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See detailFrom the Dynamically Nanostructured Liquid to the Glassy State: A Phenomenological Approach
Krüger, Jan-Kristian UL; Petersson, J.; Baller, Jörg UL et al

E-print/Working paper (2008)

Based on experimental evidences we present a phenomenological description of the thermal glass transition as a dynamical phase transition. Different susceptibilities calculated on the basis of this ... [more ▼]

Based on experimental evidences we present a phenomenological description of the thermal glass transition as a dynamical phase transition. Different susceptibilities calculated on the basis of this description are in good qualitative agreement with experimental data. As an essential feature this novel view of the glass transition reflects the kinetic as well as the transition aspect of the thermal glass transition. [less ▲]

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See detailAcoustic Profilometry Of Interphases In An Epoxy Due To Segregation and Diffusion Using Brillouin Microscopy.
Müller, Ulrich UL; Bactavatchalou, R.; Baller, Jörg UL et al

in New Journal of Physics (2008), 10(2), 023-031

Reactive network forming polymer systems like epoxies are of huge technological interest because of their adhesive properties based on specific interactions with a large variety of materials. These ... [more ▼]

Reactive network forming polymer systems like epoxies are of huge technological interest because of their adhesive properties based on specific interactions with a large variety of materials. These specific interactions alter the morphology of the epoxy within areas determined by the correlation length of these interactions. The changed morphology leads to interphases with altered (mechanical) properties. Besides these surface-induced interphases, bulk interphases do occur due to segregation, crystallization, diffusion, etc. A new experimental technique to characterize such mechanical interphases is μ-Brillouin spectroscopy (μ-BS). With μ-BS, we studied interphases and their formation in epoxies due to segregation of the constituent components and due to selective diffusion of one component. In the latter case, we will demonstrate the influence of changing the boundary conditions of the diffusion process on the shape of the interphase. [less ▲]

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See detailOrganization versus frustration: low temperature transitions in a gelatine-based gel
Philipp, Martine UL; Müller, Ulrich UL; Sanctuary, Roland UL et al

in New Journal of Physics (2008), 10

A commercial physical gel composed of gelatine, water and glycerol shows a sol–gel transition which has been resolved by optical rotation measurements by step-wise heating the gel. This transition is not ... [more ▼]

A commercial physical gel composed of gelatine, water and glycerol shows a sol–gel transition which has been resolved by optical rotation measurements by step-wise heating the gel. This transition is not observable in the longitudinal acoustic mode measured at hypersonic frequencies with Brillouin spectroscopy. Depending on the thermal treatment of the investigated material during the sol–gel transition and within the gel state, Brillouin spectroscopy reflects tremendously different hypersonic dynamics. These distinct dynamics are responsible for the formation of different glassy states at low temperatures including that of a glass-ceramic. The large variety of super-cooled and glassy states is attributed to distinct distributions of the gel's constituents within the samples. Surprisingly, the same gel state can be produced either by annealing the gel over months or by the non-equilibrium effect of thermo-diffusion (Soret effect) in the course of some minutes. [less ▲]

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See detailEffect of mixing sequence on the curing of amine-hardened epoxy/alumina nanocomposites as assessed by optical refractometry
Philipp, Martine UL; Gervais, Pierre-Colin; Sanctuary, Roland UL et al

in eXPRESS Polymer Letters (2008), 2(8), 546-552

High performance refractometry has been proven to be a useful tool to elucidate the isothermal curing process of nanocomposites. As a model system an amine-hardening epoxy filled with non-surface-treated ... [more ▼]

High performance refractometry has been proven to be a useful tool to elucidate the isothermal curing process of nanocomposites. As a model system an amine-hardening epoxy filled with non-surface-treated alumina nanoparticles was selected. The tremendous resolution of this experimental technique is used to study morphological changes within nanocomposites via the refractive index. It is shown that these morphological changes are not simply due to the curing process but also depend on the sequence of mixing the nanoparticles either first into the resin or first into the hardener. Independent of the resin/hardener composition, the type of the mixing sequence discriminates systematically between two distinct refractive index curves produced by the curing process. The difference between the two refractive index curves increases monotonically with curing time, which underlines the importance of the initial molecular environment of the nanoparticles. [less ▲]

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See detailAbout the nature of the structural glass transtion: an experimental approach
Krüger, Jan-Kristian UL; Alnot, Patrick; Baller, Jörg UL et al

in Henkel, M.; Pleimling, M.; Sanctuary, Roland (Eds.) Aging of the Glass Transition (2007)

The nature of the glassy state and of the glass transition of structural glasses is still a matter of debate. This debate stems predominantly from the kinetic features of the thermal glass transition ... [more ▼]

The nature of the glassy state and of the glass transition of structural glasses is still a matter of debate. This debate stems predominantly from the kinetic features of the thermal glass transition. However the glass transition has at least two faces: the kinetic one which becomes apparent in the regime of low relaxation frequencies and a static one observed in static or frequency-clamped linear and non-linear susceptibilities. New results concerning the so-called ?-relaxation process show that the historical view of an unavoidable cross-over of this relaxation time with the experimental time scale is probably wrong and support instead the existence of an intrinsic glass transition. In order to prove this, three different experimental strategies have been applied: studying the glass transition at extremely long time scales, the investigation of properties which are not sensitive to the kinetics of the glass transition and studying glass transitions which do not depend at all on a forced external time scale. [less ▲]

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See detailTemperature modulated Differential Scanning Calorimetry: The Dynamic Aspect of the Specific Heat Capacity and its Relation to Entropy Production
Philipp, Martine UL; Sanctuary, Roland UL; Baller, Jörg UL et al

in Beiträge zur Experimentalphysik, Didaktik und computergestützten Physik (2007)

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See detailComplex specific heat capacity of two nanocomposite systems
Sanctuary, Roland UL; Baller, Jörg UL; Krüger, Jan-Kristian UL et al

in Thermochimica Acta (2006), 445(2), 111-115

Thermal investigations on two selected model-nanocomposites have been made. They differ with regard to the type of the anorganic nanoparticles that have been filled into an organic oligomer matrix. The ... [more ▼]

Thermal investigations on two selected model-nanocomposites have been made. They differ with regard to the type of the anorganic nanoparticles that have been filled into an organic oligomer matrix. The properties of nanocomposites may vary between those of a simple mixture of independent components and those of a system, where specific interfacial interactions between the constituting parts lead to ‘new’ properties. Depending on the type of the nanoparticles filled into the matrix, the resulting properties might be closer to one or to the other extreme. We used temperature modulated differential scanning calorimetry (TMDSC) to investigate a matrix of the oligomer diglycidyl ether of bisphenol A (DGEBA) filled either with SiO2- or Al2O3-nanoparticles. The dependence of the complex specific heat capacity () on the concentration of nanoparticles shows a clear difference between the two systems as far as the glass transition of the oligomer is concerned. The SiO2 composite seems to behave more like a simple mixture, whereas the Al2O3 composite shows ‘new’ properties. [less ▲]

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See detailThe generalized Cauchy relation: a probe for local structure in materials with isotropic symmetry.
Bactavatchalou, R.; Alnot, Patrick; Baller, Jörg UL et al

in Journal of Physics. Conference Series (2006), 40

The elastic properties of the isotropic state of condensed matter are given by the elastic constants ell and c44. In the liquid state the static shear stiffness c44 vanishes whereas at sufficient high ... [more ▼]

The elastic properties of the isotropic state of condensed matter are given by the elastic constants ell and c44. In the liquid state the static shear stiffness c44 vanishes whereas at sufficient high probe frequencies a dynamic shear stiffness may appear. In that latter case the question about the existence of a Cauchy relation appears. It will be shown that a pure Cauchy relation can appear only under special conditions which are rarely fulfilled. For all investigated materials, including ceramics, liquids and glasses, a linear relation between ell and c44 called generalized Cauchy relation is observed, which, surprisingly, follows a linear transformation. [less ▲]

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See detailComment on "thermal glass transition beyond the vogel-fulcher-tammann behavior for glass forming diglycidylether of bisphenol A".
Rivera, A.; Blochowicz, T.; Porokhonskyy, V. et al

in Physical Review Letters (2005), 94(12), 129603-129604

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See detailMechanical Interphases in Epoxies as seen by Nondestructive High-Performance Brillouin Microscopy
Krüger, Jan-Kristian UL; Müller, Ulrich UL; Bactavatchalou, Ravindrakumar et al

in Adhesion - Current Research and Application (2005)

