Preparation and characterization of highly <Emphasis Type="Italic">c</Emphasis>-axis textured MgO buffer layer grown on Si(100) substrate by RF magnetron sputtering for use as growth template of ferroelectric thin film

Highly c-axis textured MgO thin films were grown directly on Si(100) substrates without any buffer layer by RF magnetron sputtering for use as growth template of ferroelectric film. We fixed the target-to-substrate spacing of 40 mm and then changed the substrate temperature, deposition pressure, and RF power to study the effect of deposition parameters on the growth of c-axis textured MgO thin films. The as-grown films were post-annealed by the rapid thermal annealing (RTA) and furnace annealing to improve the film quality. The experimental results show that the optimum deposition parameters are substrate temperature of 350 °C, oxygen pressure of 15 mTorr and RF power of 75 W. The full width at half maximum intensity (FWHM) of MgO(200) peak obtained from the XRD measurement was 0.8°, and it was further reduced to 0.5° and 0.27° after annealing by RTA and furnace, respectively. Highly c-axis textured PZT and BaTiO₃ films could be obtained on this template. Hysteresis loops of the BaTiO₃ films deposited on MgO(100) single crystalline substrate and MgO(200)/Si(100) template were measured for comparison. The results show that MgO/Si templates thus obtained are suitable for the synthesis of perovskite ferroelectric thin films.     

Epitaxial YBa<Subscript>2</Subscript>Fe<Subscript>3</Subscript>O<Subscript>8</Subscript> Films Prepared by Chemical Solution Deposition Method

YBa₂Fe₃O₈(YBFO) epitaxial films are prepared on (100) SiTrO₃ single crystal substrate by polymer-assisted non-fluorine chemical solution deposition (CSD) method. The influence of firing temperature on texture degree, microstructure, and physical properties of YBFO films is systematically investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and SQUID magnetometer. YBFO film fired at 1070 °C exhibits best epitaxial quality with FWHM value of (103) phi-scan and (005) omega-scan is 0.19° and 0.45°, respectively, and highly dense and smooth morphology. A weak ferromagnetism transition was observed at 68 K in the YBFO film.     

Nanodomain and interface structure in epitaxial BaTiO<Subscript>3</Subscript> thin films on MgO deposited by magnetron sputtering

High epitaxial quality BaTiO₃ films were deposited on the MgO (001) substrate using RF magnetron sputtering at 800 °C by manipulating processing parameters. The BaTiO₃ films have a ~200 nm thickness with a very low surface roughness but a rough interface structure with respect to the substrate. The epitaxial BaTiO₃ films have a tetragonal crystal structure (a = 4.02 Å and c = 4.11 Å) with a tetragonality (c/a) of 1.02. The c-axis of the film is parallel to the growth direction as characterized by X-ray diffraction, electron diffraction, and high-resolution transmission electron microscopy. The orientation relationship between the film and the MgO is (001)_BTO//(001)_MgO and 〈100〉_BTO//〈100〉_MgO. Epitaxial nanodomains were formed in the film with a size ranging from 3 to 20 nm. The formation of the nanodomains is associated with the rough film/substrate interface due to the modification of the substrate surface characteristics (steps, terraces, and kinks) during the process. The two-dimensional interface structure between the film and the substrate was studied and its influence on the film microstructure is discussed.     

Fabrication of conductive SrRuO<Subscript>3</Subscript> thin film and Ba<Subscript>0.60</Subscript>Sr<Subscript>0.40</Subscript>TiO<Subscript>3</Subscript>/SrRuO<Subscript>3</Subscript> bilayer films on MgO substrate

Conductive SrRuO₃ (SRO) thin films have been grown on (100) MgO substrates by pulsed laser deposition (PLD) technique. Effects of oxygen pressure and deposition temperature on the orientation of SRO thin film were investigated. X-ray diffraction (XRD) θ/2θ patterns and the temperature dependent resistivity measurements indicated that oxygen pressure of 30 Pa and deposition temperature of 700 °C were the optimized deposition parameters. A parallel-plate capacitor structure was prepared with the SRO films deposited under optimized condition as an electrode layer and Ba_0.60Sr_0.40TiO₃ (BST) thin film as the dielectric layer. XRD Φ scans indicated a epitaxial relationship between BST and SRO on MgO substrate. The dielectric constant and loss tangent measured at 10 kHz and 300 K was 427 and 0.099 under 0 V bias, and 215 and 0.062 under 8 V bias, respectively. A tunability of 49.6% has been achieved with DC bias as low as 8 V. The C–V hysteresis curve and the P–E hysteresis loop suggested that the BST films epitaxially grown on SRO/MgO have ferroelectricity at room temperature. The induced ferroelectricity was believed to originate from the compressive strain between the epitaxial BST and SRO thin films. These results show the potential application of the BST/SRO heterostructures in microelectronic devices.     

