Multifunctional composites have gained significant interest as they enable the integration of sensing and communication capabilities into structural, lightweight composites. Researchers have explored additive manufacturing processes for creating these structures through selective patterning of electrically conductive materials onto composites. Thus far, multifunctional composite performance has been limited by the conductivity of functional materials used, and the methods of integration have resulted in compromises to both structural and functional performance. Integration methods have also imposed limitations on part geometry due to an inability to adequately deposit conductive material over concave surfaces. Proposed methods of integrating functional devices within composites have been shown to negatively affect their mechanical performance. This work presents a novel method for integrating printed electronics onto the interior surfaces of closed, complex continuous fiber composite structures via the transfer of selectively printed conductive inks from additively manufactured sacrificial tooling to the composite surface. The process is demonstrated by creating multifunctional composites via embossing printed electronics onto structural composites without negatively affecting the mechanical performance of the structure. Additionally, this process expands the ability to pattern devices onto complex surfaces and demonstrates that the transferred functionality is well integrated (adhered) with the composite surface. The process is further validated through the successful completion of two separate case studies. The first is the integration of a functioning strain gauge onto an S-glass/epoxy composite, while a second process demonstration shows a composite surface featuring a band stop filter at the X-band, otherwise known as a frequency selective surface (FSS), to show the process' suitability for high performance, aerospace grade multifunctional composites. / Master of Science / Significant interest has been given in the past few decades to strong, lightweight materials for structural purposes. Among these materials, specific interest has been paid to fiber-reinforced composites, which are made of strong fibers and advanced resins. Recently, researchers have tried to use electrically conductive inks and 3D printing techniques to put antennas and other devices onto composites. These composites could possess additional functions beyond their structural purpose and are therefore called multifunctional composites. So far, the performance of multifunctional composites has been limited by the methods used to add additional functions. These methods often result in a weaker composite material and poor performance of the added devices. In this work, a new method for integrating devices onto complex-shaped composite structures is demonstrated. This is done by printing a mold for a composite, then putting a conductive ink onto the mold and transferring the ink to the composite surface. This process is demonstrated without weakening the composite. Additionally, this process allows researchers to put devices onto complex surfaces and demonstrates that the devices are secured to the composite surface. The process is used to make two separate devices and combine them with a composites surface. The first demonstration is the integration of a functioning strain gauge (used to measure a change in material dimension) onto a structural composite, while a second process demonstration shows a composite surface featuring an electromagnetic filter, otherwise known as a frequency selective surface (FSS), to show the process' suitability for high performance, aerospace grade multifunctional composites.

The mechanical characterization of the interfacial shear strength (IFSS) of carbon nanotube (CNT) coated carbon fibers and the interlaminar fracture toughness of woven fabric carbon fiber/epoxy composites toughened with CNT/epoxy interleave films is presented. The deposition of multiwalled carbon nanotubes (MWCNT) onto the surface of carbon fibers through thermal chemical vapor deposition (CVD) was used in an effort to produce a graded, multifunctional interphase region used to improve the interfacial strength between the matrix and the reinforcing fiber. Characterization of the IFSS was performed using the single-fiber fragmentation test. It is shown that the application of a MWCNT coating improves the interfacial shear strength between the coated fiber and matrix when compared with uncoated fibers. The effect of CNT/epoxy thin interleave films on the Mode I interlaminar fracture toughness of woven fabric carbon/epoxy composites is examined using the double-cantilever beam (DCB) test. Initiation fracture toughness, represented by critical strain energy release rate (GIC), is shown to improve over standard un-toughened composites using amine-functionalized CNT/epoxy thin films. Propagation fracture toughness is shown to remain unaffected using amine-functionalized CNT/epoxy thin films with respect to standard un-toughened composites.

