TY - JOUR A1 - Zhang, Luman A1 - de Greef, Nils A1 - Kalinka, Gerhard A1 - Van Bilzen, Bart A1 - Locquet, Jean-Pierre A1 - Verpoest, Ignaas A1 - Won Seo, Jin T1 - Carbon nanotube-grafted carbon fiber polymer composites: Damage characterization on the micro scale JF - Composites Part B N2 - Multiwall carbon nanotubes (CNTs) e carbon fibers (CFs)hybrid materials were produced by directly growing CNTs on CFs by means of chemical vapor deposition. For the latter, the oxidative dehydrogenation reaction of C2H2 and CO2 was applied, which allows growing CNTs without damaging the CF surface. Uni-directional nano-engineered carbon fiber reinforced composites (nFRCs) were fabricated by impregnating these hybrid materials with epoxy. The nFRCs subjected to single fiber push-out tests revealed a decrease of the interfacial shear strength (IFSS) of about 36% compared to the carbon fiber composites without CNTs. By means of transverse three-point bending tests performed on pre-notched composite beams inside a scanning electron microscope, the fracturing behavior parallel to the fibers was studied in-situ. The nFRCs showed significantly reduced fiber/matrix debonding while CNTs pull-out, CNTs bridging as well as matrix failure occurred. These results demonstrate that the presence of CNTs in nFRCs affects the stress distribution and consequently the damage Initiation as well as the damage propagation. The presence of CNTs suppresses the stress concentration at the fiber/Matrix interface and reduces the debonding of CFs from the matrix. However, our results indicate that the stress concentration shifts towards the CNTs' ends/matrix interface and causes promoted matrix failure leading to lower IFSS. KW - Carbon fibres nanotubes interface PY - 2017 DO - https://doi.org/10.1016/j.compositesb.2017.06.004 SN - 1359-8368 SN - 1879-1069 VL - 126 SP - 202 EP - 210 PB - Elsevier CY - Niederlande AN - OPUS4-42202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhandarov, S. A1 - Mäder, E. A1 - Kalinka, Gerhard A1 - Scheffler, C. A1 - Poitzsch, C. A1 - Fliescher, S. T1 - Investigation of interfacial strength parameters in polymer matrix composites: Compatibility and reproducibility JF - Advanced Industrial and Engineering Polymer Research N2 - Effects of various geometrical and physical factors, as well as the method of data reduction (analysis of experimental forceedisplacement curves) on the values of local interfacial strength parameters (local IFSS, td, and critical energy release rate, Gic) determined by means of a single fiber pull-out test are discussed. Experimental results of our pull-out tests on several fiberepolymer matrix systems showed that td and Gic weakly depended on geometrical factors. However, the pull-out test appeared to be sensitive to the conditions of specimen formation and testing, such as changing the nature of the contacting surfaces (fiber sizing) and the fiber pull-out rate. Of several methods of td and Gic Determination from a forceedisplacement curve, the most reliable and reproducible one is the approach based on the values of the maximum force recorded in a pull-out test and the interfacial frictional force immediately after fiber debonding. KW - Interface KW - Interfacial shear strength KW - Pull-out composite materials KW - Polymer matrix composites KW - Critical energy release rate KW - Geometrical factors PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-460918 DO - https://doi.org/10.1016/j.aiepr.2018.06.002 SN - 2542-5048 VL - 1 IS - 1 SP - 82 EP - 92 PB - Elsevier CY - Amsterdam AN - OPUS4-46091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wienrich, Malte A1 - Kalinka, Gerhard A1 - Greenhalgh, E.S. A1 - Carreyette, S. A1 - Bistritz, Martina A1 - Shirshova, N. A1 - Houllé, M. A1 - Asp, L. E. A1 - Bismarck, A. A1 - Fontana, Q.P.V. T1 - Impact of ionic liquid on the mechanical performance of matrix polymer for fibre reinforced materials for energy storage T2 - ECCM15 - 15th European conference on composite materials (Proceedings) N2 - For the concept of using structural materials such as carbon fibre reinforced plastics as energy storage devices, new matrix polymers are required. These polymers must provide ionic conductivity as well as adequate mechanical strength. In the EU-Project StorAGE this requirements are fulfilled by adding ionic liquid to commercial polymers. The mechanical properties of these mixtures materials were characterized by using a 3-point-bending device. In addition, single fibre pull test were performed in order to get information on the interfacial shear strength. Adding of ionic liquid has an impact on the mechanical performance of the materials. A decrease of the flexural strength and modulus of less than 10% of the value of the reference materials took part. The interfacial shear strength decreased to a value of around one third compare to the reference material. T2 - ECCM15 - 15th European conference on composite materials CY - Venice, Italy DA - 2012-06-24 KW - Multifunctional epoxy resin KW - Fibre-matrix adhesion KW - Single fibre pull-out test KW - Ionic liquid PY - 2012 SN - 978-88-88785-33-2 SP - 1 EP - 4(?) AN - OPUS4-28695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wettmarshausen, Sascha A1 - Friedrich, Jörg Florian A1 - Meyer-Plath, Asmus A1 - Kalinka, Gerhard A1 - Hidde, Gundula A1 - Weidner, Steffen T1 - Coating of carbon fibers with adhesion-promoting thin poly(acrylic acid) and poly(hydroxyethylmethacrylate) layers using electrospray ionization JF - Journal of adhesion science and technology N2 - Thin coatings of poly(acrylic acid) (PAA) and poly(hydroxyethylmethacrylate) (PHEMA) were deposited onto carbon fibers by means of the electrospray ionization (ESI) technique in ambient air. These high-molecular weight polymer layers were used as adhesion promoters in carbon fiber–epoxy resin composites. Within the ESI process, the carbon fibers were completely enwrapped with polymer in the upper 10 plies of a carbon fiber roving. As identified with scanning electron microscopy also shadowed fibers in a bundle as well as backsides of fiber rovings were pinhole-free coated with polymers (‘electrophoretic effect'). Under the conditions used, the layers have a granular structure. Residual solvent was absent in the deposit. PAA and PHEMA films did not show any changes in composition and structure in comparison with the original polymers as analyzed by X-ray photo-electron spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Single-fiber pullout tests of coated fibers embedded in epoxy resin showed significantly increased interfacial shear strength. It is assumed that chemical bonds between carbon fiber poly(acrylic acid) and epoxy resin contribute significantly to the improved interactions. KW - Adhesion promotion KW - Thin polymer layers KW - Electrospray ionization (ESI) KW - Carbon fiber–epoxy resin laminates KW - Layer topography PY - 2015 DO - https://doi.org/10.1080/01694243.2015.1040980 SN - 0169-4243 SN - 1568-5616 VL - 29 IS - 15 SP - 1628 EP - 1650 PB - VNU Science Press CY - Utrecht AN - OPUS4-34564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker A1 - Kalinka, Gerhard A1 - Loose, Florian T1 - Carbon fibre composites exemplarily research at BAM N2 - Lightweighting as a cross-cutting technology contributes significantly to achieve the European Green Deal goals. Based on, but not limited to, advanced materials and production technologies, the demand for natural resources and CO2 emmissions are reduced by lightweighting during production, as well as use phase. Therefore, lightweighting is a crucial transformation technology assisting in decoupling economic growth from resource consumption. In this manner, lightweighting contributes significantly as a key technology of relevance for many industrial sectors such as energy, mobility, and infrastructure, towards resource efficiency, climate action and economic strength, as well as a resilient Europe. To strengthen international partnerships, addressing global issues of today at the edge of science with high performance lightweight material based on carbon fibers, an overview about the BAM expertise in carbon fiber reinforced materials is given. T2 - Meeting KCarbon CY - Berlin, Germany DA - 15.06.2023 KW - Lightweighting KW - Carbon Fibers KW - Recycling KW - Push-out Test KW - multi scale testing PY - 2023 AN - OPUS4-58094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Current and future technological advancement in polymer matrix composites enabled through fundamental discoveries N2 - This presentation is a summary of the work from the past 20 years’ development of PMC-testing at the BAM-FB 5.3 with respect to safety-relevant design of advanced light weight structures in aircraft, wind turbine and automotive applications. The talk begins with wood as an example from nature, and emphasizes that load case, fiber architectural design and the production process and quality have to go hand in hand to generate an advanced light weight structure. Since PMC-relevant basic findings of mankind span across hundreds of years, high-performance composite applications today are based more on long term experiences than on breakthrough inventions of modern days. In the second part of the talk, future plans and projects of FB-5.3 are presented, specifically addressing H2-safety, circular economy, recycling by design and digitalization of PMC-technologies. T2 - Abteilungsseminar CY - Online meeting DA - 07.09.2021 KW - Polymer Matrix Composites KW - Thermo mechanical fatigue PY - 2021 AN - OPUS4-54150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tran, M.Q. A1 - Ho, K.K.C. A1 - Kalinka, Gerhard A1 - Shaffer, M.S.P. A1 - Bismarck, A. T1 - Carbon fibre reinforced poly(vinylidene fluoride): Impact of matrix modification on fibre/polymer adhesion JF - Composites science and technology N2 - The quality of interfacial interaction is dictated by the surface chemistry of the carbon fibres and the composition of the matrix. The composition of poly(vinylidene fluoride) (PVDF) was modified by the addition of maleic anhydride grafted PVDF. The surface properties of the various matrix formulations were characterised by contact angle and electrokinetic measurements. Carbon fibres were modified by industrial electrochemical oxidation and oxidation in nitric acid, or the use of a traditional epoxy-sizing of industrially oxidised fibres. The surface composition, morphology and wetting behaviour of the carbon fibres was characterised. The interaction between modified PVDF and the carbon fibres was studied by direct contact angle measurements between PVDF melt on single carbon fibres and by single fibre pull-out tests. The best wetting and adhesion behaviour was achieved between PVDF containing 5 ppm grafted maleic anhydride (MAH) and epoxy-sized carbon fibres. The addition of MAH-grafted PVDF to the unmodified PVDF caused the apparent interfacial shear strength to increase by 184%. The apparent interfacial shear strength of this fibre–matrix combination allowed for the utilisation of 100% of the yield tensile strength of PVDF. KW - A. Carbon fibres KW - A. Coupling agents KW - B. Interface KW - B. Adhesion KW - Wetting PY - 2008 DO - https://doi.org/10.1016/j.compscitech.2008.02.021 SN - 0266-3538 VL - 68 IS - 7-8 SP - 1766 EP - 1776 PB - Elsevier CY - Barking AN - OPUS4-18259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thomason, J.L. A1 - Kalinka, Gerhard T1 - A technique for the measurement of reinforcement fibre tensile strength at sub-millimetre gauge lengths JF - Composites / A N2 - The strength of composite reinforcement fibres is normally measured on samples of much greater length than the actual residual fibre lengths found in many composite materials. This is due to a number of limitations of the standard techniques which are employed. We present a description of a technique which enables values for the tensile strength of composite reinforcement fibres at short gauge lengths to be obtained. The technique is based on an adaptation of a micro-mechanical test apparatus for fibre pullout measurements. Data is presented which was obtained at gauge lengths of 180–380 µm on E-glass and S-2 glass® fibres taken from different chopped reinforcement products. The technique can be used at gauge lengths as short as 20 µm. The data indicates that the values of average fibre strength in these products are significantly below the pristine glass strength values. KW - Verstärkungsfaser KW - Kurzfaser KW - Längenabhängigkeit KW - Glass fibres KW - Strength KW - Mechanical testing KW - Festigkeit KW - Faser PY - 2001 DO - https://doi.org/10.1016/S1359-835X(00)00122-6 SN - 1359-835X VL - 32 IS - 1 SP - 85 EP - 90 PB - Elsevier CY - Oxford AN - OPUS4-12012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taketa, I. A1 - Kalinka, Gerhard A1 - Gorbatikh, L. A1 - Lomov, S. A1 - Verpoest, I. T1 - Influence of cooling rate on the properties of carbon fiber unidirectional composites with polypropylene, polyamide 6, and polyphenylene sulfide matrices JF - Advanced composite materials N2 - The longitudinal and transverse strength of three unidirectional thermoplastic prepreg systems: carbon fiber/polypropylene (CF/PP), polyamide 6 (CF/PA6), and polyphenylene sulfide (CF/PPS) are studied and analytical formulas are proposed for the estimation of matrix and fiber/matrix interface properties from composites properties. Since the matrices are semi-crystalline thermoplastics, the influence of cooling rate on the strength is statistically evaluated. While the 0° tensile strength is found to be independent of the cooling rate, the 90° tensile strength is strongly influenced by the matrix type and cooling rate. The matrix modulus increases as the cooling rate is decreased; the degree of crystallinity also increases. The matrix residual stress, interfacial shear strength, and mode II interlaminar fracture toughness are also found to depend on the cooling rate, with the trends different for different matrices. KW - Matrix residual stress KW - Thermoplastic prepreg KW - Unidirectional composites KW - Cooling rate KW - Interfacial strength PY - 2020 DO - https://doi.org/10.1080/09243046.2019.1651083 SN - 0924-3046 SN - 1568-5519 N1 - Die originale japanische Version des Artikels erschien in: Journal of the Japan Society for Composite Materials, Jg. 44, Nr. 4 (2018), S. 123-128. - The original Japanese version of the article was published in: Journal of the Japan Society for Composite Materials, vol. 44, no. 4 (2018), pp. 123-128. VL - 29 IS - 1 SP - 101 EP - 113 PB - Taylor & Francis CY - London AN - OPUS4-45433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sturm, Heinz A1 - Schulz, Eckhard T1 - Local AC current contrast on carbon fiber surfaces imaged by scanning force microscopy JF - Acta polymerica N2 - After a delamination process in a C-fiber reinforced polymer composite, the identification of the polymer residue of poly-(phenylene sulphide) on carbon fiber surfaces gives important information on the composite failure mechanism. Using scanning force microscopy (SFM) in its lateral force imaging mode or with the stiffness imaging mode, it is almost impossible to distinguish the two composite components owing to a very low material-based contrast of the local friction and compliance. The new technique using contrast based on a local AC current measurement allows a clear identification of the conducting carbon fiber and the non-conducting polymer coverage. KW - Matrix adhesion KW - Films KW - Photoconduction KW - Composites PY - 1995 DO - https://doi.org/10.1002/actp.1995.010460505 SN - 0323-7648 SN - 1521-4044 VL - 46 IS - 5 SP - 379 EP - 384 PB - Wiley-VCH Verl. CY - Weinheim, Germany AN - OPUS4-6848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sturm, Heinz A1 - Silbernagl, Dorothee A1 - Ghasem Zadeh Khorasani, Media T1 - Improving polymer matrix additives for composite structures: a focus on boehmite N2 - The aims of the Research Unit „Acting Principles of Nano-Scaled Matrix Additives for Composite Structures“ (DFG FOR 2021) are based on different synergetic pathways. Challenges are to achieve an improved damage tolerance combined with unchanged processability and a proof of the nano-based effect from molecular scale up to structural level. First of all, a comprehensive understanding of the acting mechanisms of nano-scaled ceramic additives onto polymer matrices of continuous fibre reinforced polymer composites with respect to improved matrix dominated properties is in focus. To proof of the nanoscopic and microscopic effects up to structural level; experimental investigations start on the functional correlation between the particle properties and the resulting properties of the epoxy as suspension and in the solid state. This includes tests for the resulting composite structures as well. Along the entire process chain different multi-scale simulations are performed from molecular modelling up to the macroscopic, structural level. The combination of experimental investigations and simulation methods enables a holistic understanding of the acting principles and basic mechanisms. Specialized techniques based on Scanning Force Microscopy are the basis of our analysis of physicochemical properties of the boehmite nanoparticles and their polymer environment. A surface map of mechanical properties as an input for simulations facilitate a deeper understanding of such composites across all scales. This enables us to understand the macroscopic structure-property relationship and to predict failure mechanisms as well as routes for optimization. T2 - 92nd DKG annual meeting and symposium on high performance ceramics CY - Berlin, Germany DA - 19.03.2017 KW - Boehmite nanoparticle KW - Intermodulation AFM KW - Composite structures KW - Pull-out test KW - Thermoset KW - Crack propagation energy PY - 2017 AN - OPUS4-39519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sigrüner, M. A1 - Hüsken, Götz A1 - Pirskawetz, Stephan A1 - Herz, J. A1 - Muscat, D. A1 - Strübbe, N. T1 - Pull-out behavior of polymer fibers in concrete JF - Journal of Polymer Science N2 - The bond between polymer fibers and the surrounding cementitious matrix is essential for the development of concrete reinforcement. The single fiber pull-out test (SFPT) is the standard characterization technique for testing the bond strength. However, the different phases of debonding cannot be distinguished by the SFPT. This study investigates the debonding of different polymer fibers from the surrounding cementitious matrix with a modified SFPT and proposes methods to change the SFPT setup to generate more valuable information on the debonding mechanism. The SFPT was equipped with linear variable differential transformers (LVDT), digital image correlation (DIC) and acoustic emission (AE) analysis. The results demonstrate that the modified SFPT allows a better understanding of the different phases of debonding during fiber pull-out. Furthermore, bond strength values calculated by different methods reveal that the chemical bond of the investigated polymers is not different as reported by previous studies. Deformation measurements performed using LVDTs and DIC are suitable measuring techniques to characterize the debonding mechanism in SFPT. A correlation between recorded AE and debonding phases was not found. KW - Polymer Fibres KW - Concrete KW - Pull-Out Behaviour KW - Debonding Mechanism PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582918 DO - https://doi.org/10.1002/pol.20230264 SN - 2642-4169 SP - 1 EP - 13 PB - Wiley Periodicals, LLC. AN - OPUS4-58291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shirshova, N. A1 - Bismarck, A. A1 - Greenhalgh, E.S. A1 - Johansson, P. A1 - Kalinka, Gerhard A1 - Marczewski, M.J. A1 - Shaffer, M.S.P. A1 - Wienrich, Malte T1 - Composition as a means to control morphology and properties of epoxy based dual-phase structural electrolytes JF - The journal of physical chemistry / C N2 - Structural electrolytes were prepared using a fully formulated commercially available high performance epoxy resin (MTM57) and an ionic liquid based electrolyte: lithium bis(trifluoromethylsulfonyl)imide (LiTFSI) dissolved in 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (EMIM-TFSI). Through a systematic study, the composition of the formulations was found to have a greater effect than the curing temperature on the morphology and properties of the resulting structural electrolytes. The presence of lithium salt is essential to form a structurally homogeneous electrolyte. Bicontinuous morphologies containing continuous (coarse) epoxy networks surrounded by connected spherical epoxy nodules were obtained with different length scales upon varying the lithium salt concentration. Increasing the LiTFSI concentration improved the miscibility of MTM57 with the electrolyte and decreased the characteristic length scale of the resulting bicontinuous microstructure. The properties of the structural electrolytes correlated with the morphology, showing increased Young’s modulus and decreased ionic conductivity with increasing lithium salt concentration. The miscibility of the epoxy system with the electrolyte was also improved by substitution of EMIM-TFSI with an equal weight of an aprotic organic solvent, propylene carbonate (PC); however, the window of PC concentrations which resulted in structural electrolytes with bicontinuous microstructures was very narrow; at PC concentrations above 1 wt %, gel-like polymers with no permanent mesoporosity were obtained. KW - Functional composites KW - Mechanical properties KW - Elastic properties KW - Epoxy KW - Morphology KW - Electrolyte PY - 2014 DO - https://doi.org/10.1021/jp507952b SN - 1932-7447 SN - 1089-5639 VL - 118 IS - 49 SP - 28377 EP - 28387 PB - Soc. CY - Washington, DC AN - OPUS4-34565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shirshova, N. A1 - Bismarck, A. A1 - Carreyette, S. A1 - Greenhalgh, E.S. A1 - Johansson, P. A1 - Marczewski, M.J. A1 - Jacobsson, P. A1 - Kalinka, Gerhard A1 - Shaffer, M.S.P. A1 - Wienrich, Malte A1 - Steinke, J.H.G. T1 - Correlations between mechanical properties and ionic conduction of structural electrolytes with bicontinuous morphologies T2 - ICCM19 - 19th International conference on composite materials (Proceedings) N2 - Electrolyte systems that can carry mechanical load while allowing for high levels of ionic conductivity are an important prerequisite for structural power storage devices. Introduction of structural power storage into the variety of consumer products will allow saving in weight and volume. Moreover, using a supercapacitor/battery system in hybrid electric vehicles (HEV), the supercapacitor part will extend the battery lifetime by protecting it from the high peak currents. To successfully produce structural power storage requires the development of multifunctional electrolytes where one has to simultaneously maximize mechanical properties and ionic conductivity. T2 - ICCM19 - 19th International conference on composite materials CY - Montreal, Canada DA - 28.07.2013 KW - Structural electrolyte KW - Multifunctional supercapacitor KW - Bicontinuous morphology KW - Epoxy resin KW - Ionic conductivity KW - Mechanical properties PY - 2013 SP - 72 EP - 79 AN - OPUS4-29273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shirshova, N. A1 - Bismarck, A. A1 - Carreyette, S. A1 - Fontana, Q.P.V. A1 - Greenhalgh, E.S. A1 - Jacobsson, P. A1 - Johansson, P. A1 - Marczewski, M.J. A1 - Kalinka, Gerhard A1 - Kucernak, A.R.J. A1 - Scheers, J. A1 - Shaffer, M.S.P. A1 - Steinke, J.H.G. A1 - Wienrich, Malte T1 - Structural supercapacitor electrolytes based on bicontinuous ionic liquid-epoxy resin systems JF - Journal of materials chemistry A N2 - 'Structural electrolytes' retain the desirable mechanical characteristics of structural (epoxy) resins whilst introducing sufficient ionic conductivity to operate as electrolytes in electrochemical devices. Here, a series of ionic liquid–epoxy resin composites were prepared to identify the optimum system microstructure required to achieve a high level of multifunctionality. The ionic conductivity, mechanical properties, thermal stability and morphology of the cured epoxy based structural electrolytes were studied as a function of phase composition for three fully formulated high performance structural epoxy systems. At only 30 wt% of structural resin and 70 wt% of ionic liquid based electrolyte, stiff monolithic plaques with thicknesses of 2–3 mm were obtained with a room temperature ionic conductivity of 0.8 mS cm-1 and a Young's modulus of 0.2 GPa. This promising performance can be attributed to a long characteristic length scale spinodal microstructure, suggesting routes to further optimisation in the future. KW - Epoxy KW - Ionic liquid KW - Supercapacitor PY - 2013 DO - https://doi.org/10.1039/c3ta13163g SN - 2050-7496 SN - 2050-7488 VL - 1 IS - 48 SP - 15300 EP - 15309 PB - RSC CY - London [u.a.] AN - OPUS4-29735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäferling, Michael T1 - Nanoparticle-based luminescent probes for intracellular sensing and imaging of pH JF - WIREs Nanomedicine and Nanobiotechnology N2 - Fluorescence imaging microscopy is an essential tool in biomedical research. Meanwhile, various fluorescent probes are available for the staining of cells, cell membranes, and organelles. Though, to monitor intracellular processes and dysfunctions, probes that respond to ubiquitous chemical parameters determining the cellular function such as pH, pO2, and Ca2+ are required. This review is focused on the progress in the design, fabrication, and application of photoluminescent nanoprobes for sensing and imaging of pH in living cells. The advantages of using nanoprobes carrying fluorescent pHindicators compared to single molecule probes are discussed as well as their limitations due to the mostly lysosomal uptake by cells. Particular attention is paid to ratiometric dual wavelength nanosensors that enable intrinsic referenced measurements. Referencing and proper calibration procedures are basic prerequisites to carry out reliable quantitative pH determinations in complex samples such as living cells. A variety of examples will be presented that highlight the diverseness of nanocarrier materials (polymers, micelles, silica, quantum dots, carbon dots, gold, photon upconversion nanocrystals, or bacteriophages), fluorescent pH indicators for the weak acidic range, and referenced sensing mechanisms, that have been applied intracellularly up to now. KW - pH sensing KW - Luminescent probes KW - Imaging PY - 2016 DO - https://doi.org/10.1002/wnan.1366 SN - 1939-0041 SN - 1939-5116 VL - 8 IS - 3 SP - 378 EP - 413 PB - Wiley-Blackwell CY - Hoboken, New Jersey, USA AN - OPUS4-36367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, Eckhard A1 - Kalinka, Gerhard A1 - Meretz, S. A1 - Hampe, Andreas