Cryogenic properties of SiO2/epoxy nanocomposites

SiO₂/epoxy nanocomposites were prepared using diglycidyl ether of bisphenol-F (DGEBF) type epoxy and tetraethylorthosilicate (TEOS) via the sol-gel process. Silica nanoparticles were collected after burning off the matrix resin and the silica nanoparticles were observed using TEM. The cryogenic tensile properties at 77 K and thermal expansion coefficient of the nanocomposites were studied. The tensile properties at room temperature were also given to compare with the cryogenic tensile properties. The fracture surfaces were examined with scanning electron microscopy (SEM). The effects of silica nanoparticle content have been studied on the cryogenic tensile and thermal properties of the nanocomposites. In addition, the dependence of the glass transition temperature on the silica nanoparticle content has also been examined.     

Thermal stability and crystallization kinetics of sputtered amorphous Si3N4 films

The crystallization of thin silicon nitride (Si₃N₄) films deposited on polycrystalline SiC substrates was investigated by X-ray diffractometry as a function of annealing time. The amorphous Si₃N₄ films were produced by means of reactive r.f. magnetron sputtering. Annealing at temperatures between 1300 and 1700 °C led to the formation of crystalline films composed of -Si₃N₄ and β-Si₃N₄. The fraction of β-Si₃N₄ in the films reaches approximately 40% at temperatures above 1550 °C. Both polymorphic modifications were formed simultaneously during the crystallization process. A transformation of -Si₃N₄ to β-Si₃N₄ could not be observed in the time and temperature range investigated. The crystallization process of amorphous Si₃N₄ can be described according to the Johnson–Mehl–Avrami–Kolmogorov (JMAK) formalism, assuming a three-dimensional, interface controlled grain growth from pre-existing nuclei. The rate constants show an Arrhenius behaviour with an activation enthalpy of approximately 5.5 eV.     

Fabrication and optical properties of NUV-emitting SiO2–SrB4O7:Eu glass–ceramic thin films

SiO₂–SrB₄O₇:Eu²⁺ glass–ceramic thin films were fabricated for possible application in near ultraviolet (NUV) emitting devices. Nano-sized SrB₄O₇:Eu²⁺ powders were prepared by a Pechini-type sol–gel method and a subsequent ball-milling treatment. The powders showed NUV emissions centered at 367 nm, upon irradiation with UV of shorter wavelengths, due to an allowed 4f⁶5d¹ → 4f⁷ electronic transition of Eu²⁺ ions. The glass–ceramic thin films were prepared by dip-coating of tetraethylorthosilicate (TEOS) solutions dispersed with the nano-sized SrB₄O₇:Eu²⁺ powders and a subsequent heat-treatment. It was found that the glass–ceramic thin films had relatively high thermal stability up to 800 °C in terms of the Eu²⁺ emissions. SiO₂ layers surrounding SrB₄O₇:Eu²⁺ appeared to be effective for the surface passivation of the phosphor particles.     

Effect of preparation conditions on properties of atomic layer deposited TiO2 films in Mo–TiO2–Al stacks

TiO₂ films were grown by atomic layer deposition on Mo electrodes in order to elucidate the dominating conductance mechanism and its dependence on the growth chemistry. TiCl₄ and Ti(OC₂H₅)₄ served as titanium precursors, and H₂O or H₂O₂ as oxygen precursors. The films grown at lower temperatures were amorphous. With increasing growth temperatures the crystallization first started in the TiCl₄–H₂O process. The films grown in this process were clearly leakier compared to the films grown from Ti(OC₂H₅)₄ and H₂O and from Ti(OC₂H₅)₄ and H₂O₂. In the Ti(OC₂H₅)₄-based processes, the application of H₂O₂ instead of H₂O resulted in the films with considerably lowered conductivity, although structural differences in these films were insignificant. Space–charge-limited currents were prevailing in all our amorphous Mo–TiO₂–Al packages. Measurements at different temperatures suggested quite high trap densities likely due to the presence of impurities and structural disorder, while the strong differences in conductivity seemed to be due to different densities of gap states.     

Growth and structure of epitaxial CeO2 films on yttria-stabilized ZrO2

Thirty to a hundred-nm thick epitaxial CeO₂ layers are grown on YSZ (100), (110) and (111) surfaces of yttria-stabilized ZrO₂ (YSZ) by electron beam evaporation of Ce in oxygen at reduced pressure. Their growth, structure and thermal stability are studied with several bulk and surface sensitive techniques including Rutherford backscattering spectrometry, cross-sectional high resolution electron microscopy, low energy electron diffraction and low energy reflection electron microscopy. Excellent epitaxy is obtained on all YSZ surfaces at a growth temperature of 750 K. The surfaces of films grown on (111)-oriented substrates are flat, whereas those on the other substrates are faceted into small (111) planes. The grain sizes in the films are in the 10 nm range and smaller.     

Comparison of the developed thermal stresses in Al2O3–SG, ZrO2–12%Si+Al and ZrO2–SG coating systems subjected to thermal loading

In this investigation, thermal and structure finite element analysis has been employed to analyse the thermal stresses developed in Al₂O₃–SG, ZrO₂–12%Si+A1 and ZrO₂–SG.coatings subjected to thermal loading. Systems with 0.4 mm coating thickness and 4 mm substrate material thickness were modelled. Zirconia–spherical cast iron (SG) coatings with NiAl, NiCrAlY and NiCoCrAlY interlayers were also modelled. Nominal and shear stresses at the critical interface regions (film/interlayer/substrate) were obtained. The results showed that the lowest stress levels are in ZrO₂–SG coatings. Furthermore, the interlayer thickness and material combinations have a significant influence on the level of the developed thermal stresses. It is also concluded that the finite element technique can be used to optimise the design and the processing of ceramic coatings.     

Preparation and optical properties of sol–gel derived Er-doped Al2O3–Ta2O5 films

Thin films of the system xAl₂O₃–(100 − x)Ta₂O₅–1Er₂O₃ were prepared by a sol–gel method and a dip-coating technique. The influences of the composition and the crystallization of the films on Er³⁺ optical properties were investigated. Results of X-ray diffraction indicated that the crystallization temperature of Ta₂O₅ increased from 800 to 1000 °C with increased values of x. In crystallized films, the intensities of the visible fluorescence and upconversion fluorescence tend to decrease with an increase in x values, due to the high phonon energy of Al₂O₃; the strongest fluorescence is observed in a crystallized film for x = 4 heat treated at 1000 °C. In amorphous films obtained by heat treatment at relatively low temperatures the Er³⁺ fluorescence could not be observed because strong fluorescence from organic residues remaining in the films thoroughly covered the Er³⁺ fluorescence. On the other hand, the Er³⁺ upconversion fluorescence in the amorphous films was observed to be stronger than that in the crystallized films. The strongest upconversion fluorescence is observed in an amorphous film for x = 75 heat treated at 800 °C.     

SiO2/聚四氟乙烯复合薄膜的制备及力学性能

采用空气辅助干法共混、冷压烧结并车削成膜的方法制备了SiO₂填充量为35wt%、厚度为50 μm的聚四氟乙烯（PTFE）基复合薄膜。系统研究了SiO₂颗粒粒径对SiO₂/PTFE薄膜复合材料的孔洞缺陷和力学性能等的影响,并研究了SiO₂在PTFE中的分散情况及分子间相互作用对其性能变化的影响机制。结果表明,随SiO₂粒径的逐渐增大,其在PTFE中的分散趋于均匀,同时PTFE能更好地包覆粒子,因此SiO₂/PTFE薄膜孔洞缺陷逐渐减少,力学性能逐渐增强;当SiO₂的粒径D₅₀为12 μm时,其在PTFE中的分散均匀性最佳,SiO₂/PTFE复合薄膜孔洞缺陷最少,具有较好的力学性能,断裂伸长率达19.5%,拉伸强度达9.2 MPa。      

On the optical, structural, and morphological properties of ZrO2 and TiO2 dip-coated thin films supported on glass substrates

This article reports the optical and morphological properties of dip-coated TiO₂ and ZrO₂ thin films on soda-lime glass substrates by metal-organic decomposition (MOD) of titanium^IV and zirconium^IV acetylacetonates respectively. Thermogravimetric and differential thermal analysis (DTA–TG) were performed on the precursor powders, indicating pure TiO₂ anatase and tetragonal ZrO₂ phase formation. Phase crystallization processes took place in the range of 300–500 °C for anatase and of 410–500 °C for ZrO₂. Fourier Transform Infrared Spectroscopy (FT-IR) was used to confirm precursor bidentate ligand formation with keno-enolic equilibrium character. Deposited films were heated at different temperatures, and their structural, optical and morphological properties were studied by grazing-incidence X-ray Diffraction (GIXRD) and X-Ray Photoelectron Spectroscopy (XPS), Ultraviolet Visible Spectroscopy (UV-Vis), and Atomic Force Microscopy (AFM) respectively. Film thinning and crystalline phase formation were enhanced with increasing temperature upon chelate decomposition. The optimum annealing temperature for both pure anatase TiO₂ and tetragonal ZrO₂ thin films was found to be 500 °C since solid volume fraction increased with temperature and film refractive index values approached those of pure anatase and tetragonal zirconia. Conditions for clean stoichiometric film formation with an average roughness value of 2 nm are discussed in terms of material binding energies indicated by XPS analyses, refractive index and solid volume fraction obtained indirectly by UV-Vis spectra, and crystalline peak identification provided by GIXRD.     

Synthesis and properties of chitosan/SiO2 hybrid materials

This study primarily aims to explore the strength and thermal properties of various hybrid materials that are made of tetraethoxysilane/vinyltriethoxysilane (TEOS/VTES) and chitosan in different weight ratios. It is confirmed, from micro Fourier transform infrared (micro FT-IR) and nuclear magnetic resonance (NMR) analysis, that hydrogen bonds emerge between chitosan and SiO₂ in hybrid materials. With the addition of more VTES and TEOS, the surface of the hybrid material features thick granules. In addition, the mechanical performance and thermostability of both types of hybrid are better than pure chitosan. The former is enhanced with an increasing amount of TEOS until it exceeds 2.4 g and the latter is also improved with an increasing amount of TEOS.     

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al₂O₃) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 °C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al₂O₃-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance, AC conductivity and activation energy were determined and the results are discussed.     

Structural evolution and its influence on luminescence of SiO2–SrF2–ErF3 glass ceramics prepared by sol–gel method

Er³⁺ doped SrF₂–SiO₂ transparent glass ceramics were prepared by sol–gel method and heat treatment. The decomposition of Sr²⁺–CF₃COO⁻ and the formation of SrF₂ nano-crystals were found to proceed synchronously in the xerogel. After crystallization of the xerogel, SrF₂ nano-crystals with 8–10 nm in size distributed homogenously among the glassy matrix, and the microstructure of the glass ceramic was stable under and at the temperature of 800 °C probably due to interfacial interaction between nano-crystals and glassy matrix. When heat-treated at 800 °C, the chemically bonded water in the sample was eliminated, resulting in the appearance of the visible luminescence bands of ²H_11/2, ⁴S_3/2 → ⁴I_15/2 and ⁴F_9/2 → ⁴I_15/2 transitions.     

Microstructure and properties of MoSi2–MoB and MoSi2–Mo5Si3 molybdenum silicides

MoSi₂-based intermetallics containing different volume fractions of MoB or Mo₅Si₃ were fabricated by hot-pressing MoSi₂, MoB, and Mo₅Si₃ powders in vacuum. Both classes of alloys contained approximately 5 vol.% of dispersed silica phase. Additions of MoB or Mo₅Si₃ caused the average grain size to decrease. The decrease in the grain size was typically accompanied by an increase in flexure strength, a decrease in the room temperature fracture toughness, and a decrease in the hot strength (compressive creep strength) measured around 1200 °C, except when the Mo₅Si₃ effectively became the major phase. Oxidation measurements on the two classes of alloys were carried out in air. Both classes of alloys were protected from oxidation by an in-situ adherent scale that formed on exposure to high temperature. The scale, although not analyzed in detail, is commonly recognized in MoSi₂ containing materials as consisting mostly of SiO₂. The MoB containing materials showed an increase in the scale thickness and the cyclic oxidation rate at 1400 °C when compared with pure MoSi₂. However, in contrast with the pure MoSi₂ material, oxidation at 1400 °C began with a weight loss followed by a weight gain and the formation of the protective silica layer. The Mo₅Si₃ containing materials experienced substantial initial weight losses followed by regions of small weight changes. Overall, the MoB and Mo₅Si₃ additions to MoSi₂ tended to be detrimental for the mechanical and oxidative properties.     

Influence of CaTiO3 impurity in SHS-TiN powder on the mechanical properties of ZrO2–TiN composites

Yttria-stabilised tetragonal polycrystalline ZrO₂-based composites with 40 vol.% TiN were hot pressed at 1450 °C for 1 h using a jet-milled thermally synthesized and a self-propagating high-temperature synthesis (SHS) TiN powder. The ZrO₂ phase of the SHS-TiN powder-based composites was found to be substantially coarser than for the jet-milled TiN powder-based ceramics and prone to spontaneous transformation to m-ZrO₂ and microcracking, due to the CaTiO₃ impurity in the SHS-TiN starting powder. In order to prove this, a set of experiments was performed to investigate the effect of the addition of CaO and TiO₂ on an yttria-stabilised tetragonal ZrO₂ polycrystalline (Y-TZP). The addition of 0.2 mol% of CaO to a Y-TZP ceramic was found to destabilise the t-ZrO₂ phase, whereas the addition of 1 mol% TiO₂ results in significant grain growth and the formation of less transformable t-ZrO₂. The CaTiO₃ impurity could be removed from the SHS-TiN powder by hot hydrochloric acid leaching, allowing to obtain a similar microstructure and mechanical properties as with conventional TiN powder.     

