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 U6 - 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 - 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 U6 - 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 U6 - 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 - JOUR A1 - Gunella, F. A1 - Kunisch, E. A1 - Bungartz, M. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Hortschansky, P. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. T1 - Low-dose BMP-2 is sufficient to enhance the bone formation induced by an injectable, PLGA fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia N2 - BACKGROUND CONTEXT: Bioresorbable calcium phosphate cement (CPC) may be suitable for vertebroplasty/kyphoplasty of osteoporotic vertebral fractures. However, additional targeted de- livery of osteoinductive bone morphogenetic Proteins (BMPs) in the CPC may be required to counteract the augmented local bone catabolism and support complete bone regeneration. PURPOSE: This study aimed at testing an injectable, poly (l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement (CPC) containing low-dose bone morphogenetic Protein BMP-2 in a sheep lumbar osteopenia model. STUDY DESIGN/ SETTING: This is a prospective experimental animal study. METHODS: Bone defects (diameter 5 mm) were generated in aged, osteopenic female sheep and filled with fiber-reinforced CPC alone (L4; CPC+ fibers) or with CPC containing different dosages of BMP-2 (L5; CPC+ fibers + BMP-2; 1, 5, 100, and 500g BMP-2; n=5 or 6 each). The results were compared with those of untouched controls (L1). Three and 9 months after the operation, structural and functional effects of the CPC (±BMP-2) were analyzed ex vivo by measuring (1) bone Mineral density (BMD); (2) bone structure, that is, bone volume/total volume (assessed by micro-computed tomography [micro-CT] and histomorphometry), trabecular thickness, and trabecular number; (3) bone formation, that is, osteoid volume/bone volume, osteoid surface/bone surface, osteoid thickness, mineralizing surface/bone surface, mineral Apposition rate, and bone formation rate/bone surface; (4) bone resorption, that is, eroded surface/bone surface; and (5) compressive strength. RESULTS: Compared with untouched controls (L1), CPC+ fibers (L4) and/or CPC+ fibers + BMP-2(L5) significantly improved all parameters of bone formation, bone resorption, and bone structure. These effects were observed at 3 and 9 months, but were less pronounced for some parameters at 9 months. Compared with CPC without BMP-2, additional significant effects of BMP-2 were demonstrated for bone structure (bone volume/total volume, trabecular thickness, trabecular number) and formation (osteoid surface/bone surface and mineralizing surface/bone surface), as well as for the compressive strength. The BMP-2 effects on bone Formation at 3 and 9 months were dose-dependent, with 5–100g as the optimal dosage. CONCLUSIONS: BMP-2 significantly enhanced the bone formation induced by a PLGA fiber-reinforced CPC in sheep lumbar osteopenia. A single local dose as low as ≤100g BMP-2 was sufficient to augment middle to long-term bone formation. The novel CPC+ BMP-2 may thus represent an alternative to the bioinert, supraphysiologically stiff polymethylmethacrylate cement presently used to treat osteoporotic vertebral fractures by vertebroplasty/kyphoplasty. KW - Bone regeneration KW - Computed tomography KW - Calcium phosphat cement KW - Large animal model sheep KW - Osteoporotic vertebral fracture PY - 2017 U6 - https://doi.org/10.1016/j.spinee.2017.06.005 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 11 SP - 1699 EP - 1711 PB - Elsevier Inc. AN - OPUS4-43237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bungartz, M. A1 - Kunisch, E. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Gunella, F. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. T1 - GDF5 significantly augments the bone formation induced by an injectable, PLGA fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia N2 - BACKGROUND CONTEXT: Biodegradable calcium phosphate cement (CPC) represents a promising option for the surgical treatment of osteoporotic vertebral fractures. Because of augmented local bone catabolism, however, additional targeted delivery of bone morphogenetic proteins with the CPC may be needed to promote rapid and complete bone regeneration. PURPOSE: In the present study, an injectable, poly(l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement (CPC) containing the bone morphogenetic Protein GDF5 was tested in a sheep lumbar osteopenia model. STUDY DESIGN/SETTING: This is a prospective experimental animal study METHODS: Defined bone defects (diameter 5 mm) were placed in aged, osteopenic female sheep. Defects were treated with fiber-reinforced CPC alone (L4; CPC+ fibers) or with CPC containing different dosages of GDF5 (L5; CPC+ fibers + GDF5; 1, 5, 100, and 500g GDF5; n = 5 or 6 each). The results were compared with those of untouched controls (L1). Three and 9 months postoperation, structural and functional effects of the CPC (±GDF5) were assessed ex vivo by measuring (1) bone mineral density (BMD); (2) bone structure, that is, bone volume/total volume (assessed by micro-computed tomography and histomorphometry), trabecular thickness, and trabecular number; (3) bone formation, that is, osteoid volume/bone volume, osteoid surface/bone surface, osteoid thickness, mineralized surface/bone surface, mineral apposition rate, and bone formation rate/bone surface; (4) bone resorption, that is, eroded surface/bone surface; and (5) compressive strength. RESULTS: Compared with untouched controls (L1), both CPC+ fibers (L4) and CPC+ fibers + GDF5 (L5) numerically or significantly improved all parameters of bone formation, bone resorption, and bone structure. These significant effects were observed both at 3 and 9 months, but for some parameters they were less pronounced at 9 months. Compared with CPC without GDF5, additional significant effects of CPC with GDF5 were demonstrated for BMD and parameters of bone formation and structure (bone volume/total volume, trabecular thickness, and trabecular number, as well as mineralized surface/bone surface). The GDF5 effects were dose-dependent (predominantly in the 5–100g range) at 3 and 9 months. CONCLUSIONS: GDF5 significantly enhanced the bone formation induced by a PLGA fiber-reinforced CPC in sheep lumbar osteopenia. The results indicated that a local dose as low as ≤100g GDF5 may be sufficient to augment middle to long-term bone formation. The novel CPC+ GDF5 combination may thus qualify as an alternative to the bioinert, supraphysiologically stiff poly-(methyl methacrylate) cement currently applied for vertebroplasty/kyphoplasty of osteoporotic vertebral fractures. KW - Bone regeneration KW - Computed tomography KW - Large animal model sheep KW - Osteoporotic vertebral fracture PY - 2017 U6 - https://doi.org/10.1016/j.spinee.2017.06.007 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 11 SP - 1685 EP - 1698 PB - Elsevier Inc. AN - OPUS4-43239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maenz, S. A1 - Brinkmann, O. A1 - Kunisch, E. A1 - Horbert, V. A1 - Gunella, F. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Xin, L. A1 - Günster, Jens A1 - Illerhaus, Bernhard A1 - Jandt, K. D. A1 - Bossert, J. A1 - Kinne, R. W. A1 - Bungartz, M. T1 - Enhanced bone formation in sheep vertebral bodies after minimally invasive treatment with a novel, PLGA fiber-reinforced brushite cement. N2 - Injectable, brushite-forming calcium phosphate cements (CPC) show potential for bone replacement, but they exhibit low mechanical strength. This study tested a CPC reinforced with poly(l-lactide-co-glycolide) acid (PLGA) fibers in a minimally invasive, sheep lumbar vertebroplasty model. The study aimed to test the in vivo biocompatibility and osteogenic potential of a PLGA fiber-reinforced, brushite-forming CPC in a sheep large animal model. KW - µCT KW - Vertebral KW - PLGA cement PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S152994301631066X U6 - https://doi.org/10.1016/j.spinee.2016.11.006 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 5 SP - 709 EP - 719 PB - Elsevier Science direct AN - OPUS4-40462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Illerhaus, Bernhard T1 - Hinweis zum Betrieb von Mikrofokusröntgenröhren N2 - Beim Betrieb von µFokus-Röntgenröhren entsprechend der Betriebsanleitung können schwerwiegende Schäden auftreten. KW - Hochspannungsüberschlag PY - 2017 UR - http://www.dgzfp.de/Portals/24/Zeitung/Ausgaben/Zeitung153.pdf IS - 153 SP - 18 EP - 18 PB - DGZfP AN - OPUS4-39249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -