TY - JOUR
A1 - Schnell, Alexander
A1 - Rübner, Katrin
A1 - Seher, Julia
A1 - Müller, Constanze
A1 - Müller, Anette
A1 - Liebezeit, Steffen
A1 - Fenner, Jacob
A1 - Martin, Falk
A1 - Pniok, Nicole
T1 - Manufacturing and Application of Lightweight Aggregates from Construction and Demolition Waste
N2 - The objective of the REALight project is the development of a thermal process to produce lightweight aggregates in pilot scale and the implantation of a method to recover gypsum. Beside construction and demolition waste, various industrial by‐products are studied as raw materials. The raw materials have so far been unused or used in applications with lower quality requirements. To prove the performance of the lightweight aggregates, their technical properties are tested and their use in different applications is studied, e.g., for lightweight mortars as well as lightweight concretes.
KW - Construction and demolition waste
KW - Flue gas desulfurization gypsum
KW - Industrial by-products
KW - Infra-lightweight concrete
KW - Lightweight aggregates
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604643
DO - https://doi.org/10.1002/cite.202300211
SN - 0009-286X
VL - 96
IS - 7
SP - 969
EP - 975
PB - Wiley-VCH GmbH
CY - Weinheim
AN - OPUS4-60464
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Müller, Alexander
A1 - Trappe, Volker
A1 - Hickmann, Stefan
A1 - Ortwein, H.-P
ED - Christ, Hans-Jürgen
T1 - Investigation of the infinite life of fibre-reinforced plastics using X-ray refraction topography for the in-situ, nondestructive evaluation of micro-structural degradation processes during cyclic fatigue loading
N2 - The described investigation of carbon-fibre-reinforced plastics (CFRP) documents that damage evolution can be observed by means of X-ray refractography. Comparative investigations with synchrotron technique on CFRP and grey-scale analysis on glass fibre-reinforced-plastics (GFRP) confirm these results. Moreover it was found that the fracture mechanical properties of the matrix system influence damage nucleation and propagation in the laminate during static and fatigue loads. Single-step fatigue tests were carried out on Laminates with RIM135 and LY556 matrix systems made from non-crimped fabric (NCF) or twill weave in different fibre orientations. The damage to the LY556 laminates was characterized by laminate cracks growing rapidly over the whole specimen width, whereas the damage on the RIM135 laminates was characterized by an earlier onset of micro-cracking followed by laminate cracks. The specimens were fatigued up to 108 (very high cycle fatigue (VHCF) regime) load cycles. S-N-curves of damage initiation were drawn and boundaries were identified for endurance within the VHCF regime. A phenomenology based model focusing on matrix stress was applied to reproduce the first inter-fibre failure (IFF) under static and fatigue loads.
KW - Carbon fibre-reinforced-plastics
KW - Fatigue
KW - Damage evolution
KW - X-ray refractography
KW - Very high cycle fatigue
PY - 2018
SN - 978-3-658-24531-3
DO - https://doi.org/10.1007/978-3-658-24531-3
VL - 2018
SP - 417
EP - 439
PB - Springer Spektrum
CY - Wiesbaden
ET - 1. Auflage
AN - OPUS4-50096
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Battig, Alexander
A1 - Müller, Patrick
A1 - Bertin, Annabelle
A1 - Schartel, Bernhard
T1 - Hyperbranched Rigid Aromatic Phosphorus-Containing Flame Retardants for Epoxy Resins
N2 - A rigid aromatic phosphorus-containing hyperbranched flame retardant structure is synthesized from 10-(2,5 dihydroxyphenyl)-10H-9-oxa-
10-phosphaphenanthrene-10-oxide (DOPO-HQ), tris(4-hydroxyphenyl)phosphine oxide (THPPO), and 1,4-terephthaloyl chloride (TPC). The resulting poly-(DOPO-HQ/THPPO-terephthalate) (PDTT) is implemented as a flame retardant into an epoxy resin (EP) at a 10 wt% loading. The effects on EP are compared with those of the monomer DOPO-HQ and triphenylphosphine oxide (OPPh3) as low molar mass flame retardants. The glass transition temperature, thermal decomposition, flammability (reaction to small flame), and burning behavior of the thermosets are investigated using differential scanning calorimetry, thermogravimetric analysis, pyrolysis combustion flow calorimetry, UL 94-burning chamber testing, and cone calorimeter measurements.
Although P-contents are low at only 0.6 wt%, the study aims not at attaining V-0, but at presenting a proof of principle: Epoxy resinswith PDTT show promising fire performance, exhibiting a 25% reduction in total heat evolved (THE), a 30% reduction in peak heat release rate (PHRR) due to flame inhibition (21% reduction in effective heat of combustion (EHC)), and an increase in Tg at the same time. This study indicates that rigid aromatic hyperbranched polymeric structures offer a promising route toward multifunctional flame retardancy.
KW - Hyperbranched
KW - Aromatic
KW - Phosphorus
KW - Phosphine oxide
KW - DOPO
KW - Flame retardant
KW - Xpoxy resin
KW - Rigid
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525910
DO - https://doi.org/10.1002/mame.202000731
SN - 1439-2054
VL - 306
IS - 4
SP - 731
PB - Wiley
AN - OPUS4-52591
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Müller, Alexander
T1 - Nondestructive investigation of the VHCF-endurance on cyclically loaded CFRP by X-Ray-Refractography
N2 - Carbon fiber-reinforced-plastics (CFRP) are already used under high-cycle- (HCF) and very-high-cycle-fatigue (VHCF) at relatively low loads not only in aerospace industry, but also in other growing markets like especially wind energy and increasingly also automotive industry. While the static strength of CFRP is satisfyingly predictable by means of layerwise-strenght-analysis and material data from single layers, it is more and more uncertain to predict residual strength or lifetime as the design lifetime increases. Previous studies showed that local minor cracks and inter-fiber-fracture (IFF) originate long before total failure of single layers. Reliable fatigue estimation for fiber-reinforced-plastics is not available at present. Subsequently safety-related primary structures made out of FRP are over dimensioned.
It is possible to detect the change of inner surface in a specimen by means of X-Ray-Refractography. This includes voids, intact fiber-matrix-interfaces as well as defective ones, cracks and all interfaces in plane with the X-Ray-beam. As the crack-density (including IFF) increases, the inner surface of the material correspondingly increases.
The borderline where even at high cycles no early cracks were detected was identified for selected laminates out of woven and non-crimped fabric with epoxy-matrix.
When no micro-cracks were detected up to 106 cycles, the specimens also lasted in the VHCF-regime. Furthermore for the epoxy resin LY556 in combination with carbon fiber it was distinguished that at a load minor to 50% IFF-load level, no micro cracks were detected and consequently the VHCF-endurance reached.
The integration of the set-up small-sized testing machine into the X-Ray buildup in order to achieve in-situ non-destructive detection of the crack initiation while loading the specimens (CFRP and GFRP- woven fabric and non-crimped-fabric) at the same time will increase the performance of the studies.
In earlier investigations at BAM it was shown, that the matrix has a strong influence on the micro-crack formation and finally on the total lifetime. In order to determine the influence of the matrix properties on the boarderline to infinite life, research is done on laminates while replacing the epoxy-based matrix with an equivalent one with different fracture mechanical properties.
With the evolution of early cracks and IFF monitored as well as the influence of the matrix on the crack propagation investigated we are working on an appropriate model to improve lifetime prediction in CFRP. This work is done within the priority program “infinite life” (SPP 1466) funded by Deutsche Forschungsgemeinschaft (DFG).
T2 - ECCM17
CY - München, Germany
DA - 26.06.2016
KW - X-ray
KW - CFRP
KW - FRP
KW - Micro cracks
PY - 2016
AN - OPUS4-38943
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Müller, Alexander
T1 - Nondestructive investigation of the VHCF-endurance on cyclically loaded CFRP by X-Ray-Refractography
N2 - Carbon fiber-reinforced-plastics (CFRP) are already used under high-cycle- (HCF) and very-high-cycle-fatigue (VHCF) at relatively low loads not only in aerospace industry, but also in other growing markets like especially wind energy and increasingly also automotive industry. While the static strength of CFRP is satisfyingly predictable by means of layerwise-strenght-analysis and material data from single layers, it is more and more uncertain to predict residual strength or lifetime as the design lifetime increases. Previous studies showed that local minor cracks and inter-fiber-fracture (IFF) originate long before total failure of single layers. Reliable fatigue estimation for fiber-reinforced-plastics is not available at present. Subsequently safety-related primary structures made out of FRP are over dimensioned.