In2O3 films prepared by thermal oxidation of amorphous InSe thin films

In₂O₃ thin films were prepared by the thermal oxidation of amorphous InSe films in air atmosphere. The structure, morphology and composition of the thermal annealed products were characterized by X-ray diffraction (XRD), scanning electron microscopy and energy-dispersive spectroscopy, respectively. The XRD patterns indicate that the as-deposited InSe films were amorphous and they fully transformed into polycrystalline In₂O₃ films with a cubic crystal structure in the preferential (222) orientation at a temperature around 600 °C. The optical energy gap of 3.66 eV was determined at room temperature by transmittance and reflectance measurements using UV-vis-NIR spectroscopy. A preliminary characterization shows that these films have a promising response towards NO₂ gas at a working temperature around 180 °C.     

Low-temperature ionic conductivity of the solid solution in the system ZrO2–Y2O3–Yb2O3

Compositional dependence of ionic conductivity in the system ZrO₂–Y₂O₃–Yb₂O₃ was investigated in the temperature range 573–873 K using the complex impedance technique. It was shown that the conductivity decreases with increasing concentration of Yb₂O₃ in the system ZrO₂–Y₂O₃–Yb₂O₃. Analyzing the experimental data according to the classic Arrhenius equation showed that such an experimental phenomenon can be attributed to the tighter association between Yb³⁺ and oxygen vacancy, compared with that between Y³⁺ and oxygen vacancy, which hinders the migration of oxygen vacancy in the materials.     

Photosensitivity in GeO2–SiO2 glasses and optical waveguides

Permanent refractive index changes caused by a KrF excimer laser operating at 248 nm in GeO₂–SiO₂ glasses deposited on Si (100) substrates using flame hydrolysis deposition (FHD) are presented. The sample was amorphouslike investigated by X-ray diffraction (XRD), and the ratio of Ge:Si is 14:86 from X-ray photoelectron spectroscopy (XPS) analysis. The 10-min irradiation with a KrF excimer laser (10 Hz, 187 mJ/cm²) induced a positive refractive index change of 0.341% at 1550 nm, which has achieved an international level of this field. An innovative photomask with a Cr-loaded structure coated on a UV quartz glass, was used to fabricate a 50 μm gap with a period of 100 μm waveguide grating under 1460 mJ/cm²/pulse at 6 Hz, and the diffraction patterns were observed clearly. The extinction coefficients of the samples are also measured over the range 250–1600 nm.     

Preparation of SiO2 thin films using the Cat-CVD method

Using the catalytic chemical vapor deposition (Cat-CVD) method, a-Si and SiN_x films have been the main focus of studies. SiO₂ films have not been studied because of the limited life of catalysts such as tungsten or molybdenum in an oxidative atmosphere. In this report, we describe oxide film preparation using an iridium catalyst. We determined the most appropriate catalyst material for the oxide film process by exposing heated materials in tetraethoxysilane (TEOS) or O₂ gas. As the result, it was confirmed that the Ir catalyst works in a slow oxidative atmosphere. Using the Ir catalyst, SiO₂ films were deposited in two gas combinations: TEOS and N₂O, and SiH₄ and N₂O. Although the SiO₂ film processed with the combination of TEOS and N₂O was stoichiometric, its breakdown voltage is not sufficient. The SiO₂ film processed with the combination of SiH₄ and N₂O showed good electrical property.     

Characterization of nano-crystalline ZrO2 synthesized via reactive plasma processing

Nano-crystalline ZrO₂ powder has been synthesized via reactive plasma processing. The synthesized ZrO₂ powders were characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM) and FTIR spectroscopy. The synthesized powder consists of a mixture of tetragonal and monoclinic phases of zirconia. Average crystallite size calculated from the XRD pattern shows that particles with crystallite size 20 nm or less than 20 nm are in tetragonal phase, whereas particles greater than 20 nm are in the monoclinic phase. TEM results show that particles have spherical morphology with maximum percentage of particles distributed in a narrow size from about 15 nm to 30 nm.     

Texture of copper films on Ta35Si18N47 and Ti33Si23N44 underlayers

The crystallographic texture and the grain size have been measured by X-ray diffraction techniques for about 200 nm-thick Cu films sputter-deposited on amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ underlayers, and for comparison also on TiN underlayers and oxidized silicon, all on Si (100) substrates. The (111) texture of the as-deposited Cu films increases in the sequence TiN233Si₂₃N₄₄35Si₁₈N₄₇. Amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ layers evidently promote quite effectively the growth of highly (111) textured Cu films. After vacuum annealing at 450°C for 30 min the texture of Cu rises on Ti₃₃Si₂₃N₄₄, falls on Ta₃₅Si₁₈N₄₇, while that on TiN and on SiO₂ changes little and the sequence becomes TiN235Si₁₈N₄₇33Si₂₃N₄₄. The grain size of the as-deposited Cu films increases in the sequence Ti₃₃Si₂₃N₄₄235Si₁₈N₄₇47N₅₃ and rises moderately upon annealing, least for TiN and most for SiO₂ and Ti₃₃Si₂₃N₄₄.