The effect of intragranular microstress in Al2O3—SiC nanocomposites

A theoretical model is established to investigate the intragranular particle residual stress in Al2O3-SiC nanocomposites.Using this model,we calculate the average compressive stress on the Al2O3 grain boundary(GB) and the average tensile stress within Al2O3 grains caused by SiC nanoparticles.The normal compressive stress strengthens the GB,and the average tensile stress weakens the grains.The model gives a reasonable interpretation of the strength changes of Al2O3-SiC nanocomposites with the number of SiC particles.     

X-ray spectral analysis of the interface of a thin Al<Subscript>2</Subscript>O<Subscript>3</Subscript> film prepared on silicon by atomic layer deposition

The extent and phase chemical composition of the interface forming under atomic layer deposition (ALD) of a 6-nm-thick Al₂O₃ film on the surface of crystalline silicon (c-Si) has been studied by depthresolved, ultrasoft x-ray emission spectroscopy. ALD is shown to produce a layer of mixed Al₂O₃ and SiO₂ oxides about 6–8 nm thick, in which silicon dioxide is present even on the sample surface and its concentration increases as one approaches the interface with the substrate. It is assumed that such a complex structure of the layer is the result of interdiffusion of oxygen into the layer and of silicon from the substrate to the surface over grain boundaries of polycrystalline Al₂O₃, followed by silicon oxidation. Neither the formation of clusters of metallic aluminum near the boundary with c-Si nor aluminum diffusion into the substrate was revealed. It was established that ALD-deposited Al₂O₃ layers with a thickness up to 60 nm have similar structure.     

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.     

Stress relaxation of GaN microstructures on a graphene‐buffered Al2O3 substrate

GaN microstructures were grown on c‐Al₂O₃ with a multi‐stacked graphene buffered layer using metal metal‐organic chemical‐vapor deposition. Under the same growth conditions, the nucleation of GaN was suppressed by the low surface energy of graphene, resulting in a much lower density of microstructures relative to those grown on c‐Al₂O₃. Residual stress in the GaN microstructures was estimated from the peak shift of the E₂ phonon using micro‐Raman spectroscopy. The results showed that the compressive stress of approximately 0.36 GPa in GaN on c‐Al₂O₃ caused by lattice mismatch and the difference in the thermal expansion coefficient was relaxed by introducing the graphene layer. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The structure and optical characters of the ZnO film grown on GaAs/Al2O3 substrate

In this paper ZnO films are grown on GaAs/Al₂O₃ substrates at different temperature by metal-organic chemical vapor deposition (MOCVD). The GaAs/Al₂O₃ substrates are formed by depositing GaAs layer (∼35 nm) on the Al₂O₃ substrate. The results of X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) demonstrate that most of the Ga and As atoms form Ga-As bond and the GaAs layer does not present any orientation. The characters of the ZnO films grown on GaAs/Al₂O₃ substrates are investigated by XRD, photoluminescence (PL), atomic force microscopy (AFM) and Raman scattering. Compared with ZnO film grown on Al₂O₃ substrate, ZnO film prepared by our fabrication scheme has good crystal and optical quality. Meanwhile its grain size becomes bigger according to the AFM image. Raman analysis indicates that the intrinsic defects and the in-plane tensile stress are obviously reduced in ZnO/GaAs/Al₂O₃ samples.     

晶圆键合和激光剥离工艺对GaN基垂直结构发光二极管芯片残余应力的影响

GaN基发光二极管(LED)中的残余应力状态对器件的性能和稳定性有很大影响. 通过使用三种不同的键合衬底(Al₂O₃衬底, CuW衬底和Si衬底)以及改变键合温度(290 ℃, 320 ℃, 350 ℃和380 ℃), 并且使用不同的激光能量密度(875, 945和1015 mJ·cm^-2) 进行激光剥离, 制备了不同应力状态的GaN基LED器件. 对不同条件下GaN LED进行弯曲度、Raman 散射谱测试. 实验结果表明, 垂直结构LED中的残余应力的状态是键合衬底和键合金属共同作用的结果, 而键合温度影响着垂直结构LED中的残余应力的大小. 激光剥离过程中, 一定能量密度下激光剥离工艺一般不会对芯片中的残余应力造成影响, 但是如果该工艺对GaN 层造成了微裂缝, 则会在一定程度上起到释放残余应力的作用. 使用Si衬底键合后, 外延蓝宝石衬底翘曲变大, 对应制备的GaN基垂直结构 LED中的残余应力为张应力, 并且随着键合温度的上升而变大; 而Al₂O₃和CuW衬底制备的LED中的残余应力为压应力, 但使用Al₂O₃衬底键合制备的LED中压应力随键合温度上升而一定程度变大, CuW 衬底制备的LED中压应力随键合温度上升而下降.     

Properties of an Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Si interface

The phase chemical composition of an Al₂O₃/Si interface formed upon molecular deposition of a 100-nm-thick Al₂O₃ layer on the Si(100) (c-Si) surface is investigated by depth-resolved ultrasoft x-ray emission spectroscopy. Analysis is performed using Al and Si L_{2, 3} emission bands. It is found that the thickness of the interface separating the c-Si substrate and the Al₂O₃ layer is approximately equal to 60 nm and the interface has a complex structure. The upper layer of the interface contains Al₂O₃ molecules and Al atoms, whose coordination is characteristic of metallic aluminum (most likely, these atoms form sufficiently large-sized Al clusters). The shape of the Si bands indicates that the interface layer (no more than 10-nm thick) adjacent to the substrate involves Si atoms in an unusual chemical state. This state is not typical of amorphous Si, c-Si, SiO₂, or SiO_x (it is assumed that these Si atoms form small-sized Si clusters). It is revealed that SiO₂ is contained in the vicinity of the substrate. The properties of thicker coatings are similar to those of the 100-nm-thick Al₂O₃ layer and differ significantly from the properties of the interfaces of Al₂O₃ thin layers.     

Stress, absorptance and laser-induced damage threshold properties of 355-nm HR coatings

A number of 355-nm Al₂O₃/MgF₂ high-reflectance (HR) coatings were prepared by electron-beam evaporation. The influences of the number of coating layers and deposition temperature on the 355-nm Al₂O₃/MgF₂ HR coatings were investigated. The stress was measured by viewing the substrate deformation before and after coating deposition using an optical interferometer. The laser-induced damage threshold (LIDT) of the samples was measured by a 355-nm Nd:YAG laser with a pulse width of 8 ns. Transmittance and reflectance of the samples were measured by a Lambda 900 spectrometer. It was found that absorptance was the main reason to result in a low LIDT of 355-nm Al₂O₃/MgF₂ HR coatings. The stress in Al₂O₃/MgF₂ HR coatings played an unimportant role in the LIDT, although MgF₂ is known to have high tensile stress.     

Effect of interfacial debonding and matrix cracking on mechanical properties of multidirectional composites

In composites, debonding at the fiber–matrix interface and matrix cracking due to loading or residual stresses can effect the mechanical properties. Here three different architectures — 3-directional orthogonal, 3-directional 8-harness satin weave and 4-directional in-plane multidirectional composites — are investigated and their effective properties are determined for different volume fractions using unit cell modeling with appropriate periodic boundary conditions. A cohesive zone model (CZM) has been used to simulate the interfacial debonding, and an octahedral shear stress failure criterion is used for the matrix cracking. The debonding and matrix cracking have significant effect on the mechanical properties of the composite. As strain increases, debonding increases, which produces a significant reduction in all the moduli of the composite. In the presence of residual stresses, debonding and resulting deterioration in properties occurs at much lower strains. Debonding accompanied with matrix cracking leads to further deterioration in the properties. The interfacial strength has a significant effect on debonding initiation and mechanical properties in the absence of residual stresses, whereas, in the presence of residual stresses, there is no effect on mechanical properties. A comparison of predicted results with experimental results shows that, while the tensile moduli E ₁₁, E ₃₃and shear modulus G ₁₂ match well, the predicted shear modulus G ₁₃ is much lower.     

Characterization of a new substrate for tunneling spectroscopy

An insulating layer is produced on aluminum by glow discharge in CF₄. This substrate, used as the insulator of metal-insulator-metal diodes is characterized by Inelastic Electron Tunneling Spectroscopy as an aluminum trifluoride AlF₃. The adsorption of ammonia, benzylamine. formic and propiolic acid on this substrate is investigated. A comparison between spectra of samples obtained on this insulator and on alumina for the same dopant molecules shows significant differences which are interpreted as revealing an enhanced Lewis acidity of AlF₃ relative to Al₂O₃, determined — at least in part — by an enhanced electronegativity of surface Al⁺ cations of AlF₃.     

The diffusion of silicon atoms in stack structures of La2O3 and Al2O3

The interfacial reactions and electrical characteristics of stack structures of La₂O₃ and Al₂O₃ were investigated as a function of the annealing temperature. In the case of Al₂O₃/La₂O₃/Si (ALO structure), the La₂O₃ in contact with the Si substrate was readily transformed into La-silicate by the diffusion of Si atoms, while in the case of La₂O₃/Al₂O₃/Si (LAO structure), interfacial reactions between the Al₂O₃ layer and the Si substrate were suppressed. After an annealing treatment at 700 °C, the Al₂O₃ in the ALO structure can play an effective role in blocking the hydration of La₂O₃, resulting in an unchanged interfacial layer. However, the Al₂O₃ layer in the LAO structure was unable to suppress the diffusion of Si atoms into the La₂O₃ film. When the annealing temperature reached 900 °C, both structures showed a similar depth distribution with a high content of Si atoms diffused into the films. The change in the elemental distributions via the diffusion and reaction of Si atoms affected the electrical characteristics at the interface between ALO/LAO structure and Si substrate, specifically the trap charge density (D_it) and band gap (E_g) values.     

Improving Fe3Al alloy resistance against high temperature oxidation by pack cementation process

The paper presents the results of oxidation tests of Fe₃Al-based alloys containing additions of Cr, Zr, B, and C, with and without an aluminide coating. The coating was formed by a pack cementation process in which the surface of material got enriched in aluminum. The Al-rich layer was intended to enhance the tendency of Al₂O₃ formation. The slow-growing Al₂O₃ scale provides the best corrosion protection for structural materials at high temperatures. The cyclic oxidation tests were performed in laboratory air at 1373 K. The structure and composition of oxide scales as well as their adherence were evaluated and compared for the materials with and without aluminide coatings. Surface enrichment in aluminum and effect minor addition of Zr on oxidation behavior was discussed.     

Study of microstructure and phase evolution of hot-dipped aluminide mild steel during high-temperature diffusion using electron backscatter diffraction

Mild steel was coated by hot-dipping into a molten aluminum bath. The microstructure and phase evolution in the aluminide layer during diffusion at 750 °C in static air were analyzed by electron backscatter diffraction (EBSD). The results showed that the aluminide layer of the as-coated specimen consisted of an outer aluminum topcoat, minor FeAl₃ and major Fe₂Al₅, respectively. Also, Fe₂Al₅ possessed a tongue-like morphology, which caused corresponding serration-like morphology in the steel substrate. A portion of the peaks of serration-like substrate were isolated, after short exposure at 750 °C, and accompanied by the formation of voids, which continued to appear with further exposure at 750 °C. As the aluminum topcoat was consumed, FeAl₃ phase disappeared and left an aluminide layer of Fe₂Al₅ phase. After 60 min of exposure, FeAl₂ and FeAl phases formed at the interface between Fe₂Al₅ and the steel substrate. With increasing exposure time, the voids condensed and the serration-like morphology disappeared, while FeAl₂ and FeAl phases kept growing. After prolonged exposure, the aluminide layer was composed of FeAl₂ and FeAl and possessed a flat interface between FeAl and steel substrate.     

Interfacial reactions and oxidation behavior of Al2O3 and Al2O3/Al coatings on an orthorhombic Ti2AlNb alloy

The uniform and dense Al₂O₃ and Al₂O₃/Al coatings were deposited on an orthorhombic Ti₂AlNb alloy by filtered arc ion plating. The interfacial reactions of the Al₂O₃/Ti₂AlNb and Al₂O₃/Al/Ti₂AlNb specimens after vacuum annealing at 750 °C were studied. In the Al₂O₃/Ti₂AlNb specimens, the Al₂O₃ coating decomposed significantly due to reaction between the Al₂O₃ coating and the O-Ti₂AlNb substrate. In the Al₂O₃/Al/Ti₂AlNb specimens, a γ-TiAl layer and an Nb-rich zone came into being by interdiffusion between the Al layer and the O-Ti₂AlNb substrate. The γ-TiAl layer is chemically compatible with Al₂O₃, with no decomposition of Al₂O₃ being detected. No internal oxidation or oxygen and nitrogen dissolution zone was observed in the O-Ti₂AlNb alloy. The Al₂O₃/Al/Ti₂AlNb specimens exhibited excellent oxidation resistance at 750 °C.     

The effective reinforcement of magnesium alloy ZK60A using Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles

ZK60A nanocomposite containing Al₂O₃ nanoparticle reinforcement (50 nm average size) was fabricated using solidification processing followed by hot extrusion. The nanocomposite exhibited similar grain size to the monolithic alloy, reasonable Al₂O₃ nanoparticle distribution, non-dominant (0 0 0 2) texture in the longitudinal direction, and 15% higher hardness than the monolithic alloy. Compared to the monolithic alloy (in tension), the nanocomposite exhibited lower yield strength (0.2%TYS) (−4%) and higher ultimate strength (UTS), failure strain, and work of fracture (WOF) (+13%, +170%, and +200%, respectively). Compared to the monolithic alloy (in compression), the nanocomposite exhibited lower yield strength (0.2%CYS) (−5%) and higher ultimate strength (UCS), failure strain, and WOF (+6%, +41%, and +43%, respectively). The effects of Al₂O₃ nanoparticle addition on the enhancement of tensile and compressive properties of ZK60A are investigated in this article.     

Pt–Al2O3 nanocoatings for high temperature concentrated solar thermal power applications

Nano-phased structures based on metal–dielectric composites, also called cermets (ceramic–metal), are considered among the most effective spectral selective solar absorbers. For high temperature applications (stable up to 650 °C) noble metal nanoparticles and refractory oxide host matrices are ideal as per their high temperature chemical inertness and stability: Pt/Al₂O₃ cermet nano-composites are a representative family. This contribution reports on the optical properties of Pt/Al₂O₃ cermet nano-composites deposited in a multilayered tandem structure. The radio-frequency sputtering optimized Pt/Al₂O₃ solar absorbers consist of stainless steel substrate/ Mo coating layer/ Pt–Al₂O₃/ protective Al₂O₃ layer and stainless steel substrate/ Mo coating layer /Pt–Al₂O₃ for different composition and thickness of the Pt–Al₂O₃ cermet coatings. The microstructure, morphology, theoretical modeling and optical properties of the coatings were analyzed by the x-ray diffraction, atomic force, microscopy, effective medium approximation and UV–vis specular and diffuse reflectance.     

Fabrication of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al structure by nitric acid oxidation at room temperature

A thick Al₂O₃/aluminum (Al) structure has been fabricated by oxidation of Al with 68wt% and 98wt% nitric acid (HNO₃) aqueous solutions at room temperature. Measurements of the Al₂O₃ thickness vs. the oxidation time show that reaction and diffusion are the rate-determining steps for oxidation with 68wt% and 98wt% HNO₃ solutions, respectively. Observation of transmission electron micrographs shows that the Al₂O₃ layer formed with 68wt% HNO₃ has a structure with cylindrically shaped pores vertically aligned from the Al₂O₃ surface to the Al₂O₃/Al interface. Due to the porous structure, diffusion of HNO₃ proceeds easily, resulting in the reaction-limited oxidation mechanism. In this case, the Al₂O₃/Al structure is considerably rough. The Al₂O₃ layer formed with 98wt% HNO₃ solutions, on the other hand, possesses a denser structure without pores, and the Al₂O₃/Al interface is much smoother, but the thickness of the Al₂O₃ layer formed on crystalline Al regions is much smaller than that on amorphous Al regions. Due to the relatively uniform Al₂O₃ thickness, the leakage current density flowing through the Al₂O₃ layer formed with 68wt% HNO₃ is lower than that formed with 98wt% HNO₃.     

Structure of Al2O3 thin layers synthesized on the silicon surface by atomic layer deposition

The distribution of the phase and chemical composition at an Al₂O₃/Si interface is studied by depth-resolved ultrasoft x-ray emission spectroscopy. The interface is formed by atomic layer deposition of Al₂O₃ films of various thicknesses (from several to several nanometers to several hundreds of nanometers) on the Si(100) surface (c-Si) or on a 50-nm-thick SiO₂ buffer layer on Si. L _2,3 bands of Al and Si are used for analysis. It is found that the properties of coatings and Al₂O₃/Si interfaces substantially depend on the thickness of the Al₂O₃ layer, which is explained by the complicated character of the process kinetics. At a small thickness of coatings (up to 10–30 nm), the Al₂O₃ layer contains inclusions of oxidized Si atoms, whose concentration increases as the interface is approached. As the thickness increases, a layer containing inclusions of metallic Al clusters forms. A thin interlayer of Si atoms occurring in an unconventional chemical state is found. When the SiO₂ buffer layer is used (Al₂O₃/SiO₂/Si), the structure of the interface and the coating becomes more perfect. The Al₂O₃ layer does not contain inclusions of metallic aluminum, does not vary with the sample thickness, and has a distinguished boundary with silicon.     

Influence of heat treatment on microstructure and mechanical properties of the interface in an EN AW-6082/1.4310 composite extrusion

The presented paper deals with a unidirectional steel wire reinforced aluminum matrix composite manufactured by composite extrusion. The main objective of this work was to determine the effect of heat treatment, and the influence of long solution annealing times on the composites interface regarding microstructural changes and the resulting interface strength. For evaluation of the microstructure high resolution transmission electron microscope (TEM) investigations accompanied with electron dispersive X-ray spectroscopy (EDX) were performed. It could be shown that diffusion from the steel wire into the aluminum matrix occurs and that the diffusion paths as well as particle formation is influenced by the preceded heat treatment. Diffusion paths in the range of 40–150 nm could be observed for Al, Fe, Cr and Ni. After annealing times over 5 h an extensive growth of an intermetallic reaction layer was found. The mechanical properties of the interface were determined by push-out-tests and tensile tests radial to the interface, which provided the debonding shear strength σ_deb and for the latter experiment the interfacial radial strength σ_IR. It has become apparent that debonding shear strength is highly influenced by matrix properties. In radial tensile tests the failure is predominantly controlled by the chemical bond of the interface. It was shown that interface strength of specimen with small reaction zones of about 3 μm were beneficial for the mechanical behavior in both loading conditions. Longer annealing times showed a drastic decrease of interface shear strength. It was concluded from EDX measurements and in comparison with literature that the reaction zone is dominated by the growth of Al₅Fe₂ (η-phase).     

Silicon solar cells with Al2O3 antireflection coating

The paper presents the possibility of using Al₂O₃ antireflection coatings deposited by atomic layer deposition ALD. The ALD method is based on alternate pulsing of the precursor gases and vapors onto the substrate surface and then chemisorption or surface reaction of the precursors. The reactor is purged with an inert gas between the precursor pulses. The Al₂O₃ thin film in structure of the finished solar cells can play the role of both antireflection and passivation layer which will simplify the process. For this research 50×50 mm monocrystalline silicon solar cells with one bus bar have been used. The metallic contacts were prepared by screen printing method and Al₂O₃ antireflection coating by ALD method. Results and their analysis allow to conclude that the Al₂O₃ antireflection coating deposited by ALD has a significant impact on the optoelectronic properties of the silicon solar cell. For about 80 nm of Al₂O₃ the best results were obtained in the wavelength range of 400 to 800 nm reducing the reflection to less than 1%. The difference in the solar cells efficiency between with and without antireflection coating was 5.28%. The LBIC scan measurements may indicate a positive influence of the thin film Al₂O₃ on the bulk passivation of the silicon.