Preparation of Epitaxial MgO Films Deposited by RF Magnetic Sputtering on the IBAD-MgO Substrate

We deposited epi-MgO films on the textured ion beam assisted deposition (IBAD)-MgO substrates by RF magnetic sputtering at different substrate temperatures (600–850 °C), RF powers (110–224 W) and oxygen partial pressures (19.5–58.6 mTorr). The microstructure and surface morphology of epi-MgO films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). It was found that epi-MgO films with c-axis orientation could be easily fabricated for broad parameter ranges. But the in-plane full width half maximum (FWHM) of the epi-MgO film was dependent on the parameters, and the epi-MgO film with the smallest FWHM value of 5.22° was obtained at the optimum parameters. What’s more, the GdBa₂Cu₃O₇ films deposited on the epi-MgO/IBAD-MgO substrate by RF magnetic sputtering showed c-axis orientation.     

Structure and Electrical Properties of NdBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript> Thin Films by Laser Ablation at Low Oxygen Partial Pressure

A deposition process for NdBa₂Cu₃O _y thin films by laser ablation at decreased deposition temperature was developed using substitution of oxygen with argon in the chamber during deposition. A low deposition rate is the crucial factor to obtain high-quality NBCO films. The Nd/Ba cation disorder in the film can be suppressed by an increase of the deposition temperature or by a decrease of the oxygen partial pressure during deposition. The presence of Nd/Ba disorder during deposition stimulates the introduction of oxygen into the growing film. A simple model is proposed for estimation of oxygen contents in the film using structural parameters measured with XRD techniques. Studies of the post-deposition annealing process showed ordering of the Nd/Ba sub-lattice and intense oxygen in- and out-diffusion. The temperature of the post-deposition annealing step should be chosen low enough (～400 °C) to avoid oxygen diffusion out of the NBCO film.     

Synthesis,characterization and gas sensing performance of SnO<Subscript>2</Subscript> thin films prepared by spray pyrolysis

In this work, SnO₂ thin films were deposited onto alumina substrates at 350°C by spray pyrolysis technique. The films were studied after annealing in air at temperatures 550°C, 750°C and 950°C for 30 min. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical absorption spectroscopy technique. The grain size was observed to increase with the increase in annealing temperature. Absorbance spectra were taken to examine the optical properties and bandgap energy was observed to decrease with the increase in annealing temperature. These films were tested in various gases at different operating temperatures ranging from 50–450°C. The film showed maximum sensitivity to H ₂S gas. The H₂S sensing properties of the SnO₂ films were investigated with different annealing temperatures and H ₂S gas concentrations. It was found that the annealing temperature significantly affects the sensitivity of the SnO₂ to the H ₂S. The sensitivity was found to be maximum for the film annealed at temperature 950°C at an operating temperature of 100°C. The quick response and fast recovery are the main features of this film. The effect of annealing temperature on the optical, structural, morphological and gas sensing properties of the films were studied and discussed.     

Growth and characterization of high resistivity c-axis oriented ZnO films on different substrates by RF magnetron sputtering for MEMS applications

In the present work, we report the deposition of high resistivity c-axis oriented ZnO films by RF magnetron sputtering. The deposition parameters such as RF power, target-to-substrate spacing, substrate temperature, and sputtering gas composition affect the crystallographic properties of ZnO films, which were evaluated using XRD analysis. The self-heating of the substrate in plasma during film deposition was investigated and we report that highly “c-axis oriented” ZnO thin films can be prepared on different substrates without any external heating under optimized deposition parameters. The post-deposition annealing of the film at 900 °C for 1 h in air ambient increases the intensity of (002) peak corresponding to c-axis orientation in addition with the decrease in full width at half maxima (FWHM). Bond formation of ZnO was confirmed by FTIR analysis. Grains distribution and surface roughness have been analyzed using SEM and AFM. The DC resistivity of the films prepared under different deposition conditions was measured using MIS/MIM structures and was found to be in the range of 10¹¹–10¹² Ω cm at low electric field of 10⁴ V/cm. The ZnO film of 1 μm thickness has transmittance of over 85% in the visible region. Applications of these films in MEMS devices are discussed.     

Synthesis and characterization of photosensitive TiO<Subscript>2</Subscript> nanorods by controlled precipitation route

Nanocrystalline TiO₂ thin films have been successfully synthesized by controlled precipitation route. These films are further annealed at 623 K for 2 h. The change in structural, morphological, optical, and wettability properties are studied by means of X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), scanning electron microscopy (SEM), optical absorption, and contact angle measurement. From the XRD pattern it is clear that the as-grown TiO₂ films are amorphous in nature which becomes polycrystalline after annealing. The FTIR study reveals the formation of TiO₂ compound. Scanning electron micrographs shows that the as-grown TiO₂ film consists of agglomerated nanograins well covered to the substrate surface which gets converted into vertical nanorods after annealing. As-deposited and annealed TiO₂ films showed hydrophilic behavior as water contact angles were 24° and 32°, respectively. The optical absorption study reveals the small red shift due to annealing and attributed to grain size. The annealed TiO₂ film showed conversion efficiency of 0.037% in photoelectrochemical cell with 1 M NaOH electrolyte.     

Effect of BaTiO<Subscript>3</Subscript> heat treatment on the microstructure and dielectric properties of BaTiO<Subscript>3</Subscript>-based ceramics

We have studied the effect of heat treatment of the starting BaTiO₃ powder on the dielectric properties and microstructure of X7R-type BaTiO₃-based ceramics. The results demonstrate that annealing of BaTiO₃ stabilizes the degree of tetragonality in the crystal lattice of the ceramics. Microstructural analysis shows that the annealing temperature has no effect on the average grain size of the ceramics. Increasing the BaTiO₃ annealing temperature increases the dielectric permittivity of the core phase and reduces the temperature coefficient of capacitance (TCC). We obtained an X7R-type BaTiO₃-based ceramic material (BaTiO₃ annealing temperature, 1150°C; firing temperature, 1160°C) with the following properties: ɛ_25°C = 2230, TCC = ±12% (−55 to 125°C), and tanδ_25°C = 0.013.     

Nanostructured barium titanate thin films from nanoparticles obtained by an emulsion precipitation method

Spherical non-agglomerated BaTiO₃ precursor particles of 3–5 nm size were prepared by an emulsion precipitation method that consisted of the complexation of Ba- and Ti-precursors in separate water-in-decane emulsions, followed by mixing and controlled precipitation upon reactive decomposition of tetramethyl ammonium hydroxide. Stable clear yellow dispersions with a final particle yield of ∼60% were obtained. In situ high temperature X-ray diffraction (XRD) measurements indicated that the initially amorphous particles crystallised into single-phase tetragonal BaTiO₃ at 600 °C. Thin BaTiO₃ films of 25–350 nm thickness were prepared from the precursor dispersions by spin coating or controlled deposition on Si wafers. The average crystallite size after annealing at 800 °C was approximately 26 nm, but some larger grains of 100–150 nm size were also observed. Fresnoite (Ba₂TiSi₂O₈) was likely to be formed near the interface between the oxide layer of the Si substrate and the BaTiO₃ film.     

Fabrication of biaxially textured magnesium oxide thin films by ion-beam-assisted deposition

Biaxially textured MgO thin films were grown by ion-beam-assisted deposition. The film growth parameters of film thickness, ion-to-atom arrival ratio (r-value), ion beam angle, and ion beam voltage were studied. Film characterization was performed by X-ray diffraction, pole figure analysis, and atomic force microscopy (AFM). Full-width half-maximum (FWHM) of MgO (220) ?-scans and MgO (002) ω-scans, respectively, were used to evaluate in-plane and out-of-plane film texture. MgO (220) ?-scan FWHM of 3.2° and MgO (002) ω-scan FWHM of 1.2° was achieved on amorphous Si₃N₄-coated Si substrates using a 1500-V ion source oriented at 45° to the substrate normal and an r-value of 0.90. Depositions on metallic substrates yielded MgO (220) ?-scan FWHM values of 5.2° and MgO (002) ω-scan FWHM of 2.5°. Root-mean-square surface roughness of these films as measured by AFM was ≈2.3 nm.     

Effect of substrate temperature on structural, optical and electrical properties of ZnO thin films deposited by pulsed laser deposition

ZnO thin films were grown by the pulse laser deposition (PLD) method using Si (100) substrates at various substrate temperatures. The influence of the substrate temperature on the structural, optical, and electrical properties of the ZnO thin films was investigated. All of the thin films showed c-axis growth perpendicular to the substrate surface. At a substrate temperature of 500 °C, the ZnO thin film showed the highest (002) peak with a full width at half maximum (FWHM) of 0.39°. The X-ray Photoelectron Spectroscopy (XPS) study showed that Zn was in excess irrespective of the substrate temperature and that the thin film had a nearly stoichiometrical composition at a substrate temperature of 500 °C. The photoluminescence (PL) investigation showed that the narrowest UV FWHM of 15.8 nm and the largest ratio of the UV peak to the deep-level peak of 32.9 were observed at 500 °C. Hall effect measurement systems provided information about the carrier concentration, mobility and resistivity. At a substrate temperature of 500 °C, the Hall mobility was the value of 37.4 cm²/Vs with carrier concentration of 1.36 × 10¹⁸ cm⁻³ and resistivity of 2.08 × 10⁻¹ Ω cm.     

Influence of the substrate temperature on the optical and electrical properties of Ga-doped ZnO thin films fabricated by pulsed laser deposition

Ga-doped (5 wt%) zinc oxide (GZO) thin films were fabricated on corning 1737 substrates at a fixed oxygen pressure of 200 mTorr at various substrate temperatures (100–300 °C) by using pulsed laser deposition (PLD) in order to investigate the microstructure, optical, and electrical properties of the GZO thin films. It was observed that all the thin films exhibit c-axis orientation and exhibit only a (002) diffraction peak. The GZO thin film, which was fabricated at 200 mTorr and 300 °C, showed the highest (002) orientation, and the full width at half maximum (FWHM) of the (002) diffraction peak was 0.38°. The position of the XRD peak shifted to a higher angle with increase in the substrate temperature. The optical transmittance in the visible region was greater than 85%. The Burstein-Moss effect, which causes a shift toward a high photon energy level, was observed. The electrical property indicated that the highest carrier concentration (2.33 × 10²¹ cm⁻³) and the lowest resistivity (3.72 × 10⁻⁴ Ωcm) were obtained in the GZO thin film fabricated at 200 mTorr and 300 °C.     

Chemical solution deposition of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> thin film

CaCu₃Ti₄O₁₂ (CCTO) thin film was successfully deposited on boron doped silica substrate by chemical solution deposition and rapid thermal processing. The phase and microstructure of the deposited films were studied as a function of sintering temperature, employing X-ray diffractometry and scanning electron microscopy. Dielectric properties of the films were measured at room temperature using impedance spectroscopy. Polycrystalline pure phase CCTO thin films with (220) preferential orientation was obtained at a sintering temperature of 750°C. There was a bimodal size distribution of grains. The dielectric constant and loss factor at 1 kHz obtained for a film sintered at 750°C was k ∼ 2000 and tan δ ∼ 0.05.     

Fabrication of highly c-axis textured ZnO thin films piezoelectric transducers by RF sputtering

The influence of fabrication parameters on ZnO film properties has been analyzed through conducting several experiment processes to develop an appropriate deposition condition for obtaining highly c-axis textured films. A transducer with the structure of Al/ZnO/Al/Si was fabricated at low deposition rate and under a temperature of 380 °C in a mixture of gases Ar:O₂ = 1:3, and RF power of 178 W. Pt/Ti was employed as the bottom electrode of the transducer fabricated in a suitable substrate temperature, which starts increasing at 380 °C with an increment of 20 °C for each 2 h stage of the deposition. Highly c-axis textured ZnO films have been successfully deposited on Pt/Ti/SiO₂/Si substrate under feasible conditions, including RF power of 178 W, substrate temperature of 380 °C, deposition pressure of 1.3 Pa and Ar:O₂ gas flow ratio of 50%. These conditions have been proposed and confirmed through investigating the influences of the sputtering parameters, such as substrate temperature, RF power and Ar:O₂ gas flow ratio, on the properties of ZnO films.     

Epitaxial growth of ZnO films on (100) and (001) γ-LiAlO2 substrates by pulsed laser deposition

Structural and optical properties were investigated for ZnO films grown on (100) and (001) γ-LiAlO₂ (LAO) substrates by pulsed laser deposition method. According XRD results, it is intuitionistic that (100) LAO is suitable for fabricating high quality ZnO film, while (001) LAO is unsuitable. The FWHM of XRD, stress in film and FWHM of UV PL spectra for ZnO films on (100) LAO show a decreasing with increasing substrate temperature from 300 to 600 °C. ZnO film fabricated at 600 °C has the greatest grain size, the smallest stress (0.47 Gpa) and PL FWHM value (∼85 meV). This means that the substrate temperature of 600 °C is optimum for ZnO film deposited on (100) LAO. Moreover, it was found that the UV PL spectra intensity of ZnO film is not only related to the grain size and stoichiometric, but also depends on the stress in the film.     

Dependence of Microstructure and <Emphasis Type="Italic">J</Emphasis><Subscript>c</Subscript> of YBCO Films on CeO<Subscript>2</Subscript> Cap Layers Deposited by Multi-plume PLD

In order to achieve high-performance YBa₂Cu₃O_7?x (YBCO)coated conductors (CCs) fabricated in industrial scale, it is necessary to enhance the transport properties and production speed of the CCs for use in various application forms. The transport performance of CCs depends upon the inner structure of the conductors, which make it important to analyze the microstructure and transport properties. The thickness of the buffer layer is a factor in improving speed. In this work, we deposited YBCO films on CeO₂ cap layers with different thicknesses ranging from 21 to 563 nm by multi-plume pulsed laser deposition (PLD) and investigated the dependence of the microstructure and superconducting properties of YBCO film on the thickness of CeO₂ films. The crystalline structure and surface morphology of YBCO films are systematically characterized by means of XRD, AFM, SEM and TEM. The critical current of YBCO film was measured by the conventional four-probe method at 77 K, in self-field. The results showed that the microstructure and superconducting performance of YBCO film were strongly dependent on the thickness of CeO₂ films. At the optimal CeO₂ layer thickness of 221 nm, the YBCO film exhibited a sharp in-plane and out-of-plane texture of full width at half maximum (FWHM) values of 1.5° and 2.4°, respectively, and smooth morphology of root mean square (RMS) value as low as 4.0 nm. The sharply biaxially textured YBCO films with the critical current density as high as 4.7 × 10⁶ A/cm² (77 K, in self-field) were obtained on CeO₂/MgO/Y₂O₃/Al₂O₃/C276 architecture.     

Effects of the Ar–N2 sputtering gas mixture on the preferential orientation of sputtered Ru films

We have investigated the influence of N₂ addition to the Ar sputtering gas on the crystal orientation of sputtered Ru films. An rf magnetron sputtering apparatus with a Ru target (99.9%) and a glass substrate heated to 100 °C or 300 °C was used for the deposition. The crystal structure, chemical composition and electrical properties of the resultant films were investigated. X-ray diffraction (XRD) revealed the dominant orientation at 0% N₂ to be the c-axis. With increasing proportion of N₂ in the sputtering gas at a substrate temperature of 100 °C, the intensity of the (002) peak decreased, finally disappearing at 50% N₂. This c-axis-suppressed Ru film sputtered at 50% N₂ was found to contain nitrogen by Auger electron spectroscopy (AES), but by annealing the film in vacuum at 400 °C, the nitrogen in the film was completely removed. The film orientation remained the same as before annealing. Thus, we have demonstrated a new method for depositing Ru films with a controlled preferential orientation of either c-axis oriented or c-axis suppressed.     

Rietveld analysis of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> thin films obtained by RF-sputtering

Calcium copper titanate, CaCu₃Ti₄O₁₂, CCTO, thin films with polycrystalline nature have been deposited by RF sputtering on Pt/Ti/SiO₂/Si (100) substrates at a room temperature followed by annealing at 600 °C for 2 h in a conventional furnace. The crystalline structure and the surface morphology of the films were markedly affected by the growth conditions. Rietveld analysis reveal a CCTO film with 100 % pure perovskite belonging to a space group Im3 and pseudo-cubic structure. The XPS spectroscopy reveal that the in a reducing N₂ atmosphere a lower Cu/Ca and Ti/Ca ratio were detected, while the O₂ treatment led to an excess of Cu, due to Cu segregation of the surface forming copper oxide crystals. The film present frequency -independent dielectric properties in the temperature range evaluated, which is similar to those properties obtained in single-crystal or epitaxial thin films. The room temperature dielectric constant of the 600-nm-thick CCTO films annealed at 600 °C at 1 kHz was found to be 70. The leakage current of the MFS capacitor structure was governed by the Schottky barrier conduction mechanism and the leakage current density was lower than 10^?7 A/cm² at a 1.0 V. The current–voltage measurements on MFS capacitors established good switching characteristics.