The strain and damage sensing abilities of randomly oriented multi-walled carbon nanotubes (MWCNTs) dispersed in the polymer binder of energetic composites were experimentally investigated. Ammonium perchlorate (AP) crystals served as the inert energetic and atomized aluminum as the metallic fuel, both of which were combined to create a representative fuel-oxidizer filler often used for aerospace propulsive applications. MWCNTs were dispersed within an elastomer binder of polydimethylsiloxane (PDMS), and hybrid energetics were fabricated from it, with matrix material comprised of the identified fillers. The nanocomposites were characterized based on their stress-strain response under monotonic uniaxial compression to failure, allowing for the assessment of effects of MWCNTs and aluminum powder on average compressive elastic modulus, peak stress, and strain to failure. The piezoresistive response was measured as the change in impedance with applied monotonic strain in both the mesoscopic and microscopic strain regimes of mechanical loading for each material system, as well as under ten cycles of applied compressive loading within those same strain regimes. Gauge factors were calculated to quantify the magnitude of strain and damage sensing in MWCNT-enhanced material systems. Electrical response of single-cycle thermal loading was explored with epoxy in place of the elastomer binder of the previously discussed studies. Piezoresistive response due to microscale damage from thermal expansion was observed exclusively in material systems enhanced by MWCNTs. The results discussed herein validate structural health monitoring (SHM) applications for embedded carbon nanotube sensing networks in polymer-based energetics under unprecedented cyclic loads. / Master of Science / The ability to characterize both deformation and damage in real time within materials of high energetic content, such as solid rocket propellant, is of great interest in experimental mechanics. Common energetic ammonium perchlorate, in the fonn of crystal particles, was embedded in polymer binders (ie PDMS and epoxy) and investigated under a variety of me­chanical and thermal loads. Carbon nanotubes, conductive tube-shaped molecular structures of carbon atoms, have been demonstrated in prior proofs of concept to induce substantial electrical response change when dispersed in composites which are experiencing strain. With the introduction of carbon nanotubes in the energetic composites investigated herein, the electrical response of the material systems was measured as a change in impedance with applied strain. Elastomer-bonded energel.ks were t.esl.ed under monotonic compression and cyclic compression, and expanded exploration was done on these material systems with the additional particulate of aluminum powder, allowing for varied particulate sizes and conductivity enhancement of the overall composite. The magnitude of the resulting piezoresistive change due to strain and microscale damage was observed to increase dramatically in material systems enhanced by MWCNT networks. Local heating was used to explore thermal loading on epoxy-bonded energetic material systems, and sensing of permanent damage to the­ material through its CNT network was proven through a permanent change in the electrical response which was exclusive to the CNT-enhanced material systems. These results demon­strate valid structural health monitoring (SHM) applications for embedded carbon nanotube sensing networks in particulate energetic composites, under a variety of load cases.

<p dir="ltr">The demand and utilization of fiber-reinforced composites are increasing in various sectors, including aerospace, civil engineering, and automotive industries. Non-destructive methods are necessary for monitoring fiber-reinforced composites due to their complex and often visually undetectable failure modes. An emerging method for monitoring composite structures is through the integration of self-sensing capabilities. Self-sensing in nanocomposites can be achieved through nanofiller modifications, which involve introducing an adequate amount of nanofillers into the matrix, such as carbon nanotubes (CNTs) and carbon nanofillers (CNFs). These fillers form an electrically well-connected network that allows the electrical current to travel through conductive pathways. The disruption of connectivity of these pathways, caused by mechanical deformations or damages, results in a change in the overall conductivity of the material, thereby enabling intrinsic self-sensing.</p><p dir="ltr">Currently, the majority of predictive modeling attempts in the field of self-sensing nanocomposites have been dedicated to microscale piezoresistivity. There has been a lack of research conducted on the modeling of strain-induced resistivity changes in macroscale fiber-matrix material systems. As a matter of fact, no analytical macroscale model that addresses the impact of continuous fiber reinforcement in nanocomposites has been presented in the literature. This gap is significant because it is impossible to make meaningful structural condition predictions without models relating observed resistivity changes to the mechanical condition of the composite. Accordingly, this dissertation presents a set of three research contributions. The overall objective of these contributions is to address this knowledge gap by developing and validating an analytical model. In addition to advancing our theoretical understanding, this model provides a practical methodology for predicting the piezoresistive properties of continuous fiber-reinforced composites with integrated nanofillers.</p><p dir="ltr">To bridge the above-mentioned research gap, three scholarly contributions are presented in this dissertation. The first contribution proposes an analytical model that aims to predict the variations in resistivity within a material system comprising a nanofiller-modified polymer and continuous fiber reinforcement, specifically in response to axial strain. The fundamental principle underlying our methodology involves the novel use of the concentric cylindrical assembly (CCA) homogenization technique to model piezoresistivity. The initial step involves the establishment of a domain consisting of concentric cylinders that represent a continuous reinforcing fiber phase wrapped around by a nanofiller-modified matrix phase. Subsequently, the system undergoes homogenization to facilitate the prediction of changes in the axial and transverse resistivity of the concentric cylinder as a consequence of longitudinal deformations. The second contribution investigates the effect of radial deformations on piezoresistivity. Here, we demonstrate yet another novel application of the CCA homogenization technique to determine piezoresistivity. This contribution concludes by presenting closed-form analytical relations that describe changes in axial and transverse resistivity as functions of externally applied radial strain. The third contribution involves computationally analyzing piezoresistivity in fiber-reinforced laminae by using three-dimensional representative volume elements (RVE) with a CNF/epoxy matrix. By comparing the single-fiber-based analytical model with the computational model, we can investigate the impact of interactions between multiple adjacent fibers on the piezoresistive properties of the material. The study revealed that the differences between the single-fiber CCA analytical model and the computational model are quite small, particularly for composites with low- to moderate-fiber volume fractions that undergo relatively minor deformations. This means that the analytical methods herein derived can be used to make accurate predictions without resorting to much more laborious computational methods.</p><p dir="ltr">In summary, the impact of this dissertation work lies in the development of novel analytical closed-form nonlinear piezoresistive relations. These relations relate the electrical conductivity/resistivity changes induced by axial or lateral mechanical deformations in directions parallel and perpendicular to the reinforcing continuous fibers within fiber-reinforced nanocomposites and are validated against in-depth computational analyses. Therefore, these models provide an important and first-ever bridge between simply observing electrical changes in a self-sensing fiber-reinforced composite and relating such observations to the mechanical state of the material.</p>

Orientador: Edson Cocchieri Botelho / Resumo: Este trabalho de pesquisa consiste na obtenção e caracterizações térmica, mecânica, reológica e elétrica de compósitos multifuncionais obtidos a partir da utilização de fibras de carbono (FC), resina furfurílica (RF) e nanotubos de carbono (CNT) para aplicações aeroespaciais. O uso de uma bioresina como fonte alternativa ao petróleo em compósitos multifuncionais e a avaliação dos ganhos de propriedades na utilização de nanotubos de carbono (0, 1,3 e 2,5% em volume) associados a fibras contínuas de carbono (tecido plain weave) são os objetivos principais deste trabalho. O desenvolvimento deste trabalho de pesquisa estabelece os parâmetros de processo mais adequados para a obtenção de compósitos multifuncionais com propósitos estruturais, térmicos e/ou elétricos. Neste trabalho, os compósitos multifuncionais foram processados com a utilização de moldagem por compressão a quente, sendo esta uma das contribuições desta dissertação. Após processados, os laminados foram avaliados a partir de ensaios mecânicos (cisalhamento interlaminar por compression shear test (CST), impacto a baixas velocidades, DCB (Double Cantilever Beam test), ENF (End Notched Flexure) e fadiga); assim como, a partir de análises térmicas (DMA (Análise Dinâmico-Mecânica), DSC (Calorimetria Exploratória Diferencial), TGA (Análise Termogravimétrica) e TMA (Análise Termomecânica)), ensaios elétricos, análises morfológicas (MO (Microscopia Óptica), MEV (Microscopia Eletrônica de Varredura) e ultrassom) e análises ... (Resumo completo, clicar acesso eletrônico abaixo) / Doutor