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Item Design of Experiment to Determine the Effect of the Geometric Variables on Tensile Properties of Carbon Fiber Reinforced Polymer Composites(MDPI AG, 2023-05) Janicki, Joseph C.; Egloff, Matthew C.; Bajwa, Dilpreet S.; Amendola, Roberta; Ryan, Cecily A.; Cairns, Douglas S.Carbon fiber reinforced polymers (CFRPs) are increasingly used in the aerospace industry because of their robust mechanical properties and strength to weight ratio. A significant drawback of CFRPs is their resistance to formability when drawing continuous CFRPs into complex shapes as it tends to bridge, resulting in various defects in the final product. However, CFRP made from Stretch Broken Carbon Fiber (SBCF) aims to solve this issue by demonstrating superior formability compared to conventional continuous CFRPs. To study and validate the performance of SBCF, a statistical design of the experiment was conducted using three different types of CFRPs in tow/tape form. Hexcel (Stamford, CT, USA) IM7-G continuous carbon fiber impregnated with Huntsman (The Woodlands, TX, USA) RDM 2019-053 resin system, Hexcel SBCF impregnated with RDM2019-053 resin, and Montana State University manufactured SBCF impregnated with Huntsman RDM 2019-053 resin were tested in a multitude of forming trials and the data were analyzed using a statistical model to evaluate the forming behavior of each fiber type. The results show that for continuous fiber CFRP tows forming, Fmax and Δmax do not show statistical significance based on temperature fluctuations; however, in SBCF CFRP tows forming, Fmax and Δmax is dominated by the temperature and geometry has a low statistical influence on the Fmax. The lower dependence on tool geometry at higher temperatures indicates possibly superior formability of MSU SBCF. Overall findings from this research help define practical testing methods to compare different CFRPs and provide a repeatable approach to creating a statistical model for measuring results from the formability trials.Item Formability Characterization of Fiber Reinforced Polymer Composites Using a Novel Test Method(ASTM International, 2021-10) Janicki, Joseph C.; Egloff, Matthew C.; Amendola, Roberta; Ryan, Cecily A.; Bajwa, Dilpreet S.; Dilpreet S., Alexey; Cairns, Douglas S.Fiber reinforced polymer composites are often used as a replacement for metal alloys because of the superior strength to weight ratio. However, a major drawback of these materials is the lack of formability caused by the low strain to failure ratio that does not allow the material to follow tooling contours into deep drawn shapes or tight radii. Composite materials have a multiscale hierarchical structure where micro and meso scale effects (fiber and tow scales) contribute to the macro structural response (laminate scale). In particular, during forming, different deformation occurs simultaneously at every scale. Currently, the amount of quantifiable and comparable forming data for both continuous and discontinuous fiber reinforced polymer composites, including a multi-scale understanding of the deformation response, is limited because of the lack of a testing system. This article proposes a novel test method and an apparatus called “the forming fixture” for testing the tow formability of fiber reinforced polymer composites by determining the required load to form an uncured resin impregnated fiber tow sample into a stretch drawn profile. Test results from forming of Hexcel (Stamford, CT) IM7-G continuous carbon fiber impregnated with Huntsman (The Woodlands, TX) RDM 2019-053 resin system, in the temperature range of 21°C–121°C, are discussed to demonstrate the use of the proposed apparatus including representative data. Results showed consistency and repeatability, validating the reliability of the novel method. The test aided in defining the forming behavior of the material in real time both visually (e.g. sample failure location) and as forming load versus displacement curves. A novel forming metrics, relating the maximum drawing depth with no failure and the maximum forming load, is defined to compare and select different fiber and resin formulations. Widespread adoption of the forming fixture will reduce reliance on a “trial and error” approach during the the forming process.Item Physical and chemical mechanisms that influence the electrical conductivity of lignin-derived biochar(2021-10) Kane, Seth; Ulrich, Rachel; Harrington, Abigail; Stadie, Nicholas P.; Ryan, Cecily A.Lignin-derived biochar is a promising, sustainable alternative to petroleum-based carbon powders (e.g., carbon black) for polymer composite and energy storage applications. Prior studies of these biochars demonstrate that high electrical conductivity and good capacitive behavior are achievable. However, these studies also show high variability in electrical conductivity between biochars (– S/cm). The underlying mechanisms that lead to desirable electrical properties in these lignin-derived biochars are poorly understood. In this work, we examine the causes of the variation in conductivity of lignin-derived biochar to optimize the electrical conductivity of lignin-derived biochars. To this end, we produced biochar from three different lignins, a whole biomass source (wheat stem), and cellulose at two pyrolysis temperatures (900 °C, 1100 °C). These biochars have a similar range of conductivities (0.002 to 18.51 S/cm) to what has been reported in the literature. Results from examining the relationship between chemical and physical biochar properties and electrical conductivity indicate that decreases in oxygen content and changes in particle size are associated with increases in electrical conductivity. Importantly, high variation in electrical conductivity is seen between biochars produced from lignins isolated with similar processes, demonstrating the importance of the lignin’s properties on biochar electrical conductivity. These findings indicate how lignin composition and processing may be further selected and optimized to target specific applications of lignin-derived biochars.Item Biomineralization of Plastic Waste to Improve the Strength of Plastic-Reinforced Cement Mortar(2021-04) Kane, Seth; Thane, Abby; Espinal, Michael; Lunday, Kendra; Armagan, Hakan; Phillips, Adrienne J.; Heveran, Chelsea M.; Ryan, Cecily A.The development of methods to reuse large volumes of plastic waste is essential to curb the environmental impact of plastic pollution. Plastic-reinforced cementitious materials (PRCs), such as plastic-reinforced mortar (PRM), may be potential avenues to productively use large quantities of low-value plastic waste. However, poor bonding between the plastic and cement matrix reduces the strength of PRCs, limiting its viable applications. In this study, calcium carbonate biomineralization techniques were applied to coat plastic waste and improved the compressive strength of PRM. Two biomineralization treatments were examined: enzymatically induced calcium carbonate precipitation (EICP) and microbially induced calcium carbonate precipitation (MICP). MICP treatment of polyethylene terephthalate (PET) resulted in PRMs with compressive strengths similar to that of plastic-free mortar and higher than the compressive strengths of PRMs with untreated or EICP-treated PET. Based on the results of this study, MICP was used to treat hard-to-recycle types 3–7 plastic waste. No plastics investigated in this study inhibited the MICP process. PRM samples with 5% MICP-treated polyvinyl chloride (PVC) and mixed type 3–7 plastic had compressive strengths similar to plastic-free mortar. These results indicate that MICP treatment can improve PRM strength and that MICP-treated PRM shows promise as a method to reuse plastic waste.Item Incorporation of Carbon Nanofillers Tunes Mechanical and Electrical Percolation in PHBV:PLA Blends(2018-12) Arroyo, Jesse; Ryan, Cecily A.Biobased fillers, such as bio-derived cellulose, lignin byproducts, and biochar, can be used to modify the thermal, mechanical, and electrical properties of polymer composites. Biochar (BioC), in particular, is of interest for enhancing thermal and electrical conductivities in composites, and can potentially serve as a bio-derived graphitic carbon alternative for certain composite applications. In this work, we investigate a blended biopolymer system: poly(lactic acid) (PLA)/poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV), and addition of carbon black (CB), a commonly used functional filler as a comparison for Kraft lignin-derived BioC. We present calculations and experimental results for phase-separation and nanofiller phase affinity in this system, indicating that the CB localizes in the PHBV phase of the immiscible PHBV:PLA blends. The addition of BioC led to a deleterious reaction with the biopolymers, as indicated by blend morphology, differential scanning calorimetry showing significant melting peak reduction for the PLA phase, and a reduction in melt viscosity. For the CB nanofilled composites, electrical conductivity and dynamic mechanical analysis supported the ability to use phase separation in these blends to tune the percolation of mechanical and electrical properties, with a minimum percolation threshold found for the 80:20 blends of 1.6 wt.% CB. At 2% BioC (approximately the percolation threshold for CB), the 80:20 BioC nanocomposites had a resistance of 3.43 x 108 as compared to 2.99 x 108 for the CB, indicating that BioC could potentially perform comparably to CB as a conductive nanofiller if the processing challenges can be overcome for higher BioC loadings.Item Incorporation of carbon nanofillers tunes mechanical and electrical percolation in PHBV:PLA blends(2018-12) Arroyo, Jesse; Ryan, Cecily A.Biobased fillers, such as bio-derived cellulose, lignin byproducts, and biochar, can be used to modify the thermal, mechanical, and electrical properties of polymer composites. Biochar (BioC), in particular, is of interest for enhancing thermal and electrical conductivities in composites, and can potentially serve as a bio-derived graphitic carbon alternative for certain composite applications. In this work, we investigate a blended biopolymer system: poly(lactic acid) (PLA)/poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV), and addition of carbon black (CB), a commonly used functional filler as a comparison for Kraft lignin-derived BioC. We present calculations and experimental results for phase-separation and nanofiller phase affinity in this system, indicating that the CB localizes in the PHBV phase of the immiscible PHBV:PLA blends. The addition of BioC led to a deleterious reaction with the biopolymers, as indicated by blend morphology, differential scanning calorimetry showing significant melting peak reduction for the PLA phase, and a reduction in melt viscosity. For the CB nanofilled composites, electrical conductivity and dynamic mechanical analysis supported the ability to use phase separation in these blends to tune the percolation of mechanical and electrical properties, with a minimum percolation threshold found for the 80:20 blends of 1.6 wt.% CB. At 2% BioC (approximately the percolation threshold for CB), the 80:20 BioC nanocomposites had a resistance of 3.43 × 108 Ω as compared to 2.99 × 108 Ω for the CB, indicating that BioC could potentially perform comparably to CB as a conductive nanofiller if the processing challenges can be overcome for higher BioC loadings.Item Code to calculate interfacial interactions for polymer blends and composites(Montana State University, 2018-12) Arroyo, Jesse; Ryan, Cecily A.This code uses the Owens-Wendt theory to calculate surface energies of polymers and fillers from contact angle measurements and predict phase separation and nanofiller localization based on interfacial tensions. This code predicts the morphology of a 2-phase polymer blend and the localization of a nano-particulate using the geometric mean equation, and contact angles of each polymer.Item Assessment of models for anaerobic biodegradation of a model bioplastic: Poly(hydroxybutyrate-co-hydroxyvalerate)(2017-03) Ryan, Cecily A.; Billington, Sarah L.; Criddle, Craig S.Kinetic models of anaerobic digestion (AD) are widely applied to soluble and particulate substrates, but have not been systematically evaluated for bioplastics. Here, five models are evaluated to determine their suitability for modeling of anaerobic biodegradation of the bioplastic poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV): (1) first-order kinetics with and without a lag phase, (2) two-step first-order, (3) Monod (4) Contois, and (5) Gompertz. Three models that couple biomass growth with substrate hydrolysis (Monod, Contois, and Gompertz) gave the best overall fits for the data , with reasonable estimates of ultimate CH4 production. The particle size limits of these models were then evaluated. Below a particle size of 0.8 mm, rates of hydrolysis and acetogenesis exceeded rates of methanogenesis with accumulation of intermediates leading to a temporary inhibition of CH4 production. Based on model fit and simplicity, the Gompertz model is recommended for applications in which particle size is greater than 0.8 mm.Item Methodology to assess end-of-life anaerobic biodegradation kinetics and methane production potential for composite materials(2017-04) Ryan, Cecily A.; Billington, Sarah L.; Criddle, Craig S.Composites made with bio-based resins are promising candidates for replacement of conventional plastic composites made with petroleum-based resins in many applications (e.g., decking, paneling, furniture, molded automotive parts). For any such applications, end-of-life management needs consideration. Here, we describe a methodology to assess end-of-life anaerobic degradation to methane (CH4) within landfills or anaerobic digestion (AD) facilities in batch anaerobic microcosms. The core methodology combines stoichiometric considerations, chemical oxygen demand (COD) analysis, a CH4 production assay, and modeling. Additional analyses, such as thermogravimetric analysis (TGA), can complement this core set of analyses. We apply the methodology to injection molded poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) composites with wood fiber (WF) (0%, 20%, 40%) and two fiber-matrix compatibilization treatments that enhance in-service performance: (1) hydrophobic silane treatment of the WF and (2) grafting of hydrophilic maleic anhydride groups to the PHBV matrix. The methodology successfully quantifies process kinetics, ultimate CH4 production capacity, and biodegradability, and allows comparison to reference materials (positive controls).Item Biocomposite Fiber-Matrix Treatments that Enhance In-Service Performance Can Also Accelerate End-of-Life Fragmentation and Anaerobic Biodegradation to Methane(2017-07) Ryan, Cecily A.; Billington, Sarah L.; Criddle, Craig S.Biodegradable resins can enhance the environmental sustainability of wood-plastic composites (WPCs) by enabling methane (CH4) recovery via anaerobic digestion (AD). An under appreciated step in biocomposite AD is the role of cracking and fragmentation due to moisture uptake by the wood fiber (WF) fraction. Here, we use batch microcosms to simulate AD at end-of-life and to assess the effects of fiber-matrix treatments used to retard in-service moisture uptake. The composites evaluated were injection molded poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) with WF (0, 20%) using two fiber-matrix compatibilization treatments: (1) hydrophobic silane treatment of the wood fiber and (2) grafting of hydrophilic maleic anhydride groups to the PHBV matrix. Both treatments accelerated rates of mass loss and CH4 production by a factor of 1.2-2.3 compared to neat PHBV. The fragmentation rate, as measured by mass loss, increased significantly for treated samples compared to untreated samples. A ranking of test samples from lowest to highest rates of mass loss gave the following sequence: neat PHBV ~ maleated PHBV < PHBV plus untreated WF < maleated PHBV plus untreated WF < PHBV plus silane-treated WF. Compared to the untreated samples, maleic anhydride treatment increased the mass loss rate by 30%, and silane treatment increased the mass loss rate by 92%. Onset of cracking in silane-treated composites was observed at 2 weeks (using X-ray micro-computed tomography). At the same time, solid mass loss and CH4 production peaked, implicating cracking and physical disintegration as the rate-limiting step for accelerated anaerobic degradation. When modified to account for bioplastic matrix degradation, a previously derived moisture-induced damage model could predict the onset of composite fragmentation at end-of-life. These results are significant for design of bio-WPCs and demonstrate that treatments designed to improve in-service performance can also improve end-of-life options.