularly used in materials science to correlate structural properties with macroscopic properties and to optimize manufacturing processes. The X-ray beam energy must be adapted to the sample properties, such as size and density. If both strongly and weakly absorbing materials are present, the contrast to the weakly absorbing materials is lost, resulting in image artifacts and a poor signal-tonoise ratio (SNR). One particular example is a low-temperature co-fired ceramics (LTCC), in which metal connections are embedded in a ceramic matrix and form 3-dimensional conducting structures. This article describes a method of combining SXCT scans acquired at different beam energies, significantly reducing metal artifacts, and improving image quality. We show how to solve the difficult task of merging the scans at low and high beam energy. Our proposed merging approach achieves up to 35 % improvement in SNR within ceramic regions adjacent to metallic conductors. In this way, previously inaccessible regions within the ceramic structure close to the metallic conductors are made accessible. The paper further discusses methodological requirements, limitations, and potential extensions of the presented multi-energy SXCT merging technique. KW - Synchrotron computed tomography KW - Reconstruction algorithm KW - High dynamic range KW - Data merging KW - Low-temperature cofired ceramics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652339 DO - https://doi.org/10.1016/j.tmater.2025.100079 SN - 2949-673X VL - 9 SP - 1 EP - 10 PB - Elsevier CY - Amsterdam AN - OPUS4-65233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Characterization of Beta-Alumina Solid Electrolyte by Coin Cell Testing N2 - All solid-state batteries (ASSBs) are the subject of widespread research, one reason being their predicted increased safety [1]. Variants of beta-alumina solid electrolyte (BASE), a promising solid electrolyte for sodium ion batteries, exhibit ion conductivities up to 5 mS/cm at room temperature, which motivates targeted research and testing [2]. Dedicated measurement cells for conductivity measurements and cycling of ASSBs are available, providing even pressure and temperature control. However, these are often costly and thus unsuitable for long-term studies with many cells. In contrast, coin cells are a practical and scalable approach for such ASSB studies, despite poor pressure control and other influencing factors that may affect the reproducibility of results [3]. This study investigates the extent to which reliable measurement data can be obtained from symmetrical Na/BASE/Na coin cells. Therefore, several testing procedures and different cell architectures are considered. The experiments are supported by an electrical equivalent circuit model. The modeling approach and both measured and numerically simulated data are presented. The coin cell results are compared to data acquired using a designated ASSB setup (CompreCell and CompreFrame by RHD). T2 - XIXth Conference of the EuropeanCeramic Society / SBS6 InternationalSodium Battery Symposium CY - Dresden, Germany DA - 01.09.2025 KW - Beta aluminate solid electrolyte KW - Coin cell PY - 2025 AN - OPUS4-64055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Widjaja, Martinus Putra A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Multi-Energy High Dynamic Range (HDR) Synchrotron X-ray Computed Tomography applied to LTCC samples N2 - Synchrotron X-ray computed tomography (SXCT) is regularly used in materials science to correlate structural properties with macroscopic properties and to optimize manufacturing processes. The X-ray beam energy must be adapted to the sample properties, such as size and density. If both strongly and weakly absorbing materials are present, the contrast to the weakly absorbing materials is lost, resulting in image artifacts and a poor signal-to-noise ratio (SNR). One example is a low-temperature co-fired ceramics (LTCC), in which metal connections are embedded in a ceramic matrix and form 3-dimensional conducting structures. This article describes a method of combining SXCT scans acquired at different beam energies, significantly reducing metal artifacts, and improving image quality. We show how to solve the difficult task of merging the scans at low and high beam energy. Our proposed merging approach achieves up to 35% improvement in SNR within ceramic regions adjacent to metallic conductors. In this way, previously inaccessible regions within the ceramic structure close to the metallic conductors are made accessible. The paper further discusses methodological requirements, limitations, and potential extensions of the presented multienergy SXCT merging technique. T2 - iCT 2026 CY - Linz, Austria DA - 10.02.2026 KW - Synchrotron x-ray CT KW - Multi-energy CT KW - Low-Temperature cofired ceramics PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655848 SP - 1 EP - 7 CY - e-Journal of Nondestructive Testing AN - OPUS4-65584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-1. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - TDEP2023: Finite-temperature and anharmonic response properties of solids in theory and practice CY - Linköping, Sweden DA - 21.08.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - 4th International Symposium on Negative Thermal Expansion and Related Materials (ISNTE-4) CY - Padua, Italy DA - 04.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - 16th International conference on materials chemistry (MC16) CY - Dublin, Ireland DA - 03.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - George, Janine A1 - Mieller, Björn A1 - Stawski, Tomasz T1 - ZrV2O7 negative thermal expansion (NTE) material N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder. T2 - SALSA Make and Measure Conference CY - Berlin, Germany DA - 13.09.2023 KW - NTE KW - Composites KW - TEM PY - 2023 AN - OPUS4-58367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Markötter, Henning ED - Petzow, G. ED - Mücklich, F. T1 - Machine learning assisted characterization of a Low Temperature Cofired Ceramic (LTCC) module measured by synchrotron computed tomography N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Taagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 SN - 978-3-88355-422-8 VL - 54 SP - 136 EP - 141 PB - Deutsche Gesellschaft für Materialkunde e.V CY - Sankt Augustin AN - OPUS4-51298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Practical breakdown voltage calculations using dielectric breakdown strength reference values N2 - Dielectric breakdown is a catastrophic failure of ceramic substrates and insulators. The use of dielectric breakdown strength (DBS) reference values for the dimensioning of such components is not straightforward, as the DBS depends on sample thickness and electrode area. This fact also hampers a valid comparison of data taken from different literature sources. Based on the empirically confirmed proportionality of DBS to the reciprocal square root of sample thickness and an approach to account for the influence of electrode area on the failure probability, a practical equation is derived to calculate the breakdown voltage for arbitrary sample thickness and electrode area from one set of DBS reference data. To validate the equation, the AC DBS of commercial alumina substrates with thicknesses ranging from 0.3 mm to 1.0 mm was performed using different printed electrodes with varying areas. The breakdown voltages comprise a range from 18 kV for thick samples to 8.5 kV for thin samples, resulting in DBS values from 17 kV/mm for 1.0 mm thick samples to 29 kV/mm for 0.3 mm thin samples, all made from the same material. The influence of electrode area is comparatively smaller. The results calculated with the proposed equation are in reasonable accordance with the measured data. Thus, the equation can be applied for a proper comparison of literature DBS data measured in different setups and for a reasonable estimation of breakdown voltages in DBS tests and applications based on reference data. T2 - Electroceramics Conference XVII CY - Online meeting DA - 24.08.2020 KW - Ceramics KW - Dielectric breakdown KW - Weibull distribution PY - 2020 AN - OPUS4-51151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -