TY - JOUR A1 - Müller, Patrick A1 - Morys, Michael A1 - Sut, Aleksandra A1 - Jäger, Christian A1 - Illerhaus, Bernhard A1 - Schartel, Bernhard T1 - Melamine poly(zinc phosphate) as flame retardant in epoxy resin: Decomposition pathways, molecular mechanisms and morphology of fire residues N2 - Synergistic multicomponent systems containing melamine poly(metal phosphate)s have been recently proposed as flame retardants. This work focuses on the decomposition pathways, molecular mechanisms and morphology of the fire residues of epoxy resin (EP) flame retarded with melamine poly(zinc phosphate) (MPZnP) to explain the modes of action and synergistic effects with selected synergists (melamine polyphosphate (MPP) and AlO(OH), respectively). The total load of flame retardants was always 20 wt.%. The decomposition pathways were investigated in detail via thermogravimetric Analysis coupled with Fourier transform infrared spectroscopy. The fire residues were investigated via elemental analysis und solid-state nuclear magnetic resonance spectroscopy. The morphology of intumescent fire residues was investigated via micro-computed tomography and scanning electron microscopy. EP + (MPZnP + MPP) formed a highly voluminous residue that showed structural features of both EP + MPZnP and EP + MPP, resulting in a highly effective protection layer. EP + (MPZnP + AlO(OH)) preserved the entire quantity of phosphorus content during combustion due to the Formation of Zn₂P₂O₇ and AlPO₄. KW - Melamine poly(metal phosphate) KW - Flame retardancy KW - Epoxy resin KW - Solid-state NMR KW - Micro-computed tomography KW - Fire residue PY - 2016 DO - https://doi.org/10.1016/j.polymdegradstab.2016.06.023 SN - 0141-3910 VL - 130 SP - 307 EP - 319 PB - Elsevier AN - OPUS4-36863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morys, Michael A1 - Illerhaus, Bernhard A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Revealing the inner secrets of intumescence: Advanced standard time temperature oven (STT Mufu+)—my‐computed tomography approach N2 - Intumescent coatings have been used for fire protection of steel for decades, but there is still a need for improvement and adaptation. The key parameters of such coatings in a fire Scenario are thermal insulation, foaming dynamics, and cohesion. The fire resistance tests, large furnaces applying the standard time temperature (STT) curve, demand coated full‐scale components or intermediate‐scale specimen. The STT Mufu+ (standard time temperature muffle furnace+) approach is presented. It is a recently developed bench‐scale testing method to analyze the performance of intumescent coatings. The STT Mufu+ provides vertical testing of specimens with reduced specimen size according to the STT curve. During the experiment, the foaming process is observed with a high‐temperature endoscope. Characteristics of this technique like reproducibility and resolution are presented and discussed. The STT Mufu+ test is highly efficient in comparison to common tests because of the reduced sample size. Its potential is extended to a superior research tool by combining it with advanced residue analysis (μ‐computed tomography and scanning electron microscopy) and mechanical testing. The benefits of this combination are demonstrated by a case study on 4 intumescent coatings. The evaluation of all collected data is used to create performance‐based rankings of the tested coatings. KW - Bench‐scale fire testing KW - Computed tomography KW - Fire resistance KW - Intumescence KW - Residue analysis KW - Standard time temperature furnace PY - 2017 DO - https://doi.org/10.1002/fam.2426 SN - 0308-0501 SN - 1099-1018 VL - 41 IS - 8 SP - 927 EP - 939 PB - Wiley AN - OPUS4-42754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morys, Michael A1 - Illerhaus, Bernhard A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Revealing the inner secrets of intumescent chars by advanced small scale tests combined with µ-CT N2 - Testing of intumescent coatings for Steel is usually done in intermediate scale or even full scale experiments and is hence quite expensive. We developed two complementary small scale tests, simulating fully developed Tire. First is a strongly modified electrical muffle furnace, which is now able to follow the Standard temperature-time curve (according EN 1363-1) for 90 min in a very accurate manner. Düring the experiment backside temperatures are recorded and the growth of the char is observed with a custom made high temperature endoscope. Second is a testing apparatus based on a propane-oxygen-bumer for direct severe flame impingement of coated samples, reaching temperatures