The evolution of nanoscale properties is measured during the thermally triggered curing of an industrial epoxy adhesive. We use x-ray photon correlation spectroscopy (XPCS) to track the progression of the curing reaction through the local dynamics of filler particles that reflect the formation of a thermoset network. Out-of-equilibrium dynamics are resolved through identification and analysis of the intensity–intensity autocorrelation functions obtained from XPCS. The characteristic time scale and local velocity of the filler is calculated as functions of time and temperature. We find that the dynamics speed up when approaching the curing temperature (Tcure), and decay rapidly once Tcure is reached. We compare the results from XPCS to conventional macroscale characterization by differential scanning calorimetry (DSC). The demonstration and implementation of nanoscale characterization of curing reactions by XPCS proves useful for future development and optimization of epoxy thermoset materials and other industrial adhesive systems.

Additive manufacturing (AM) is a promising technique to rapidly produce polymeric materials into complex 3-dimensional (3D) geometries. While AM is widespread and relevant for a range of applications, implementation in industry has outpaced our fundamental understanding of polymer dynamics and structure development during the printing process. Characterization and quantification of such dynamics is necessary to optimize final material properties and design future materials and processes for 3D printing. Here, we utilize X-ray photon correlation spectroscopy (XPCS) to measure spatial and time-resolved, out-of-equilibrium dynamics during direct ink write (DIW) 3D printing. Specifically, we investigate the progression of structural dynamics in a dual cure (UV/thermal) nanocomposite during and directly after printing. As the filament is printed and cured in situ, the relaxation processes of the cross-linking network are measured through the dynamics of inorganic filler particles. The characteristic relaxation time of the dynamics is calculated through the intensity–intensity autocorrelation function g 2 and directly correlated to the printing process parameters, such as printhead velocity and UV light intensity. The time-resolved evolution of nanoscale dynamics follows a power-law dependence as the filament is cured. Bulk rheological characterizations reveal the macroscopic solidification of the resin, providing correlation of material properties across a wide range of length and time scales. The measurement of multiscale, out-of-equilibrium dynamics provides insight into the development of structure in polymer nanocomposite filaments during 3D printing and is used to further understand the influence of such parameters on the AM process.

Chemical conversion coating as an effective corrosion inhibition has wide range of applications in industries and is of great expectation to be environmentally friendly and costeffective. Zirconium-based (Zr-based) conversion coating using hexafluorozirconic acid with copper (Cu) additive on low carbon steel which improves anticorrosion and adhesion properties was studied using synchrotron X-ray and electron-based techniques. To understand the elemental evolution during coating formation process, in situ synchrotron X-ray fluorescence (XRF) microscopy has been applied to observe Zr, Cu, iron (Fe), and zinc (Zn) concentration evolution. By quantifying the density, average size, and size distribution of the cluster as a function of time and temperature, the growth mechanism of the coating can be concluded as a reaction-controlled mechanism. X-ray absorption near edge structure and X-ray photoelectron spectroscopy (XPS) were used to characterize the composition of the Cu-rich clusters embedded in the coating which was determined to be mainly Cu 2 O, Cu, and CuF 2 ; the cluster composition varies from the surface to the internal region as determined by the depth-profiling of XPS. Our study shed light on the chemical and morphological evolution in environmentally friendly surface conversation coating and demonstrated new methodology in studying the coating formation via in situ synchrotron XRF.

The sintering processing–structure–property relationship of a multiscale silver materials is investigated: microparticles with nanofeatures, particularly on their three‐dimensional (3D) morphology. The target application is to replace conventional lead‐based solders in advanced electronic manufacturing. Unlike lead‐based solders, silver powders are suited to satisfy increasingly demanding mechanical, electrical, and thermal requirements, meanwhile being free of health effect. Sintering the material at a low temperature and without applied pressure are desirable conditions, which results in a preferred use of silver nanoparticles, as nanofeatures have higher driving force to sinter with the decrease in particle size. However, nanosized powders present potential health/environmental effects. To address the trade‐off between the benefits and shortcomings of nano‐ versus microparticles, this work studies a novel multiscale silver paste, namely micron‐sized powders with nanosized features. To get quantitative 3D visualization of micro‐ and nanoscale features, ptychographic X‐ray computed nanotomography is applied. The correlations between conditions (thermal aging, pressure, and substrate metallization), mechanical properties, and morphological parameters are established. Using novel 3D X‐ray nanoimaging technique, it is demonstrated that one can design multiscale materials while balancing complex demands required in advanced electronics manufacturing and research directions in materials design and characterization.

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