It is possible to detect the change of inner surface in a specimen by means of X-Ray-Refractography. This includes voids, intact fiber-matrix-interfaces as well as defective ones, cracks and all interfaces in plane with the X-Ray-beam. As the crack-density (including IFF) increases, the inner surface of the material correspondingly increases.
The borderline where even at high cycles no early cracks were detected was identified for selected laminates out of woven and non-crimped fabric with epoxy-matrix.
When no micro-cracks were detected up to 106 cycles, the specimens also lasted in the VHCF-regime. Furthermore for the epoxy resin LY556 in combination with carbon fiber it was distinguished that at a load minor to 50% IFF-load level, no micro cracks were detected and consequently the VHCF-endurance reached.
The integration of the set-up small-sized testing machine into the X-Ray buildup in order to achieve in-situ non-destructive detection of the crack initiation while loading the specimens (CFRP and GFRP- woven fabric and non-crimped-fabric) at the same time will increase the performance of the studies.
In earlier investigations at BAM it was shown, that the matrix has a strong influence on the micro-crack formation and finally on the total lifetime. In order to determine the influence of the matrix properties on the boarderline to infinite life, research is done on laminates while replacing the epoxy-based matrix with an equivalent one with different fracture mechanical properties.
With the evolution of early cracks and IFF monitored as well as the influence of the matrix on the crack propagation investigated we are working on an appropriate model to improve lifetime prediction in CFRP. This work is done within the priority program “infinite life” (SPP 1466) funded by Deutsche Forschungsgemeinschaft (DFG).
T2 - MSE 2016
CY - Darmstadt,Germany
DA - 27.09.2016
KW - CFRP
KW - FRP
KW - X-Ray
KW - Micro cracking
PY - 2016
AN - OPUS4-38945
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Spange, S.
A1 - Seifert, Alexander
A1 - Müller, Hansjörg
A1 - Hesse, S.
A1 - Jäger, Christian
T1 - Fabrication of chromophoric xerogels by senergistic combination of nucleophilic aromatic substitution and the sol-gel process
N2 - The nucleophilic substitution of fluorine of aromatic compounds with n-aminoalkyl trialkoxysilanes and consecutive sol-gel process have been used for the fabrication of various chromophoric sol-gel materials. The displacement of the fluoro substituent of an activated aromatic molecule occurs by a primary or secondary amino group of (CH3O)3Si-(CH2)3-NHR [R- = H-; CH3-, (CH3O)3Si-(CH2)3-] in tetraalkoxysilane or alcohol as solvent and the sol-gel process can be carried in the same vessel. The HF formed is trapped by a tertiary amine and simultaneously serves as the catalyst for the sol-gel process. Various aromatic compounds have been checked for this purpose: 1-(4-fluorophenyl)-2-nitroethylene, 1-(4-fluorophenyl)-2,2-dicyanoethylene, 4-fluorobenzonitrile, 4-fluoronitrobenzene, 4,4prime-difluorobenzophenone, 4,4prime-difluorobenzil, 7,7prime-difluorodibenzylideneacetone, tetrafluoro-p-benzoquinone, and 1,5-difluoro-2,4-dinitrobenzene. Mono and disubstitution has been studied by UV/Vis- and solid state NMR spectroscopy of the xerogels.
PY - 2003
DO - https://doi.org/10.1023/A:1020789318803
SN - 0928-0707
SN - 1573-4846
VL - 26
SP - 77
EP - 81
PB - Kluwer Academic Publ.
CY - Dordrecht
AN - OPUS4-2128
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wang, Y.
A1 - Ulbricht, Alexander
A1 - Schmidt, F.
A1 - Müller, Bernd R.
A1 - Kupsch, Andreas
A1 - Schwitalla, A.D.
T1 - Micro-CT analysis and mechanical properties of low dimensional CFR-PEEK specimens additively manufactured by material extrusion
N2 - Material extrusion of thermoplastic polymers enables the realization of complex specific designs with high performance composites. The present study aims at evaluating the mechanical properties of carbon fiberreinforced semi-crystalline thermoplastic polymer polyether ether ketone (CFR-PEEK) manufactured by material extrusion and correlating them with results obtained by micro-CT. Samples in the shape of small bars were provided by Kumovis (Munich, Germany). The determination of surface roughness and density was followed by three-point bending tests. To reveal the pore distribution as well as the fusion quality of CFR PEEK when applied with external forces, micro-CT scans were performed with an X-ray microscope before and after the mechanical test to localize the sites where the fracture is generated. The density of CFR-PEEK bars indicated that they had superior mechanical properties compared with our previous study on unfilled 3D printed PEEK (bending modulus: (5.4 ± 0.5) GPa vs. (1.05 ± 0.05) GPa to (1.48 ± 0.10) GPa; bending strength: (167 ± 11) MPa vs. (51 ± 15) to (193 ± 7) MPa). Micro-CT analyses revealed the local 3D-distribution of voids. Voids of 30 μm diameter are nearly spherical and make up the main part of the total porosity. The larger the voids, the more they deviate from a spherical shape. Significant lack-of-fusion voids are located between the deposited filaments. By growing and merging, they act as seeds for the forming fracture line in the region of the flexural specimens where the maximum local tensile stresses occurred under bending load. Our work provides a detailed analysis of printed PEEK with fiber additive and relates this with mechanical properties.
KW - CFR-PEEK
KW - Material extrusion (MEX)
KW - FFF
KW - Surface topography
KW - Bending property
KW - Micro-CT
PY - 2023
DO - https://doi.org/10.1016/j.jmbbm.2023.106085
SN - 1751-6161
VL - 146
SP - 1
EP - 9
PB - Elsevier Ltd.
AN - OPUS4-58112
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Rübner, Katrin
A1 - Schnell, Alexander
A1 - Müller, Anette
T1 - Comparative study of lightweight expanded aggregates made from masonry rubble or clay
N2 - Lightweight aggregates can be manufactured from masonry rubble by a thermal expanding process pursuing the idea of feedstock recycling. Throughout a series of research projects, the manufacturing process has been developed, optimized and scaled up. Various test results prove that the engineering properties of the new expanded masonry rubble aggregates are similar to those of traditional expanded clays. The aggregates show a heterogeneous and macroporous pore structure. The grains consist of cracks, cavities, large bulky pores and a solid skeleton containing small capillary pores as well as partly melted areas. But which differences and similarities exist to expanded clay aggregates, which are made from a relatively homogeneous clayey raw material? To answer this question, comparative studies on the chemical, physical, mineralogical and microstructural characteristics of expanded masonry rubble aggregates and commercial expanded clay aggregates have been conducted. In our contribution, results of particle shape and porosity measurements, mercury intrusion porosimetry and electron microscopy are presented. The microstructural characteristics are correlated with engineering properties, such as water absorption and particle strength.
KW - Lightweight aggregates
KW - Expanded aggregates
KW - Expanded granules
KW - Expanded clay
KW - Masonry rubble
KW - Chemical recycling
PY - 2023
SN - 978-2-35158-238-1
VL - 137
SP - 93
EP - 121
PB - RILEM Publications S.A.R.L.
CY - Champs-sur-Marne, France
AN - OPUS4-64752
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Silvestroni, L.
A1 - Kupsch, Andreas
A1 - Müller, Bernd R.
A1 - Ulbricht, Alexander
A1 - Wieder, Frank
A1 - Fritsch, Tobias
A1 - Sciti, D.
A1 - Bruno, Giovanni
T1 - Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
N2 - In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
KW - Ceramic matrix composites
KW - Synchrotron X-ray refraction radiography
KW - X-ray computed tomography
KW - Scanning electron microscopy
KW - High-temperature ceramics
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597712
DO - https://doi.org/10.1016/j.jeurceramsoc.2024.02.048
SN - 0955-2219
VL - 44
IS - 8
SP - 4853
EP - 4862
PB - Elsevier Ltd.
