Improvement of the thermo-oxidative stability of biobased poly(butylene succinate) (PBS) using biogenic wine by-products as sustainable functional fillers. - In: Polymers, ISSN 2073-4360, Bd. 15 (2023), 11, 2533, S. 1-23
Biobased poly(butylene succinate) (PBS) represents one promising sustainable alternative to petroleum-based polymers. Its sensitivity to thermo-oxidative degradation is one reason for its limited application. In this research, two different varieties of wine grape pomaces (WPs) were investigated as fully biobased stabilizers. WPs were prepared via simultaneous drying and grinding to be used as bio-additives or functional fillers at higher filling rates. The by-products were characterized in terms of composition and relative moisture, in addition to particle size distribution analysis, TGA, and assays to determine the total phenolic content and the antioxidant activity. Biobased PBS was processed with a twin-screw compounder with WP contents up to 20 wt.-%. The thermal and mechanical properties of the compounds were investigated with DSC, TGA, and tensile tests using injection-molded specimens. The thermo-oxidative stability was determined using dynamic OIT and oxidative TGA measurements. While the characteristic thermal properties of the materials remained almost unchanged, the mechanical properties were altered within expected ranges. The analysis of the thermo-oxidative stability revealed WP as an efficient stabilizer for biobased PBS. This research shows that WP, as a low-cost and biobased stabilizer, improves the thermo-oxidative stability of biobased PBS while maintaining its key properties for processing and technical applications.
Comparison of the properties of biogenic wine by-products stabilized biocomposites compounded with a miniaturized single-screw extruder and a co-rotating twin-screw extruder. - In: Engineering for a changing world, (2023), 2.3.010, S. 1-13
Bioplastics research is hindered by high material prices and limited availability of biopolymers. For conventional compounding, even on lab-scale, large quantities of material are required. In this study, an alternative process for compounding biocomposites was evaluated to investigate the potential of wine-derived biogenic by-products as functional fillers. Formulations based on poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) and wine grape pomace (WP) with filler contents up to 10 wt.-% were prepared. The materials were processed with a modified miniaturized single-screw extruder (MSE) and compared to a lab-scale twin-screw extruder (TSE). Thermal and rheological properties of the materials were determined using GPC, MFR, DSC, TGA and OIT. The mixing quality of both extruders was evaluated by optical microscopy imaging. The results revealed that the MSE represents an efficient alternative for research purposes, but differences in the dominant degradation mechanisms during processing must be considered. Thermal analysis showed that WP successfully suppressed the thermo-oxidative degradation of PHBV.
Influence of the recycling process parameters on CFRTP waste properties. - In: Engineering for a changing world, (2023), 2.3.002, S. 1-12
Nowadays, the combination of continuous fibers and thermoplastic polymers as the matrix to continuous fiber-reinforced thermoplastics (CFRTP) is receiving increasing attention due to their potential advantages such as excellent weight-specific mechanical properties, short cycle times, storability, repeated meltability, good formability and the use of alternative joining processes enabling automated large volume manufacturing processes which allow various applications in different industries including transportation, construction among others. As the production rate of these materials increases, the amount of waste for disposal increases, for which recycling strategies need to be established to ensure the sustainability of CFRTP. Hence, these recycling strategies must be developed and evaluated economically and ecologically to close the loop and achieve a circular economy to process recycled fiber-reinforced pellets from CFRTP waste to valuable products e.g., by injection molding. This study presents a mechanical recycling approach from CFRTP waste to injection molded test specimens and evaluates the impact of the individual recycling steps along the recycling chain on the fiber length as the fiber length is detrimental to the resulting mechanical properties. First, the CFRTP waste processability is investigated and conditions for size reduction by cutting and shredding into feedstock for extrusion are defined. Second, fiber-reinforced pellets are produced by twin-screw extrusion. The fiber volume content and the process parameters screw speed and temperature during compounding are varied and the influence of these parameters on the fiber length is determined. Third, the extruded pellets are further processed by injection molding. Here, the influence of screw speed, back pressure, and processing temperature as well as the initial fiber length in the extruded granules on the resulting properties is investigated. Quantitative correlations between material properties and processing parameters are presented and suggestions for gentle processing during recycling are given.
