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Register a new userThe role of etching anisotropy in the fabrication of freestanding oxide microstructures on SrTiO3(100), SrTiO3(110), and SrTiO3(111) substrates
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The release process for the fabrication of freestanding oxide microstructures relies on appropriate, controllable and repeatable wet etching procedures. SrTiO3 is among the most employed substrates for oxide thin films growth and can be decomposed in HF:water solution. Such process is strongly anisotropic and is affected by local defects and substrate cut-plane. We analyze the etching behavior of SrTiO3 substrates having (100), (110), and (111) cut-planes during immersion in a 5% HF:water solution. The etching process over the three substrates is compared in terms of pitting, anisotropy, macroscopic etch rate and underetching effects around HF-resistant (La,Sr)MnO3 thin film micropatterns. The release of targeted structures, such as the reported (La,Sr)MnO3 freestanding microbridges, depends on the substrate crystallographic symmetry and on the in-plane orientation of the structures themselves along the planar directions. By comparing the etching evolution at two different length scales, we distinguish two regimes for the propagation of the etching front: an intrinsic one, owning to a specific lattice direction, and a macroscopic one, resulting from the mixing of different etching fronts. We report the morphologies of the etched SrTiO3 surfaces and the geometries of the underetched regions as well as of the microbridge clamping zones. The reported analysis will enable the design of complex MEMS devices by allowing to model the evolution of the etching process required for the release of arbitrary structures made of oxide thin films deposited on top of STO.
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In recent years, striking discoveries have revealed that two-dimensional electron liquids (2DEL) confined at the interface between oxide band-insulators can be engineered to display a high mobility transport. The recognition that only few interfaces appear to suit hosting 2DEL is intriguing and challenges the understanding of these emerging properties not existing in bulk. Indeed, only the neutral TiO2 surface of (001)SrTiO3 has been shown to sustain 2DEL. We show that this restriction can be surpassed: (110) and (111) surfaces of SrTiO3 interfaced with epitaxial LaAlO3 layers, above a critical thickness, display 2DEL transport with mobilities similar to those of (001)SrTiO3. Moreover we show that epitaxial interfaces are not a prerequisite: conducting (110) interfaces with amorphous LaAlO3 and other oxides can also be prepared. These findings open a new perspective both for materials research and for elucidating the ultimate microscopic mechanism of carrier doping.
We analyze the basic structural units of simple reconstructions of the (111) surface of SrTiO3 using density functional calculations. The prime focus is to answer three questions: what is the most appropriate functional to use; how accurate are the energies; what are the dominant low-energy structures and where do they lie on the surface phase diagram. Using test calculations of representative small molecules we compare conventional GGA with higher-order methods such as the TPSS meta-GGA and on-site hybrid methods PBE0 and TPSSh, the later being the most accurate. There are large effects due to reduction of the metal d oxygen sp hybridization when using the hybrid methods which are equivalent to a dynamical GGA+U, which leads to rather substantial improvements in the atomization energies of simple calibration molecules, even though the d-electron density for titanium compounds is rather small. By comparing the errors of the different methods we are able to generate an estimate of the theoretical error, which is about 0.25eV per 1x1 unit cell, with changes of 0.5-1.0 eV per 1x1 cell with the more accurate method relative to conventional GGA. An analysis of the plausible structures reveals an unusual low-energy TiO2-rich configuration with an unexpected distorted trigonal biprismatic structure. This structure can act as a template for layers of either TiO or Ti2O3, consistent with experimental results as well as, in principle, Magnelli phases. The results also suggest that both the fracture surface and the stoichiometric SrTiO3 (111) surface should spontaneously disproportionate into SrO and TiO2 rich domains, and show that there are still surprises to be found for polar oxide surfaces.
The evolution of the atomic structure of LaAlO3 grown on SrTiO3 was investigated using surface x-ray diffraction in conjunction with model-independent, phase-retrieval algorithms between two and five monolayers film thickness. A depolarizing buckling is observed between cation and oxygen positions in response to the electric field of polar LaAlO3, which decreases with increasing film thickness. We explain this in terms of competition between elastic strain energy, electrostatic energy, and electronic reconstructions. The findings are qualitatively reproduced by density-functional theory calculations. Significant cationic intermixing across the interface extends approximately three monolayers for all film thicknesses. The interfaces of films thinner than four monolayers therefore extend to the surface, which might affect conductivity.
We report the existence of confined electronic states at the (110) and (111) surfaces of SrTiO3. Using angle-resolved photoemission spectroscopy, we find that the corresponding Fermi surfaces, subband masses, and orbital ordering are different from the ones at the (001) surface of SrTiO3. This occurs because the crystallographic symmetries of the surface and sub-surface planes, and the electron effective masses along the confinement direction, influence the symmetry of the electronic structure and the orbital ordering of the t2g manifold. Remarkably, our analysis of the data also reveals that the carrier concentration and thickness are similar for all three surface orientations, despite their different polarities. The orientational tuning of the microscopic properties of two-dimensional electron states at the surface of SrTiO3 echoes the tailoring of macroscopic (e.g. transport) properties reported recently in LaAlO3/SrTiO3 (110) and (111) interfaces, and is promising for searching new types of 2D electronic states in correlated-electron oxides.
The crystal structures of LaAlO3 films grown by pulsed laser deposition on SrTiO3 substrates at oxygen pressure of 10-3 mbar or 10-5 mbar, where kinetics of ablated species hardly depend on oxygen background pressure, are compared. Our results show that the interface between LaAlO3 and SrTiO3 is sharper when the oxygen pressure is lower. Over time, the formation of various crystalline phases is observed while the crystalline thickness of the LaAlO3 layer remains unchanged. X-ray scattering as well as atomic force microscopy measurements indicate three-dimensional growth of such phases, which appear to be fed from an amorphous capping layer present in as-grown samples.
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