far above 1500 °C. Our small scale samples are coated Steel plates of a size of 75 x 75 x 2 mm3. The structure-propertyrelation between additives, thermal properties and morphology of the char were examined using a well determined series of samples consisting of basic composition mixed with different additives. With the burner-testing-apparatus we studied the behavior of a high performance coating, which shows a transformation of the carbonaceous char into a ceramic foam at temperatures as high as 1600 °C. Nondestructive micro-computed tomography was used to characterize the morphology of the char. According to the structure of the foams we used different analytic methods like cell-detection or wallthickness-analysis. Additional scanning electron and optical microscopy were performed. The combination of the CT-data with the measured backside temperatures of the different samples provides us a deep understanding of the interaction between isolating properties and morphology of intumescent chars. T2 - Fire and materials 2015 - 14th International conference and exhibition CY - San Francisco, CA, USA DA - 02.02.2015 PY - 2015 SP - 478 EP - 483 PB - Interscience Communications AN - OPUS4-32710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morys, Michael A1 - Illerhaus, Bernhard A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Variation of intumescent coatings revealing different modes of action for good protection performance N2 - Thermal insulation and mechanical resistance play a crucial role for the performance of an intumescent coating. Both properties depend strongly on the morphology and morphological development of the foamed residue. Small amounts (4 wt%) of fiberglass, clay and a copper salt, respectively, are incorporated into an intumescent coating to study their influence on the morphology and Performance of the residues. The bench scale fire tests were performed on 75 x 75 x 2 mm³ coated steel plates according to the standard time–temperature curve in the Standard Time Temperature Muffle Furnace+ (STT Mufu+). It provided information about foaming dynamics (expansion rates) and thermal insulation. Adding the copper salt halved the expansion height, whereas the clay and fiberglass Change the height of the residue only moderately. The time to reach 500 °C was improved by 31% for clay and 15% for the other two fillers. Nondestructive micro computed tomography is used to assess the inner structure of the residues. A transition of the residue from a black, carbonaceous foam with closed cells into an inorganic, residual open cell sponge occurs at high temperatures. This transition is due to a loss of carbon; the change in microstructure is analyzed by scanning electron microscopy. Additional mechanical tests are performed and interpreted with respect to the results of the morphology analysis. Adding clay or copper salt improved the mechanical resistance tested by a factor 4. The additives significantly influence the thickness and foaming Dynamics as well as the inner structure of the residues, whereas their influence on insulation Performance is moderate. In conclusion, different modes of action are observed to achieve similar insulation performance during the fire test. KW - Intumescence KW - Coating KW - Bench scale fire testing KW - Computed tomography KW - Fire resistance PY - 2017 DO - https://doi.org/10.1007/s10694-017-0649-z SN - 0015-2684 SN - 1572-8099 VL - 53 IS - 4 SP - 1569 EP - 1587 PB - Springer AN - OPUS4-40751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morys, Michael A1 - Illerhaus, Bernhard A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Size is not all that matters: Residue thickness and protection performance of intumescent coatings made from different binders N2 - In addition to the acid source, charring agent, and blowing agent, the binder is a crucial part of an intumescent coating. Its primary task is to bind all compounds, but it also acts as a carbon source and influences the foaming process. A series of intumescent coatings based on five different binders was investigated in terms of insulation, foaming, mechanical impact resistance, and residue morphology. The Standard Time-Temperature modified Muffle Furnace (STT MuFu+ ) was used for the bench-scale fire resistance tests and provided data on temperature and residue thickness as well as well-defined residues. The residue morphology was analyzed by nondestructive m-computed tomography and scanning electron microscopy. A moderate influence of the binder on insulation performance was detected in the set of coatings investigated, whereas the foaming dynamics and thickness achieved were affected strongly. In addition, the inner structure of the residues showed a rich variety. High expansion alone did not guarantee good insulation. Furthermore, attention was paid to the relation between the microstructure transition induced by carbon loss due to thermo-oxidation of the char and the development of the thermal conductivity and thickness of the coatings during the fire test. KW - Intumescence KW - Morphology analysis KW - Computed tomography KW - Fire resistance KW - Bench-scale fire test KW - Fire protective coating PY - 2017 DO - https://doi.org/10.1177/0734904117709479 SN - 0734-9041 SN - 1530-8049 VL - 35 IS - 4 SP - 284 EP - 302 PB - Sage AN - OPUS4-40766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Illerhaus, Bernhard A1 - Spreemann, M. T1 - Making use of phase-contrast in dimensional muCT-measurements of weakly absorbing objects N2 - The effects of refraction (phase-contrast) are normally considered as disturbances in high-resolution μCT-measurements. We show that in the case of small objects with low absorption a single-distance phase-retrieval algorithm not only reduces the edge enhancement, but also raises the signal-to-noise ratio sufficiently to allow dimensional measurements. This is exemplified at an optical element for optical fibre connectors. T2 - Conference on industrial computed tomography (ICT) 2014 CY - Wels, Austria DA - 25.02.2014 PY - 2014 SN - 978-3-8440-2557-6 SN - 1610-4773 SP - 405 EP - 410 PB - Shaker Verlag GmbH AN - OPUS4-30325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Myrach, Philipp A1 - Röllig, Mathias A1 - Jonietz, Florian A1 - Illerhaus, Bernhard A1 - Meinel, Dietmar A1 - Richter, U. A1 - Miksche, R. ED - Chimenti, Dale E. ED - Bond, Leonard J. T1 - Characterization of pores in high pressure die cast aluminum using active thermography and computed tomography N2 - Larger high pressure die castings (HPDC) and decreasing wall thicknesses are raising the issue of casting defects like pores in aluminum structures. Properties of components are often strongly influenced by inner porosity. As these products are being established more and more in lightweight construction (e.g. automotive and other transport areas), non-destructive testing methods, which can be applied fast and on-site, are required for quality assurance. In this contribution, the application of active thermography for the direct detection of larger pores is demonstrated. The analysis of limits and accuracy of the method are completed by numerical simulation and the method is validated using computed tomography. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - flash thermography KW - aluminum KW - pores KW - computed tomography PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940580 VL - 1706 SP - 110009-1 EP - 110009-8 PB - AIP Publishing LLC CY - Melville, New York, USA AN - OPUS4-35848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kinne, R. W. A1 - Gunnella, F. A1 - Kunisch, E. A1 - Heinemann, S. A1 - Nies, B. A1 - Maenz, S. A1 - Horbert, V. A1 - Illerhaus, Bernhard A1 - Huber, R. A1 - Firkowska-Boden, I. A1 - Bossert, J. A1 - Jandt, K. D. A1 - Sachse, A. A1 - Bungartz, M. A1 - Brinkmann, O. T1 - Performance of calcium phosphate cements in the augmentation of sheep vertebrae - An ex vivo study N2 - Oil-based calcium phosphate cement (Paste-CPC) shows not only prolonged shelf life and injection times, but also improved cohesion and reproducibility during application, while retaining the advantages of fast setting, mechanical strength, and biocompatibility. In addition, poly(L-lactideco-glycolide) (PLGA) fiber reinforcement may decrease the risk for local extrusion. Bone defects (diameter 5 mm; depth 15 mm) generated ex vivo in lumbar (L) spines of female Merino sheep (2–4 years) were augmented using: (i) water-based CPC with 10% PLGA fiber reinforcement (L3); (ii) Paste-CPC (L4); or (iii) clinically established polymethylmethacrylate (PMMA) bone cement (L5). Untouched (L1) and empty vertebrae (L2) served as controls. Cement performance was analyzed using micro-computed tomography, histology, and biomechanical testing. Extrusion was comparable for Paste-CPC(-PLGA) and PMMA, but significantly lower for CPC + PLGA. Compressive strength and Young’s modulus were similar for Paste-CPC and PMMA, but significantly higher compared to those for empty defects and/or CPC + PLGA. Expectedly, all experimental groups showed significantly or numerically lower compressive strength and Young’s modulus than those of untouched controls. Ready-to-use Paste-CPC demonstrates a performance similar to that of PMMA, but improved biomechanics compared to those of water-based CPC + PLGA, expanding the therapeutic arsenal for bone defects. O, significantly lower extrusion of CPC + PLGA fibers into adjacent lumbar spongiosa may help to reduce the risk of local extrusion in spinal surgery. KW - Sheep KW - PMMA KW - Calcium phosphate bone cement KW - Oil-based KW - Ready-to-use KW - Water-based KW - Micro-CT KW - Compressive strength KW - Young’s modulus PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569072 DO - https://doi.org/10.3390/ma14143873 SN - 1996-1944 VL - 14 IS - 14 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-56907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bienge, J.-E. A1 - Illerhaus, Bernhard A1 - Epperlein, J. ED - Szallies, agrathaer GmbH, Isabell T1 - Blick in den Boden N2 - Computertomographische Untersuchungen in einer Studie zum vergleichenden Wurzelwachstum von Raps unter verschiedenen Bedingungen der Bodenbearbeitung. T2 - 20 Jahre Praxisversuch Lietzen Ackerbau und Forschung auf dem Weg in die Zukunft Feldtag in der Komturei Lietzen CY - Komturei Lietzen, Germany DA - 19.5.2016 KW - Computer Tomographie PY - 2016 SP - 28 EP - 29 AN - OPUS4-38144 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - μCT begleitete in-situ Druckversuche an spongiösem Knochen - Vergleich(ende Bestimmung) des experimentellen und simulierten Verschiebungsfeldes mit der simulierten internen Spannung N2 - Untersuchungen haben gezeigt, dass sich ältere Schafe gut als Modell für die mi-nimalinvasive Behandlung von Osteoporose eignen [1]. Um einen Behandlungs-effekt nachzuweisen, wird dabei unter anderem die Belastungsfähigkeit des Kno-chens durch Druckversuche an kleinen Zylindern aus den behandelten und unbe-handelten Knochen bestimmt. Diese hatten hier einen Durchmesser von 10 mm und eine Höhe von 13 mm. Für den in-situ Druckversuch wurde eine Deben CT5000 verwendet. In einer Serie von Druckerhöhungen wurden die Proben je-weils tomographiert. Dabei ergab sich zunächst, dass mit der µCT innerhalb der Knochen im oberen und unteren Bereich schon Brüche nachgewiesen werden können, obwohl die gemessene Kraftaufnahmekurve keine Unstetigkeit zeigt. Deswegen wurden die starren Probenaufnehmer der Deben Anordnung durch bewegliche Aufnehmer ergänzt, die eine leichte Verkippung der belasteten Ober-flächen ausgleichen können. Ein Vergleich der gemessenen und der aus den µCT-Daten berechneten Verschiebungsfelder ergab trotz der komplexen Struktur der Knochen gute Übereinstimmungen. Diese Verschiebungen wurden dann mit den aus den µCT Daten simulierten mechanischen Druckversuchen, Von-Mise-Spannungen und daraus berechneten Verschiebungen verglichen. (VGStudioMax Simulation). T2 - DGZfP-Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Computer Tomographie KW - In-situ Druckversuch KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448827 UR - https://www.ndt.net/?id=23080 SN - 978-3-940283-92-4 VL - DGZfP BB 166 SP - 1 EP - 7 PB - DGZfP CY - Berlin AN - OPUS4-44882 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - Serial in situ compression of spongiosa cylinder observed by μCT, compared to simulated stress, strain, and movement N2 - Minimally invasive injection of calcium phosphate cement into bone defects in aged sheep vertebrae has been used as a model for the treatment of osteoporotic vertebral fractures. One of the therapeutic criteria is a compression test of non-treated or treated vertebral bodies. In the present study, an in situ compression test with a stepwise load increase was performed with small spongiosa cylinders from the vertebrae under continuous monitoring by μCT. This allows localization of bone cracks and the visualization of correct placement and form of the bone cylinder. In addition, the effects of an uneven load distribution on the sample due to an irregular shape and a subsequent underperformance of the test sample can be excluded by controlling its shape under increasing load. There was a good agreement between the measured data and those obtained by simulated load-dependent transformation on the basis of a digital volume correlation between consecutive compression tests on the bone surface under the assumption of homogeneous bone material. Mechanic simulation was executed by directly using structural voxel data, resulting in maps of Von Mise stresses and predicted displacements. T2 - 12th ECNDT CY - Gothenburg, Sweden DA - 11.6.2018 KW - Computed tomography KW - In-situ compression KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453317 SN - 978-91-639-6217-2 SP - 0162, 1 EP - 7 AN - OPUS4-45331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -