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Eingeladener Vortrag
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Scanning force microscopy (SFM) has been used to assess the local mechanical properties of fibre-reinforced polymers. Using a sinusoidal displacement modulation (DM) and lock-in technique the method allows to characterize local viscoelastic properties with a high lateral resolution. The simultaneous measurement of the local electrical conductivity is proposed which facilitates the interpretation of the mechanical data. The investigation of cross-sections perpendicular to the axis of carbon fibres embedded in PPS delivers some information about the change in local stiffness within the interfacial region. As a first approach, assuming a single-exponential decrease in local stiffness along a radial line from fibre to polymer we find characteristic decay lengths which are distributed in a range between 20 and 80nm. Further, a modified DM-mode is proposed which is expected to provide a contrast enhancement of the signal which is related to local stiffness. This can be achieved by installing an additional feedback loop which keeps constant the amplitude of dynamic indentation (CDI-mode).
Liquid chromatography in combination with spectroscopic methods like matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) or nuclear magnetic resonance (NMR) spectroscopy is a powerful method to characterize silsesquioxanes and silsesquioxane mixtures. As new examples, the formation of silsesquioxyl-substituted silsesquioxanes [(n-octyl)7(SiO1.5)8]2O and [(n-octyl)7(SiO1.5)8O]2[(n-octyl)6(SiO1.5)8] as well as the cage rearrangement of octa-[(n-heptyl)silsesquioxane] to larger structur es [(n-heptyl)SiO1.5)]n up to n=28 are shown.
The physical properties as well as the thickness of the interphase between polymer and reinforcing phase are generally expected to show a strong influence on the macroscopic mechanical properties of composite materials. In this study the scanning force microscope (SFM) has been applied for detecting stiffness gradients near the interface between copper and epoxide. In displacement modulation mode the load exerted by the tip is modulated sinusoidally by vibrating the normal position of the cantilever or the sample. The corresponding amplitude of dynamic cantilever bending is related to local surface stiffness. Thus, using the SFM, the local mechanical properties of the surface under investigation can be probed. When scanning the tip across the reinforcement/polymer interface, the polymeric interphasial zone can be identified with the observed stiffness gradient. For a commercial epoxide based on diglycidyl ether of bisphenol A (DGEBA) cured with an amine-containing hardener, a stiffness gradient was detected that could be fitted by a Gaussian profile typical for diffusional processes. The width of the stiffness gradient was 280 nm. The observation is discussed in terms of interface-induced segregation processes between resin and hardener, as well as heat conduction mechanisms that can occur during the exothermic curing reaction. Both mechanisms are diffusional in nature and, via the local network structure, are expected to show some influence on the local stiffness of the cured epoxy. Copyright © 2000 John Wiley & Sons, Ltd.
Beyond measuring the topography of surfaces, scanning force microscopy (SFM) has proved to be valuable both for mapping of various materials properties and for modifying surfaces via lithography techniques. Thus, SFM has gained relevance as a surface analysis technique as well as a tool for nanoscale engineering purposes. Different kinds of tip-sample interactions are exploitable, e.g. mechanical, thermal and electrical ones. Owing to its versatility, SFM has found plenty of applications in polymer science. Among others, the examples reported on in this review article encompass issues related to commodity polymers, various polymer-based composites, polymer blends, or ferroelectric polymers. For instance, stiffness imaging is elucidated as a technique for detecting interphases occurring in composites with inorganic fillers. The described applications are mainly related to mechanical and electrical tip-sample interactions. The respective fundamentals are outlined as well as some aspects of the measurement of materials contrasts. The presented techniques of nano-scale modification are a dynamical sort of plowing lithography and electrical poling, both performed by means of SFM-probes.
Poly(methyl methacrylate) (PMMA) surfaces have been modified by dynamic plowing lithography. The resulting modified structures, presenting regions of different densities and stiffnesses, have been studied by forcedisplacement curves. The elasto-plastic response, the stiffness, and the adhesion of the modified samples have been characterized. Forcedisplacement curves are able to distinguish between unmodified PMMA and two different structures resulting from the lithography, i.e. compressed PMMA and low density PMMA. In particular, the low density regions are made up of cluster-like globular particles, whose elasto-plastic response and adhesion are measured and whose contribution to the total elasto-plastic response and to the adhesion has been studied in detail.
Mapping of local mechanical and thermal properties - The Scanning Force Microscope in Tribology
(2001)
The fracture toughness in the fiber-matrix composite by means of the single fiber pull-out test can be achievable, if it is possible to measure the compliance of partial debonded fiber, which necessitates a stable crack propagation and the determination of the corresponding crack length. A combination of high stiff test equipment and a simultaneous monitoring of the photo-elastic pattern of the embedded fibers with the help of polarization microscope enables to measure crack length and determination of Gc [Hampe, A and Marotzke, C. (1997). The Energy Release Rate of the Fiber/Polymer Matrix Interface: Measurement and Theoretical Analysis, J. Reinf. Plast. and Compo., 16: 341-352.]. This method is well-known for glass fiber-amorphous polymer composite. In this investigation, we tried to implement the same technique to C-fiber with amorphous and semi-crystalline polymer composites. The energy release rate (ERR) of the fiber-matrix interface was evaluated for the carbon fiber-reinforced in polycarbonate (PC) by interfacial crack propagation arising in the single fiber pullout test. Further, the crack propagation at the fiber-matrix interface with different matrix morphology was discussed with the use of photo-elastic pattern observed with the aid of polarization microscope.
Die in zunehmenden Maße Mitte der 80er Jahre einsetzende Substitution von metallischen Materialien z. B. durch hochleistungsfähige polymere Werkstoffe und Verbundwerkstoffe wurde u. a. von der DGM zum Anlass genommen, ihre zukünftigen Aufgaben neu zu definieren und gleichzeitig mit der Gründung des Fachausschusses "Gefüge und Eigenschaften von Polymerwerkstoffen" dieser neuen Entwicklung in der Materialkunde auf dem Gebiet der Kunststoffe und ihrer Anwendungen Rechnung zu tragen.
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.
An advanced equipment for single-fibre pull-out test designed to monitor the fracture process
(1995)
Pull-out of Single Fibres
(1994)
Viscoelastic properties of the interphase in fibre reinforced polymers - measurement and simulation
(1999)
It is highly desirable to improve attractive interactions between carbon fibers and unreactive thermoplastic matrices to the possible maximum. This could be achieved by a simple grafting process to create a covalently bonded interface or interlayer, which should result in cohesive interactions between the polymer-grafted fibers and the same matrix material, leading to a better adhesion strength in the obtained composite material. Here, we are describing the grafting of styrene onto unmodified and unsized carbon fibers via free-radical bulk polymerization in the presence of fibers. After grafting, the surface properties of the carbon fiber approach those of pure polystyrene which was proven by contact angle and zeta ({zeta}) potential measurements. As indicated by the water contact angle, the carbon fiber surface becomes more hydrophobic. Scanning electron microscopy (SEM) provides evidence of grafted polymer. This simple procedure results in a continuous polystyrene coating. The fiber diameter increases significantly after polymer grafting. The adhesion and fracture behavior between the original and polystyrene-grafted carbon fibers to a polystyrene (VESTYRON®) matrix was characterized using the single-fiber pull-out test. There is a considerable increase in the measurable adhesion, i.e., the interfacial shear strength IFSS, by almost 300% between the grafted fibers and polystyrene as compared to untreated original fibers. Two planes of interfacial failure could be distinguished; first in the fiber coating interface leading to lower interfacial shear strength and second in the PS-matrix-PS-coating interphase resulting in a higher interfacial shear strength. In addition to the improved adhesion, there are also clear differences in the pull-out behavior between the nongrafted and grafted fibers. After the initial debonding process corresponding to the maximal pull-out force is completed, the pull-out force is increasing again.
Composites of carbon fiber and cyanate ester matrix have been investigated. The research has been focused on the interfacial behaviour. The influence of carbon fiber surface treatments, sizing and oxidation, and also modification of thermoset matrix by the addition of a thermoplastic, has been analysed. In order to relate the interfacial behaviour with the characteristics of the components, a physico-chemical characterisation of the carbon fibers and of the cyanate ester resins has been carried out. Thereafter, the apparent interfacial shear strength, the interlaminar shear strength and the Mode II delamination fracture toughness, GIIC, have been measured by pull-out test, short beam-shear test, and end-notched flexure test, respectively. For fractographic analysis the surfaces of laminates fractured under Mode II deformation have also been examined by scanning electron microscopy.
Atmospheric-plasma fluorination was used to introduce fluorine functionalities onto the surface of carbon fibers without affecting their bulk properties. The interfacial adhesion between atmospheric-plasma-fluorinated carbon fibers and poly(vinylidene fluoride) (PVDF) was studied by means of direct wetting measurements and single fiber pullout tests. Measured contact angles of PVDF melt droplets on modified carbon fibers show that short exposure times of carbon fibers to atmospheric-plasma fluorination (corresponding to a degree of surface fluorination of F/C = 0.01 (1.1%)) leads to improved wettability of the fibers by PVDF melts. The apparent interfacial shear strength as a measure of practical adhesion, determined by the single-fiber pullout test, increases by 65% under optimal treatment conditions. The improved practical adhesion is not due to the formation of transcrystalline regions around the fibers or a change of the bulk matrix crystallinity or to an increased surface roughness; it seems to be due to the compatibilization of the interface caused of the atmospheric-plasma fluorination of the carbon fibers.
A simple method of creating defined PMMA and poly (MMA-co-Cz) electrocoatings on carbon fibres is described. The electrodeposition of poly methylmethacrylate (PMMA) onto unsized, unmodified carbon fibres was performed by simple constant current electrolyses of methylmethacrylate (MMA) monomer in dimethylformamide (DMF) solutions and the pure liquid monomer using sodium nitrate and lithium perchlorate as supporting electrolytes. The presence of polymeric coatings successfully attached to the carbon fibres was verified by scanning electron microscopy and photoelectron spectroscopy (XPS).
Performing the electrolysis in dilute MMA in DMF solutions ([MMA] < 5 M) results in the deposition of powder-like polymer on the carbon fibre electrodes. Increasing the MMA concentration in the DMF solution results in a homogeneous PMMA coating of the carbon fibres. The degree of grafting or coating increases with increasing MMA concentration, except when pure MMA is used without solvent.
The adhesive strength between the electrocoated carbon fibres and a PMMA matrix was determined using the single fibre pull-out test. It was found that the interfacial fracture behaviour of all carbon fibre/PMMA model composites is rather brittle. The adhesion strength between the unmodified carbon fibres and the PMMA matrix was equal to the cohesive strength of the polymer matrix itself. Nevertheless, the electrodeposition of thin and homogeneous PMMA coatings resulted in much improved adhesion strengths.
Two different approaches to investigate the local complex conductivity and the surface charge with Scanning Force Microscopy (SFM) techniques are presented. It is shown that the measurement of local electrical properties with SFM leads to interesting information about the composition of electrically heterogeneous surfaces
With an extended contact and non-contact mode scanning force microscope samples with different heterogeneous electrical properties can be characterized. The contact mode method allows the determination of local electric conductivities of heterogeneous systems at the sample surfaces. An interpretation of this behaviour can be obtained in combination with other SFM modes such as topography, friction and compliance used simultaneously. The non-contact mode SFM allows to get more information about the local surface charge of heterogeneous samples. In this paper two new SFM approaches will be discussed on examples of carbon-fibre reinforced, organic and ceramic materials
Applying a high-frequency lateral vibration between tip and sample in a scanning force microscope (SFM), a harmonically modulated lateral (friction) force image can be obtained using lock-in techniques. Harmonically modulated lateral force microscopy (HM-LFM) offers several advantages compared with standard lateral force microscopy (LFM). After a brief investigation of the scan velocity dependence of LFM and HM-LFM, two samples were investigated. First, the surface of a poly(acrylonitrile-co-styrene)/polybutadiene blend (ABS) was used to demonstrate the ability of the new technique to decrease the stick effects of the SFM tip. Second, an interface between two chemically very similar polymers was prepared by melting polypropylene (PP) and poly(propene-block-ethene) (PP-block-PE) films on each other. After cutting, the surface roughness of this sample was very high. It is shown that only HM-LFM clearly resolves the local micromechanical properties without artefacts.
The surface properties of original high strength and preoxidized high modulus carbon fibers were altered by electrocopolymerizing acryl amide and carbazole and therefore depositing a copolymer coating onto the fibers. Scanning electron microscopy and zeta-potential measurements confirmed the presence of a rough but dense and continuous electrocoating with a basic surface character. Therefore, lsquogoodrsquo adhesion behavior between the electrocoated carbon fibers and an epoxy resin matrix should be expected. The interfacial adhesion was measured using the single fiber pull-out and single fiber indentation test. It was shown that only lsquointermediatersquo adhesion was present between the carbon fibers and the electrocoating, but superior adhesion between the coating and epoxy resin exists. The single fiber model composites always failed at the fiber/electrocoating interface. However, as shown by using the indentation test, the interfacial adhesion between fibers and electrocoating can be significantly improved if preoxidized fibers are used as substrate for electropolymerization. A very high tensile strength for the electrocoating can be expected as derived from the single fiber pull-out tests.
In this study an attempt is made to investigate the influence of surface treatments such as oxidation and sizing on a high-strength carbon fibre in respect of interfacial adhesion in composite materials with a cyanate matrix. For analysing the fibre/resin interfacial adhesion the single-fibre pull-out technique has been used. The interfacial shear strengths obtained by this technique have been compared with results of interlaminar shear strength measurements corresponding to woven composite plates. In order to clarify the nature of this interfacial adhesion, both morphological (by atomic force microscopy, AFM) and chemical characterisation (by Fourier transform infrared, FTIR), have also been carried out.