Piezoelectric Response in WO3-x Thin Films by Aluminum Clustering

doi:10.21203/rs.3.rs-384370/v1

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Piezoelectric Response in WO3-x Thin Films by Aluminum Clustering

https://doi.org/10.21203/rs.3.rs-384370/v1

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We report piezoelectric response of d₃₃ = 35 ± 5 pm V^− 1 on aluminum doped tungsten trioxide thin films (Al-WO_3 − x), prepared by RF-sputtering and post annealing treatment in air atmosphere. Using XPS characterization indicate a stoichiometry of WO_2.7 and Raman a distorted octahedral tungsten vibration mode of monoclinic WO₃ at 236.9 cm^− 1, 691 cm^− 1 and 803 cm^− 1 corresponding to O-W-O chemical bonds. The grazing incidence X-ray diffraction revealed a non-centrosymmetric monoclinic (P2₁/c) and tetragonal (P4/nmm) mixed phases of WO_3 − x with islands of piezoelectric domains as observed by atomic force microscope, additionally atom probe tomography revealed diffusion of aluminum ions from Al₂O₃ substrate.

Physical Medicine & Rehab

Materials Chemistry

tungsten trioxide

aluminum

piezoelectric

atom probe tomography

materials.

Outstanding applications in the field of Internet of Things (IoT) [1]–[3] and micro-electromechanical systems (MEMS) [4, 5] have increased the demand for environmentally friendly, low cost, and reliable materials to fabricate several types of sensors, actuators and power components [6–9]. This has expanded the interest on properties such as electrochromism and piezoelectricity in various materials [10–12]. Piezoelectric materials have gained importance in modern day technology due their wide range of applications, from positioners in electronic microscopes, crystal oscillators, sound and vibration sensors, and energy harvesting devices [13–19]. Piezoelectricity occurs mainly in non-centrosymmetric structures [20]–[23], which refers to those lacking an inversion point, i.e., a point or atom position at specific coordinates inside the Bravais unit cell, with respect to a crystallographic plane; in the spatial distribution this causes uneven distribution of electronic states and when a mechanical force is applied part of those accumulated electron charges are released, causing a piezoelectric response, as described extensively in the literature [21], [24]–[28]. Several materials can exhibit piezoelectricity to some degree, this includes ceramic materials [20], [29], polymers [23, 24] and semiconductors [31], with lead zirconate titanate, also known as PZT, is one of most common piezoelectric ceramics as reported in the literature, with remarkable piezoelectric response derived from interaction at morphotropic phase boundary (MPB) [25]. Sustainable environmental concerns and also that it is an insulator [27, 28] has caused an intensified on-going research worldwide in search for lead-free conducting piezoelectric materials [27, 29, 30], and previous investigations in the materials field indicate that piezoelectric semiconductors are potential candidates due to intrinsic piezoelectricity and conductivity [36]. Also, some binary compounds such as ZnO and AlN, have been considered attractive piezoelectric materials and currently are under extensive research [25, 32], some reports indicates addition of ZnO or WO₃ as dopants in PZT or in BaTiO₃–SrTiO₃ ceramics can induce piezo-response [33–36]. Recently, Chen et al. successfully used ZnO-WO_3 − x nanorods for piezoelectric-photoelectrochemical water splitting due to intrinsic ZnO piezoelectricity and the fact that WO_3 − x charge carrier concentration can be tuned in function of oxygen vacancies [42]. Corby et al. found that vacancy concentration of 2% for stoichiometric oxides meaning oxygen concentration, can maximize photocurrent in water splitting performance [43], similar to the results reported by Soltani et al. [44]. Kim et al. reported piezoelectric response in an oxygen-deficient WO_2.96 film with a d₃₃ coefficient of 7.9 pm/V, attributed to the non-centrosymmetric structures within film thickness, that corresponds to monoclinic and tetragonal phases [45]. In this communication, we are reporting piezoelectric response for aluminum doped WO₃ thin films annealed at 400°C, along with extensive characterization by grazing incidence X-ray diffraction (GIXRD) and atom probe tomography (APT).

Piezoelectric response by PFM

WO₃ thin films were deposited on sapphire with a resulting thickness of 225 nm and subsequently annealed at various temperatures, see experimental methods section. A piezoelectric response was found in the film annealed at 400°C, determined by characterization using piezo force microscopy technique in dual AC resonance tracking (DART) mode, as described extensively in [22, 26–28, 46, 47]. The surface topography of this film is shown in Fig. 1a, and Fig. 1b) and 1c) corresponds to the piezo force microscopy signal phase before and after measurements, revealing a local hysteresis loops; hysteresis loops corresponding to red circles, where piezo response domains appear as yellow, white and violet colored regions show polarization direction piezoelectric domains, as described by Kholkin et al. [27]. The white regions are positive domains, i.e., polarization pointing towards the bottom electrode, which occurred by switching domains as observed in hysteresis loops shown in Fig. 1e. Furthermore, ferroelectric behavior was observed in the sample annealed at 400°C from hysteresis loops in phase and piezoelectric coefficient (d₃₃) versus AC applied bias voltage as shown in Fig. 1f. The piezoelectric coefficient was determined by positioning the cantilever across a large grain of Al-WO_3 − x (red circle). The amplitude (nm) versus AC bias voltage (V) exhibited a butterfly loop as presented in Fig. 1d and it is related to piezoelectric deformation under an applied AC bias voltage demonstrating a local polarization switching behavior [28]. The latter indicates that a phase difference of 180° polarization switching under DC bias voltage related to the existence of piezoelectric domains and local d₃₃ coefficient can be estimated by (V-V₁)d₃₃ = D-D₁, where D is the measured piezoelectric deformation or amplitude, V is applied voltage, D₁ is the piezoelectric deformation, and V₁ is the applied voltage at the intersection as described by Roelofs et al. [28]. The coercive voltage (2.7 V) was evaluated using the equation (V_c⁺-V_c⁻)/2 where V_c⁺ and V_c⁻ are the forward and reverse coercive bias voltages, respectively. The piezoelectric coefficient (d₃₃) of 35 ± 5 pmV^− 1 was measured at the maximum voltage of 10 V for the film annealed at 400°C, which is four times higher than that reported by Kim et al. [45] for WO_2.9 and the highest value found in the literature for this material, indicating a potential use in piezoelectric devices [48].

The measured d₃₃ coefficient is assume to occur due to non-centrosymmetric phases in combination with potential oxygen vacancies and aluminum doping induced a different stoichiometric composition of WO_3 − x films, mainly for those processed at 400°C in agreement with reports as found in the literature [38, 48–57]. And confirmed by XPS measurements (Supplemental material) which reveals a stoichiometry of WO_2.7 in the surface of the film annealed at 400°C and in agreement with grazing incidence x-ray diffraction (GIXRD) and atom probe tomography (APT) as presented in this communication.

Crystallographic structure as determined by GIXRD

As presented in Fig. 2, an evolution of crystallinity occurred on the films from room temperature to annealing process at 400°C and 550 ºC corresponding to polycrystalline amorphous structure, reflections at 23.1° corresponds to (001), (021) and (121) and corresponds to monoclinic WO_3 − x phase (γ-WO_3 − x) [57], [59]–[61] with space group P2₁/c, a tetragonal WO_3 − x phase (α-WO_3 − x) with P4/nmmspace group is formed for sample at 400°C in agreement with literature [61, 62]. The Raman spectra indicate a distorted octahedral tungsten vibration mode of monoclinic WO_3 − x at 236.9 cm^− 1, 691 cm^− 1 and 803 cm^− 1 attributed to bending O-W-O bonds and symmetric/antisymmetric stretching of W-O bonds (see supplemental material). However, as the annealing temperature increased and evolution of phases occurred with γ-WO_3 − x or α-WO_3 − x for 500°C and 550°C, respectively as observed. Furthermore, diffractions at ~ 37º which corresponds to (111) planes of metallic aluminum (FCC), only appear at 400°C and not at 500°C and 550°C, our believe is that aluminum clusters is formed by interdiffusion from sapphire substrates (Al₂O₃) during annealing process, in agreement with Li et al. oxygen vacancies can promote defects and dislocation; and potentially can induce diffusion of aluminum ions on lattice sites within WO₃ [64]; because critical temperature of aluminum diffusion is reached at above 300°C in agreement with previous reports, and revealed by atom probe tomography, Fig. 3. Thus, segregated aluminum induces formation of mixed α-WO_3 − x and γ-WO_3 − x phases in agreement with previous reports [52], [65]; as it is described usually heavy metallic ions like induces recrystallization in thin films [66]. Also, metallic species such as gold (Au) induces phase change from triclinic to monoclinic in WO₃ [67]. In here, we were able to determine that aluminum is diffused creating changes on the electronic states mainly on island form over film and mixed monoclinic and tetragonal (α-WO_3 − x and γ-WO_3 − x) specially when is processed at 400°C, in agreement with Ahart et al. [25] and Ibrahim et al. [68] who explained in detail that mixed phases can produce a morphotropic phase boundary (MPB).

Chemical distribution by atom probe tomography

In order to investigate chemical volume distribution a series of atom probe tomography characterizations were completed, which is an abrasive technique used to obtain time of flight mass spectrometry from events occurred due to laser pulse ionic evaporation at high-vacuum as described in the literature [69], for all APT measurements a well-defined interface between WO₃ film and Al₂O₃ substrate was revealed. From mass spectrum it was possible to achieve chemical composition distribution mainly at the WO₃ film thickness (0-400nm) and traces of aluminum, oxygen and tungsten was found as shown in Fig. 3. Tungsten concentration remains around 27% during annealing process and oxygen concentration is about 70% at 400 ºC with strong traces of aluminum (~ 3%) which forms clusters, as shown in Fig. 3a; it is our believe this clusters are formed during annealing process by ionic diffusion from sapphire substrate due to voids occurred by oxygen vacancies which allowed aluminum ions to undergo onto WO₃ [56], [65], which is in agreement with mixed phases as encountered by grazing incidence x-ray diffraction. For sample processed at 500°C lower concentration (> 1%) of aluminum ions is found and corresponds mainly to α-WO_3 − x as shown in Fig. 3b and no traces of grain boundaries was found for all samples.

We report a piezoelectric response with d₃₃ = 35 ± 5 p/V for Al-WO_3 − x in thin films processed at 400°C. The grazing incidence x-ray and atom probe indicates that piezo-response effect is caused by aluminum diffusion creating mixed phase between γ-WO_3 − x (monoclinic) and α-WO_3 − x (tetragonal) corresponding to a non-centrosymmetric. And we found that at elevated annealing temperatures (> 400°C) film recrystallizes in α-WO_3 − x followed by γ-WO_3 − x causing a reorder to piezoelectric domains, as confirmed by atom probe tomography where no clustering of aluminum was encountered for sample processed at 500°C.

RF magnetron sputtering

The tungsten trioxide (WO₃) thin films were deposited by radio frequency magnetron sputtering technique using a 99.99% pure WO₃disk as target and Al₂O₃ as substrate. The base pressure was set up to 1×10^-6 Torr before allowing Ar into the chamber as plasma source. The deposition rate was 1 Å/s, at a working pressure of 3 mTorr and 225 W of RF power. The wafer was cut into several samples for subsequent annealing process at temperatures of 300 ˚C, 400 ˚C, 500 ˚C and 550 ˚C, for 45 min with a 15 min ramp down, in air. A film thickness of ~220 nm was measured for the as-deposited film using profilometry.

Piezo Force Microscopy (PFM)

Domain imaging, switching and piezoelectric hysteresis loops were investigated by piezoresponse force microscopy (PFM) using the Dual AC Resonance Tracking (DART) mode, in a commercial Atomic Force Microscope (AFM) model Infinity 3D Asylum Research with two internal lock-ins amplifiers. The PFM was operated in vertical mode with an AC voltage amplitude of 5 V_pk-pk and at a drive frequency of 398 kHz far below the resonance of the cantilever, applied between the bottom electrode and the Pt/Ir conductive tip during imaging PFM. To achieve the measurement of local polarization (hysteresis loops) a voltage of -10 to 10 V_pk-pk was applied using the spectroscopy PFM mode.

Grazing Incidence X-Ray Diffraction (XRD)

Crystallographic structure was obtained with the aid of Panalytical Empyrean system, with Cu_Kα radiation source (λ=1.54 Å) at an operating accelerating voltage of 40 kV and an emission current of 30 mA. Scanning angle was varied from 20˚ to 80˚ with a step size of 0.05˚.

Atom Probe Tomography (APT)

Three-dimensional chemical distribution for W, O and Al was obtained with a Cameca® LEAP 4000X high-resolution system, equipped with a UV laser (λ ∼ 355 nm). All measurements were taken at a set temperature of 50 K with an evaporation rate of 0.2 and a laser frequency of 100 kHz. The laser beam was set to 20 pJ/V, and all data were reconstructed from SEM images using the Cameca IVAS© 3.6.14 package. Additional samples were prepared by directly coating the micro tip coupons provided by the CAMECA with the multilayer sputtering system. The samples were prepared by annular milling with the aid of the focused ion-beam (FIB) instrument models FEI© Strata or Zeiss Auriga, both equipped with dual beam. The surface was protected with an additional platinum layer deposited from a precursor gas within the SEM-FIBs to reduce amorphization of film matrix.

Authors Contribution

P.M.P.D, M.R., J.N. and O.A.L.G. completed all sample preparation at Center for Integrated Nanotechnologies-Albuquerque, NM. J.L.E.C. and P.M.P.D. performed the Raman measurements. T.B. and M.H. performed atom probe tomography characterization at Karlsruhe Nano and Micro Facility. A. H.M. mesure piezo-electric properties at Centro de Investigación en Materiales Avanzados-Chihuahua. J. L. and Y. G. performed XPS measurements at University of Texas at El Paso. Data analysis was completed by P.M.P.D., H.C. and O.A.L. G.; and manuscript was mainly typed by P.M. P.D., O. A. L.G., J.L.E.C., M.H. and M.R.

Acknowledgments

Authors thank: Center for Integrated Nanotechnologies, an Office of Science User Facility operated for the U.S. Department of Energy (DOE) Office of Science. Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-AC04-94AL85000 under external user proposal #2018AU0133. We are grateful to the Karlsruhe Micro and Nano Facility (KNMF) of Karlsruhe Institute of Technology for usage of Atom Probe Tomography and FIB instruments and to IAM-WK of Karlsruhe Institute of Technology. The Laboratorio Nacional de Nanotecnología of Centro de Investigación en Materiales Avanzados (CIMAV-Chihuahua) for the usage of electron microscopy and characterization equipment. P. Pineda-Domínguez and M. Ramos thank Dirección General de Vinculación e Intercambio of Universidad Autónoma de Ciudad Juárez for travel award support and Instituto de Ingeniería y Tecnología of UACJ. Pineda-Domínguez thank the graduate scholarship sponsor program of Consejo Nacional de Ciencia y Tecnología-México, scholarship number 956889.

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Piezoelectric Response in WO3-x Thin Films by Aluminum Clustering

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