Influence of the processing on the properties of continuous fiber reinforced thermoplastic sheets prepared by extrusion. - In: AIP conference proceedings, ISSN 1551-7616, Bd. 2884 (2023), 1, 050005, S. 050005-1-050005-14
Continuous fiber reinforced thermoplastics (CFRT) are composite materials consisting of continuous fibers and a thermoplastic matrix and offer outstanding mechanical properties, low densities, short cycle times and recyclability. CFRT can be classified into unidirectional tapes and sheets utilizing various semi-finished textiles as reinforcement. CFRT sheets are of interest for area measured products or multiaxial loads. Various discontinuous and semi-continuous methods to prepare CFRP sheets are described in the literature. All these methods either feature high cycle times or high investment costs and require double melting of the polymer, e.g., first to produce a polymer film and second to produce the CFRT sheet. An energy efficient alternative to produce CFRT sheets is extrusion, which allows to spare one melting step. A twin-screw extruder melts the polymer, which is then conveyed by a melt pump to the film extrusion dies and applied to both sides of the semi-finished textile, which is wetted and consolidated using a calendar. Due to the high melt viscosity and the line load at the calendar the major challenge is to achieve full void-free impregnation of the semi-finished textile. The mechanical properties of a CFRT sheet are determined by fiber and void volume content. Hence, the influence of the processing conditions on the fiber and void volume content as well as the mechanical properties were examined applying a parametric study of the die temperature, the haul-off speed, and the gap between the calendar rolls. The properties of the extruded CFRT sheets were compared to compression molded sheets. The fiber volume content was directly adjusted by the haul-off speed and the extruder throughput. An increasing die temperature lowers the melt viscosity and results in an increased fiber volume content. Scanning electron microscopy shows complete macro impregnation between the fiber bundles but not completely wetted individual filaments within fiber bundles.
Investigation of the fiber length and the mechanical properties of waste recycled from continuous glass fiber-reinforced polypropylene. - In: Recycling, ISSN 2313-4321, Bd. 8 (2023), 6, 82, S. 1-20
This paper explores the mechanical recycling of continuous fiber-reinforced thermoplastics (CFRTPs) waste into injection molded products, focusing on the influence of recycling parameters on fiber length and mechanical properties. CFRTPs are gaining attention for their promising attributes, including weight-specific mechanical properties, short cycle times, storability, and recyclability, making them suitable for diverse applications. However, as CFRTP production rates rise, recycling strategies become crucial for sustainability. This study investigates the processability of CFRTP waste, defines size reduction conditions, and evaluates the impact of various compounding parameters such as temperature, screw speed, and fiber volume content during extrusion. The research findings indicate that higher screw speeds lead to fiber length reduction, whereas elevated temperatures result in longer fibers. Increased fiber volume intensifies interactions, resulting in shorter lengths. Additionally, the study examines the influence of injection molding parameters such as back pressure, screw speed, and initial fiber length on the resulting fiber length and mechanical properties of injection molded specimens, emphasizing the need for precise parameter control to optimize performance in recycled CFRTPs. Key findings are that increasing the initial fiber length from 260 μm to 455 μm results in an average fiber length after injection molding of 225 μm and 341 μm, respectively. This implies that longer initial fibers are more prone to breakage. Regarding the mechanical properties, increasing back pressure from 20 bar to 60 bar results in a reduction in Young’s modulus of approximately 40 MPa. Higher screw speed also reduces modulus by approximately 70 MPa due to intensified fiber-screw interactions. However, back pressure and screw speed have neutral effects on the tensile strength and the elongation at break.
Investigation on the influence of process parameters on the mechanical properties of extruded bio-based and biodegradable continuous fiber-reinforced thermoplastic sheets. - In: Polymers, ISSN 2073-4360, Bd. 15 (2023), 18, 3830, S. 1-14
The use of bio-based and biodegradable matrix materials in fiber-reinforced polymers (FRPs) is an approach to reduce the consumption of fossil resources and the amount of polymer waste. This study aims to assess the influence of the process parameters on the resulting mechanical properties of extruded bio-based and biodegradable continuous fiber-reinforced thermoplastics (CFRTPs) in the form of sheets. Therefore, the impregnation temperature during the production of PLA/flax fiber composites is varied between 220 ˚C and 280 ˚C, and the consolidation pressure, between 50 bar and 90 bar. A design of experiments approach is used. Fiber contents of 28.8% to 34.8% and void contents of 6.8% to 15.5% are determined for the composites by optical measurements. To assess the mechanical properties, tensile tests are performed. Using the evaluation software Minitab, a strong negative influence of the consolidation pressure on the tensile modulus and the tensile strength is observed. Increasing the pressure from 50 bar to 90 bar results in a reduction in the tensile modulus of 50.7% and a reduction in the tensile strength of 54.8%, respectively. It is assumed that this is due to fibers being damaged by the external force exerted onto the materials during the consolidation process in the calender. The influence of the impregnation temperature on the mechanical properties cannot be verified.
Extrusion as an energy-efficient manufacturing process for thermoplastic organosheets. - In: Sheet Metal 2023, (2023), 43, S. 345-352
Organosheets combine the advantages of reinforcement fibers and thermoplastic polymers. By pairing these two materials, composites with outstanding mechanical properties and low densities can be produced. These semi-finished products can be further processed into complex and functionalized components by thermoforming or injection molding. There are a number of different manufacturing processes for continuous fiber reinforced thermoplastics (CFRT), however, most of them require long production times and recurrent melting of the polymer resulting in high energy and manufacturing costs. This study presents a novel extrusion process, that enables a continuous production of reinforced thermoplastic sheets with only one melting step. Due to the high energy efficiency and wide range of processible materials, this process shows a high potential for an economical production of CFRT. To investigate the extrusion process in more detail, the influence of the processing and the flow behavior of the polymer on the impregnation quality and the mechanical properties of the composites were studied. The results showed increasing fiber volume contents with lower polymer viscosities. Furthermore, higher die temperatures and pressures resulted in higher fiber volume contents and thus in higher mechanical properties. The experiments also revealed that a complete impregnation can currently not be achieved without an additional small double belt press due to the line load of the calender, the high viscosity of the melt and the short impregnation time.
Aushärteüberwachung von Klebstoffen durch luftultraschallinduzierte und geführte Wellen. - Ilmenau, 2023. - 1 Band (verschiedene Seitenzählung)
Technische Universität Ilmenau, Dissertation 2023
Klebstoffsysteme finden zunehmend Anwendung in den verschiedensten Industriesegmenten und substituieren oder ergänzen oftmals konventionell angewandte Verbindungsverfahren wie das Schweißen und Nieten. Gleichzeitig bestehen zahlreiche, genormte Prüfverfahren, um die Aushärtung von Klebstoffen zu charakterisieren. Diese beschränken sich auf die Untersuchung von Probenkleinstmengen im Labor auf Basis von z. B. rheologischen und kalorimetrischen Verfahren. Die dabei erzielten Ergebnisse können aufgrund ungleicher Rahmenbedingungen nicht direkt auf die Gegebenheiten in einem industriellen Produktionsumfeld übertragen werden. Die zu Grunde liegenden Ursachen sind vielfältig. In den meisten Fällen ist etwa ein direkter Messzugang zum Klebstoff bedingt durch die vorhandenen Fügepartner nicht gegeben und Umgebungsbedingungen wie Temperatur und Luftfeuchtigkeit weichen gleichermaßen wie die betrachtete Menge an Klebstoff von den genannten Laborprüfungen ab. Im industriellen Umfeld kaum etabliert, aber im Stand der Technik und Wissenschaft beschrieben, sind hingegen zerstörungsfreie Methoden zur Prüfung von applizierten Klebstoffen. Zu diesen gehören beispielsweise die Terahertz-, berührende Ultraschall- und Kernspinresonanztechnik. Wesentliche Nachteile wie eine nicht berührungslose Arbeitsweise, die die Untersuchung klebriger Oberflächen behindert, eine geringe Eindringtiefe, aus der Informationen gewonnen werden können, einschränkende Anforderungen an die elektrische Leitfähigkeit der untersuchbaren Materialsysteme sowie letztlich hohe Systemkosten sind Gründe für eine geringe Anwenderakzeptanz. Diesen Verfahren steht ein neuer Prüfansatz auf Basis mittels Luftultraschall induzierter, geführter Wellen entgegen. Dieser erlaubt eine verhältnismäßig kostengünstige, wegintegrale Aushärteüberwachung von Klebstoffen über lange Strecken hinweg, ohne einen direkten Zugang zum Klebstoff zu erfordern. Die vorliegende Dissertation erforscht das Messprinzip und die damit verbundenen Vor- und Nachteile, demonstriert unmittelbar die Verfahrenseignung durch Betrachtung unterschiedlicher Klebstoffsysteme, untersucht den Einfluss wesentlicher Prüfrahmenbedingungen, zeigt Anwendungsmöglichkeiten sowie erkannte Limitationen auf und bietet anschließend Umgehungsstrategien zur Überwindung der genannten Limitationen z. B. durch Anwendung von sogenannten Pulskompressionsmethoden an.
Application of capacitive sensors and controlled injection pressure to minimize void formation in resin transfer molding. - In: Polymer composites, ISSN 1548-0569, Bd. 44 (2023), 3, S. 1658-1671
Void formation as a result of irregular resin flow at the flow front is discussed and a practical method for reducing void formation during resin transfer molding (RTM) is introduced. In this study, a sensor system is developed for in situ measurement of resin velocity inside a closed cavity. Assisted by the acquired data, a resin injection system is augmented to automatically adjust the injection pressure and achieve a uniform flow front velocity. It is proven, that the developed system is suited to monitor the resin flow front and is able to sufficiently control flow velocity of a linear flow front. Test specimen produced by this method show significantly reduced void contents in comparison to a common resin transfer molding process.
Optical detection of void formation mechanisms during impregnation of composites by UV-reactive resin systems. - In: Journal of composites science, ISSN 2504-477X, Bd. 6 (2022), 11, 351, S. 1-15
During the impregnation of reinforcement fabrics in liquid composite molding processes, the flow within fiber bundles and the channels between the fiber bundles usually advances at different velocities. This so-called “dual-scale flow” results in void formation inside the composite material and has a negative effect on its mechanical properties. Semi-empirical models can be applied to calculate the extent of the dual-scale flow. In this study, a methodology is presented that stops the impregnation of reinforcement fabrics at different filling levels by using a photo-reactive resin system. By means of optical evaluation, the theoretical calculation models of the dual-scale flow are validated metrologically. The results show increasingly distinct dual-scale flow effects with increasing pressure gradients. The methodology enables the measurability of microscopic differences in flow front progression to validate renowned theoretical models and compare simulations to measurements of applied injection processes.