CY - Amsterdam
AN - OPUS4-59771
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Markötter, Henning
A1 - Müller, Bernd R.
A1 - Kupsch, Andreas
A1 - Evsevleev, Sergei
A1 - Arlt, T.
A1 - Ulbricht, Alexander
A1 - Dayani, Shahabeddin
A1 - Bruno, Giovanni
T1 - A Review of X-Ray Imaging at the BAMline (BESSY II)
N2 - The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications.
KW - Material science
KW - Radiography
KW - Refraction
KW - Tomography
KW - X-ray imaging
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572417
DO - https://doi.org/10.1002/adem.202201034
SN - 1438-1656
SP - 1
EP - 22
PB - Wiley VHC-Verlag
AN - OPUS4-57241
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Trappe, Volker
A1 - Müller, Alexander
A1 - Hickmann, Stefan
T1 - Infinite life of CFRP evaluated non-destructively with X-ray-refraction topography in-situ mechanical loading
N2 - Carbon Fibre Reinforced Plastics (CFRP) are more and more used in modern civil aircrafts. These days the whole fuselage is made of this material (B787; A350). Due to strict certification standards the normal in-service loading gives a low stress level compared to the static and even the fatigue strength of the material. Hence CFRP are assumed to have an infinite life. To evaluate this assumption, fatigue tests on CFRP-specimens were performed up to 108 load cycles and the first inter-fibre failure was evaluated non-destructively by accompanying Xray-refraction topography. A tensile testing machine was integrated in a small angle X-ray scattering (SAXS) setup. X-ray refraction topography was performed while the CFRP samples were tensile loaded. This non-destructive technique enables the detection of micro-cracking and inter-fibre failure especially for CFRP. For Glass Fibre Reinforced Plastic (GFRP) X-ray refraction and in-situ loading has already been successfully used. The increase of inner surfaces due to inter fibre failure was measured as a function of the stress state. Fatigue tests were performed at and below the limit of inter-fibre failure strength. State of the art is to assume the failure of the samples under cyclic loading as the fatigue life. Accompanying non-destructive X-ray refraction measurements reflects the damage state and enables to trace its evolution even if the total failure of the specimens does not occur. This investigation technique is of high interest to give the engineer a design value of infinite life which is practically often reached due to knock down factors of certification standards. Finally the infinite life was found for cyclic fatigue loaded CFRP-samples even under high inter fibre transverse and shear loading investigated up to 108 load cycles.
T2 - 19th World Conference on Non-Destructive Testing
CY - Munich, Germany
DA - 13.06.2016
KW - CFRP
KW - NDT
KW - Fatigue
KW - Damage evolution
PY - 2016
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-375015
UR - https://www.ndt.net/?id=19360
SN - 978-3-940283-78-8
VL - 2016
SP - 1
EP - 9
PB - DGZFP
CY - Berlin
AN - OPUS4-37501
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel HE
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
KW - Myrcene
KW - Anionic polymerization
KW - MALDI TOF MS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649039
DO - https://doi.org/10.1002/pi.6772
SN - 0959-8103
SP - 1
EP - 8
PB - Wiley
AN - OPUS4-64903
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel H. E.
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - The kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations.
KW - MALDI-TOF MS
KW - Anionic polymerization
KW - β‐myrcene
KW - Kinetics
KW - Reaction order
KW - Activation energy
KW - Microstructure
KW - Quantum chemical calculations
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630900
DO - https://doi.org/10.1002/pi.6772
SN - 1097-0126
SP - 1
EP - 8
PB - Wiley
CY - New York, NY
AN - OPUS4-63090
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel HE
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
KW - Myrcene
KW - Anionic polymerization
KW - Reaction order
KW - Activation energy
KW - Microstructure
KW - Quantum chemical calculation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636840
DO - https://doi.org/10.1002/pi.6772
SN - 0959-8103
SP - 1
EP - 8
PB - Wiley
AN - OPUS4-63684
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -