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Ferroelectric Properties of Ion-Irradiated Bismuth Ferrite Layers Grown Via Molecular- Beam Epitaxy

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Ferroelectric Properties of Ion-Irradiated Bismuth Ferrite Layers Grown Via Molecular- Beam Epitaxy Ferroelectric properties of ion-irradiated bismuth ferrite layers grown via molecular- beam epitaxy Cite as: APL Mater. 7, 111101 (2019); https://doi.org/10.1063/1.5125809 Submitted: 27 August 2019 . Accepted: 10 October 2019 . Published Online: 01 November 2019 Antonio B. Mei , Sahar Saremi , Ludi Miao , Matthew Barone, Yongjian Tang , Cyrus Zeledon, Jürgen Schubert , Daniel C. Ralph, Lane W. Martin , and Darrell G. Schlom ARTICLES YOU MAY BE INTERESTED IN Self-assembly and properties of domain walls in BiFeO3 layers grown via molecular-beam epitaxy APL Materials 7, 071101 (2019); https://doi.org/10.1063/1.5103244 Photovoltaic, photo-impedance, and photo-capacitance effects of the flexible (111) BiFeO3 film Applied Physics Letters 115, 112902 (2019); https://doi.org/10.1063/1.5120484 Improved optoelectronic properties in solution-processed epitaxial rare-earth-doped BaSnO3 thin films via grain size engineering Applied Physics Letters 115, 162105 (2019); https://doi.org/10.1063/1.5115526 APL Mater. 7, 111101 (2019); https://doi.org/10.1063/1.5125809 7, 111101 © 2019 Author(s). APL Materials ARTICLE scitation.org/journal/apm Ferroelectric properties of ion-irradiated bismuth ferrite layers grown via molecular-beam epitaxy Cite as: APL Mater. 7, 111101 (2019); doi: 10.1063/1.5125809 Submitted: 27 August 2019 • Accepted: 10 October 2019 • Published Online: 1 November 2019 Antonio B. Mei,1,a) Sahar Saremi,2 Ludi Miao,3 Matthew Barone,1 Yongjian Tang,4 Cyrus Zeledon,1 Jürgen Schubert,5 Daniel C. Ralph,4,6 Lane W. Martin,2,7 and Darrell G. Schlom1,6 AFFILIATIONS 1 Department of Materials Science and Engineering, Cornell University, Ithaca, New York 14853, USA 2Department of Materials Science and Engineering, University of California, Berkeley, Berkeley, California 94720, USA 3Laboratory of Atomic and Solid State Physics, Cornell University, Ithaca, New York 14853, USA 4Physics Department, Cornell University, Ithaca, New York 14853, USA 5Peter Grünberg Institute (PGI-9) and JARA-Fundamentals of Future Information Technology, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany 6Kavli Institute at Cornell for Nanoscale Science, Ithaca, New York 14853, USA 7Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720, USA a)[email protected] ABSTRACT We systematically investigate the role of defects, introduced by varying synthesis conditions and by carrying out ion irradiation treat- ments, on the structural and ferroelectric properties of commensurately strained bismuth ferrite BixFe2−xO3 layers grown on SrRuO3-coated DyScO3(110)o substrates using adsorption-controlled ozone molecular-beam epitaxy. Our findings highlight ion irradiation as an effective approach for reducing through-layer electrical leakage, a necessary condition for the development of reliable ferroelectrics-based electronics. © 2019 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). https://doi.org/10.1063/1.5125809., s I. INTRODUCTION composition, structure, and ferroelectric properties of epitax- ial BixFe2−xO3 layers grown via adsorption-controlled ozone BiFeO3 crystalizes in a rhombohedrally distorted perovskite molecular-beam epitaxy. Structural characterization reveals that sto- structure (space group #161, R3c) and exhibits the combination of ichiometric films, for which bismuth and iron concentrations are ferroelectricity and spin-canted weak ferromagnetism.1–3 At room equal (i.e., x ≈ 1.00), exhibit the highest crystalline and ferroelec- temperature, the polar and magnetic order parameters are cou- tric domain perfection. The leakage characteristics of these high- pled. As a result, when ferroelectric domains are poled, magnetic quality layers are found to be similar to defective layers grown near moments reorient deterministically.2,4,5 Voltage-controlled mag- the single-phase field boundaries (i.e., x ≠ 1.00). Through film leak- netism is important for enabling low-power spintronic devices that age is dramatically reduced by irradiating both stoichiometric and operate efficiently and independently of current-based switching nonstoichiometric samples with He+ ions. mechanisms, including Oersted induction and spin-transfer torque.6 Utilizing BiFeO for practical voltage-controlled spintronics, how- 3 II. FILM GROWTH ever, requires overcoming reliability challenges currently limiting 7 ferroelectric-based devices. Key among these is reducing through- BixFe2−xO3 layers are grown to a thickness of ≃200 nm on 8–10 film leakage. SrRuO3-coated (110)o-oriented DyScO3 substrates (o subscripts In this letter, we investigate the influence of growth con- denote orthorhombic indices in the nonstandard Pbnm setting) via ditions and postdeposition ion-irradiation treatments on the adsorption-controlled molecular-beam epitaxy in a Veeco GEN10 APL Mater. 7, 111101 (2019); doi: 10.1063/1.5125809 7, 111101-1 © Author(s) 2019 APL Materials ARTICLE scitation.org/journal/apm −8 −6 system (base pressure PBase = 1 × 10 Torr = 1.3 × 10 Pa). SrRuO3 is selected as an epitaxial bottom electrode11 due to its relatively low electrical resistivity (170 μΩ-cm at room temperature)12 and lattice match with the DyScO3 substrate (lattice mismatch m = 0.6%). The SrRuO3 electrodes are deposited as described in Refs. 12 and 13 to thicknesses of ≃20 nm. BixFe2−xO3 films are grown subsequently ○ without breaking vacuum at growth temperatures Ts between 550 C and 650 ○C, estimated using a thermocouple in indirect contact with the growth surface. Iron (99.995% pure) and bismuth (99.9999% pure) are simulta- neously14 supplied to the growth surface from effusion cells oper- ating at temperatures near 1250 ○C and 650 ○C, respectively. Iron 13 −2 −1 fluxes are fixed at JFe = 2.4 × 10 cm s , yielding bismuth ferrite deposition rates of 1.1 nm/min; bismuth fluxes are varied 13 −2 −1 13 −2 −1 between JBi = 4.8 × 10 cm s and 38.4 × 10 cm s , cor- responding to JBi/JFe flux ratios spanning 2 through 16. High bis- muth fluxesJ ( Bi/JFe ≫ 1) promote the incorporation of bismuth into the growing film, compensating for the desorption of volatile 15 BiOx species. Elemental oxygen is supplied via atmospheric mixtures consist- FIG. 1. Composition and structure of epitaxial BixFe2−xO3/SrRuO3/DyScO3(110)o ing of 20% O2 and 80% O3. The deposition pressure is maintained heterostructures. (a) Variability chart showing film bismuth fractions x vs incident −5 −3 16,17 at 1 × 10 Torr (1.3 × 10 Pa), corresponding to an equivalent metal flux ratios JBi/JFe and deposition temperatures Ts. The broken lines connect 16 −2 −1 18,12,19 ozone flux of JO3 ≈ 10 cm s . The use of strong oxidants points grown at the same temperature Ts. Diffuse and coherent labels refer to RSM peak shapes [see the inset in (b)]. (b) JBi/JFe vs Ts parameter space governing and high ozone fluxesJ ( O3 /JFe ≈ 500) suppress the formation of oxygen vacancies, which engender mobile electrons.20 the adsorption-controlled growth of BixFe2−xO3 layers via ozone molecular-beam epitaxy. White regions denote phase-pure layers; blue and red areas indicate mixed-phase films with2 Fe O3 and Bi2O2.5 inclusions, respectively; striped (non- A. Structure and composition striped) regions identify regimes where RSMs carried out about BixFe2−xO3 002p reflections (inset) display diffuse (coherent) peak shapes. The dimensions ofthe −2 Initial film growth experiments focus on determining the RSMs are 0.08 × 0.13 nm . (c) XRD θ-2θ diffracted intensities near 002p film and effects of incident flux ratios 2 ≤ JBi/JFe ≤ 16 and deposition tem- substrate reflections fromx Bi Fe2−xO3 layers. (d) Corresponding film out-of-plane ○ ○ lattice parameters a vs bismuth fractions x. peratures 550 C ≤ Ts ≤ 650 C on the composition and structure of the BixFe2−xO3 layers grown on SrRuO3/DyScO3(110)o. Figure 1(a) is a variability chart21 showing film bismuth fractions x determined from BixFe2−xO3 layers using Rutherford deposition temperatures and bismuth fluxes, the fundamental film 22–24 backscattering spectrometry. Measured x values span 0.90 reflections display diffuse features; at higher T and J /J values, ○ ○ s Bi Fe (JBi/JFe = 4, Ts = 650 C) through 1.05 (JBi/JFe = 16, Ts = 600 C). the peaks exhibit coherent profiles. In the remainder of this letter, Increasing Ts and reducing JBi/JFe result in lower film bismuth fac- we focus on the latter set of films, for which the structural quality is ○ tions x; in particular, we find that a 50 C increase in Ts has an effect superior. on x equivalent to a two-fold reduction in JBi/JFe. The loss of bis- Figure 1(c) shows diffracted θ-2θ x-ray intensities collected muth at higher temperatures results from thermally activated BiOx near 002 film and substrate peaks from Bi Fe O layers (p sub- 25–27 p x 2−x 3 desorption. scripts denotes pseudocubic indices) grown along the isoflux JBi/JFe ○ The phase composition and structural perfection of as- = 16 and isotherm Ts = 650 C lines. As the film bismuth frac- deposited films are investigated using x-ray diffraction (XRD) θ-2θ tion x is increased, film reflections shift to slightlyθ lower2 values, scans and reciprocal space maps (RSM). The findings are summa- resulting in out-of-plane lattice parameter values a which grow 29 rized as a function of incident metal flux ratios JBi/JFe and deposi- linearly with composition x [Fig. 1(d)]. The variation in a val- tion temperatures Ts in Fig. 1(b). Three structurally distinct growth ues suggests a changing
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