Optimization of ZnO/Ag/ZnO multilayer electrodes obtained by Ion Beam Sputtering for optoelectronic devices

We investigated the electrical and optical properties of ZnO/Ag/ZnO multi-layer electrodes obtained by ion beam sputtering for flexible optoelectronic devices. This multi-layer structure has the advantage of adjusting the layer thickness to favor antireflection and the surface plasmon resonance of the metallic layer. Inserting a thin (Ag) metallic layer between two (ZnO) oxide layers decreases the sheet resistance while widening the optical transmittance window in the visible. We found that the optimal electrode is made up of a 10 nm thin Ag layer between two 35 nm and 20 nm thick ZnO layers, which resulted in a low sheet resistance (R_sq = 6 Ω/square), a high transmittance (T ≥ 80% in the visible) and the highest figure of merit of 1.65 × 10^-2 square/Ω.     

Nanoindentation and micro-mechanical fracture toughness of electrodeposited nanocrystalline Ni-W alloy films

Nanocrystalline nickel-tungsten alloys have great potential in the fabrication of components for microelectromechanical systems. Here the fracture toughness of Ni-12.7 at.%W alloy micro-cantilever beams was investigated. Micro-cantilevers were fabricated by UV lithography and electrodeposition and notched by focused ion beam machining. Load was applied using a nanoindenter and fracture toughness was calculated from the fracture load. Fracture toughness of the Ni-12.7 at.%W was in the range of 1.49-5.14 MPa √m. This is higher than the fracture toughness of Si (another important microelectromechanical systems material), but considerably lower than that of electrodeposited nickel and other nickel based alloys.     

Porous silicon oxide sacrificial layers deposited by pulsed-direct current magnetron sputtering for microelectromechanical systems

The development of silicon oxide layers with high etch rates to be used as sacrificial layers in surface micromachining for microsystems fabrication poses a great technological challenge. In this work, we have investigated the possibility of obtaining easily removable silicon oxide layers by pulsed-direct current (DC) magnetron reactive sputtering. We have carried out a comprehensive study of the influence of the deposition parameters (total pressure and gas composition) on the composition, residual stress and lateral etch rate in fluoride wet solutions of the films. This study has allowed to determine the sputtering conditions to deposit, at high rates (up to 0.1 μm/min), silicon oxide films with excellent characteristics for their use as sacrificial layers. Films with roughness around 5 nm rms, residual stress below 100 MPa and very high lateral etch rate (up to 5 μm/min), around 70 times higher than for thermal silicon oxide, have been achieved. The structural characteristics of these easily removable silicon oxide layers have been assessed by infrared spectroscopy and atomic force microscopy, which have revealed that the films exhibit a porous structure, related to very specific sputter conditions. Finally, the viability of these films has been demonstrated by using them as sacrificial layer in the fabrication process of AlN-based microresonators.     

Intrinsic stress effect on fracture toughness of plasma enhanced chemical vapor deposited SiNx:H films

The apparent fracture toughness for a series of plasma enhanced chemical vapor deposition SiN_x:H films with intrinsic film stress ranging from 300 MPa tensile to 1 GPa compressive was measured using nanoindentation. The nanoindentation results show the measured fracture toughness for these films can vary from as high as > 8 MPa⋅√m for films in compression to as low as < 0.5 MPa⋅√m for the films in tension. Other film properties such as density, Young's modulus, and hydrogen content were also measured and not observed to correlate as strongly with the measured fracture toughness values. Various theoretical corrections proposed to account for the presence of intrinsic or residual stresses in nanoindent fracture toughness measurements were evaluated and found to severely underestimate the impact of intrinsic stresses at thicknesses ≤ 3 μm. However, regression analysis indicated a simple linear correlation between the apparent fracture toughness and intrinsic film stress. Based on this linear trend, a stress free/intrinsic fracture toughness of 1.8 ± 0.7 MPa⋅√m was determined for the SiN_x:H films.     

Single-crystal SiC thin-film produced by epitaxial growth and its application to micro-mechanical devices

This paper deals with the fabrication process of single-crystal silicon carbide (SiC) thin-films and its application to microdevice. SiC thin-film was synthesized using molecular beam epitaxy, where single-crystal SiC layer was grown on single-crystal silicon (Si) substrate. Using lithography and etching process, microscopic cantilevers were fabricated. Typical dimensions of the cantilevers were 10-60 μm in length, 10-30 μm in width, typically 180 nm in thickness. Young's modulus estimated from bending test was almost the same with that of bulk material. Finally, an application is demonstrated where nickel was deposited on the cantilever and biomorphic actuation was carried out. The displacement at the tip was about 2 μm when the temperature change was 40 K. The time constant of the step response was about 0.07 s.     

Thin film removal mechanisms in ns-laser processing of photovoltaic materials

The removal of thin films widely used in photovoltaics (amorphous silicon, tin oxide, zinc oxide, aluminum, and molybdenum) is studied experimentally using multi-kHz Q-switched solid-state lasers at 532 nm and 1064 nm wavelengths. The processing (“scribing”) is performed through the film-supporting glass plate at scribing speeds of the order of m/s. The dependence of the film removal threshold on the laser pulse duration (8 ns to 40 ns) is investigated and the results are complemented by a multi-layer thermal model used for numerical simulations of the laser-induced spatio-temporal temperature field within the samples. Possible film removal mechanisms are discussed upon consideration of optical, geometrical, thermal and mechanical properties of the layers.     

