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Organisationseinheit der BAM
Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation
(2017)
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.
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.
In Kooperation zwischen dem Institut für Kunststoffverarbeitung (IKV) und der Bundesanstalt für Materialforschung und -prüfung (BAM) wurde das mechanische Verhalten unter Druck- und Zugbelastung unterschiedlicher morphologischer Strukturen teilkristalliner Thermoplaste (PP und POM) untersucht. Im Ergebnis steigt der E-Modul sowohl der druck- wie auch zugbelasteten Prüfkörper aus spritzgegossenem PP und POM mit gröberem Gefüge an. Probekörper mit scherinduziertem Gefüge zeigen einen hohen Einfluss des Kristallisationsgrads auf den E-Modul.
Pull-out of Single Fibres
(1994)
Fatigue Behaviour of High-Performance Fibre-Reinforced Composites with a Thermoplastic Matrix
(1990)
An advanced equipment for single-fibre pull-out test designed to monitor the fracture process
(1995)
Viscoelastic properties of the interphase in fibre reinforced polymers - measurement and simulation
(1999)
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.
A mathematical model for the description of the overall crystallization of polymers has been developed which separates the pure geometric spreading of the semicrystalline superstructures from the increasing crystallinity inside these entities. The model uses the Avrami theory for the geometric part and a freely optional function for the increasing local crystallinity. The two functions are combined by a mathematical procedure called convolution. The free option of the local crystallinity function enables this model to permit calculation of this function, which is not accessible to direct measurement. Thus with given Avrami parameters and measured values of the time-dependent overall crystallinity, this function of the local crystallinity (secondary crystallization function) can be calculated. The model has been applied to test data produced by computer simulations.
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.
Investigations on the cold crystallization of pure and filled PETP by dielectric measurements
(1993)
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.
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 180380 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.
The interaction between direct fluorinated carbon fibres and various fluoropolymers (ethylene-chlorotrifluoroethylene, poly vinylidene fluoride, fluorinated ethylene propylene copolymer and tetrafluoroethylene-perfluoro alkoxy vinyl ether copolymer) was studied by means of direct wetting measurements between fibres and the polymer melts and single fibre pull-out tests. The results of both techniques allow the adhesion behaviour between the fibres and the matrices to be predicted. The results obtained show that a low degree of surface fluorination of carbon fibres leads to an improved wettability between the fibres and fluoropolymer melts and this is an indicator for an improved thermodynamic work of adhesion. The apparent interfacial shear strength as measure of practical adhesion, determined by the single fibre pull-out test, increases with increasing degree of surface fluorine content up to a maximum, which depends on the degree of fluorination of the matrix used. The improved interaction between the fibre and the matrix is due to an enhanced compatibility at the fibre/matrix interface.
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.