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Direct inkjet printing of functional inks is an emerging and promising technique for the fabrication of electrochemical energy storage devices. Electrochromic energy devices combine electrochromic and energy storage functions, providing a rising and burgeoning technology for next-generation intelligent power sources. However, printing such devices has, in the past, required additives or other second phase materials in order to create inks with suitable rheological properties, which can lower printed device performance. Here, tungsten oxide nanocrystal inks are formulated without any additives for the printing of high-quality tungsten oxide thin films. This allows the assembly of novel electrochromic pseudocapacitive zinc-ion devices, which exhibit a relatively high capacity (≈260 C g−1 at 1 A g−1) with good cycling stability, a high coloration efficiency, and fast switching response. These results validate the promising features of inkjet-printed electrochromic zinc-ion energy storage devices in a wide range of applications in flexible electronic devices, energy-saving buildings, and intelligent systems.
Microalloyed steels contain small quantities (≤ 0.5 wt%) of the microalloying elements Ti, Nb, V. Judicious combination of TMCP parameters and microalloyed steel composition leads to formation of desirable nm-sized carbide, nitride, carbonitride inclusions which improve steel mechanical properties. TMCP optimisation relies on understanding the interrelation between TMCP parameters and precipitate properties. A characterisation routine was developed in the group to provide statistically meaningful data on precipitates size distribution and chemical composition.[1] Precipitates with diameters below 10nm could not be investigated with the existing routine. Such precipitates are of interest because they play a key role in precipitation hardening. This thesis extends the existing characterisation routine to sub-10nm precipitates extracted from microalloyed steels. Electrolytic extraction was investigated as alternative extraction process to reduce undesired particle loss during chemical extraction. The suitability of various electrolytes to provide a stable colloidal suspension for colloidal analysis was assessed. Chemically extracted precipitates underwent differential centrifugation to isolate sub-10nm precipitates and enable their size and chemical composition characterisation. Improvements in precipitate analysis were achieved by implementation of speed-ramp analytical ultracentrifugation and precipitate number density determination.
Particle number densities are a crucial parameter in the microstructure engineering of microalloyed steels. We introduce a new method to determine nanoscale precipitate number densities of macroscopic samples that is based on the matrix dissolution technique (MDT) and combine it with atom probe tomography (APT). APT counts precipitates in microscopic samples of niobium and niobium-titanium microalloyed steels. The new method uses MDT combined with analytical ultracentrifugation (AUC) of extracted precipitates, inductively coupled plasma–optical emission spectrometry, and APT. We compare the precipitate number density ranges from APT of 137.81 to 193.56 × 1021 m−3 for the niobium steel and 104.90 to 129.62 × 1021 m−3 for the niobium-titanium steel to the values from MDT of 2.08 × 1021 m−3 and 2.48 × 1021 m−3. We find that systematic errors due to undesired particle loss during extraction and statistical uncertainties due to the small APT volumes explain the differences. The size ranges of precipitates that can be detected via APT and AUC are investigated by comparison of the obtained precipitate size distributions with transmission electron microscopy analyses of carbon extraction replicas. The methods provide overlapping resulting ranges. MDT probes very large numbers of small particles but is limited by errors due to particle etching, while APT can detect particles with diameters below 10 nm but is limited by small-number statistics. The combination of APT and MDT provides comprehensive data which allows for an improved understanding of the interrelation between thermo-mechanical controlled processing parameters, precipitate number densities, and resulting mechanical-technological material properties.
