Alpha-alumina is known to exhibit photo-luminescent (PL) properties, mainly characteristic R-lines that shift according to applied stress. In addition to showing excellent PL properties, polymers with embedded alumina nanoparticles have been shown to improve the overall composite mechanical properties. While the use of the PL properties to develop stress-sensing materials using an alumina-epoxy material has been success- fully shown in compression, the properties have not been developed for tension. In this study, the PL response of variable volume fraction alumina-epoxy composites will be determined under tensile conditions. It is expected that increasing the volume fraction of alumina nanoparticles will increase the sensitivity of the particles PL emission shift to applied stress. Three tensile alumina-epoxy specimens of 21.0%, 31.2%, and 34.5% volume fractions were manufactured and tested under tensile static loads. The results of this experiment will determine the piezospectroscopic (PS) coeffi cient and calibration of bulk alumina nanocomposites in tension. A linear region was identified in the PS response of the nanocomposite to the applied tensile load. The PS coeffi cient of this linear region increased as the volume fraction of the nanocomposite increased. To demonstrate the application of structural composites with stress sensing capabilities, alumina nanoparticles were integrated in the manufacturing of a carbon fiber composite specimen. The results of the stress-sensing composite mechanical experiment showed that alumina nanoparticles were able to detect changes in stress. The results for both the bulk nanocomposite calibrations and the application of stress-sensing alumina nanoparticles in a carbon-fiber composite will advance the development of this novel stress-sensing method.

Particulate composites are widely used in many aerospace and military applications as energetic materials, armor materials or coatings and their behavior under dynamic loads have gained increasing significance. The addition of modifiers such as alumina nanoparticles generally facilitates the improvement of the mechanical strength to density ratio due to high specific area and particle rigidity. This allows for sufficient particlematrix bonding and therefore improved stiffness and load transfer in the composite. Photo-luminescent α-alumina nanoparticles when embedded in an epoxy matrix allow for the added benefit of in situ measurements at low strain rates to provide stress-sensitive information using the particle piezospectroscopic (PS) property. To investigate the low strain rate behavior, cylindrical specimens of alumina-epoxy composites with varying volume fractions of alumina were fabricated using a casting process to ensure minimal surface finishing and reduced manufacturing time. The results illustrate the capability of alumina nanoparticles to act as diagnostic sensors to measure the stress-induced shifts of the spectral R-line peaks resulting from low compressive strain rates. The range of PS coefficients measured, -3.15 to -5.37 cm−1/GP a for R1 and -2.62 to -5.39 cm−1/GP a for R2, correlate well with static test results of similar volume fractions. Results reveal a general trend of increasing sensitivity of the PS coefficients with increasing strain rate when compared to similar materials under static conditions. In contrast to static results, at a given strain rate, the PS coefficients show varying degrees of sensitivity for each iii volume fraction. This information can be used to determine the time-dependent microscale stresses the nanoparticles sustain during composite loading. Additionally, this work facilitates failure prediction by monitoring upshifts in the PS information. Calibration of the in situ diagnostic stress sensing capabilities of varying volume fractions of alumina nanocomposites under quasi-static strain rates in this work sets the precedent for future studies at high strain rates.

Carbon ber composites have become popular in aerospace structures and applications due to their light weight, high strength, and high performance. Recently, scientists have begun investigating hybrid composites that include fibers and particulate fillers, since they allow for advanced tailoring of mechanical properties, such as improved fatigue life. This project investigated a hybrid carbon ber reinforced polymer (HCFRP) that includes carbon fiber and additional alumina nanoparticle fillers, which act as embedded nano stress-sensors. Utilizing the piezospectroscopic e ect, the photo-luminescent spectral signal of the embedded nanoparticles has been monitored as it changes with stress, enabling non-contact stress detection of the material. The HCRFPs stress-sensitive properties have been investigated in-situ using a laser source and a tensile mechanical testing system. Hybrid composites with varying mass contents of alumina nanoparticles have been studied in order to determine the e ect of particle content on the overall stress sensing properties of the material. Additionally, high resolution photo-luminescent maps were conducted of the surfaces of each sample in order to determine the particulate dispersion of samples with varying alumina content. The dispersion maps also served as a method of quantifying particulate sedimentation, and can aid in the improvement of the manufacturing process. The results showed that the emitted photo-luminescent spectrum can indeed be captured from the embedded alumina nanoparticles, and exhibits a systematic trend in photo-luminescent peak shift with respect to stress. The stress maps showed a linear increase in peak shift up to a certain critical stress, and matched closely with the DIC strain results. Therefore, the non-contact stress sensing results shown in this work have strong implications for the future of structural health monitoring and nondestructive evaluation (NDE) of aerospace structures.

