We report on the use of an atmospheric pressure, open-air plasma treatment to remove Li2CO3 species from the surface of garnet-type tantalum-doped lithium lanthanum zirconium oxide (Li6.4La3Zr1.4Ta0.6O12, LLZTO) solid-state electrolyte pellets. The Li2CO3 layer, which we show forms on the surface of garnets within 3 min of exposure to ambient moisture and CO2, increases the interface (surface) resistance of LLZTO. The plasma treatment is carried out entirely in ambient and is enabled by use of a custom-built metal shroud that is placed around the plasma nozzle to prevent moisture and CO2 from reacting with the sample. After the plasma treatment, N2 compressed gas is flowed through the shroud to cool the sample and prevent atmospheric species from reacting with the LLZTO. We demonstrate that this approach is effective for removing the Li2CO3 from the surface of LLZTO. The surface chemistry is characterized with X-ray photoelectron spectroscopy to evaluate the effect of process parameters (plasma exposure time and shroud gas chemistry) on removal of the surface species. We also show that the open-air plasma treatment can significantly reduce the interface resistance. This platform demonstrates a path towards open-air processed solid-state batteries.
1 December 2014 in Journal of Magnesium and Alloys
Direct electroless Ni–P plating was done on AZ91D magnesium alloy by immersing magnesium AZ91D samples into a bath containing Nickel sulphate. The nucleation mechanism of Ni–P deposits on the AZ91D magnesium alloy in the presence of surfactants and nano-additives was studied by using SEM. The electroless Ni–P deposits were preferentially nucleated on the βMg17Al12 phase of AZ91D magnesium alloy. Ni–P coating was coated uniformly in the presence of surfactants. Effect of surfactant C-Tab with varying quantities was studied. Addition of surfactant C-Tab homogenized the Ni–P deposition on AZ91D magnesium alloy surface. The effect produced by surfactant C-Tab was maximum with minimum addition (1 g/l) of surfactant C-Tab further increase in the surfactant C-Tab quantity did not brought much changes in morphology. Effect of surfactant SLS was studied using SEM. Surfactant SLS when incorporated in small amounts (6 g/l and 12 g/l) only exerted a slight influence in Ni–P deposition on AZ91D alloy surface. However Ni–P deposition was more uniform and spread throughout the surface with the addition of SLS surfactant (18 g/l). Effect of nano additives Al2O3, ZnO, SiO2 were studied. Nano additive Al2O3 enhanced the deposition of Ni–P on AZ91D alloy when added in 0.6 g/l quantity. SiO2 addition also gave the same results. ZnO addition influenced the Ni–P deposition on AZ91D alloy positively. Ni–P surface coating was coated more uniform and spread throughout the surface with the addition of surfactants and nano-additives
1 July 2019 in Journal of Vacuum Science & Technology A
Wafer bonding can be substituted for heteroepitaxy when manufacturing specific heterojunction-based devices. Devices manufactured using wafer bonding include multijunction solar cells, integrated sensors, heterogeneously integrated photonic devices on Si (such as high-performance laser diodes), Mach-Zehnder modulators, photodetectors, optical filters, and surface acoustic wave devices. In these devices, creating heterointerfaces between different semiconductors with heavily mismatched lattice constants and/or significant thermal expansion mismatch presents significant challenges for heteroepitaxial growth. High costs and poor yields in heavily mismatched heteroepitaxy can be addressed by wafer bonding in these optoelectronic devices and sensors, including the LiTaO3/Si and LiTaO3/SiO2 heterostructures. In the present work, heterostructure formation between piezoelectric LiTaO3 (100) and Si (100) and α-quartz SiO2 (100) is investigated via wafer bonding. Direct bonding is selected instead of heteroepitaxy due to a significant thermal expansion mismatch between LiTaO3 and Si-based materials. The coefficient of thermal expansion (CTE) of LiTaO3 is 18.3 × 10−6/K. This is 1 order of magnitude larger than the CTE for Si, 2.6–2.77 × 10−6/K and 25–30 times larger than the CTE for fused SiO2 and quartz (which ranges 0.54–0.76 × 10−6/K). Thus, even at 200 °C, a 4 in. LiTaO3/Si bonded pair would delaminate with LiTaO3 expanding 300 μm in length while Si would expand only by 40 μm. Therefore, direct wafer bonding of LiTaO3/Si and LiTaO3/SiO2 is investigated with low temperature (T < 500 K) Nano-Bonding™, which uses surface energy engineering (SEE). SEE is guided by fast, high statistics surface energy measurements using three liquid contact angle analysis, the van Oss/van Oss–Chaudhury–Good theory, and a new, fast Drop Reflection Operative Program analysis algorithm. Bonding hydrophobic LiTaO3 to hydrophilic Si or SiO2 is found to be more effective than hydrophilic LiTaO3 to hydrophobic Si or SiO2 temperatures for processing LiTaO3 are limited by thermal decomposition LiTaO3 into Ta2O5 at T ≥ 180 °C due to Li out-diffusion as much as by LiTaO3 fractures due to thermal mismatch.
State-of-the-art solid-state electrolytes (SSEs) are limited in their energy density and processability based on thick, brittle pellets, which are generally hot pressed in vacuum over the course of several hours. We report on a high-throughput, open-air process for printable thin-film ceramic SSEs in a remarkable one-minute time frame using a lithium lanthanum titanium oxide (LLTO)-based SSE that we refer to as robust LLTO (R-LLTO). Powder XRD analysis revealed that the main phase of R-LLTO is polycrystalline LLTO, accompanied by selectively retained crystalline precursor phases. R-LLTO is highly dense and closely matched to the stoichiometry of LLTO with some heterogeneity throughout the film. A minimal presence of lithium carbonate is identified despite processing fully in ambient conditions. The LLTO films exhibit remarkable mechanical properties, demonstrating both flexibility with a low modulus of ∼35 GPa and a high fracture toughness of >2.0 . We attribute this mechanical robustness to several factors, including grain boundary strengthening, the presence of precursor crystalline phases, and a decrease in crystallinity or ordering caused by ultrafast processing. The creation of R-LLTO-a ceramic material with elastic properties that are closer to polymers with higher fracture toughness-enables new possibilities for the design of robust solid-state batteries.
21 August 2019 in Journal of 3D Printing in Medicine
The current approach of modifying standardized prosthetics for orthopedic, dental and maxillofacial implants made from conventional manufacturing techniques have been found inconvenient to customiz...