Microstructure and mechanical properties of continuous Al2O3 fibre reinforced Ni45Al45Cr7.5Ta2.5 alloy (IP75) matrix composites

Single crystalline Al₂O₃ fibres (sapphire), coated with the NiAl alloy IP75 by physical vapour deposition (PVD), were assembled to fabricate composites by means of diffusion bonding. The microstructure and chemistry of both as-coated fibre and as-diffusion bonded composites were investigated by electron microscopy and microanalysis. The interface shear stress for complete debonding was measured by fibre push-out tests at room temperature, and the composite tensile strength was measured at 900°C and 1100°C. An amorphous layer with a thickness of about 400?nm formed between the fibre and the matrix during the PVD process and was maintained during diffusion bonding. A Laves phase precipitated along NiAl grain boundaries in the IP75 matrix. This caused a lower tensile strength of the IP75/Al₂O₃ composite at high temperatures compared to as-cast monolithic IP75 and rendered the composite useless for structural applications.     

Oxidation behaviour of SiC coatings

Amorphous silicon carbide (SiC) films were deposited on silicon substrates by radio-frequency magnetron sputtering. The films were oxidized in air in the temperature range 400–900 °C and for times from 1 to 16 h. Neutron reflectivity measurements provided information on the thickness, density and roughness of the SiC and on the formed SiO₂ layers. Fourier transform infrared spectroscopy was used to determine the bond structure of the formed SiO₂ and changes in the bonding of SiC after exposure at the oxidation temperature. The surface morphology of the oxidized films was characterized by atomic force microscopy measurements. The oxidation kinetics is initially fast and as the SiO₂ layer is formed it slows down. The SiC consumption varies linearly with time at all oxidation temperatures. Exposure of the SiC at the oxidation temperature affects its density and to some degree its bond structure, while the formed SiO₂ has density and bond structure as that formed by oxidation of Si under the same conditions. PACS  66.30.Ny; 68.47.Gh; 68.55.J-     

Fabrication of silicon nanowires

2 at 750 °C and 850 °C. The oxide and interface morphology are characterized by cross-sectional scanning electron microscope images. It is found that the oxidized nanowire following oxidation at 750 °C still keeps its pentagon shape even if it has been oxidized for 19 h. However, the oxidized samples at 850 °C become circular in shape. The oxidation-temperature dependence of the sample shapes is discussed. Our results should be useful in generating silicon nanowires coated with SiO₂ in microelectronic technology with careful selection of the SiO₂ growth temperatures. Received: 26 September 1997/Accepted: 8 December 1997     

Interfacial microstructure and reaction at the spin-coated fluorinated polyimide/Al interface: surface-enhanced X-ray diffraction and TEM studies

2 multilayers by means of X-ray diffraction, transmission electron microscopy, and an ellipsometer. The FPI precursor, a solution of PMDA/6FDA/TFMOB/PPD was spin-coated onto the Al layer and then cured at 400 °C for one hour. It is found that the moisture and oxygen from the FPI layer released during thermal treatment can lead to the oxidation of the interface between the Al and the FPI. The TEM cross-sectional images and the electron diffraction patterns indicate that the oxidized interface is amorphous. The oxidation product is identified to be Al₂O₃. The oxidation onset temperature is determined to be 415 °C, which is slightly higher than the curing temperature. The oxidation of the FPI/Al interface results in an increase in the electrical resistance of the Al layer, and thus may lead to a reduction in its effective electrical thickness. Received: 21 May 1997/Accepted: 27 May 1997     

Optical excitation and emission processes of Si-QD/SiO2 multilayer films with different SiO2 layer thicknesses

Si-rich oxide/SiO₂ multilayer films with different SiO₂ layer thicknesses have been deposited by the plasma enhanced chemical vapor deposition technique, and crystallized Si quantum dot (Si-QD)/SiO₂ multilayer films are obtained after annealing at 1100 ^°C. The photoluminescence (PL) intensity of the multilayer films increases significantly with increasing SiO₂ layer thickness, and the PL peak shifts from 1.25 eV to 1.34 eV. The PL excitation spectra indicate that the maximal PL excitation intensity is located at 4.1 eV, and an excitation–transfer mechanism exists in the excitation processes. The PL decay time for a certain wavelength is a constant when the SiO₂ thickness is larger than 2 nm, and a slow PL decay process is obtained when the SiO₂ layer is 1 nm. In addition, the PL peak shifts toward high energy with decreasing temperature only when the SiO₂ layer is thick enough. Detailed analyses show that the mechanism of PL changes from the quantum confinement effect to interface defects with decreasing SiO₂ layer thickness.     

Thermal stability of Cu–Nb nanolamellar composites fabricated via accumulative roll bonding

In situ annealing within a neutron beam line and ex situ annealing followed by transmission electron microscopy were used to study the thermal stability of the texture, microstructure, and bi-metal interface in bulk nanolamellar Cu/Nb composites (h?=?18?nm individual layer thickness) fabricated via accumulative roll bonding, a severe plastic deformation technique. Compared to the bulk single-phase constituent materials, the nanocomposite is two orders of magnitude higher in hardness and significantly more thermally stable, e.g., no observed recrystallization in Cu at temperatures as high as 85% of the melting temperature. The nanoscale h?=?18?nm individual layer thickness is maintained up to 500°C, the lamellar structure thickens but is maintained up to 700°C, and recrystallization is suppressed even up to 900°C. With increasing temperature, the texture sharpens, and among the interfaces found in the starting material, the {112}_Cu?||?{112}_Nb interface with a Kurdjumov-Sachs orientation relationship shows the greatest thermal stability. Our results suggest that thickening of the individual layers under heat treatment coincides with thermally driven removal of energetically unfavorable bi-metal interfaces. Thus, we uncover a temperature regime that maintains the lamellar structure but alters the interface distribution such that a single, low energy, thermally stable interface prevails.     

Catalytic action of gold atoms on the oxidation of Si(111) surfaces

Auger spectroscopy, electron energy loss spectroscopy and ion depth profiling techniques, under ultra high vacuum conditions, have been used in a comparative study of the oxidation of clean and gold precovered silicon (111) surfaces. Exposure of a Si surface covered by a few Au monolayers to an oxygen partial pressure induces the formation of SiO₄ tetrahedra even at room temperature. In contrast, oxidation under the same conditions of a clean Si(111) surface leads to the well known formation of a chemisorbed oxygen monolayer. In the case of the Au covered surfaces, the enhancement of the oxide growth is attributed to the presence of an AuSi alloy where the hybridization state of silicon atoms is modified as compared to bulk silicon. This Au catalytic action has been investigated with various parameters as the substrate temperature, oxygen partial pressure and Au coverage. The conclusions are two fold. At low temperature (T < 400°C), gold atoms enhance considerably the oxidation process. SiO₄ tetrahedra are readily formed even at room temperature. Nevertheless, the SiO₂ thickness saturates at about one monolayer, this effect being attributed to the lack of Si atoms alloyed with gold in the reaction area. By increasing the temperature (from 20°C to ～400°C), silicon diffusion towards the surface is promoted and a thicker SiO₂ layer can be grown on top of the substrate. In the case of the oxidation performed at temperature higher than 400°C, the results are similar to the one obtained on a clean surface. At these temperatures, the metallic film agglomerates into tridimensional crystallites on top of a very thin AuSi alloyed layer. The fact that the latter has no influence on the oxidation is attributed to the different local arrangement of atoms at the sample surface.     

Identification of optimal ALD process conditions of Nd2O3 on Si by spectroscopic ellipsometry

Variable angle spectroscopic ellipsometry (VASE) is used to investigate the thickness and optical properties of Nd₂O₃ films deposited by atomic layer deposition (ALD) at various process conditions. It is found that the films exhibit good thickness uniformity and an almost constant growth rate of 0.42 ?/cycle in the temperature region of 290–330 °C. Further examination of the imaginary part of the dielectric functions of the selected samples demonstrates that all optically observable dielectric-related defects are located in the interface layer between the silicon substrate and the native oxide rather than in the bulk Nd₂O₃ layer. And, the defects within the band gap of the interface are found to be strongly affected by the deposition temperature. In the deposition temperature range of 300–320 °C, only one absorption peak of 3.53 eV besides the silicon substrate’s critical features is observed, indicating that the Si/SiO₂/Nd₂O₃ stacks contain the fewest interfacial defects. Then the optimal ALD process condition for Nd₂O₃ is determined as Nd(thd)₃ (thd = 2,2,6,6,-tetramethyl-3,5-heptanedionato) evaporation temperature: 185 °C, deposition temperature: 300–320 °C, saturation condition: Nd(thd)₃ and pulse time longer than 0.5 s.     

The microstructure of SiO thin films: from nanoclusters to nanocrystals

The microstructure and electronic structure of silicon-rich oxide (SRO) films were investigated using transmission electron microscopy and electron energy loss spectroscopy as the main analytical techniques. The as-deposited SRO film was found to be a single phase SiO_1.0, as suggested by its electronic structure characteristics determined by the valence electron energy loss spectrum. This single phase undergoes a continuous but incomplete phase decomposition to Si and SiO₂ for films annealed between 300 and 1100°C. The resulting Si phase first appears as ～2?nm-diameter amorphous clusters which grow to larger sizes at higher annealing temperatures, but only crystallize at a critical temperature between 800 and 900°C. This cluster/matrix configuration of the SRO films is consistent with the appearance of the interface plasmon and its oscillator strength as a function of the nanoparticle size. Three separate stages were identified in the sequence of annealed films that were characterized by the presence of single-phase SiO, amorphous silicon nanoclusters, and silicon nanocrystals, respectively. The presence of amorphous silicon nanoclusters in the intermediate stage, the mean size of which can be controlled via annealing, may offer an alternative to silicon nanocrystal composites for optical applications.     

Formation of atomically smooth SiO2/SiC interfaces at ∼120 °C by use of nitric acid oxidation method

Conventional thermal oxidation of SiC requires heating at ∼1100 °C. In the present study, we have developed a method of oxidizing SiC at low temperatures (i.e., ∼120 °C) to form relatively thick silicon dioxide (SiO₂) layers by use of nitric acid. When 4H-SiC(0 0 0 1) wafers are immersed in 40 wt% HNO₃ at the boiling temperature of 108 °C and the boiling is kept for 5 h after reaching the azeotropic point (i.e., 68 wt% HNO₃ at 121 °C), 8.1 nm thick SiO₂ layers are formed on the SiC substrates. High resolution transmission electron microscopy measurements show that the SiO₂/SiC interface is atomically flat and the SiO₂ layer is uniform without bunching. When SiC is immersed in an azeotropic mixture of HNO₃ with water from the first, the SiO₂ thickness is less than 0.3 nm. The metal-oxide-semiconductor (MOS) diodes with the SiO₂ layer formed by the nitric acid oxidation method possess a considerably low leakage current density.     

Thermal oxidation temperature dependence of 4H-SiC MOS interface

The thermal oxidation temperature dependence of 4H-silicon carbide (SiC) is systematically investigated using X-ray photoelectron spectroscopy (XPS) and capacitance-voltage (C-V) measurements. When SiC is thermally oxidized, silicon oxycarbides (SiC_xO_y) are first grown and then silicon dioxide (SiO₂) is grown. It is identified by XPS that the SiO₂ films fall into two categories, called SiC-oxidized SiO₂ and Si-oxidized SiO₂ in this paper. The products depend on thermal oxidation temperature. The critical temperature is between 1200 and 1300 °C. The interface trap density (D_it) of the sample possessing Si-oxidized SiO₂, at thermal oxidation temperature of 1300 °C, is lower than SiC-oxidized SiO₂ at and below 1200 °C, suggesting that a decrease of the C component in SiO₂ film and SiO₂/SiC interface by higher oxidation temperature improves the metal-oxide-semiconductor (MOS) characteristics.     

Fabrication of coaxial nanowire heterostructures: SiO x nanowires with conformal TiO2 coatings

Silica nanowires, grown via the active oxidation of a silicon substrate, have been coated with TiO₂ using two coating methods: solution-based deposition of Ti-alkoxides and atomic layer deposition. Analysis of as-deposited and annealed films shows that it is possible to produce stable conformal coatings of either the anatase or rutile phases of TiO₂ on nanowires with diameters greater than 100 nm when annealed between 500–600°C and 800–900°C, respectively, with annealing at higher temperatures (1050°C) producing coatings with a highly facetted rutile morphology. The efficacy of the process is shown to depend on nanowire diameter, with nanowires having diameters less than about 100 nm fusing together during solution-based coating and decomposing during TiO₂ atomic layer deposition. The use of a suitable buffer layer is shown to be an effective means of minimizing nanowire decomposition. Finally, annealing coated nanowires under active oxidation conditions (1100°C) is shown to be an effective technique for depositing additional conformal SiO _x coatings, thereby providing a means of fabricating multi-layered coaxial nanostructures.     

Influence of sintering temperature and pH on the phase transformation,particle size and anti-reflective properties of RHA nano silica powders

Nano silica powders were synthesized from rice husk ash, the most silica-rich raw material, using alkaline extraction followed by acid precipitation. The phase transformation during sintering, the influence of sintering temperature and pH on the particle size and anti-reflective properties of nano silica were investigated. The results showed that the amorphous SiO₂ sintered at 600°C were transformed to a cristobalite structures completely during the sintering process at 800°C and 1100°C. With the increasing sintering temperature and pH, the particle size distributions (d₅₀) were increased respectively in the range of 62–84, 192–240, and 283–329?nm at sintering temperatures of 600°C, 800°C, and 1100°C. When the sintering temperatures were increased at 1100°C, 98.15% and 96.84% of transmittances were obtained respectively at the highest and lowest points of the anti-reflection band and could be used for anti-reflective applications.     

Morphology, composition and thermal stability of thin SiO2/HfO2 layers grown on silicon by electron-beam evaporation in vacuum

The results of integrated studies of thin-film structures based on silicon and hafnium dioxides on silicon grown by electron-beam evaporation in vacuum are presented. The surface morphology, structural and phase composition of these films depending on the annealing temperature within 500–1100°C are studied. Special consideration is given to the change in the state of the interfaces after annealing. It is determined that annealing in a flow of nitrogen with the addition of oxygen (～10 vol %) at 700°C does not lead to structural and phase changes in the films, but the intensity of the electron paramagnetic resonance (EPR) spectra of uncompensated bonds on the HfO₂-Si interface decreased. Annealing at higher temperatures stimulates crystallization of the HfO₂ films and hafnium silicate is formed on the SiO₂-HfO₂ interface and suboxide SiO _x appears on the HfO₂-Si interface.     

Optical and electrical properties of Ge-implanted SiO2 layers on n-Si and p-Si

Ge ions of 100 keV were implanted into a 120 nm-thick SiO₂ layer on n-Si at room temperature while those of 80 keV were into the same SiO₂ layer on p-Si. Samples were, subsequently, annealed at 500°C for 2 h to effectively induce radiative defects in the SiO₂. Maximum intensities of sharp violet photoluminescence (PL) from the SiO₂/n-Si and the SiO₂/p-Si samples were observed when the samples have been implanted with doses of 1×10¹⁶ and 5×10¹⁵ cm⁻², respectively. According to current–voltage (I–V) characteristics, the defect-related samples exhibit large leakage currents with electroluminescence (EL) at only reverse bias region regardless of the type of substrate. Nanocrystal-related samples obtained by an annealing at 1100°C for 4 h show the leakage at both the reverse and the forward region.     

Structural investigations of silicon nanostructures grown by self-organized island formation for photovoltaic applications

The self-organized growth of crystalline silicon nanodots and their structural characteristics are investigated. For the nanodot synthesis, thin amorphous silicon (a-Si) layers with different thicknesses have been deposited onto the ultrathin (2 nm) oxidized (111) surface of Si wafers by electron beam evaporation under ultrahigh vacuum conditions. The solid phase crystallization of the initial layer is induced by a subsequent in situ annealing step at 700 °C, which leads to the dewetting of the initial a-Si layer. This process results in the self-organized formation of highly crystalline Si nanodot islands. Scanning electron microscopy confirms that size, shape, and planar distribution of the nanodots depend on the thickness of the initial a-Si layer. Cross-sectional investigations reveal a single-crystalline structure of the nanodots. This characteristic is observed as long as the thickness of the initial a-Si layer remains under a certain threshold triggering coalescence. The underlying ultra-thin oxide is not structurally affected by the dewetting process. Furthermore, a method for the fabrication of close-packed stacks of nanodots is presented, in which each nanodot is covered by a 2 nm thick SiO₂ shell. The chemical composition of these ensembles exhibits an abrupt Si/SiO₂ interface with a low amount of suboxides. A minority charge carrier lifetime of 18 µs inside of the nanodots is determined.     

Modification of Optical Characteristics of a Polymer Composite Material under Irradiation

Polymer composites based on polystyrene and modified SiO₂ are synthesized. Effect of the SiO₂ concentration on the surface (thermostatic) properties of the composites is analyzed. Surfaces of composites with different SiO₂ concentrations are microscopically studied. Minor amounts of spherical agglomerates are obtained at relatively high SiO₂ concentrations, and the size of the agglomerates may amount to 80 μm at a SiO₂ concentration of 30 wt %. Variations in the integral absorbance of solar radiation are studied for the polymer composites irradiated with vacuum-UV radiation at a temperature of 125°C.     

Specific features of plastic relaxation of a metastable Ge x Si1 − x layer buried between a silicon substrate and a relaxed germanium layer

Heterostructures Ge/Ge _x Si_{1 ? x} /Si(001) grown by molecular beam epitaxy have been investigated using atomic scale high-resolution electron microscopy. A germanium film (with a thickness of 0.5–1.0 μm) grown at a temperature of 500°C is completely relaxed. An intermediate Ge_0.5Si_0.5 layer remains in a strained metastable state, even though its thickness is 2–4 times larger than the critical value for the introduction of 60° misfit dislocations. It is assumed that the Ge/GeSi interface is a barrier for the penetration of dislocations from a relaxed Ge layer into the GeSi layer. This barrier is overcome during annealing of the heterostructures for 30 min at a temperature of 700°C, after which dislocation networks having different degrees of ordering and consisting predominantly of edge misfit dislocations are observed in the Ge/GeSi and GeSi/Si(001) heteroboundaries.     

Curie temperatures of CoPt ultrathin continuous films

The effects of layer thickness and thermal annealing on Curie temperature have been studied for CoPt ultrathin continuous layers in AlN/CoPt multilayer structures. It is found that there exists a critical thickness below which Curie temperature rapidly decreases due to the loss of spin-spin interactions in the vicinity of interface. After high temperature annealing, the in-plane lattice constant of CoPt film is increased and the exchange coupling parameter is decreased. Consequently, Curie temperatures decrease for some films with large thickness, compared with as-deposited state. Upon annealing at 600?^°C, CoPt undergoes ordering transformation, which also contributes to the degradation of the Curie temperature. However, when the CoPt film thickness is below 2?nm, the Curie temperature is increased after annealing. Especially for 1?nm thick film, the Curie temperature is strikingly increased from 173?^°C to 343?^°C after annealing at 600?^°C. This effect is attributed to the out-of-plane lattice deformation of CoPt thin layers in AlN/CoPt multilayer structures.     

Preparation of PEO ceramic coating on Ti alloy and its high temperature oxidation resistance

Ceramic coatings were prepared in Na₂SiO₃–Na₂CO₃–NaOH system by pulsed bi-polar plasma electrolytic oxidation on Ti–6Al–4V alloy. The phase composition, structure and the elemental distribution of the coatings were studied by XRD, SEM and energy dispersive spectroscopy, respectively. The thermal shock resistance of the coated samples at 850 °C was evaluated by the thermal shock tests. The high temperature oxidation resistance of the coating samples at 500 °C was investigated. The results showed that the coating was mainly composed of rutile- and anatase TiO₂, Increasing the concentration of Na₂SiO₃, TiO₂ content decreased gradually while the thickness of the coating increased. There were a large amount of micro pores and sintered particles on the surface of the coatings. Increasing concentration of Na₂SiO₃, the sintered particles on the surface turned large, and the Si content increased while the Ti content decreased gradually. When the concentration of Na₂SiO₃ was 15 g/L, the thermal shock resistance of the coatings was better than that of the coatings that prepared under other Na₂SiO₃ concentrations. The coating samples prepared under the optimized technique process based on the thermal shock tests improved the high temperature oxidation resistance at 500 °C greatly, whether considering the isothermal oxidation or the cyclic oxidation.