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Flux Pinning Mechanism in BaSnO{sub 3}-Added GdBa{sub 2}Cu{sub 3}O{sub 7-x} Films with Different Thickness

Types of flux pinning mechanism in pure and BaSnO{sub 3} (BSO)-added GdBa{sub 2}Cu{sub 3}O{sub 7-x} (GdBCO) superconducting films have been determined by using the Dew-Hughes model. We have found that as the BSO content increases up to 4 wt%, dominant pinning mechanism of GdBCO films has changed from normal surface pinning due to intrinsic linear defects to normal point pinning by BSO addition. Careful analysis on the scaling of the flux pinning for the 4 wt% BSO-doped GdBCO films with various film thicknesses revealed that the pinning mechanism came from the hybrid pinning of two kinds of pinning types. In addition to the normal point pinning by BSO addition, another type of Δκ-pinning was observed to be prominent in the thinner films in low magnetic field region as normal point pinning was deteriorated. Through the EXAFS analysis, it was found that the Δκ-pinning is possibly originated from the oxygen deficiency in localized position. These results suggested that film thickness directly affects the flux pinning mechanism of the BSO-doped GdBCO films, and in the application point of view, an optimization of the film thickness may be crucial to operate normal point pinning induced by BSO addition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Study of the physical properties of CuS thin films grown by SILAR method

CuS thin films were obtained using the SILAR method on an amorphous glass substrate. All experiments were performed at room temperature. CuS thin films were deposited at 30, 40, 50 and 60 cycles, respectively. Structural, morphological and optical properties of the structures that increase the thickness of nanostructured CuS thin films were investigated. X-ray diffraction, scanning electron microscopy, atomic force microscopy, RAMAN and optical absorption measurements were carried out in order to examine the physical properties of CuS thin films. As a result of the analysis, we can say that the thickness increase positively affects the crystal structure of CuS thin films. In addition, the energy bandgap range of CuS thin films ranged from 2.22 to 1.78 eV. Analysis results of CuS thin films using SILAR method show that thickness is an important factor for thin film studies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microstructural, optical and electrical properties of CdS thin films grown by spray pyrolysis technique as a function of substrate temperature

In this research, nanocrystalline cadmium sulfide thin films were produced by the spray pyrolysis technique on glass substrates. The effects of substrate temperature in the range 400–550 °C on the structural, morphological, optical, and electrical properties of the thin films were investigated. The thin films have been characterized by investigating their X-ray diffraction, field emission scanning electron microscope (FE-SEM), and optical absorption (UV–Vis) measurements. X-ray analysis revealed that thin films were a polycrystalline structure with the hexagonal phase in all cases and by increasing in substrate temperature, crystallite size decreases, and dislocation density increases. The FE-SEM images showed that the surface of the thin films is uniform, homogeneous and without cracks. The average sizes of the grains are at the range of 210–235 nm. The obtained values for optical band gap have been in the range of 2.18–2.41 eV, where the value of optical band gap for the thin films decreases by increasing substrate temperature. The Urbach energies of the thin films increase as the substrate temperature is increased. When substrate temperature increased from 400 to 550 °C, electrical resistivity increased from 531 to 2817 Ω cm, carrier concentration decreased from 15.96 × 10{sup 14} to 3.71 × 10{sup 14} cm{sup −3}, Hall mobility decreased from 7.37 to 5.98 cm{sup 2}/V s. Hall effect analysis indicated that the thin films exhibited n-type conductivity.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Mechanical and Frictional Performance of Ta and Ta-Ag Alloy Films Deposited at Different Sputtering Powers

The mechanical and tribological properties of tantalum and its alloy films are greatly influenced by their phase transformation. In this study, Ta and Ta-Ag films were prepared on carbon steel substrate by DC magnetron sputtering with various sputtering powers. The amorphous and nanocrystalline Ta and Ta-Ag film were produced at different sputtering powers from 40 to 110 W. The frictional properties of Ta and Ta-Ag films were investigated by rubbing against Si{sub 3}N{sub 4} ball from RT to 700 °C. The nanocrystalline Ta-Ag films shows higher hardness values (12 GPa) compared with amorphous phase. The nanocrystalline Ta90-Ag8 film shows a low friction coefficient of about 0.20-0.30 when rubbing against Si{sub 3}N{sub 4} ball at 700 °C. The segregation of Ag can effectively reduce friction coefficients of Ta-Ag film at 700 °C. The Ta-Ag films show high structure stability even after friction at 700 °C.

36 MATERIALS SCIENCE↗

Growth, microstructure and electrical properties of sputter-deposited hafnium oxide (HfO2) thin films grown using HfO2 ceramic target

Hafnium oxide (HfO₂) thin films have been made by radio-frequency (rf) magnetron-sputtering onto Si(100) substrates under varying growth temperature (Ts). HfO₂ ceramic target has been employed for sputtering while varying the Ts from room temperature to 500⁰C during deposition. The effect of Ts on the growth and microstructure of deposited HfO₂ films has been studied using grazing incidence x-ray diffraction (GIXRD), X-ray photoelectron spectroscopy (XPS), and high-resolution scanning electron microscopy (HR-SEM) coupled with energy dispersive x-ray spectrometry (EDS). The results indicate that the effect of Ts is significant on the growth, surface and interface structure, morphology and chemical composition of the HfO₂ films. Structural characterization indicates that the HfO₂ films grown at Ts<200 ⁰C are amorphous while films grown at Ts>200 ⁰C are nanocrystalline. An amorphous-to-crystalline transition occurs at Ts=200 ⁰C. Nanocrystalline HfO₂ films crystallized in a monoclinic structure with a (-111) orientation. XPS measurements indicated the high surface-chemical quality and stoichiometric nature of the grown HfO₂ films. An interface layer (IL) formation occurs due to reaction at the HfO₂-Si interface for HfO₂ films deposited at Ts>200 ⁰C. The thickness of IL increases with increasing Ts. XPS and EDS at the HfO₂-Si cross-section indicate the IL is a (Hf, Si)-O compound. The electrical characterization using capacitance-voltage measurements indicate that the dielectric constant decreases from 25 to 16 with increasing Ts.

36 MATERIALS SCIENCE↗

Water film-driven Mn (oxy)(hydr)oxide nanocoating growth on rhodochrosite

Minerals exposed to moist air stabilize thin water films that drive a score of chemical reactions of great importance to water-unsaturated terrestrial environments. In this study, we identified Mn (oxy)(hydr)oxide nanocoatings formed by the dissolution, oxidation and precipitation of Mn in oxygenated water films grown on rhodochrosite (MnCO 3 ) microparticles. Nanocoatings that could be identified by vibrational spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and (scanning and transmission) electron microscopy formed in water films containing the equivalent of at least 7 monolayers (~84 H 2 O/nm 2 ). These films were formed by exposing microparticles to moist air with at least 50% relative humidity (RH). Films of neutral pH reacted up to 14% of the Mn II located in the topmost ~5 nm region of the microparticles in atmospheres of up to 90% RH for 7 d. These reactions produced MnOOH, birnessite (MnO 2 ) and hausmannite (Mn 3 O 4 ) nanoparticles of low crystallinity, while exposure to atmospheric air for 1 yr. converted only 2% of Mn II in this region to MnOOH. In contrast, reactions in alkaline water films converted up to ~75% of the Mn II but only after 16 d of reaction. These films produced MnOOH and MnO 2 of low crystallinity, as well as crystalline hausmannite. Kinetic modeling of the time-resolved growth of the Mnsingle bondO stretching vibrational bands of these nanocoatings revealed two concurrent reaction processes. A 1 rst -order process was assigned to nucleation events terminating only after a few hours, and a 0-order process was assigned to the sustained growth of nanocoatings from these nuclei over longer reaction time. By identifying nanocoatings formed by water film-driven reactions on rhodochrosite, our study adds new insight into mineralogical transformations relevant to anoxic–oxic boundaries in water-unsaturated environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thin film combinatorial sputtering of Al-Ce alloys: Investigating the phase separation of as-deposited solid solutions and determining the coefficient of thermal expansion

Al x Ce 100–x thin films with a composition range of ~75.0 < x < 99.5 at% (36.5 < x < 97.5 wt%) were synthesized via combinatorial co-sputtering from an Al and an Al 50 Ce 50 target. The crystal structure, phase fraction, film morphology, electrical resistivity, and temperature-dependent coefficients of thermal expansion (CTE) are all correlated to the Al x Ce 100–x composition. The as-deposited films form a metastable solid-solution, and annealing leads to the formation of the thermodynamically stable two-phase system of Al and the α-Al 11 Ce 3 intermetallic. Temperature dependent x-ray diffraction (XRD) reveals that the two phases expand independently of one another, and the thin film Al temperature-dependent CTE is similar to bulk Al. The thin film Al 11 Ce 3 intermetallic phase has a nearly constant CTE of ~1.5 × 10 –5 /°C within the temperature range studied (25–550 °C). To confirm the thin film Al 11 Ce 3 results, bulk stoichiometric Al 11 Ce 3 and +/- 1 wt% Ce samples were prepared and the CTE of each was measured with the same conditions. A Rietveld analysis of the bulk data enabled an estimation of the CTE in each of the 3 orthorhombic lattice parameters, which displayed anisotropic behavior. The thin film and bulk CTE measurements were in very good agreement. Estimations of the temperature dependent CTE of the two-phase alloys are made via the Reuss and Voigt models. Finally, by demonstrating the efficacy of the approach, more complex multi-component rapid materials discovery of low CTE Al-alloys can be pursued via the combinatorial thin film synthesis and XRD measurement.

36 MATERIALS SCIENCE↗

Direct processing of PbZr 0.53 Ti 0.47 O 3 films on glass and polymeric substrates

This work reports on direct crystallization of PbZr 0.53 Ti 0.47 O 3 (PZT) thin films on glass and polymeric substrates, using pulsed thermal processing (PTP). Specifically, xenon flash lamps deliver pulses of high intensity, short duration, broadband light to the surface of a chemical solution deposited thin film, resulting in the crystallization of the film. Structural analysis by X-ray diffraction (XRD) and transmission electron microscopy show the existence of perovskite structure in nano-sized grains (≤5 nm). Local functional analysis by band excitation piezoelectric spectroscopy and electrostatic force microscopy confirm the presence of a ferroelectric phase and retention of voltage-written polarization for multiple days. Based on structural and functional analyses, strategies are discussed for optimization of pulse voltage and duration for the realization of crystalline ferroelectric thin films. For ~200 nm-thick PZT films on glass substrates, 500 μs-long pulses were required for crystallization, starting with 100 pulses at 350 V, 10 or 25 pulses at 400 V and in general lower number of pulses at higher voltages (resulting in higher radiant energy). Overall power densities of >6.4 kW/cm 2 were needed for appearance of peaks corresponding to the perovskite phase in the XRD. Films on glass processed at 350–400 V had a higher degree of 111-oriented perovskite grains. Higher applied radiant energy (through increased pulse voltage or count) resulted in more random and/or partially 001-oriented films. For ~1 μm-thick PZT films on polymeric substrates, 10 to 25 250 μs-long pulses at voltages ranging between 200 to 250 V, corresponding to power densities of ~2.8 kW/cm 2 , were optimal for maximized perovskite phase crystallization, while avoiding substrate damage.

36 MATERIALS SCIENCE↗

Enhancement of photoelectric catalytic activity of TiO{sub 2} film via Polyaniline hybridization

A Polyaniline (PANI)/TiO{sub 2} film coated on titanium foil was successfully prepared using the sol-gel method followed by a facile chemisorption. Compared with pristine TiO{sub 2}, the photocatalytic (PC) and photoelectrocatalytic (PEC) degradation rates of 2,4-dichlorophenol (2,4-DCP) with the PANI/TiO{sub 2} film were enhanced by 22.2% and 57.5%, respectively. 2,4-DCP can be mineralized more effectively in the presence of PANI/TiO{sub 2} film. The best PEC degradation efficiency of 2,4-DCP with the PANI/TiO{sub 2} film was acquired at an external potential of 1.5 V with a layer of 1 nm thick PANI. The PANI/TiO{sub 2} film was characterized by Raman spectra, Fourier transform infrared spectra (FT-IR), Auger electron spectroscopy (AES), and electrochemical analysis. These results indicated that there was a chemical interaction on the interface of PANI and TiO{sub 2}. This interaction may be of significance to promote the migration efficiency of carriers and induce a synergetic effect to enhance the PC and PEC activities. - Graphical abstract: The effect of PANI content on 2,4-DCP degradation with initial concentration of 50 mg/L, external potential=1.5 V. Inset: degradation rate constants of various PANI/TiO{sub 2} films. Highlights: > Polyaniline/TiO{sub 2} film was prepared using the sol-gel method followed by chemisorption. > Photoelectrocatalytic degradation rate of 2,4-dichlorophenol was enhanced by 57.5%. > The modification of Polyaniline to TiO{sub 2} film caused a rapid charge separation. > Best degradation efficiency was acquired at 1.5 V with 1 nm thick PANI.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Recent progress in nanostructured multiferroic Bi{sub 2}FeCrO{sub 6} thin films

We report the latest progress on the growth and characterization of Bi{sub 2}FeCrO{sub 6} (BFCO), a recently discovered multiferroic system. BFCO thin films and nanostructures exhibit exceptional multiferroic properties at room temperature. The growth of pure BFCO thin films on STO substrates is possible only in a narrow window of deposition parameters (i.e., Oxygen pressure pO{sub 2}=1.2 Multiplication-Sign 10{sup -2} mbar and around a substrate temperature T{sub S}=680 Degree-Sign C). The epitaxial growth stabilizes the metastable single phase of this material and promotes the Fe/Cr cation ordering in both thin films and nanostructures. This cationic ordering which is responsible for good magnetic properties of BFCO is also at the origin of pronounced photovoltaic (PV) properties observed in the epitaxial films grown on STO substrates. The results indicate that the ferroelectric polarization plays a dominant role in the observed PV effect. - Graphical abstract: (Top) Crystal structure of BFCO thin films deposited on (1 1 1)-oriented SrTiO3:Nb substrates and direct evidence of the presence of cationic ordering Fe/Cr in the films. (Bottom) Control of the crystal orientation and the shape of the epitaxial nanostructures by the orientation of the niobium-doped STO substrates. Highlights: Black-Right-Pointing-Pointer Growth optimization of Bi{sub 2}FeCrO{sub 6} (BFCO) thin films and nanostructures by pulsed laser deposition. Black-Right-Pointing-Pointer Ordered BFCO single phase have been stabilized by epitaxial strain. Black-Right-Pointing-Pointer Arbitrary patterns of heteroepitaxial multiferroic BFCO nanostructures have been fabricated by PLD combined with nanostenciling. Black-Right-Pointing-Pointer Experimental characterizations revealed the excellent multiferroic character of BFCO thin films and nanostructures. Black-Right-Pointing-Pointer Unprecedentedly high power conversion efficiency for ferroelectrics was observed in 125 nm-thick highly ordered BFCO films.Graphical abstract legend.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Study of the crystallographic phase change on copper (I) selenide thin films prepared through chemical bath deposition by varying the pH of the solution

Copper (I) selenide thin films with orthorhombic and cubic structure were deposited on glass substrates by using the chemical bath deposition technique. The effects of the solution pH on the films growth and subsequently the structural, optical and electrical properties of the films were studied. Films with orthorhombic structure were obtained from baths wherein both metal complex and hydroxide coexist; while films with cubic structure were obtained from baths where the metal hydroxide there is no present. The structural modifications are accompanied by changes in bandgap energy, morphology and electrical resistivity of the films. - Graphical abstract: “Study of the crystallographic phase change on copper (I) selenide thin films prepared through chemical bath deposition by varying the pH of the solution” by M. G. Sandoval-Paz, C. A. Rodríguez, P. F. Porcile-Saavedra, C. Trejo-Cruz. Display Omitted - Highlights: • Copper (I) selenide thin films were obtained by chemical bath deposition. • Orthorhombic to cubic phase change was induced by varying the reaction solution pH. • Orthorhombic phase is obtained mainly from a hydroxides cluster mechanism. • Cubic phase is obtained mainly from an ion by ion mechanism. • Structural, optical and electrical properties are presented as a function of pH.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Growth of different phases and morphological features of MnS thin films by chemical bath deposition: Effect of deposition parameters and annealing

Manganese sulfide thin films have been deposited on glass slides by chemical bath deposition (CBD) method. The effects of preparative parameters such as deposition time, bath temperature, concentration of precursors, multi-layer deposition, different source of manganese, different complexing agent and thermal annealing on structural and morphological film properties have been investigated. The prepared thin films have been characterized using the X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). It exhibit the metastable forms of MnS, the hexagonal γ-MnS wurtzite phase with preferential orientation in the (002) plane or the cubic β-MnS zinc blende with preferential orientation in the (200) plane. Microstructural studies revealed the formation of MnS crystals with different morphologies, such as hexagons, spheres, cubes or flowers like. - Graphical Abstract: We report the preparation of different phases of manganese sulfide thin films (γ, β and α-MnS) by chemical bath deposition method. The effects of deposition parameters such as deposition time and temperature, concentrations of precursors and multi-layer deposition on MnS thin films structure and morphology were investigated. The influence of thermal annealing under nitrogen atmosphere at different temperature on MnS properties was also studied. Different manganese precursors as well as different complexing agent were also used. - Highlights: • γ and β-MnS films were deposited on substrate using the chemical bath deposition. • The effect of deposition parameters on MnS film properties has been investigated. • Multi-layer deposition was also studied to increase film thickness. • The effect of annealing under N{sub 2} at different temperature was investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Water droplet behavior on superhydrophobic SiO{sub 2} nanocomposite films during icing/deicing cycles

This work investigates water droplet behavior on superhydrophobic (water contact angle value of 162 ± 1°) SiO{sub 2} nanocomposite films subjected to repetitive icing/deicing treatments, changes in SiO{sub 2} nanocomposite film surface morphology and their non-wetting characteristics. During the experiment, water droplets on SiO{sub 2} nanocomposite film surface are subjected to a series of icing and deicing cycles in a humid (∼ 70% relative humidity) atmosphere and the resulting morphological changes are monitored and characterized using atomic force microscopy (AFM) and contact angle measurements. Our data show that the formation of the frozen or thawed water droplet, with no further shape change, on superhydrophobic SiO{sub 2} nanocomposite film, is obtained faster within each cycle as the number of the icing/deicing cycles increases. After 10 icing and deicing cycles, the superhydrophobic SiO{sub 2} nanocomposite film had a water contact angle value of 146 ± 2° which is effectively non-superhydrophobic. AFM analysis showed that the superhydrophobic SiO{sub 2} nanocomposite film surface area under the water droplet undergoes gradual mechanical damage during the repetitive icing/deicing cycles. We propose a possible mechanism of the morphological changes to the film surface that take place during the consecutive icing/deicing experiments. - Highlights: • Superhydrophobic film is subjected to repetitive icing/deicing treatments. • Water droplet shape transition is recorded and characterized thereafter. • Atomic force microscopy and contact angle measurements are performed. • The surface undergoes gradual mechanical damage during repetitive icing/deicing. • Mechanism for the observed surface morphological changes is suggested.

36 MATERIALS SCIENCE↗

X-ray microstructural analysis of nanocrystalline TiZrN thin films by diffraction pattern modeling

A detailed microstructural characterization of nanocrystalline TiZrN thin films grown at different substrate temperatures (T{sub S}) was carried out by X-ray diffraction (XRD). Total diffraction pattern modeling based on more meaningful microstructural parameters, such as crystallite size distribution and dislocation density, was performed to describe the microstructure of the thin films more precisely. This diffraction modeling has been implemented and used mostly to characterize powders, but the technique can be very useful to study hard thin films by taking certain considerations into account. Nanocrystalline films were grown by using the cathodic pulsed vacuum arc technique on stainless steel 316L substrates, varying the temperature from room temperature to 200 °C. Further surface morphology analysis was performed to study the dependence of grain size on substrate temperature using atomic force microscopy (AFM). The crystallite and surface grain sizes obtained and the high density of dislocations observed indicate that the films underwent nanostructured growth. Variations in these microstructural parameters as a function of T{sub S} during deposition revealed a competition between adatom mobility and desorption processes, resulting in a specific microstructure. These films also showed slight anisotropy in their microstructure, and this was incorporated into the diffraction pattern modeling. The resulting model allowed for the films' microstructure during synthesis to be better understood according to the experimental results obtained. - Highlights: • Mobility and desorption competition generates a critical temperature. • A microstructure anisotropy related to the local strain was observed in thin films. • Adatom mobility and desorption influence grain size and microstrain.

36 MATERIALS SCIENCE↗

Influence of the microstructure on the resulting 18R martensitic transformation of polycrystalline Cu−Al−Zn thin films obtained by sputtering and reactive annealing

We report the influence of the microstructure on the martensitic transformation in polycrystalline Cu−Zn−Al thin films with 18R structure. The films are grown in two steps. First, Cu−Al thin films are obtained by DC sputtering. Second, the Zn is introduced in the Cu−Al thin films by the annealing them together with a bulk Cu−Zn−Al reference. The crystalline structure of the films was analyzed by X-ray diffraction and transmission electron microscopy. The martensitic transformation temperature was measured by electrical transport using conventional four probe geometry. It was observed that temperatures above 973 K are necessary for zincification of the samples to occur. The resulting martensitic transformation and its hysteresis (barrier for the transformation) depend on the grain size, topology and films thickness. - Highlights: • Polycrystalline Cu−Al−Zn thin films with nanometric grain size are sintered. • Influence of thermal annealing process on the microstructure is analyzed. • Martensitic transformation of Cu−Al−Zn thin films is strongly affected by the microstructure.

36 MATERIALS SCIENCE↗

Characterization of nanostructured photosensitive (NiS){sub x}(CdS){sub (1-x)} composite thin films grown by successive ionic layer adsorption and reaction (SILAR) route

Highlights: {yields} Thin films of (NiS){sub x}(CdS){sub (1-x)} with variable composition (x = 1 to 0) were deposited onto glass substrates by the successive ionic layer adsorption and reaction (SILAR) method. {yields} The structural, surface morphological and electrical characterizations of the as deposited and annealed films were studied. {yields} The bandgap and activation energy of annealed (NiS){sub x}(CdS){sub (1-x)} film decrease with improvement in photosensitive nature. -- Abstract: Recently ternary semiconductor nanostructured composite materials have attracted the interest of researchers because of their photovoltaic applications. Thin films of (NiS){sub x}(CdS){sub (1-x)} with variable composition (x = 1-0) had been deposited onto glass substrates by the successive ionic layer adsorption and reaction (SILAR) method. As grown and annealed films were characterised by X-ray diffraction, scanning electron microscopy and EDAX to investigate structural and morphological properties. The (NiS){sub x}(CdS){sub (1-x)} films were polycrystalline in nature having mixed phase of rhombohedral and hexagonal crystal structure due to NiS and CdS respectively. The optical and electrical properties of (NiS){sub x}(CdS){sub (1-x)} thin films were studied to determine compsition dependent bandgap, activation energy and photconductivity. The bandgap and activation energy of annealed (NiS){sub x}(CdS){sub (1-x)} film decrease with improvement in photosensitive nature.

36 MATERIALS SCIENCE↗

Sol–gel synthesis and electrical characterization of Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12} thin films

Graphical abstract: Display Omitted Highlights: ► Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12} (BLT) thin films on Pt/TiO{sub 2}/SiO{sub 2}/Si substrates prepared by sol–gel. ► Ethylacetoacetate (EAA) used as a replacement for highly toxic 2-methoxyethanol. ► 0.4 μm thick BLT film has 2P{sub r} ∼ 21 μC/cm{sup 2} and 2E{sub c} of ∼195 kV/cm at 300 kV/cm, εr = 140 and tan δ = 0.025, 1 kHz. ► BLT films with improved dielectric response when prepared form ethylacetoacetate (EAA). -- Abstract: Lanthanum bismuth titanate (Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12}) (BLT) thin films on Pt/TiO{sub 2}/SiO{sub 2}/Si substrates were prepared by sol–gel using ethylacetoacetate (EAA) as a replacement for the highly toxic 2-methoxyethanol. EAA is used as a modifier to stabilize the metal alkoxide. At 450 °C films are amorphous. After annealing at 650 °C films are crystalline and present good dielectric and ferroelectric properties. A 0.4 μm thick BLT film exhibits 2P{sub r} of ∼21 μC/cm{sup 2} and 2E{sub c} of ∼195 kV/cm at 300 kV/cm. The dielectric constant and dielectric losses of these BLT films at 1 kHz are 140 and 0.025, respectively.

36 MATERIALS SCIENCE↗

Effects of He (90%)/H{sub 2} (10%) plasma treatment on electric properties of low dielectric constant SiCOH films

In microelectronics industry, integration of the low dielectric constant (low-k) material films is a continuing issue due to the decreasing device feature size. To improve electric properties, various post-deposition treatments of the low-k material films can be used. In this work, we used room temperature treatment of He/H{sub 2} plasma and investigated the effects of plasma treatment on the electrical properties of low-k SiOCH films. Plasma treatment time changed from 300 to 1800 s. After treatment, the dielectric constant was decreased from 2.9 to 2.48, and the thickness of the low-k SiCOH films changed by only ∼5%. The leakage current densities of the low-k SiCOH films were decreased to ∼10{sup −11} A/cm{sup 2}, with treatment time ≥600 s. The breakdown occurred only around 2 V for films plasma-treated for 600 and 900 s. However, for 1800 s treatment time, the breakdown voltage was enhanced dramatically and breakdown occurred at applied voltage higher than 40 V. The surface composition change of the films after treatment was investigated by X-ray photoelectron spectroscopy (XPS). As the plasma treatment time was increased, the intensities of C-C/C-H and C-Si peaks were decreased while the intensities of Si-O and C-O peaks were increased. It is thought that increase of oxygen content of the SiCOH film, after plasma treatment, contributed to leakage current reduction and breakdown voltage increase.

36 MATERIALS SCIENCE↗