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See detailA Reply to the Comment by A. Rivera et al.
Krüger, Jan-Kristian UL; Britz, Thomas; Baller, Jörg UL et al

in Physical Review Letters (2005), 94

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See detailDifferent glassy states, as indicated by a violation of the generalized Cauchy relation.
Krüger, Jan-Kristian UL; Britz, Th; le Coutre, A. et al

in New Journal of Physics (2003), 5(80), 1-11

Using Brillouin spectroscopy as a probe for high-frequency clamped acoustic properties, a shear modulus can be measured in addition to the longitudinal modulus already well above the thermal glass ... [more ▼]

Using Brillouin spectroscopy as a probe for high-frequency clamped acoustic properties, a shear modulus can be measured in addition to the longitudinal modulus already well above the thermal glass transition. On slow cooling of the liquid through the thermal glass transition temperature Tg, both moduli show a kink-like behaviour and the function follows a generalized Cauchy relation (gCR) defined by the linear relation , which completely hides the glass transition. In this work we show experimentally that on fast cooling this linear transformation becomes violated within the glassy state, but that thermal ageing drives the elastic coefficients towards the gCR, i.e. towards a unique glassy state. [less ▲]

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See detailCauchy-like relation between elastic constants in amorphous materials.
Krüger, Jan-Kristian UL; Baller, Jörg UL; Britz, Th et al

in Physical Review. B, Condensed Matter and Materials Physics (2002), 66(1), 012206-012210

It is well known that in addition to the longitudinal modulus, viscoelastic liquids show a shear stiffness at sufficiently high probe frequencies due to structural relaxations. For probe frequencies that ... [more ▼]

It is well known that in addition to the longitudinal modulus, viscoelastic liquids show a shear stiffness at sufficiently high probe frequencies due to structural relaxations. For probe frequencies that are large compared to the structural relaxation frequency, the measured elastic longitudinal and shear moduli become so-called clamped properties (c11∞ and c44∞, respectively). During freezing or polymerization of amorphous liquids, these clamped moduli behave in a strongly nonlinear fashion as a function of temperature or polymerization time. Based on Brillouin spectroscopy data we will show that there exists a linear relation between c11∞ and c44∞ over a large temperature or polymerization time range. Surprisingly, the parameters of this linear relation between the elastic moduli vary only little for different materials. Implications for the nonlinear elastic behavior at the glass transition will be discussed on the basis of mode Grüneisen parameters. [less ▲]

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See detailThermal Glass Transition Beyond the Vogel-Fulcher-Tammann Behavior for Glass Forming Diglycidylether of Bisphenol A
Krüger, Jan-Kristian UL; Britz, Th; Baller, Jörg UL et al

in Physical Review Letters (2002), 89

For the low molecular weight fragile liquid diglycidyl ether of bisphenol A we report, based on Brillouin and dielectric spectroscopy, on a thermal glass transition where the relaxation time of the α ... [more ▼]

For the low molecular weight fragile liquid diglycidyl ether of bisphenol A we report, based on Brillouin and dielectric spectroscopy, on a thermal glass transition where the relaxation time of the α process does not go to infinity. Instead, the structural α relaxation disappears spontaneously at the transition point. That discontinuity in relaxation time coincides with a kink in the longitudinal hypersonic velocity and determines unambiguously the transition from the liquid to the glassy state. [less ▲]

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See detailFreezing of Nano-Scaled Fractal Molecules: Dendrimers
Krüger, Jan-Kristian UL; Veith, M.; Elsässer, R. et al

in Ferroelectrics (2001), 259(1-4), 27-36

Within this paper we present mono-disperse dendrimers as a new class of ideal canonical glass formers where the frustration mechanism originates from the self similar intramolecular order. Because of ... [more ▼]

Within this paper we present mono-disperse dendrimers as a new class of ideal canonical glass formers where the frustration mechanism originates from the self similar intramolecular order. Because of their fractal intramolecular structure these dendrimers are hardly able to build up a three dimensional translation symmetry necessary to form the crystalline state. Instead they show an unconventional dynamic and static freezing behavior at rather low temperatures. Based on temperature modulated differential scanning calorimetry (TMDSC) and Brillouin spectroscopy (BS) we give further evidences for the existence of an ideal primary glass transition with a thermal glass transition temperature which increases with the generation index of the fractal molecule. However, the primary glass transitions of higher generations do not completely erase the memory of the fractal intramolecular mobility but allow the survival of dynamic processes significant for the freezing of the constituting molecular unit. [less ▲]

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See detailSurface Induced Order in Organic and Anorganic Materials on Nano-Structured Poly-tetrafluoroethylene.
Krüger, Jan-Kristian UL; Fischer, C.; Baller, Jörg UL et al

in Frontiers in Science and Technology, Advanced Physics Studies Press (2000),7th FSRC FERROELECTRICS-2000 (2000)

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See detailElastic properties of single-crystalline and consolidated nano-structured yttrium oxide at room temperature.
Baller, Jörg UL; Krüger, Jan-Kristian UL; Birringer, R. et al

in Journal of Physics : Condensed Matter (2000), 12(25), 5403-5409

High resolution Brillouin spectroscopy was used to characterize the elastic stiffness properties of consolidated nano-crystalline yttrium oxide as well as of the related single-crystalline state. Defect ... [more ▼]

High resolution Brillouin spectroscopy was used to characterize the elastic stiffness properties of consolidated nano-crystalline yttrium oxide as well as of the related single-crystalline state. Defect enriched grain boundaries are discussed as sources for the extremely soft elastic properties of the nano-crystalline state. [less ▲]

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See detailOn the Influence of Nano-Scaling on the Glass Transition of Molecular Liquids
Krüger, Jan-Kristian UL; Holtwick, R.; le Coutre, Andre et al

in Nanostructured Materials (1999), 12(1), 519-522

The nature of the glass transition is still a matter of debate. We used temperature modulated DSC (TMDSC) and Brillouin spectroscopy ( BS ) to investigate the freezing behaviour of canonical glasses ... [more ▼]

The nature of the glass transition is still a matter of debate. We used temperature modulated DSC (TMDSC) and Brillouin spectroscopy ( BS ) to investigate the freezing behaviour of canonical glasses ( salol and di-n-butyl-phtalate (DBP)) confined to controlled pore glasses (CPG) with pore diameters between 2.5 and 20 nm. The temperature behaviour of the heat capacity of the composite system deviates from the bulk fluid properties and we interpret the remaining kink-like anomaly at Tg as a static glass transition. In smaller pores Tg is only slightly shifted to lower temperatures. This operative Tg is in good agreement with sound velocity data showing a sharp kink at Tg. The working hypothesis of the existence of a static glass transition is supported by the fact that the -relaxation process disappears with decreasing pore diameter. [less ▲]

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See detailExistence of An Intrinsic Glass Transition In A Silicon Rubber: Hypersonic Versus Calorimetric Properties
Krüger, Jan-Kristian UL; Mesquida, P.; Baller, Jörg UL

in Physical Review. B, Condensed Matter and Materials Physics (1999), 60(14), 10037-10041

Time-domain temperature-modulated differential scanning calorimetry and high-performance Brillouin spectroscopy have been used as experimental techniques in order to investigate the effect of the thermal ... [more ▼]

Time-domain temperature-modulated differential scanning calorimetry and high-performance Brillouin spectroscopy have been used as experimental techniques in order to investigate the effect of the thermal glass transition on the specific heat as well as on the acoustic properties, quantities which are intimately related by thermodynamics, but measured at completely different frequencies. Using a siloxane as a model substance, we demonstrate the efficiency of hypersonic relaxations until thermal freezing of the material. Introducing the optoacoustic dispersion function as a sensitive measure for structural relaxations, we show that the high-frequency α relaxations are truncated by the thermal glass transition instead of dying out at much higher temperatures. Moreover, the extrapolated static compliance of the rubbery state goes to zero close to but below the thermal glass transition temperature Tg, indicating the existence of an acoustic instability which is reminiscent of the so-called Kauzmann paradox. [less ▲]

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