T1 - Pull-out of Single Fibres JF - Kunststoffe : bilingual edition, German + English KW - Verstärkungsfaser KW - Verbundwerkstoffe KW - Interface KW - Adhäsion KW - Reibung KW - Haftung KW - Thermoplast PY - 1994 SN - 0945-0084 VL - 84 IS - 5 SP - 25 EP - 26 PB - Hanser CY - München AN - OPUS4-11989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, Eckhard A1 - Kalinka, Gerhard A1 - Auersch, W. T1 - Effect of Transcrystallization in Carbon Fiber Reinforced Poly(p/phenylene sulfide) Composites on the Interfacial Shear Strength Investigated with the Single Fiber Pull-Out Test JF - Journal of macromolecular science B N2 - The effect of transcrystallinity in carbon fiber reinforced poly(p-phenylene sulfide (PPS) composites on the apparent shear strength was investigated with the single fiber pull-out test. Transcrystalline zones around the reinforcing fibers do not seem to improve the adhesion level significantly. Neighbor fibers hinder the formation of the transcrystalline zone and a ductile fracture behavior can be observed. However, the apparent strength level is slightly higher for composites containing such reinforcing neighbor fibers compared with single fiber composite samples. During annealing a brittle interface can be formed in the multifiber composite yielding a higher level of the apparent shear strength. KW - Thermoplaste KW - Kristallisation KW - Transkristallisation KW - Interface KW - Verbundwerkstoffe KW - Pull-out KW - Haftung KW - Adhäsion KW - Reibung PY - 1996 DO - https://doi.org/10.1080/00222349608220393 SN - 0022-2348 SN - 1525-609X VL - 35 IS - 3-4 SP - 527 EP - 546 PB - Dekker Chemistry CY - New York, NY AN - OPUS4-11987 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Eckhard A1 - Kalinka, Gerhard T1 - Effect of Transcrystallization in Carbon Fibre Reinforced Poly(p-phenylene sulfide) Composites on the Interfacial Shear Strength Investigated with the Single Fibre Pull-out Test T2 - Europhysics Conference on Macromolecular Physics T2 - Europhysics Conference on Macromolecular Physics CY - Prague, Czech Republic DA - 1995-07-17 PY - 1995 AN - OPUS4-12084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Eckhard A1 - Kalinka, Gerhard A1 - Sturm, Heinz A1 - Munz, Martin T1 - Investigations of the mechanical behaviour of heterogeneous polymeric systems and fibre reinforced composites using micro indentation and scanning force microscopy T2 - Special Lectures, 18. Disc. Conf. And 56the PMM.: Mech. Behaviour of polymeric materials T2 - Special Lectures, 18. Disc. Conf. And 56the PMM.: Mech. Behaviour of polymeric materials CY - Prague, Czech Republic DA - 1998-07-20 PY - 1998 AN - OPUS4-12092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Eckhard A1 - Kalinka, Gerhard A1 - Leistner, André A1 - Sturm, Heinz A1 - Munz, Martin A1 - Hampe, Andreas T1 - Investigation of polymeric composites reinforced with high oriented short glass fibres using the single fibre push-out test T2 - Euro-Conf. Surfaces and Interfaces in Polymers and Composites T2 - Euro-Conf. Surfaces and Interfaces in Polymers and Composites CY - Lausanne, Switzerland DA - 1997-06-03 PY - 1997 AN - OPUS4-6439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Eckhard A1 - Kalinka, Gerhard A1 - Sturm, Heinz A1 - Munz, Martin T1 - Investigation on mechanical behaviour of heterogeneous polymeric systems and fibre reinforced composites using micro indentation and scanning force microscopy T2 - 18th Disc. Conf. and 56th PMM T2 - 18th Disc. Conf. and 56th PMM CY - Prague, Czech Republic DA - 1998-07-20 PY - 1998 AN - OPUS4-6451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schukar, Vivien A1 - Kusche, Nadine A1 - Kalinka, Gerhard A1 - Habel, Wolfgang T1 - Field deployable fiber bragg grating strain patch for long-term stable health monitoring applications JF - Applied sciences N2 - A fiber Bragg grating (FBG) strain patch specially adapted for long-term and high-strain applications has been developed and characterized. The design concept for the patch is based on a glass-fiber reinforced plastic (gfrp) carrier material. The developed concept for the FBG integration into the carrier material was derived from reliable integration procedure of FBG sensors into composite structures. The patches' temperature sensitivity, strain gauge factor, fiber–matrix interface adhesion and fatigue behavior were characterized. As a result, FBG strain patches with linear temperature and strain behavior, as well as excellent fatigue resistance, were developed and can be used as part of a monitoring system for advanced composite materials in aerospace structures or wind turbine power plants. KW - Fiber Bragg grating KW - Patch KW - Strain gauge factor KW - Temperature sensitivity KW - Push-out test KW - Validation KW - Fatigue behavior PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-276271 DO - https://doi.org/10.3390/app3010039 SN - 2076-3417 VL - 3 IS - 1 SP - 39 EP - 54 PB - MDPI CY - Basel AN - OPUS4-27627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schukar, Vivien A1 - Baitinger, Eugen A1 - Kusche, Nadine A1 - Steinke, F. A1 - Habel, Wolfgang T1 - Use of spectral conditions to separate strain and temperature effects in fibre Bragg grating sensors embedded in load-carrying anisotropic laminates JF - Experimental mechanics N2 - This work presents a further development of the methods of simultaneous determination of temperature and axial strain using a single fibre Bragg grating (FBG). The reflected spectrum of composite-embedded FBG sensors has been analyzed in order to separate temperature and load effects. We found out that during the curing process of the laminates, a superstructure has been introduced on the FBG. Analyzing this effect, a temperature and strain separation was implemented by simply calculating and comparing the integrated intensity of the spectral response signal. A mathematical four-parametric model has been developed to calculate the reflected spectrum of a superstructured fibre Bragg grating. The mathematically achieved data has been evaluated with experimentally determined data from fibre Bragg gratings embedded in glass-fibre reinforced composite materials. KW - Fibre Bragg grating KW - Patch KW - Four-parametric KW - model KW - Superstructure KW - Temperature KW - Strain PY - 2013 DO - https://doi.org/10.1007/s11340-013-9773-y SN - 0014-4851 SN - 1741-2765 VL - 54 IS - 3 SP - 421 EP - 429 PB - Springer CY - Norwell, Mass. AN - OPUS4-29452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schreier, Andy T1 - Distributed Brillouin sensing in polymer optical fibers N2 - A brief overview about the results obtained within the BAM PhD framwork. T2 - Meeting of the Terahertz-Photonics-Group at IHF, Technische Universität Braunschweig CY - Braunschweig, Germany DA - 17.07.2019 KW - Brillouin KW - Distributed sensing KW - Polymer optical fibre PY - 2019 AN - OPUS4-48501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilder, Constanze A1 - Schukar, Marcus A1 - Steffen, Milan A1 - Krebber, Katerina T1 - Structural health monitoring of composite structures by distributed fibre optic sensors T2 - 5th International symposium on NDT in aerospace N2 - Structural Health Monitoring of composite materials gains in importance with the increasing use of Composite structures for safety-related applications, e.g. in aerospace. Because of the material properties of composites, defects often occur inside the structures and raise the demand for integrated sensors. The advantages of optical fibres predestine them not only for the surface-application on composite structures but also for the Integration into composite structures. Even without quasi-distributed sensors such as FBGs or LPGs, the optical fibre itself can be used to measure the structure and occurring events over the entire fibre length by distributed sensing techniques. This paper presents the surface-application of polyimide coated silica optical fibres onto PEEK specimens and the integration of copper and polyimide coated silica optical fibres into an AS-4/PEEK Composite to be used as distributed fibre optic sensors for SHM. Results from distributed measurements by optical backscatter reflectometry based on Rayleigh backscattering are shown. T2 - 5th International symposium on NDT in aerospace CY - Singapore DA - 13.11.2013 KW - Structural health monitoring (SHM) KW - Composite structures KW - Optical fibre KW - Distributed fibre optic sensors KW - Optical backscatter reflectometry PY - 2013 SN - 1435-4934 SP - 1 EP - 7 AN - OPUS4-29687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radl, S. A1 - Kreimer, M. A1 - Manhart, J. A1 - Griesser, T. A1 - Moser, A. A1 - Pinter, G. A1 - Kalinka, Gerhard A1 - Kern, W. A1 - Schlögl, S. T1 - Photocleavable epoxy based materials JF - Polymer N2 - The present study aims at the development of photodegradable epoxy based materials comprising o-nitrobenzyl ester links that undergo well defined bond cleavage in response to UV irradiation. New bi-functional epoxy based monomers bearing o-nitrobenzyl ester groups are synthesized and thermally cured with an anhydride hardener to yield photosensitive polymers and duromers. The UV induced changes in solubility are exploited for the preparation of positive-type photoresists. Thin patterned films are obtained by photolithographic processes and characterized by microscopic techniques. The results evidence that sensitive resist materials with good resolution and high contrast behavior can be accomplished. Along with resist technology, the applicability of o-nitrobenzyl chemistry in the design of recyclable polymer materials with thicknesses in the millimeter range is evaluated. By monitoring the thermo-mechanical properties upon UV illumination, a distinctive depletion of storage modulus and glass transition temperature is observed with increasing exposure dose. Additionally, single fiber pull-out tests are carried out revealing a significant decrease of the interfacial adhesion at the fiber-matrix interface due to the phototriggered cleavage reaction. KW - Epoxy based network KW - Photocleavage KW - o-Nitrobenzyl ester KW - Adhesion KW - Mechanical properties KW - Interfacial shear strength PY - 2015 DO - https://doi.org/10.1016/j.polymer.2015.05.055 SN - 0032-3861 SN - 1873-2291 VL - 69 SP - 159 EP - 168 PB - Elsevier Ltd. AN - OPUS4-34566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Paulick, C. A1 - Kalinka, Gerhard T1 - Helical zirconia (TZP) springs manufacturing and testing under mechanical and thermal load N2 - Helical springs with a rectangular cross-section have been machined from sintered and grinded hollow cylinders with high geometrical precision and good reproducibility. Such springs made from tetragonal zirconia polycrystal (TZP) ceramic show excellent edge quality because of high fracture toughness and bending strength of the starting material. Hence, springs with desired geometric dimension and tailored spring constant can be manufactured for highly demanding applications at high temperatures and in harsh environments. Prior to any practical use, application limits of springs under mechanical and thermal load have to be analyzed. Therefore, different displacement experiments were carried out on the helical TZP springs. - Dynamic displacement tests at various temperatures from -15°C to +60°C using a piezo actor to load/unload springs with frequencies between 1 and 40 Hz: Springs remained undamaged and the spring constants were not altered, even after more than one million cycles of compression loading. - Long-time displacement measurements under static tensile loading at room temperature with a high-precision interferometer test facility: Significant spring elongation under constant strain was surprisingly proved over a period of many hours already at room temperature. - Creeping experiments for 48 h under static compression load at different temperatures up to 1000 °C: After cooling down and load removing no permanent length reduction of springs was observed for test temperatures up to 700 °C. However, reshaping of TZP springs by plastic deformation is possible at higher temperatures and opens up additional possibilities for spring design and manufacturing. T2 - German Ceramic Society, Annual Meeting 2018 CY - München, Germany DA - 09.04.2018 KW - Ceramic springs KW - Manufacturing KW - Mechanical and thermal testing PY - 2018 AN - OPUS4-44728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Kalinka, Gerhard T1 - Deformation behavior of alumina and zirconia springs at room temperature N2 - At high temperatures and in harsh environments ceramic springs are often superior to metallic springs and allow for innovative solutions. A recently proposed application involves ceramic springs with metallized surfaces as capacitive force sensor. A strictly linear stress-strain characteristic of the spring is a precondition for such a sensor. Helical ceramic springs with rectangular cross-section have been produced from sintered hollow cylinders. Alumina, ATZ, Y-TZP, and Ce-TZP springs with identical dimensions were characterized and compared regarding deformation behavior. Spring deformation was investigated under various load scenarios. Dynamic compression was performed with deformation speeds from 0.3 to 30 mm/min. Spring constants of alumina springs are strain rate independent. By contrast, Y-TZP spring constant increases by approximately 3 % within the experimental framework. A high-precision test facility was developed to characterize spring displacement in nm range under static tensile load over long periods of time. Spring elongation with asymptotic course was observed for zirconia containing materials at room temperature. This effect is particularly strong in the case of Y-TZP. Up to 0.3 % time-dependent elongation was measured after 24 h under constant load. Deformation is completely reversible after unloading. Alumina springs do not show any time-dependent deformation under identical test conditions. Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs at room temperature was proved in both test series. It is supposed, that pseudo-elasticity caused by stress-induced phase transformation from tetragonal to monoclinic is responsible for this special behavior of TZP springs. T2 - D-A-CH Keramiktagung CY - Leoben, Austria DA - 06.05.2019 KW - Phase transformation KW - Ceramic spring KW - Force-distance diagram KW - Deformation behavior PY - 2019 AN - OPUS4-48026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, T. A1 - Kalinka, Gerhard A1 - Mieller, Björn T1 - Manufacturing and deformation behavior of alumina and zirconia helical springs at room temperature JF - Journal of the American Ceramic Society N2 - Ceramic helical springs with identical dimensions were produced by hard machining from alumina, alumina toughened zirconia (ATZ), and tetragonal zirconia polycrystals (TZP) stabilized with different oxides. According to the results of the spring constant determination under deformation rates of 3 mm/min, the deformation behavior of all ceramic springs obeys to Hook’s law. However, variation of the deformation rate, tests under constant load, and spring recovery behavior revealed differences in the deformation behavior of alumina, TZP, and ATZ springs. Alumina springs exhibited time-independent deformation in all tests. In contrast, anelastic deformation at room temperature was demonstrated in all springs containing TZP. This deformation is completely reversible over a period of several days. Anelastic behavior is particularly pronounced in Y-TZP springs, whereas Ce-TZP springs exhibit comparatively very low but still reliably detectable anelasticity. Oxygen vacancies in the TZP ceramic are considered the most likely explanation for the anelastic behavior of TZP springs at room temperature. KW - Alumina KW - Creep KW - Elastic properties KW - Zirconia PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571858 DO - https://doi.org/10.1111/jace.19085 SN - 0002-7820 SP - 1 EP - 14 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-57185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Qian, Hui A1 - Bismarck, A. A1 - Greenhalgh, E.S. A1 - Kalinka, Gerhard A1 - Shaffer, M.S.P. T1 - Hierarchical composites reinforced with carbon nanotube grafted fibers: The potential assessed at the single fiber level JF - Chemistry of materials N2 - The feasibility of reinforcing conventional carbon fiber composites by grafting carbon nanotubes (CNTs) onto the fiber surface has been investigated. Carbon nanotubes were grown on carbon fibers using the chemical vapor deposition (CVD) method. Iron was selected as the catalyst and predeposited using the incipient wetness technique before the growth reaction. The morphology of the products was characterized using scanning electron microscopy (SEM), which showed evidence of a uniform coating of CNTs on the fiber surface. Contact angle measurements on individual fibers, before and after the CNT growth, demonstrated a change in wettability that can be linked to a change of the polarity of the modified surface. Model composites based on CNT-grafted carbon fibers/epoxy were fabricated in order to examine apparent interfacial shear strength (IFSS). A dramatic improvement in IFSS over carbon fiber/epoxy composites was observed in the single fiber pull-out tests, but no significant change was shown in the push-out tests. The different IFSS results were provisionally attributed to a change of failure mechanism between the two types of tests, supported by fractographic analysis. KW - Composites KW - Nano tubes KW - Grafting KW - Interface PY - 2008 DO - https://doi.org/10.1021/cm702782j SN - 0897-4756 SN - 1520-5002 VL - 20 IS - 5 SP - 1862 EP - 1869 PB - American Chemical Society CY - Washington, DC AN - OPUS4-34568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Qian, H. A1 - Kalinka, Gerhard A1 - Chan, K.L.A. A1 - Kazarian, S.G. A1 - Greenhalgh, E.S. A1 - Bismarck, A. A1 - Shaffer, M.S.P. T1 - Mapping local microstructure and mechanical performance around carbon nanotube grafted silica fibres: Methodologies for hierarchical composites JF - Nanoscale N2 - The introduction of carbon nanotubes (CNTs) modifies bulk polymer properties, depending on intrinsic quality, dispersion, alignment, interfacial chemistry and mechanical properties of the nanofiller. These effects can be exploited to enhance the matrices of conventional microscale fibre-reinforced polymer composites, by using primary reinforcing fibres grafted with CNTs. This paper presents a methodology that combines atomic force microscopy, polarised Raman spectroscopy, and nanoindentation techniques, to study the distribution, alignment and orientation of CNTs in the vicinity of epoxy-embedded micrometre-scale silica fibres, as well as, the resulting local mechanical properties of the matrix. Raman maps of key features in the CNT spectra clearly show the CNT distribution and orientation, including a ‘parted’ morphology associated with long grafted CNTs. The hardness and indentation modulus of the epoxy matrix were improved locally by 28% and 24%, respectively, due to the reinforcing effects of CNTs. Moreover, a slower stress relaxation was observed in the epoxy region containing CNTs, which may be due to restricted molecular mobility of the matrix. The proposed methodology is likely to be relevant to further studies of nanocomposites and hierarchical composites. KW - Nanotubes KW - Silica fibres KW - Nano indentation KW - Mapping PY - 2011 DO - https://doi.org/10.1039/c1nr10497g SN - 2040-3364 SN - 2040-3372 VL - 3 IS - 11 SP - 4759 EP - 4767 PB - RSC Publ. CY - Cambridge AN - OPUS4-34718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pommet, M. A1 - Juntaro, J. A1 - Heng, J.Y.Y. A1 - Mantalaris, A. A1 - Lee, A.F. A1 - Wilson, K. A1 - Kalinka, Gerhard A1 - Shaffer, M.S.P. A1 - Bismarck, A. T1 - Surface modification of natural fibers using bacteria: depositing bacterial cellulose onto natural fibers to create hierarchical fiber reinforced nanocomposites JF - Biomacromolecules N2 - Triggered biodegradable composites made entirely from renewable resources are urgently sought after to improve material recyclability or be able to divert materials from waste streams. Many biobased polymers and natural fibers usually display poor interfacial adhesion when combined in a composite material. Here we propose a way to modify the surfaces of natural fibers by utilizing bacteria (Acetobacter xylinum) to deposit nanosized bacterial cellulose around natural fibers, which enhances their adhesion to renewable polymers. This paper describes the process of modifying large quantities of natural fibers with bacterial cellulose through their use as substrates for bacteria during fermentation. The modified fibers were characterized by scanning electron microscopy, single fiber tensile tests, X-ray photoelectron spectroscopy, and inverse gas chromatography to determine their surface and mechanical properties. The practical adhesion between the modified fibers and the renewable polymers cellulose acetate butyrate and poly(l-lactic acid) was quantified using the single fiber pullout test. KW - Composires KW - Bacteria KW - Surface KW - Cellulose natural fibers PY - 2008 DO - https://doi.org/10.1021/bm800169g SN - 1525-7797 VL - 9 IS - 6 SP - 1643 EP - 1651 PB - ACS Publ. CY - Washington, DC, USA AN - OPUS4-23162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plichta, T. A1 - Sirjovona, V. A1 - Zvonek, M. A1 - Kalinka, Gerhard A1 - Cech, V. T1 - The Adhesion of Plasma Nanocoatings Controls the Shear Properties of GF/Polyester Composite JF - Polymers N2 - High-performance fibre-reinforced polymer composites are important construction materials based not only on the specific properties of the reinforcing fibres and the flexible polymer Matrix but also on the compatible properties of the composite interphase. First, oxygen-free (a-CSi:H) and oxygen-binding (a-CSiO:H) plasma nanocoatings of different mechanical and tribological properties were deposited on planar silicon dioxide substrates that closely mimic E-glass. The nanoscratch test was used to characterize the nanocoating adhesion expressed in terms of critical normal load and work of adhesion. Next, the same nanocoatings were deposited on E-glass fibres, which were used as reinforcements in the polyester composite to affect its interphase properties. The shear properties of the polymer composite were characterized by macro- and micromechanical tests, namely a short beam shear test to determine the short-beam strength and a single fibre push-out test to determine the interfacial shear strength. The results of the polymer composites showed a strong correlation between the short-beam strength and the interfacial shear strength, proving that both tests are sensitive to changes in fibre-matrix adhesion due to different surface modifications of glass fibres (GF). Finally, a strong correlation between the shear properties of the GF/polyester composite and the adhesion of the plasma nanocoating expressed through the work of adhesion was demonstrated. Thus, increasing the work of adhesion of plasma nanocoatings from 0.8 to 1.5 mJ·m−2 increased the short-beam strength from 23.1 to 45.2 MPa. The results confirmed that the work of adhesion is a more suitable parameter in characterising the level of nanocoating adhesion in comparison with the critical normal load. KW - Mechanical properties KW - Plasma nanocoatings KW - Glass fibre KW - Polymer composite KW - Short-beam strength KW - Interfacial shear strength KW - Work of adhesion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521844 DO - https://doi.org/10.3390/polym13040593 VL - 13 IS - 4 SP - 593 PB - MDPI CY - Basel,Schweiz AN - OPUS4-52184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Palantöken, Sinam A1 - Bethke, K. A1 - Zivanovic, V. A1 - Kneipp, Janina A1 - Rademann, Klaus A1 - Kalinka, Gerhard T1 - Cellulose hydrogels physically crosslinked by glycine: Synthesis, characterization, thermal and mechanical properties JF - Journal of Applied Polymer Science N2 - Biopolymers are very efficient for significant applications ranging from tissue engineering, biological devices to water purification. There is a tremendous potential value of cellulose because of ist being the most abundant biopolymer on earth, swellability, and functional groups to be modified. A novel, highly efficient route for the fabrication of mechanically stable and natural hydrogels is described in which cellulose and glycine are dissolved in an alkaline solution of NaOH and neutralized in an acidic solution. The dissolving temperature and the glycine amount are essential parameters for the self-assembly of cellulose chains and for Tuning the morphology and the aggregate structures of the resulting hydrogels. Glycine plays the role of a physical crosslinker based on the Information obtained from FTIR and Raman spectra. Among the prepared set of hydrogels, CL5Gly30 hydrogels have the highest capacity to absorb water. The prepared CL5Gly30 gels can absorb up to seven times their dry weight due to its porous 3-D network structure. CL5Gly10 hydrogel exhibits 80% deformation under 21 N force executed. The method developed in this article can contribute to the application of heavy metal adsorption in aqueous solutions for water purification and waste management. KW - Biopolymer KW - Cellulose KW - Hydrogel KW - Natural KW - Synthesis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486845 DO - https://doi.org/10.1002/APP.48380 SN - 1097-4628 SN - 0021-8995 VL - 136 SP - 48380, 1 EP - 11 PB - Wiley CY - USA AN - OPUS4-48684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, H. A1 - Kalinka, Gerhard A1 - Hinrichsen, G. T1 - Investigations on the cold crystallization of pure and filled PETP by dielectric measurements JF - Acta polymerica N2 - The cold crystallization of pure and filled poly(ethylene terephthalate) (PETP) after quenching from the melt has been investigated by dielectric measurements in two different modes: The first one using constant heating-rate (in the temperature range from 320 to 480 K) and the second one under isothermal conditions (at 378 K). The complex dielectric constant (ε´, tan δ) is influenced by crystallization. Two α-relaxation regions are identified: The αa-relaxation region from the pure amorphous phase and the α´-relaxation region from the spherulitic phase. The investigations on the filled systems (PETP + 10% aramid puple, PETP + 30% short glass fibres) prove that an influence of the fillers on the time delay and rate of crystallization and on the geometry of the growing spherulites exists. KW - Verbundwerkstoffe KW - Gefüllte Kunststoffe KW - Elektrische Eigenschaften KW - Verlustfaktor KW - Dielektrische Analyse PY - 1993 SN - 0323-7648 SN - 1521-4044 VL - 44 IS - 1 SP - 25 EP - 28 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Munz, Martin A1 - Chung, Jae Un A1 - Kalinka, Gerhard ED - Possart, W. T1 - Mapping Epoxy Interphases T2 - Adhesion : current research and applications T2 - 7th European Conference on Adhesion ; 7th EURADH CY - Freiberg, Germany DA - 2004-09-01 KW - Interface KW - Interphase KW - Epoxy KW - Copper (Cu) KW - Polyvinylpyrrolidone (PVP) KW - AFM/SFM KW - DSI KW - EDX/EDS KW - Stiffness KW - Modulus KW - Interdiffusion PY - 2005 SN - 3-527-31263-3 VL - 7 SP - 103 EP - 123 PB - Wiley-VCH CY - Weinheim AN - OPUS4-10894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munz, Martin A1 - Sturm, Heinz A1 - Kalinka, Gerhard T1 - On the stiffness gradient at the interface between an amine-cured epoxy and a thermoplast T2 - 6. Workshop 'Rasterkraftmikroskopie in der Werkstoffwissenschaft' an der Uni Erlangen, Inst. für Werkstoffwissenschaften veranstaltet vom Arbeitskreis 'Rastersondenmikroskopie in der Werkstoffwissenschaft' im Fachausschuss Metallographie der Deutschen Gesellschaft für Materialkunde (DGM) T2 - 6. Workshop 'Rasterkraftmikroskopie in der Werkstoffwissenschaft' an der Uni Erlangen, Inst. für Werkstoffwissenschaften veranstaltet vom Arbeitskreis 'Rastersondenmikroskopie in der Werkstoffwissenschaft' im Fachausschuss Metallographie der Deutschen Gesellschaft für Materialkunde (DGM) CY - Erlangen, Germany DA - 2005-02-17 PY - 2005 AN - OPUS4-7137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marotzke, Christian A1 - Kalinka, Gerhard ED - Zachariev, G. T1 - Microscopical Failure Processes in Fiber Reinforced Polymers - Mechanical Aspects of the Adhesion between Fiber and Matrix T2 - Proceedings of the 11th International Conference on Mechanics and Technology of Composite Materials T2 - 11th International Conference on Mechanics and Technology of Composite Materials CY - Sofia, Bulgaria DA - 2006-10-02 KW - Composite materials KW - Failure process KW - Adhesion PY - 2006 SP - 37 EP - 42 PB - Bulgarian Academy of Sciences CY - Sofia AN - OPUS4-14027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marotzke, Christian A1 - Kalinka, Gerhard T1 - Local failure processes in fiber reinforced polymers T2 - ICCM17 - 17th International conference on composite materials (Proceedings) N2 - The breakage of a fiber and its effect on the strain energy is studied in a model composite, this is, a single fiber embedded in a dogbone specimen. The fracture process is recorded by an acoustic emission device, the crack patterns are monitored under a microscope. A finite element analysis is performed in order to estimate the energy released by different failure scenarios. The abilities and limitations of the acoustic emission analysis in characterizing different failure types in fiber reinforced composites are evaluated. T2 - ICCM17 - 17th International conference on composite materials CY - Edinburgh, UK DA - 2009-07-27 KW - Fiber KW - Interface KW - Composite material KW - Failure KW - Acoustic emission KW - Fracture mechanics KW - Energy release rate KW - Finite element analysis PY - 2009 IS - D7:8 SP - 1 EP - 10 CY - Edinburgh, UK AN - OPUS4-21295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marotzke, Christian A1 - Kalinka, Gerhard T1 - Microscopical failure processes in fiber reinforced polymers - Mechanical aspects of the adhesion between fiber and matrix T2 - 11th International Conference on Mechanics and Technology of Composite Materials T2 - 11th International Conference on Mechanics and Technology of Composite Materials CY - Sofia, Bulgaria DA - 2006-10-02 PY - 2006 AN - OPUS4-13239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marotzke, Christian T1 - Strength of composite structural parts - role of the fiber/matrix interface T2 - SEICO 11 - SAMPE Europe - 32nd International technical conference - New Material Characteristics to cover New Application Needs (Proceedings) N2 - The strength of laminates distinctly depends on the transverse strength of the laminas. The transverse failure is dominated by the adhesion between fiber and matrix. Usual strength criteria however do not take into account the adhesive strength explicitly. The determination of the interface strength is performed on the micromechanical scale using single fiber specimens. The fibers are loaded under off-axis loading while the debonding is monitored under a microscope. The stresses acting in the Interface are calculated by finite element analyses. It is found that for off-axial angles up to 35° interfacial debonding is the dominant failure mode while fiber breakage takes place at lower angles. The occurrence of fiber breakage and debonding under off-axis loading shows that the restriction to two potential failure planes - perpendicular or parallel to the fibers - as applied in common failure criteria has to be put in question. T2 - SEICO 11 - SAMPE Europe - 32nd International technical conference CY - Paris, France DA - 28.03.2011 KW - Composites KW - Strength KW - Adhesion PY - 2011 SN - 978-3-9523565-3-1 IS - Session 3B SP - 250 EP - 257 AN - OPUS4-23680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüders, C. A1 - Kalinka, Gerhard A1 - Li, Wei A1 - Sinapius, M. A1 - Wille, T. T1 - Experimental and numerical multiscale approach to thermally cycled FRP JF - Composite Structures N2 - Due to the different thermal expansion of the constituent materials, cyclic thermal loading of FRP induces alternating stresses in the material at two scales: at the micro scale (level of fibre–matrix-interaction) and at the macro scale (level of the multidirectional laminate). Especially the micro scale effect is not comprehensively investigated yet. Additionally, computational investigations mostly neglect this effect due to the homogenous modelling of the composite material. As this effect is assumed to significantly contribute to the fatigue of FRP at thermal loads, the present paper suggests an experimental and numerical multiscale approach including Experiments at the different involved material scales to separately observe the effects acting at these scales. The approach also includes numerical modelling for each scale to complement the knowledge gained from the Experiments and to create a basis for the consideration of the micro effect even in macroscopic fatigue models treating homogeneous modelled composites. The main focus of the contribution is to bring the overall Approach up for discussion, rather than to present the multiscale modelling details. KW - Fatigue KW - Thermal cycling KW - Fibre reinforced plastic KW - Cryogenic KW - Carbon Fibre KW - Epoxy Resin PY - 2020 DO - https://doi.org/10.1016/j.compstruct.2020.112303 SN - 0263-8223 VL - 244 SP - 112303 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-50844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lamoriniere, S. A1 - Mitchell, P. J. A1 - Ho, K. A1 - Kalinka, Gerhard A1 - Shaffer, M. S. P. A1 - Bismarck, A. T1 - Carbon nanotube enhanced carbon Fibre-Poly(ether ether ketone) interfaces in model hierarchical composites JF - Composites Science and Technology N2 - Poly (ether ether ketone) (PEEK) has a high continuous service temperature, excellent mechanical properties, and good solvent and abrasion resistance, which can be further improved through the addition of carbon nanotubes (CNTs). CNT-PEEK nanocomposites are promising matrices for continuous carbon fibre composites; powder processing can mitigate the high melt viscosities in these systems. In this study, model single fibre (hierarchical) composites were produced by embedding sized and desized carbon fibres in nanocomposite CNTPEEK powders followed by single fibre pull-out tests to assess interfacial characteristics. Carbon fibre-PEEK interfacial shear strength is typically 40–45 MPa. Increasing CNT loadings increased fibre-matrix interfacial shear strength linearly up to ~70 MPa at 5.0 wt%, which was attributed to the CNT-based mechanical modification of the PEEK matrix. Apparent interfacial shear strength was inversely correlated with the embedded fibre length irrespective of carbon fibre sizing or CNT loading, indicating brittle fracture of the fibre-matrix interface. Pulled out carbon fibres were still coated with the matrix, which indicated strong adhesion at the interface in all samples, likely related to a transcrystalline region. Adhesion was, however, negatively affected by the presence of epoxy sizings. Frictional shear strength was independent of embedded fibre length and CNT content for all samples. KW - Keywords: Poly(ether ether ketone) KW - Carbon fibres KW - Carbon nanotubes KW - Interfacial strength KW - Debonding PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550052 DO - https://doi.org/10.1016/j.compscitech.2022.109327 SN - 0266-3538 VL - 221 SP - 1 EP - 8 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-55005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, T. A1 - Kalinka, Gerhard A1 - Auer, C. A1 - Hinrichsen, G. T1 - Computer Simulation of Crystallization Kinetics in FIber-Reinforced Composites JF - Journal of applied polymer science KW - Verbundwerkstoffe KW - Thermoplaste KW - Kristallisation KW - Kristallisationskinetik KW - Erstarrung KW - Avrami KW - Modellrechnung KW - Simulation PY - 1994 SN - 0021-8995 SN - 1097-4628 VL - 51 SP - 399 EP - 406 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-11992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krauklis, A. E. A1 - Starovka, O. A1 - Gibhardt, D. A1 - Aouissi, H. A. A1 - Burlakovs, J. A1 - Sabalina, A. A1 - Fiedler, Bodo A1 - Kalinka, Gerhard T1 - Reversible and irreversible effects on the epoxy GFRP fiber-matrix interphase due to hydrothermal aging JF - Composites Part C N2 - Epoxy R-Glass Fiber-Reinforced Polymer (GFRP) composite plates were hydrothermally aged at 60 ◦C for 23, 75, and 133 days. The water content reached 0.97 wt%, 1.45 wt% and 1.63 wt%, respectively. The studied GFRP matrix was inert to hydrolysis or chain scission, allowing for investigation of irreversible changes in the fiber-matrix interphase due to hydrothermal aging upon re-drying. During each period, a subset of the specimens was removed from the water bath and dried in a chamber. The weight loss upon drying was explained with epoxy leaching (impurities), sizing-rich interphase hydrolysis, glass fiber surface hydrolysis, accumulated degradation products escaping, and water changing state from bound to free. The influence of hydrothermal aging on the fiber-matrix interfacial properties was investigated. Lower interfacial strength of hydrothermally aged (wet) samples was attributed to plasticization of the epoxy, plasticization and degradation of the sizing-rich interphase (including formation of hydrolytic flaws), and hydrolytic degradation of the glass fiber surface. The kinetics of epoxy-compatible epoxysilane W2020 sizing-rich interphase hydrolysis provided an estimate of ca. 1.49%, 4.80%, and 8.49% of the total composite interphase degraded after 23, 75, and 133 days, respectively. At these conditions, the interface lost 39%, 48%, and 51% of its strength. Upon re-drying the specimens, a significant part of the interfacial strength was regained. Furthermore, an upward trend was observed, being 13%, 10% and 3% strength, respectively; thus, indicating a possibility of partial recovery of properties. KW - GFRP KW - Hydrothermal Ageging KW - Interphase KW - Water Diffusion KW - Desorption KW - Interfacial Strength PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581554 DO - https://doi.org/10.1016/j.jcomc.2023.100395 SN - 2666-6820 VL - 12 SP - 1 EP - 9 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-58155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - Sahin, M. A1 - Schlögl, S. A1 - Wang, J. A1 - Kaynak, B. A1 - Mühlbacher, I. A1 - Ziegler, W. A1 - Kern, W. A1 - Grützmacher, H. T1 - Tailoring the interfaces in glass fiber-reinforced photopolymer composites JF - Polymer N2 - The present work provides a comparative study on the interface and adhesion properties of surface modified single glass fibers embedded in an acrylate matrix. To facilitate a covalent bonding at the fibermatrix interface, the fibers are functionalized with selected organosilanes that comprise either passive (unsaturated C¼C bonds of methacrylate moieties) or photoactive functionalities (photocleavable bis(acyl)phosphane oxide groups). Immobilization of the functional silanes is carried out by a classic silanization reaction involving a condensation reaction across the surface hydroxyl groups of the inorganic glass fibers. The change of the physico-chemical properties of the fibers due to desizing and subsequent surface modification is monitored by X-ray photoelectron spectroscopy and zeta potential measurements. In addition, scanning electron microscopy is used to follow the changes in surface morphology. After the modification step, the desized and modified single fibers are embedded in a photocurable acrylate resin formulation. By performing single fiber pull-out tests, maximum pull-out force, friction strength and apparent interfacial shear strength are determined as a function of the coupled silanes. The results reveal that the attached organosilanes lead to a significant increase in adhesion strength, whilst the performance of the photo-cleavable organosilane is superior to the passive methacryl-functional derivative. KW - Photocleavable organosilanes KW - Fiber-matrix interface KW - Photopolymer composites KW - Single fiber pull-out test KW - Surface modification PY - 2018 DO - https://doi.org/10.1016/j.polymer.2018.03.020 SN - 0032-3861 VL - 141 SP - 221 EP - 231 PB - Elsevier Ltd. CY - New York AN - OPUS4-44784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - Leistner, André A1 - Hampe, Andreas T1 - Characterisation of the fibre/matrix interface in reinforced polymers by the push-in technique JF - Composites science and technology N2 - The push-in test is the only micromechanical test method that is not restricted to artificial fibre/matrix arrangements, but allows the in situ characterisation of interfaces in composites fabricated and stressed under realistic conditions. However, with the application of this method to reinforced polymers some problems arise both in the mathematical model for evaluating test data and in the practical performance of the test. Because in some cases the deformation of the relatively compliant polymeric matrices cannot be neglected, an extension of the existing model is required. For this purpose, the elastic energy of the material around the debonded part of the fibre is estimated and included in the energy-balance analysis. Because of the small diameter of the fibres usually used for reinforcing polymers, a test apparatus was designed which ensures a high positioning accuracy in the xy plane as well as in the z direction. In order to minimise thermal and mechanical influences, the microscope for fibre selection and the force sensor/indenter are directly connected together and the apparatus is designed to be stiff in all components. A solid-state bending joint guarantees very precise control of the axial movement. Three examples of the application of this easy-to-handle and low-cost test apparatus are presented briefly in the paper: assess fibre/matrix combinations, measures to improve the interfacial adhesion and the influence of water on the interface. KW - Interface KW - Test method KW - Characterisation KW - Indentation KW - Push-in PY - 1997 SN - 0266-3538 VL - 57 IS - 8 SP - 845 EP - 851 PB - Elsevier CY - Barking AN - OPUS4-12011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - Hinrichsen, G. T1 - Two-dimensional computer simulation of spherulite formation by branching lamellae JF - Acta polymerica KW - Thermoplaste KW - Kristallisation KW - Sphärolithe KW - Lamellen KW - Modellrechnungen PY - 1997 SN - 0323-7648 SN - 1521-4044 VL - 48 SP - 256 EP - 261 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-12004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - ElAbshihy, K. T1 - Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation JF - Composite Interfaces N2 - Characterization of the size and mechanical properties of interphases is essential when designing multicomponent materials. When nanoindentation is used to investigate the size and mechanical properties of an interphase, a common challenge is that the indenter or the stress zone formed around it are often restricted by the reinforcement, making it difficult to distinguish the mechanical property variations caused by the interphase itself from those caused by the boundary effect. In this work, a testing system was developed that allows determining the indent affected zone and accounting for it in the interphase measurements of an epoxy/Cu system. Using finite element analysis, we confirmed the validity of the proposed system. Nanoindentation was used to investigate the Interphase between copper and two different epoxy systems; amine-cured and anhydride-cured. Nanoindentation results showed that a copper layer that is only 10 nm thick still exhibits a constriction effect on the indentations in its vicinity. The amine-cured epoxy did not show any sign of interphase existence using the introduced method. However, a soft interphase with a thickness of ~1.7 μm was measured on theanhydride-cured epoxy. Furthermore, we show that the proposed system can be used to determine the interphase thickness as well as its relative mechanical properties regardless of the indentation depth. This system can be further used for investigating other polymer/metal interphases to better understand the factors influencing them, thus helping engineer the interphase size and properties to enhance composite performance. KW - Interphase KW - Polymer-metal KW - Epoxy KW - Copper KW - Composites KW - Nanoindentation PY - 2017 DO - https://doi.org/10.1080/09276440.2017.1286878 SN - 0927-6440 SN - 1568-5543 VL - 24 IS - 9 SP - 833 EP - 848 PB - Taylor & Francis CY - UK AN - OPUS4-39128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -