Soft actuation methods are a developing field of robotics deemed suitable for physical human-robot interactions due to the adaptability of materials and compliant structures. Thermo-active soft actuators are a subset of these which convert thermal energy to mechanical work in the form of elongation, bending, or twisting to conform to the environment. This study is divided into three major studies that all use actuators with a working principle of phase-change fluid vaporizing for expansion with applied heat from a Peltier. The first study evaluates the bandwidth and efficiency between (i) traditional Joule heating, and (ii) Peltier heating, finding that Peltier heating can considerably improve the operational bandwidth of the actuator. The second study uses a thin membrane actuator placed in a braided mesh to form a McKibben muscle capable of lifting 5N, and formed into a gripper capable of manipulating objects within the environment. The third study uses actuators of a solid, hollow and flexible Peltier embedded silicone structure and are evaluated and optimized in order to increase actuation speed, finding that the embedded flexible Peltier design was able to elongate over 50% of its original height in 20 seconds. The overall aim of all of these studies was to improve bandwidth, efficiency, actuator lifetime, and create more symmetrical actuation and deactuation cycles.

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Energy storage within hypersonic aircraft is becoming increasingly important with the development of more sophisticated electronic components and is an integral piece of expanding their overall capabilities. Hypersonics not only produce large external thermal loads, but also an abundance of internal thermal loads from components such as power electronics, avionics, and batteries. Additionally, limited volume within such vehicles introduces additional constraints. Thus, having efficient heat sinks that are capable of storing much of these heat loads is imperative. Passive thermal management systems, i.e., heat sinks, are preferable in most applications because they do not require power input to operate, and they are typically smaller than active systems such as coolant loops. In identifying and developing heat sinks with increased energy storage capability, an exhaustive search of available phase change materials (PCMs) is conducted. PCMs have been used in hypersonic vehicles in the past as a means of energy storage. Additionally, the use of energy-consuming endothermic reactions is considered. An innovative PCM-endothermic reaction hybrid approach is also developed. Both thermodynamic and transient/quasi-stationary models are developed for each of these proposed heat sink technologies. Prototypes are then developed for the best candidates to validate the models and draw conclusions on each heat sink's performance. Both the thermodynamic modeling and experimental results presented in this paper suggest that PCMs, endothermic reactions, and, especially, the hybrid system show greater energy storage capabilities than what is being used in hypersonic vehicles currently. / Master of Science / Hypersonic vehicles are an important topic of interest in the aerospace and defense industries. To be classified as hypersonic, a vehicle must travel at or above Mach 5, which is at least five times the speed of sound. Hypersonic vehicles often travel at high altitudes and a common application of the technology is in missiles. One major hurdle in developing hypersonic technologies at lower altitudes is that because of the high speeds, the outside skin temperature of the vehicle can reach thousands of degrees. Clearly, these temperatures can affect the heat load on the inside of the vehicle as can the thermal energy release of internal components such as the power electronics, the avionics, etc. To deal with these internal heat loads, innovative energy storage solutions are needed to efficiently and effectively store the thermal energy released internally. One approach considered here is the use of phase change materials (PCMs) as a storage medium. Melting such a material requires large amounts of energy and occurs at constant temperature. This is much more advantageous than heating a material in which only the temperature rises. Another approach considered in this thesis is that of using a chemical reaction, which requires energy input to proceed. Such a reaction is called an endothermic reaction and often results in a temperature decrease. Thus, simply mixing a set of reactants and adding energy helps cool the system. A final approach considered is a hybrid one, which combines a PCM material and an endothermic reaction. Such an approach combines the advantages of both. Each of these approaches are modeled thermodynamically to better understand how devices based on them work. Physical prototypes are then designed, built, and tested to confirm their performance. Both the modeling and experimental results presented in this thesis suggest that these devices show significantly improved energy storage capabilities over the devices currently used in hypersonic vehicles.

Thermal energy storage (TES) consists in storing heat for a later use, thereby reducing the gap between energy availability and demand. The most diffused materials for TES are the organic solid-liquid phase change materials (PCMs), such as paraffin waxes, which accumulate and release a high amount of latent heat through a solid-liquid phase change, at a nearly constant temperature. To avoid leakage and loss of material, PCMs are either encapsulated in inert shells or shape-stabilized with porous materials or a nanofiller network. Generally, TES systems are only a supplementary component added to the main structure of a device, but this could unacceptably rise weight and volume of the device itself. In the applications where weight saving and thermal management are both important (e.g. automotive, portable electronics), it would be beneficial to embed the heat storage/management in the structural components. The aim of this thesis is to develop polymer composites that combine a polymer matrix, a PCM and a reinforcing agent, to reach a good balance of mechanical and TES properties. Since this research topic lacks a systematic investigation in the scientific literature, a wide range of polymer/PCM/reinforcement combinations were studied in this thesis, to highlight the effect of PCM introduction in a broad range of matrix/reinforcement combinations and to identify the best candidates and the key properties and parameters, in order to set guidelines for the design of these materials. The thesis in divided in eight Chapters. Chapter I and II provide the introduction and the theoretical background, while Chapter III details the experimental techniques applied on the prepared composites. The results and discussion are then described in Chapters IV-VII. Chapter IV presents the results of PCM-containing composites having a thermoplastic matrix. First, polyamide 12 (PA12) was melt-compounded with either a microencapsulated paraffin (MC) or a paraffin powder shape-stabilized with carbon nanotubes (ParCNT), and these mixtures were used as matrices to produce thermoplastic laminates with a glass fiber fabric via hot-pressing. MC was proven more suitable to be combined with PA12 than ParCNT, due to the higher thermal resistance. However, also the MC were considerably damaged by melt compounding and the two hot-pressing steps, which caused paraffin leakage and degradation, as demonstrated by the relative enthalpy lower than 100 %. Additionally, the PCM introduction decreased the mechanical properties of PA12 and the tensile strength of the laminates, but for the laminates containing MC the elastic modulus and the strain at break were not negatively affected by the PCM. Higher TES properties were achieved with the production of a semi-structural composite that combined PA12, MC and discontinuous carbon fibers. For example, the composite with 50 wt% of MC and 20 wt% of milled carbon fibers exhibited a total melting enthalpy of 60.4 J/g and an increase in elastic modulus of 42 % compared to the neat PA. However, the high melt viscosity and shear stresses developed during processing were still responsible for a not negligible PCM degradation, as also evidenced by dynamic rheological tests. Further increases in the mechanical and TES properties were achieved by using a reactive thermoplastic matrix, which could be processed as a thermosetting polymer and required considerably milder processing conditions that did not cause PCM degradation. MC was combined with an acrylic thermoplastic resin and the mixtures were used as matrices to produce laminates with a bidirectional carbon fabric, and for these laminates the melting enthalpy increased with the PCM weight fraction and reached 66.8 J/g. On the other hand, the increased PCM fraction caused a rise in the matrix viscosity and so a decrease in the fiber volume fraction in the final composite, thereby reducing the elastic modulus and flexural strength. Dynamic-mechanical investigation evidenced the PCM melting as a decreasing step in ’; its amplitude showed a linear trend with the melting enthalpy, and it was almost completely recovered during cooling, as evidenced by cyclic DMA tests. Chapter V presents the results of PCM-containing thermosetting composites. A further comparison between MC and ParCNT was performed in a thermosetting epoxy matrix. First, ParCNT was mixed with epoxy and the mixtures were used as matrices to produce laminates with a bidirectional carbon fiber fabric. ParCNT kept its thermal properties also in the laminates, and the melting enthalpy was 80-90 % of the expected enthalpy. Therefore, ParCNT performed better in thermosetting than in thermoplastic matrices due to the milder processing conditions, but the surrounding matrix still partially hindered the melting-crystallization process. Therefore, epoxy was combined with MC, but the not optimal adhesion between the matrix and the MC shell caused a considerable decrease in mechanical strength, as also demonstrated by the fitting with the Nicolais-Narkis and Pukanszky models, both of which evidenced scarce adhesion and considerable interphase weakness. However, the Halpin-Tsai and Lewis-Nielsen models of the elastic modulus evidenced that at low deformations the interfacial interaction is good, and this also agrees with the data of thermal conductivity, which resulted in excellent agreement with the Pal model calculated considering no gaps at the interface. These epoxy/MC mixtures were then reinforced with either continuous or discontinuous carbon fibers, and their characterization confirmed that the processing conditions of an epoxy composite are mild enough to preserve the integrity of the microcapsules and their TES capability. For continuous fiber composites, the increase in the MC fraction impaired the mechanical properties mostly because of the decrease in the final fiber volume fraction and because the MC phase tends to concentrate in the interlaminar region, thereby lowering the interlaminar shear strength. On the other hand, a small amount of MC enhanced the mode I interlaminar fracture toughness (Gic increases of up to 48 % compared to the neat epoxy/carbon laminate), as the MC introduced other energy dissipation mechanisms such as the debonding, crack deflection, crack pinning and micro-cracking, which added up to the fiber bridging. Chapter VI introduces a fully biodegradable TES composite with a thermoplastic starch matrix, reinforced with thin wood laminae and containing poly(ethylene glycol) as the PCM. The wood laminae successfully acted as a multifunctional reinforcement as they also stabilized PEG in their inner pores (up to 11 wt% of the whole laminate) and prevent its leakage. Moreover PEG was proven to increase the stiffness and strength of the laminate, thereby making the mechanical and TES properties synergistic and not parasitic. Finally, Chapter VII focused on PCM microcapsules. The synthesis of micro- and nano-capsules with an organosilica shell via a sol-gel approach clarified that the confinement in small domains and the interaction with the shell wall modified the crystallization behavior of the encapsulated PCM, as also evidenced by NMR and XRD studies and confirmed by DSC results. In the second part of Chapter VII, a coating of polydpamine (PDA) deposited onto the commercial microcapsules MC. The resulting PDA coating was proven effective to enhance the interfacial adhesion with an epoxy matrix, as evidenced by SEM micrographs. XPS demonstrated that the PDA layer was able to react with oxirane groups, thereby evidencing the possibility of forming covalent bond with the epoxy matrix during the curing step.

Active substances can be stabilized to be protected from undesirable reactions, aggregation, and leaking, which would keep the intended functions of the active substances without premature degradation. Among such active substances are paraffin-based organic phase change materials (PCMs) and essential oils (EOs), which feature attractive characteristics, e.g., high latent heat of fusion and inherent antimicrobial activity. However, their high volatility requires an effective stabilization strategy. Petroleum-based synthetic polymers have often been employed to stabilize PCMs and EOs by encapsulation and complexation pathways. Despite their proven effectiveness, these polymers are from non-renewable resources, and non-degradable and often toxic, which has prompted a need to develop a substitute arising from natural polymers that are environmentally benign, biodegradable, and sustainable. Valorization of biomass in this regard would add extra value to biomass otherwise burned or wasted. This dissertation will present the development of microcapsules and inclusion complexes consisting of a hydrophobic active substance core and a polysaccharidic shell originating from biomass. The first two chapters will explain the introduction and experimental details. Chapter 3 will present the microencapsulation of n-hexadecane as PCM via oil-in-water (O/W) Pickering emulsions stabilized by unmodified cellulose nanofibrils (CNFs) through a sonochemical technique. Chapter 4 will investigate the incorporation of the PCM-CNF microcapsules into TEMPO-oxidized CNF films for building application. Finally, Chapter 5 will show the synthesis of EOs-beta cyclodextrin (βCD) inclusion complexes as a guest-host system through a sonochemical technique.

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