Chemical Solution Deposition of Functional Oxide Thin Films
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As an example, single crystalline anatase TiO 2 thin films have been epitaxially grown on silicon by ALD as a potential platform for memories based on resistive switching [ 44 ]. The growth of crystalline oxides on Si by combining physical and chemical methods is also a matter of current research that in the recent years has enhanced the integration of novel functional oxides with multiple applications. A new approach combining MBE and PAD has been recently introduced by the authors for the growth of integrated functional oxide thin films on silicon substrates.
PAD is a wet chemical method introduced by Jia et al. The polymer plays a significant role in the process by controlling the desired viscosity of the precursor without gelling and additionally, binding the metal ions to prevent premature precipitation and the further formation of metal-oxide oligomers. This process leads to a homogeneous distribution of the metal precursors in the solution. Polyethyleneimine PEI and its derivatives are the most frequently used polymers in PAD and metal nitrates, metal chlorides, metal acetates, or metal hydroxides are among the source of metals widely used.
As an aqueous solution system, PAD is less dependent on expensive or sensitive metalorganic precursors, thereby lowering the environmental impact, if compared to other chemical solution methods. As an example, PAD was shown to produce films of high quality and abrupt interfaces were obtained in epitaxial multilayers [ 34 , 50 ]. The strain state of the cobaltite film and its influence on the physical properties are currently under investigation. We found that the structural quality and the sharpness of the interfaces are similar in the layers grown by MBE and by PAD. Figure 3. Nanostructured surfaces are interesting in many fields as a result of their many applications including electronic devices, storage media, and as substrates for the production of more complex structures.
Notice that periodically organized mesoporous architectures exhibit unexpected electrochemical, catalytic and photo-catalytic properties.
Disentangling Epitaxial Growth Mechanisms of Solution Derived Functional Oxide Thin Films
As a result, mesoporous networks work as a connected solid network that allows fast transport of electrons, oxygen ions or protons. The construction of porous and hierarchically structured materials is accomplished by bridging together sol-gel chemistry, multiple templating, and advanced processing, namely Integrative Chemistry Strategy.
The main chemical routes and strategies in this direction have been thoroughly described in several review articles [ 51 — 53 ]. Oxide nanostructures of high quality and low aspect-ratio ratio of out-of-plane to in-plane dimensions can be obtained by self-assembly patterning methods based on CSD.
In self-assembly of oxide nanostructures, solution precursors are spin-coated on a substrate pursued by a high temperature annealing. The shape of the nanostructures and their distribution are largely determined by the misfit strain between the substrate and the functional oxide itself. The shape of the nanoislands can be stabilized by the convenient selection of the substrate's crystallographic orientation. The main improvement of these self-assembly techniques are the low costs, their simple processing, and the absence of patterning conditions.
However, to-date high quality crystalline oxides have been established only for epitaxially grown structures and the nanostructures size, shape and precise position cannot be efficiently controlled. The CSD process is so far an adaptable method that can be assembled with the use of molds or templates with high aspect ratio nanopores infiltrated with the convenient chemical precursors. This results in the fabrication of low or high aspect ratio oxide nanostructures [ 56 ].
As an example, porous Si and alumina templates as well as polymers patterned through e-beam, ion beam or photo-lithography, and block co-polymers in self-assembly have been described as successful templates [ 57 — 60 ]. Nevertheless, submicron size nanostructures in a well-defined arrangement are required for many interesting applications such as ferroelectric or ferromagnetic memory applications.
High-density ferroelectric nanostructure arrays have been fabricated using a heated AFM tip on sol-gel precursor films deposited onto platinized or plain Si substrates [ 62 ]. In addition, fully functional arrays of ferroelectric and ferromagnetic nanostructures can be prepared by electron-beam direct writing EBDW [ 63 , 64 ]. In EBDW, the chemical reactions are narrowly activated in a metallorganic thin film after irradiation with an EB under adequate energy and dose and the required pattern is impressed by scanning the EB over the sample.
The pattern is completed by dissolving the unexplored area in a precise solvent and further converted into metal oxide by thermal annealing. In the past decades, most of the works on the growth of crystalline oxide thin films on silicon have been based on a layer-by-layer approach to heteroepitaxy. The main techniques used to this purpose have been MBE or PLD after adjusting the growth conditions during the deposition to avoid silicon surface oxidation. However, such techniques cannot be used to grow integrated functional oxide nanostructures and thick films.
In the last years, CSD showed up as a versatile bottom-up approach to generate nanostructured surfaces and thicker films. In this regard, the authors recently established that the combination of soft chemistry and epitaxial growth expands opportunities for the controlled growth of functional oxide nanostructures on silicon. As an example, Carretero-Genevrier et al. In this work authors employed industrial dip-coating method to produce quartz thin films on -silicon substrates of controllable thicknesses from sol-gel precursors.
The dip-coating process was executed in four stages: i immersion of the silicon substrate inside the sol-gel solution of the coating material at a constant speed, ii deposition of the thin layer on the silicon substrate while it is pulled up at a constant speed for a good control of the thickness of the film, iii drainage of the excess liquid from the surface of the substrate; and iv evaporation of the solvent and gelification of sol-gel precursors forming the thin film.
In that case, other polymorphs of silica did not show an equal mismatch with the silicon substrate thus, preventing the stabilization of other crystalline silica phases [ 65 ]. This particular growth mechanism was coupled along with the CSD methodology to control the nanostructuration of piezoelectric quartz thin films. The piezoelectric functionality of these nanostructured films was completely preserved and no important differences between the piezoelectric force microscopy PFM response inside and outside regions of the pore were found [ 67 ].
Figure 4. Note that this growth mechanism is prepared by a dip-coating process. During the gelification and drying of films, strontium, barium or calcium ions were uniformly distributed within the amorphous silica matrix. After crystallization thin films maintain the initial porous structure achieved at room temperature. Compared to standard method of production of quartz films, top down technology based on cutting and polishing of large hydrothermally grown crystals, this bottom-up approach that produces nanostructured quartz films allows obtaining much thinner films with thicknesses between and nm.
As a consequence, quartz films obtained by this novel approach could find applications in the future in the field of electromechanical devices because thanks to its thicknesses below nm these are expected to present higher resonance frequencies. Moreover, the authors have recently evidenced that epitaxial quartz films on silicon are intrinsically chiral. In this work, a comparative evaluation of the surface energies of the two possible trapezoidal habits in the P3 1 21 and P3 2 21 quartz space groups was performed.
This work importantly opens new perspectives in the field of enantioselective surface chemistry and in the mechanisms governing crystallization of chiral pure systems [ 68 ]. Analogously, it is possible to take advantage of the catalytic devitrification process of the silica native layer at the silicon interface for the epitaxial stabilization of complex oxide nanowires on silicon as shown by Carretero-Genevrier et al. In that case, the authors used supported track etched polymeric templates as a nanoreactor for the confined growth and further stabilization of epitaxial oxide nanowires on silicon [ 69 ].
Figure 5. A FE-SEM Cross-sectional image of the porous polymer template after infiltration of nanopores with the precursor solution. Precursor nanocolumns that maintain the dimensions of the initial template nanopores are developed. These nanoparticles will act as seeds for the growth of manganate nanowires under high temperature conditions i.
In addition, the close contact of the silica native layer with the alkaline-earth metal cations present in the precursor solution during the thermal treatment assists the devitrification of the silica native layer.
Staff View: Chemical solution deposition of functional oxide thin films /
This combination has shown to be a powerful technique for structural, chemical and magnetic analysis down to the atomic scale [ 73 ]. It is worth mentioning that neither appreciable inter-diffusion of Si into the nanowires nor any trace of Sr on the quartz layer was detected by EELS studies see Figure 6.
Figure 6. Notice that both filled symbols and open symbols in the plot mean fields experimented parallel, and orthogonal to the substrate surface respectively. This finding suggests that Mn shells are less than half-filled and that the origin of ferromagnetism may reside in a double-exchange-like mechanism. The different disposition and arrangement of La and Sr cations in the new structure of the nanowires might well affect the Mn-O bonds of MnO 6 octahedra.
In addition to the solution template-based growth methodology, the authors are investigating a novel strategy for the epitaxial integration of oxides nanowires on different substrates. This new procedure consists in the use of the MBE technology to allow the metallic evaporation under atomic oxygen inside the pores of supported track etched polymer templates see Figure 7.
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The epitaxial relationship of BaTi 5 O 11 and its influence on the physical properties are currently under investigation. This finding proves once more that the confined growth of metastable phases within nanopores combined with an epitaxial growth offers interesting opportunities for the further integration of functional oxide nanowires on silicon substrates.
Figure 7. Scheme of an O-MBE setup that shows the epitaxial integration of oxides nanowires on silicon through a metallic evaporation under atomic oxygen inside the pores of a supported track etched polymer templates. Along this review we have provided an overview showing the most successful strategies used to monolithically integrate functional complex oxide thin films and nanostructures on silicon.
Importantly, the interplay of parameters such as chemical reactivity, crystallographic structure epitaxial misfit, interface, and surface energies is crucial for the nucleation and the final crystallographic phase stabilization of nanostructures. A special emphasis has been put on the combination of chemical solutions deposition methodology with physical methods MBE in order to obtain novel functional oxide heterostructures on silicon.
We have shown the power of coupling solution chemistry and epitaxial growth. This combination of physics, chemistry and processing allows nanostructured, epitaxial crystalline thin films and nanostructures. Another strategy presented in this review, is based on the controlled catalytic devitrification of the silica native layer at the silicon interface which makes possible the integration of novel functional oxide thin films and nanostructures on silicon.
In this direction, we have shown in detail the development of nanostructured piezoelectric epitaxial quartz films grown on silicon, and the epitaxial stabilization of complex oxide nanowires with enhanced magnetic properties. The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest. We thank David Montero and L. Picas for technical support. We also thank P. Regreny, C. Botella, J. Goure for technical assistance on the Nanolyon technological platform. J Appl Phys.
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