Improved barium fluoride process YBa2Cu3)7-x films via post-anneal monitoring

The continuous monitoring of the conversion, of Y, Cu and BaF₂ precursors to form superconductor thin films has been achieved using a fluorine-specific-ion electrode immersed in an effluent gas-washing cell. High-quality thin films of YBa₂Cu₃O_7-x deposited on NdGaO₃, LaA10₃ and LaGaO₃, have been produced by limiting the wet oxygen annealing phase of the post-deposition anneal. When the films were over-annealed in humidified oxygen the superconducting transition temperature as measured by inductive methods and the crystal quality, determined by x-ray rocking curves were degraded.     

Influence of La substitution on the electrical properties of metal-ferroelectric (BiFeO3)-insulator (CeO2)-semiconductor nonvolatile memory structures

Metal-multiferroic (La-substituted BiFeO₃)-insulator (CeO₂)-semiconductor (MFIS) capacitors has been fabricated. The crystalline phase and amount of La³⁺ substitution at Bi-site were investigated by XRD and XPS in the postannealing temperature range from 500 to 700 °C, respectively. The microstructure and interfacial layer between CeO₂ and Si substrate were characterized by HRTEM. The memory windows as functions of insulator film thickness and DC power for La were measured. The maximum memory window is about 1.9 V under ±6 V applied voltage. The ferroelectric polarization increases with increasing substitution amount. The morphologies of La-substituted BiFeO₃ films were also studied by AFM.     

Direct measurement of interfacial structure in epitaxial Gd2O3 on GaAs (0 0 1) using scanning tunneling microscopy

The epitaxial growth of Gd₂O₃ on GaAs (0 0 1) has given a low interfacial density of states, resulting in the demonstration of the first inversion-channel GaAs metal-oxide-semiconductor field-effect transistor. Motivated by the significance of this discovery, in this work, cross-sectional scanning tunneling microscopy is employed herein to obtain precise structural and electronic information on these epitaxial films and interfaces. At the interface, the interfacial stacking of Gd₂O₃ films is directly correlated with the stacking sequence of the substrate GaAs. Additionally, from the local electronic states across the gate oxides, the spatial extent of the GaAs wavefunctions into the oxide dielectric may suggest a minimum Gd₂O₃ thickness to be of bulk properties.     

Epitaxy of BaTiO3 thin film on Si(0 0 1) using a SrTiO3 buffer layer for non-volatile memory application

In this study we report the epitaxial growth of BaTiO₃ films on Si(0 0 1) substrate buffered by 5 nm-thick SrTiO₃ layer using both MBE and PLD techniques. The BaTiO₃ films demonstrate single crystalline, (0 0 1)-oriented texture and atomically flat surface on SrTiO₃/Si template. The electrical characterizations of the BaTiO₃ films using MFIS structures show that samples grown by MBE with limited oxygen pressure during the growth exhibit typical dielectric behavior despite post deposition annealing process employed. A ferroelectric BaTiO₃ layer is obtained using PLD method, which permits much higher oxygen pressure. The C-V curve shows a memory window of 0.75 V which thus enable BaTiO₃ possibly being applied to the non-volatile memory application.     

Epitaxial anatase HfO2 on high-mobility substrate for ultra-scaled CMOS devices

On the basis of ab initio simulations, the formation of an epitaxial phase that has the anatase structure has been proposed as the microscopic mechanism responsible for the preferential orientation of monoclinic HfO₂ films on the high-mobility (0 0 1) oriented Ge and GaAs substrates. In fact, the oriented monoclinic structure follows the in-plane axis of the anatase phase as proved by X-ray scattering measurements. The fact that epitaxial HfO₂ anatase has no bulk counterpart is explained by our calculations as due to the unfavorable Helmholtz free energy of anatase phase when the condition of epitaxy is released.     

Epitaxial Growth of High-J c NdBa2Cu3O7−δ Films on RABiTS by Pulsed Laser Deposition

NdBa₂Cu₃O_7−δ (NdBCO) films were grown on rolling-assisted biaxially textured substrates (RABiTS) via pulsed laser deposition. c-Axis-oriented epitaxial NdBCO films with high performance were obtained under optimal deposition conditions. Transmission electron microscopy analysis shows that the NdBCO film grown on RABiTS has a clear interface with a CeO₂ cap layer and a nearly perfect lattice structure. The NdBCO film exhibits higher T _c of 93.7 K and better in-field J _c in magnetic fields and at all field orientations, compared to pure YBCO films.     

Epitaxial growth and electrical conductance of metal(CoSi2)/insulator(CaF2) nanometer-thick layered structures on Si (111)

Epitaxial growth of a metal (CoSi₂) /insulator (CaF2) nanometer-thick layered structure on Si(111) was demonstrated and the resistivity of CoSi₂ epilayer in this structure was investigated. An epitaxial CoSi₂ layer on CaF₂ was obtained by the two-step growth technique,i.e. solid phase epitaxy with the epitaxial Si layer grown in the first step and Co deposited in the second step. This technique was shown to be effective to avoid the Co agglomeration on CaF₂ layer observed in the co-evaporation of Si and Co. An epitaxial CaF₂ layer was formed on CoSi₂/CaF₂ at low substrate temperature (450°C) with partially ionized and accelerated CaF₂ beam, to avoid Co agglomeration in the CoSi₂/CaF₂ underlayer as well. Obtained results showed a single-crystalline nature in reflection high-energy electron diffraction (RHEED) and transmission electron microscopy (TEM) observations. The resistivity of a few nm-thick CoSi₂ epilayers embedded by CaF₂ has been investigated. We studied thickness and annealing temperature dependence of resistivity and showed that a minimum resistivity of 30 μΩ cm was obtained in a 2 nm-thick CoSi₂ sample annealed at 860°C.     

LaNiO3 and Cu3Ge contacts to YBa2Cu3O7-x films

Metallization of high-T_c superconductors using low resistivity metal oxides and Cu-Ge alloys has been investigated on high quality pulsed laser deposited epitaxial YBa₂Cu₃O_7-x (YBCO) films. Epitaxial LaNiO₃ (LNO) thin films have been grown on YBCO films at 700°C using pulsed laser deposition. The specific resistivity of LNO was measured to be 50 μΩ-cm at 300K which decreases to 19 μΩ-cm at 100K indicating good metallicity of the LNO films. The contact resistance of LNO-YBCO thin film interface was found to be reasonably low (of the order of 10^-4Ω-cm² at 77K) which suggests that the interface formed between the two films is quite clean and LNO can emerge as a promising metal electrode-material to YBCO films. A preliminary investigation related to the compatibility of Cu₃Ge alloy as a contact metallization material to YBCO films is discussed. The usage of other oxide based low resistivity materials such as SrRuO₃ (SRO) and SrVO₃ (SVO) for metallization of high-T_c YBCO superconductor films is also discussed.     

Atomic-layer-deposited Al2O3 and HfO2 on GaN: A comparative study on interfaces and electrical characteristics

Al₂O₃, HfO₂, and composite HfO₂/Al₂O₃ films were deposited on n-type GaN using atomic layer deposition (ALD). The interfacial layer of GaON and HfON was observed between HfO₂ and GaN, whereas the absence of an interfacial layer at Al₂O₃/GaN was confirmed using X-ray photoelectron spectroscopy and transmission electron microscopy. The dielectric constants of Al₂O₃, HfO₂, and composite HfO₂/Al₂O₃ calculated from the C-V measurement are 9, 16.5, and 13.8, respectively. The Al₂O₃ employed as a template in the composite structure has suppressed the interfacial layer formation during the subsequent ALD-HfO₂ and effectively reduced the gate leakage current. While the dielectric constant of the composite HfO₂/Al₂O₃ film is lower than that of HfO₂, the composite structure provides sharp oxide/GaN interface without interfacial layer, leading to better electrical properties.     

The electronic structures and optical properties of BaTiO3 and SrTiO3 using first-principles calculations

The electronic-energy band structures and total density of states (TDOS) for bulk BaTiO₃ and SrTiO₃ were calculated by the first-principles calculations using density-functional theory and local-density approximation. The calculated band structure of BaTiO₃ and SrTiO₃ show the energy band gaps of 1.81 and 1.92 eV at the Γ point in the Brillouin zone, respectively. The optical properties of the both perovskites in the core-level spectra are investigated by the first principles under scissor approximation. The optical constants like refractive index and extinction coefficient of both BaTiO₃ and SrTiO₃ were derived from the calculated real and imaginary parts of the dielectric function. The calculated spectra were compared with the experimental results for BaTiO₃, SrTiO₃ in good agreement.     

Ag(Ta,Nb)O3 thin-film interdigital capacitors for microwave applications

Epitaxial silver tantalate-niobate Ag(Ta,Nb)O₃ (ATN) films have been grown on LaAlO₃(0 0 1) single crystals by pulsed laser ablation of stoichiometric AgTa_0.38Nb_0.62O₃ ceramic target. Extensive X-ray diffraction analysis reveals epitaxial relationship between the ATN film and LaAlO₃(0 0 1) substrate. Micrometer size interdigital capacitor structures have been defined photolithographically on the top surface of ATN films. ATN/LaAlO₃ thin-film capacitors exhibit superior overall performance: loss tangent as low as 0.0033 at 1 MHz, dielectric permittivity 224 at 1 kHz, weak frequency dispersion of 5.8% in 1 kHz to 1 MHz range. Dielectric permittivity and loss tangent were also measured at the microwave range. Conformal mapping techniques were employed to extract dielectric properties of ATN film on substrate at the microwave frequency range. Theoretical properties of conformal mapping techniques for interdigital capacitors and CPW microstrip lines were discussed.     

Engineered oxide thin films as 100% lattice match buffer layers for YBCO coated conductors

One of the most important qualities of buffer layers for RE-BCO coated conductors’ growth is close lattice match with RE-BCO. However, there is no natural material with a 100% lattice match with RE-BCO. In this study mixtures of europium oxide (Eu₂O₃) and ytterbium oxide (Yb₂O₃), (Eu_1−uYb_u)₂O₃ (0.0u1.0), were investigated as a candidate buffer layer that could have same lattice parameter as YBa₂Cu₃O_7−δ(YBCO). Because the pseudocubic lattice parameter of Eu₂O₃ is bigger, and that of Yb₂O₃ is smaller than lattice parameter of YBCO, and the mixed oxides with appropriate ratio would have same lattice parameter of YBCO. The mixtures were prepared using metal-organic precursor by sol–gel process, and it was found that all mixed samples are single phase, complete solid solutions, and have same crystal system over the whole range of “u”. Lattice parameters of mixed (Eu_1−uYb_u)₂O₃ oxide powders were changed between 10.86831 and 10.42828 Å which are lattice parameter of Eu₂O₃ and Yb₂O₃, respectively by changing the ratio of Eu/Yb in the mixture. Phase and lattice parameter analysis revealed that pseudocubic lattice parameter of (Eu_0.893Yb_0.107)₂O₃ is 3.82 Å which is same as the lattice parameter of YBCO. Textured (Eu_0.893Yb_0.107)₂O₃ buffer layers were grown on biaxially textured-Ni (1 0 0) substrates. The solution was prepared from Europium and Ytterbium 2,4-pentadioanate, and was deposited on the Ni substrates using a reel-to-reel sol–gel dip coating system. The textured films were annealed at 1150 °C for 10 min under 4% H₂–Ar gas flow. Extensive texture analysis has been done to characterize the texture of (Eu_0.893Yb_0.107)₂O₃ buffer layers. X-ray diffraction (XRD) of the buffer layer showed strong out-of-plane orientation on Ni tape. The (Eu_0.893Yb_0.107)₂O₃ (2 2 2) pole figure indicated a single cube-on-cube textured structure. The omega and phi scans revealed good out-of-plane and in-plane alignments. The full-width-at-half-maximum (FWHM) values of omega and Phi scan of (Eu_0.893Yb_0.107)₂O₃ films were 6.45° and 7.70°, respectively. ESEM micrographs of the films revealed pinhole-free, crack-free and dense microstructures.     

WO3/NiWO4复合薄膜的制备及其光电化学性能

采用两步水热法在导电玻璃(FTO)上制备了WO₃/NiWO₄复合薄膜。通过XRD,SEM表征了WO₃/NiWO₄复合薄膜的组成结构及微观形貌,利用UV-Vis、光电流测试、光电催化测试和交流阻抗测试分析了WO₃/NiWO₄复合薄膜的光电性能。结果表明:WO₃/NiWO₄复合薄膜相较于WO₃薄膜具有更好的光吸收特性、光电流密度和光电催化活性,其中水热反应3h的WO₃/NiWO₄复合薄膜的光电化学性能最佳。WO₃/NiWO₄-3h在1.4V(vs.Ag/AgCl)时的光电流密度为1.94mA/cm²,光电催化210min对亚甲基蓝溶液的降解效率为57.1%。交流阻抗图谱表明WO₃/NiWO₄薄膜的电荷转移电阻小于WO₃薄膜,光电化学性能更优。     

Electrodepositing ZnxMnyOz alloys from zinc oxide to manganese oxide

Electrodeposition has emerged as a practical and simple method to synthesise semiconductor materials under different forms, thin films or nanostructured layers. This work reports on the cathodic electrodeposition of ZnMnO thin layers using both zinc and manganese chlorides as precursors. The composition of thin films can be varied from binary zinc oxide to manganese oxide varying the Mn/(Mn+Zn) ratio between 0 and 1. The composition of Zn_xMn_yO_z films was obtained by energy dispersive spectroscopy. Zn_1−xMn_xO films with Mn/Zn ratio less than 10% exhibit a crystalline wurtzite structure typical of ZnO fully oriented in the (0 0 2) direction. Higher Mn content leads to deformation of the ZnO lattice and the wurtzite structure is no longer maintained. X-ray photoelectron spectroscopy points out that Mn₃O₄ tends to be deposited when a high Mn/Zn ratio is used in the starting solution. Magnetic measurements on films with Mn/(Zn+Mn) ratio near 1 reveal magnetic characteristics similar to Mn₃O₄ compounds. The transmission spectra of Zn_xMn_yO_z show the typical absorption edge of crystalline ZnO while the wurtzite structure is maintained and it shifts to higher wavelengths when Mn content increases.     

Defect formation in epitaxial oxide dielectric layers due to substrate surface relief

Defects were characterized in epitaxial (001) CeO₂ films deposited and planarizedin situ on patterned (001) LaAlO₃ substrates by ion beam assisted deposition (IBAD). A hill and valley structure with steps running parallel to the [100] LaAlO₃ axis was produced on the surface of the substrate by photolithography and ion beam etching prior to film deposition. A conformai epitaxial CeO₂ layer of ∼ 100 nm thickness was deposited on the heated substrate by e-beam evaporation. Lattice-matching between the e-beam film and the substrate was of the type: (001) CeO₂∥(001) LaAlO₃ and [110] CeO₂∥[100] LaAlO₃. Evaporative deposition of additional film onto the conformai layer was accompanied by bombardment with a 500 eV argon/oxygen ion beam to promotein situ planarization. Extreme lattice misfit for the orientation (001) CeO₂∥(001)LaAlO₃ and [001] CeO₂∥[001] LaAlO₃ caused formation of dislocations in the e-beam CeO₂ film in the vicinity of individual ledges in the substrate surface. Coherence of the CeO₂ film was locally lost in the step regions of the hill and valley structure. The large patterned steps, which are composed of numerous adjacent ledges in the LaAlO₃ surface, caused nucleation of CeO₂ with a tilt misalignment of up to ∼5‡ about the substrate [100]. Nucleation and growth of nonepitaxial CeO₂ crystallites was observed along the step regions of the film during the IBAD portion of deposition. Defect formation in the e-beam ceria layer due to substrate surface relief indicates that “lattice engineering≓ of multilayer epitaxial structures may not be possible when nonplanar surfaces are created during device fabrication. The IBAD CeO₂ layer was more defective than the conformai layer deposited without the impinging ion beam, even in the portions of the film where epitaxy was maintained throughout both layers.     

Low temperature cleaning of Si by a H2/AsH3 plasma prior to heteroepitaxial growth of GaAs by metalorganic chemical vapor deposition (MOCVD)

A method using a H₂/AsH₃ plasma to clean the Si surface before GaAs heteroepitaxy was investigated and the dependence of the effectiveness of this treatment on arsine partial pressure was studied. Thin GaAs-on-Si films deposited on the plasma-cleaned Si were analyzed using plan-view TEM, HRXTEM and SIMS. Although not optimized, this method of Si cleaning makes heteroepitaxial deposition of GaAs possible. Some roughening of the Si surface was observed and a possible explanation is offered. Using the results of this study, thick (2.5–3.0μm) epitaxial GaAs films were then deposited and their quality was evaluated using RBS, XTEM and optical Nomarski observation. All Si surface cleaning and GaAs deposition were carried out at temperatures at or below 650°.     

Epitaxial growth of Dy2O3 thin films on epitaxial Dy-germanide films on Ge(0 0 1) substrates

Ultra-thin films of Dy are grown on Ge(0 0 1) substrates by molecular beam deposition near room temperature and immediately annealed for solid phase epitaxy at higher temperatures, leading to the formation of DyGe_x films. Thin films of Dy₂O₃ are grown on the DyGe_x film on Ge(0 0 1) substrates by molecular beam epitaxy. Streaky reflection high energy electron diffraction (RHEED) patterns reveal that epitaxial DyGe_x films grow on Ge(0 0 1) substrates with flat surfaces. X-ray diffraction (XRD) spectrum suggests the growth of an orthorhombic phase of DyGe_x films with (0 0 1) orientations. After the growth of Dy₂O₃ films, there is a change in RHEED patterns to spotty features, revealing the growth of 3D crystalline islands. XRD spectrum shows the presence of a cubic phase with (1 0 0) and (1 1 1) orientations. Atomic force microscopy image shows that the surface morphology of Dy₂O₃ films is smooth with a root mean square roughness of 10 Å.     

Infrared spectroscopy and X-ray diffraction studies on the crystallographic evolution of La2O3 films upon annealing

Rare earth oxides (REOs) have lately received extensive attention in relation to the continuous scaling down of non-volatile memories (NVMs). In particular, La₂O₃ films are promising for integration into future NVMs because they are expected to crystallize above 400 °C in the hexagonal phase (h-La₂O₃) which has a higher κ value than the cubic phase (c-La₂O₃) in which most of REOs crystallize. In this work, La₂O₃ films are grown on Si by atomic layer deposition using La(C₅H₅)₃ and H₂O. Within the framework of the h-La₂O₃ formation, we systematically study the crystallographic evolution of La₂O₃ films versus annealing temperature (200-600 °C) by Fourier transform infrared spectroscopy (FTIR) and grazing incidence X-ray diffraction (GIXRD). As-grown films are chemically unstable in air since a rapid transformation into monoclinic LaO(OH) and hexagonal La(OH)₃ occurs. Vacuum annealing of sufficiently thick (>100 nm) La(OH)₃ layers induces clear changes in FTIR and GIXRD spectra: c-La₂O₃ gradually forms in the 300-500 °C range while annealing at 600 °C generates h-La₂O₃ which exhibits, as inferred from our electrical data, a desirable κ ∼ 27. A quick transformation from h-La₂O₃ into La(OH)₃ occurs due to H₂O absorption, indicating that the annealed films are chemically unstable. This study extends our recent work on the h-La₂O₃ formation.     

Polypyrrole, α-Fe2O3 and their hybrid nanocomposite sensor: An impedance spectroscopy study

Polypyrrole (PPy), α-Fe₂O₃ and their hybrid nanocomposites have been successfully prepared using chemical polymerization, sol–gel and solid state synthesis method respectively. Films of PPy, α-Fe₂O₃ and PPy/α-Fe₂O₃ nanocomposites were deposited on glass substrates using spin coating technique and characterized using FTIR, XPS, FESEM, TEM techniques as well as their gas sensing performance were studied towards NO₂ gas. FTIR and XPS study confirms the formation of PPy, α-Fe₂O₃ and PPy/α-Fe₂O₃ hybrid nanocomposites. FESEM studies revealed that, the films consists of porous granular type of morphology. TEM analysis revealed that the hybrid composite is in nano range. Impedance spectroscopy studies in presence of air and after exposure of NO₂ gas were carried out on PPy, α-Fe₂O₃ and PPy/α-Fe₂O₃ hybrid nanocomposite films in the frequency range of 20 Hz–10 MHz. Impedance spectroscopy results demonstrate that, the impedance is mainly contributed by the potential barrier at grain boundaries of the films. With the help of impedance spectroscopy results, sensing mechanism between PPy, α-Fe₂O₃ and PPy/α-Fe₂O₃ hybrid nanocomposite films and NO₂ gas molecules was studied and explored.     

Microwave properties of epitaxial large-area Ca-doped YBa2Cu3O7−δ thin films on r-plane sapphire

Ca doping of YBa₂Cu₃O_7−δ (YBCO) is well known to enhance the critical current density in large-angle grain boundaries for example of bicrystals. However, up to now no data are available on microwave properties of epitaxial Ca-doped YBa₂Cu₃O_7−δ thin films on r-plane sapphire with CeO₂ buffer layer.Therefore, first results are presented for large-area pulsed laser deposition (PLD) grown Ca_xY_1−xBa₂Cu₃O_7−δ films on 3-in. diameter sapphire wafers. The PLD process is optimised for undoped YBCO thin films and shows high reproducibility for YBCO. The microwave surface resistance R_s at 8.5 GHz of Ca-doped YBCO (x=0.1) thin films shows clear reduction (up to 20%) with respect to that of YBCO for temperatures from about 20–50 K. In addition, microwave surface resistance R_s of Ca-doped YBCO is lower than that of YBCO even for enhanced microwave surface magnetic field up to about 20 mT for temperatures 20 and 40 K.