Ultra-high temperature ceramics (UHTCs), such as ZrB2-based ceramic composites, have been identified as next generation candidate materials for leading edges and nose cones in hypersonic air breathing vehicles. Mechanical performance of ceramic composites play an important role in the ultra-high temperature applications, therefore SiC is added to ZrB2 as a strengthening phase to enhance its mechanical performance. The high melting temperatures of both ZrB2 and SiC, as well as the ability of SiC to form SiO2 refractory oxide layers upon oxidation make ZrB2-SiC ceramics very suitable for aerospace applications. Thermal residual stresses appearing during processing are unavoidable in sintered ZrB2-SiC ceramic composites. Residual microstresses appear at the microstructural level (intergranular microstresses) or at the crystal structure level (intragranular microstresses). These microstresses are of enormous importance for the failure mechanisms in ZrB2-SiC ceramics, such as ratio of the trans- and intergranular fracture; crack branching or bridging, microcracking, subcritical crack growth and others, as they govern crack propagation–induced energy dissipation and affect the toughness and strength of the ceramic material. Therefore, understanding the evolution of residual stress state in processed ZrB2-SiC ceramic composites and accurate measurements of these stresses are of high priority. In the present research the ZrB2-17vol%SiC, ZrB2-32vol%SiC, and ZrB2-45vol%SiC ultra-high temperature particulate ceramic composites were sintered using both Hot Pressing (HP) and Spark Plasma Sintering (SPS) techniques. The mechanical performance of the ZrB2-SiC composites was investigated using 3- and 4-point bending techniques for measurements of instantaneous fracture strength and fracture toughness. Resonant Ultrasound Spectroscopy was used for measurement of Young's, shear, and bulk moduli as well as Poisson's ratio of the composites. The distribution of thermal residual stresses and the effect of the applied external load on their re-distribution was studied using micro-Raman spectroscopy. Piezospectroscopic coefficients were determined for all compositions of ZrB2-SiC ceramic under study and their experimentally obtained values were compared with the piezospectroscopic coefficients both published in the literature and calculated using theoretical approach. Finally, the novel ZrB2-IrB2-SiC ceramic composites were also produced using Spark Plasma Sintering (SPS), where IrB2 powder was synthesized using mechanochemical route. It is expected that the IrB2 additive phase might contribute to the improved overall oxidation resistance of ZrB2 based ultra-high temperature ceramic composites.

Particulate composites are widely used in many aerospace applications such as protective coatings, adhesives, or structural members of a body and their mechanical properties and behavior have gained increasing significance. The addition of modifiers such as alumina generally leads to improved mechanical properties. This addition also enables the non-invasive study of the load transfer between the particle and the matrix. Understanding the load transfer between the particulate and the matrix material is the first step to understanding the behavior and mechanical properties of the composite as a whole. In this work, samples with an isolated alumina particle embedded in an epoxy matrix were created to replicate the ideal assumptions for many particulate mechanics models. In separate experiments, both photo stimulated luminescent spectroscopy (PSLS) and synchrotron radiation were used to collect the spectral emission and diffraction rings, respectively, from the mechanically loaded samples. The PSLS data and XRD data are shown to be in qualitative agreement that as particle size is increased, the load transferred to the particle also increased for the range of particle sizes tested. This trend of increasing load transfer with increasing particle size is compared with the classical Eshelby model. Results from this work provide experimental insight into the load transfer properties of particulate composites and can serve to experimentally validate the theoretical load transfer models that currently exist.

The durability of Thermal Barrier Coatings (TBCs) used on the turbine blades of aircraft and power generation engines has been known to be affected by sand particle ingression comprised of Calcium-Magnesium-Alumina-Silicate (CMAS). Previous studies have shown that these effects present themselves through variations in the thermomechanical and thermochemical properties of the coating. This study investigated the impact of CMAS ingression on the Yttria Stabilized Zirconia Topcoat (YSZ) and Thermally Grown Oxide (TGO) strain in sprayed Thermal Barrier Coating (TBC) samples of varying porosity with and without CMAS ingression. In-Situ Synchrotron X-ray Diffraction measurements were taken on the sample under thermal loading conditions from which the YSZ and TGO peaks were identified and biaxial strain calculations were determined at high temperature. Quantitative strain results are presented for the YSZ and TGO during a thermal cycle. In-plane strain results for YSZ near the TGO interface for a complete thermal cycle are presented, for a 6% porous superdense sample with CMAS infiltration. The outcomes from this study can be used to understand the role of CMAS on the strain tolerance of the TBC coating. It is well known that under engine operational conditions the development of the TGO layer, with large critical stresses, has been linked to failure of the coating. The growth of the TGO manifests as undulations in a series of peaks and troughs. Understanding the mechanics of the oxide layer at these locations provides significant information with respect to the failure mechanisms of the TBC coating. This study investigated the stress at the peak and trough of a TGO undulation for a cycled Dense Vertically Cracked (DVC) plasma sprayed TBC sample through photo-luminescence (PL) spectroscopy. High resolution nanoscale stress maps were taken nondestructively in the undulation of the TGO. Preliminary results from first line mapping of TGO peak and trough scan, at a resolution of 200 nm, have shown a non-uniform TGO stress variation. The results obtained from this study can be used to understand the stress variation in the peak and trough of a DVC sample's TGO undulation and how it contributes to the life of the TBC coating.

Coatings utilizing the piezospectroscopic (PS) effect of alpha alumina could enable on the fly stress sensing for structural health monitoring applications. While the PS effect has been historically utilized in several applications, here by distributing the photo-luminescent material in nanoparticle form within a matrix, a stress sensing coating is created. Parallel to developing PS coatings for stress sensing, the multi-scale mechanics associated with the observed PS response of nanocomposites and their coatings has been applied to give material property measurements, providing an understanding of particle reinforced composite behavior. Understanding the nanoparticle-coating-substrate mechanics is essential to interpreting the spectral shifts for stress sensing of structures. In the past, methods to experimentally measure the mechanics of these embedded nano inclusions have been limited, and much of the design of these composites depend on computational modeling and bulk response from mechanical testing. The PS properties of Chromium doped alumina allow for embedded inclusion mechanics to be revisited with unique experimental setups that probe the particles state of stress under applied load to the composite. These experimental investigations of particle mechanics will be compared to the Eshelby theory and its derivative theories in addition to the nanocomposite coating mechanics. This work discovers that simple nanoparticle load transfer theories are adequate for predicting PS properties in an intermediate volume fraction range. With fundamentals of PS nanocomposites established, the approach was applied to selected experiments to prove its validity. In general it was observed that the elastic modulus values calculated from the PS response were similar to that observed from macroscale strain measurements such as a strain gage. When simple damage models were applied to monitor the elastic modulus, it was observed that the rate of decay for the elastic modulus was much higher for the PS measurements than for the strain gage. A novel experiment including high resolution PS maps with secondary strain maps from digital image correlation is reviewed on an open hole tension, composite coupon. The two complementary measurements allow for a unique PS response for every location around the hole with a spatial resolution of 400 microns. Progression of intermediate damage mechanisms was observed before digital image correlation indicated them. Using the PS nanocomposite model, elastic modulus values were calculated. Introducing an elastic degradation model with some plastic deformation allows for estimation of material properties during the progression of failure. This work is part of a continuing effort to understand the mechanics of a stress sensing PS coating. The mechanics were then applied to various experimental data that provided elastic property calculations with high resolution. The significance is in the experimental capture of stress transfer in particulate composites. These findings pave the way for the development of high resolution stress-sensing coatings.