Titanium monoxide ultra-thin coatings evaporated onto polycrystalline copper films

We evaporated polycrystalline copper thin films of thickness between 10 and 100 nm on silicon substrates with their native oxide under ultra-high-vacuum conditions. Some of them were exposed to air for a period ranging from 1 day to 2 weeks. X-ray photoelectron spectroscopy (XPS) revealed a clean copper surface with a trace of oxygen. These films that were exposed to air presented oxides in the state Cu(II), the amount of CuO depended on the time that the film was exposed to air. Subsequently, we deposited TiO ultra-thin films on polycrystalline copper substrates. Both these thin films were formed by electron beam evaporation. XPS spectra showed that the surface of the titanium monoxide (TiO) films was contamination-free. An evaporation of 0.3 nm of TiO reduced the native oxide of the copper substrates from Cu(II) to Cu(I) or Cu(0) and transformed the TiO into TiO₂ at the interface. Low-energy ion spectroscopy showed that the complete coverage of the substrates depends on the thickness of the copper films. For 10 nm copper thin films the complete coverage occurred at 1.5 nm of TiO, and for 100 nm it occurred at 2.0 nm of TiO. In samples exposed to air, the complete coverage occurred at a film thickness slightly higher than those treated under ultra-high-vacuum conditions.     

Measuring the fracture toughness of ultra-thin films with application to AlTa coatings

An experimental technique is presented for measuring the fracture toughness of brittle thin films. In this technique, long rectangular membranes are fabricated from the film of interest using standard silicon micromachining techniques. A focused ion beam is then used to introduce pre-cracks of different lengths along the centerline of the membranes and the membranes are pressurized until rupture. The fracture stress of the membrane is measured as a function of pre-crack length and the fracture toughness of the film is determined from a simple fracture mechanics analysis. The technique is applicable to a wide range of materials and is especially suited for ultra-thin films. We have demonstrated the experimental procedure for a 150 nm AlTa intermetallic film and obtained a room-temperature fracture toughness of K _1c = 4.44 ± 0.21 MPam^1/2.     

Transmission electron microscopy study of Ni–Si nanocomposite films

Nickel induced crystallization of amorphous Si (a-Si) films is investigated using transmission electron microscopy. Metal-induced crystallization was achieved on layered films deposited onto thermally oxidized Si(3 1 1) substrates by electron beam evaporation of a-Si (400 nm) over Ni (50 nm). The multi-layer stack was subjected to post-deposition annealing at 200 and 600 °C for 1 h after the deposition. Microstructural studies reveal the formation of nanosized grains separated by dendritic channels of 5 nm width and 400 nm length. Electron diffraction on selected points within these nanostructured regions shows the presence of face centered cubic NiSi₂ and diamond cubic structured Si. Z-contrast scanning transmission electron microscopy images reveal that the crystallization of Si occurs at the interface between the grains of NiSi₂ and a-Si. X-ray absorption fine structure spectroscopy analysis has been carried out to understand the nature of Ni in the Ni–Si nanocomposite film. The results of the present study indicate that the metal induced crystallization is due to the diffusion of Ni into the a-Si matrix, which then reacts to form nickel silicide at temperatures of the order of 600 °C leading to crystallization of a-Si at the silicide–silicon interface.     

Electrically active, doped monocrystalline silicon nanoparticles produced by hot wire thermal catalytic pyrolysis

Doped silicon nanoparticles have successfully been produced by hot wire thermal catalytic pyrolysis at 40 mbar and a filament temperature of 1800 °C, using a mixture of silane and diborane or phosphine. All particles are monocrystalline with shapes ranging from an octahedron to varying degrees of truncation of this basic shape, with an average diameter of 22 nm. To determine the doping activity, the resistivity of the nanopowders was measured at successive compression levels. While boron doped particles have clean surfaces and are electrically active, with compacted powder having a resistivity of the order of 10³ Ω m, phosphorus doped particles are covered by an oxide layer whose thickness increases from 0.3 nm to 0.6 nm with higher phosphine concentrations. Furthermore, the phosphor atoms are localised at the interface to this surface layer, where they are electrically inactive. These powders have a resistivity in the order of 10⁷ Ω m.     

Visible light emission from silicon dioxide with silicon nanocrystals

An electroluminescent MOS structure was developed using silicon wafers covered by thermal silicon dioxide containing silicon nanocrystals. Efficiency of the structure was sufficient for observation to be possible with the naked eye in daylight conditions under DC polarization. Silicon nanocrystals were produced using silicon ion implantation followed by subsequent annealing at 1100 °C in a nitrogen atmosphere. Three separate bands of emitted light at wavelengths of ∼400-500 nm (blue), ∼500-600 nm (green), and ∼650-850 nm (red) were observed and found to be related to specific regions of the implanted silicon concentration profile. For a single energy implant, each of the emitted light bands originated from a separate depth region of the silicon dioxide layer containing silicon nanocrystals. The spectrum of the emitted light was found to depend on the excess silicon concentration profile. For practical applications, the color of the emitted light can be controlled by adjustment of the implantation parameters and MOS structuring process.     

Improvement of electro-physical properties of ultra-thin PECVD silicon oxynitride layers by high-temperature annealing

Ultra-thin (5 and 6 nm) silicon oxynitride layers have been fabricated by the plasma-enhanced chemical vapour deposition (PECVD) process. Split experiments with annealing of the deposited dielectric layers were performed using the RTP reactor and a standard furnace, both at 900 °C. Possible changes in properties, structure and chemical composition of the obtained layers were investigated by means of spectroscopic ellipsometry, X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS) and electrical characterisation of manufactured test structures (metal-insulator-semiconductor (MIS) capacitors and MISFETs). The results achieved have shown that annealing at high temperature causes improvement of the properties of ultra-thin silicon oxynitride layers (e.g. lower interface traps density, lower leakage currents within the dielectric layer and lower charge-pumping currents of the MISFETs). The observed improvement in electro-physical properties can be attributed to the increase of the SiON phase. Moreover, comparison between the physical thickness and the equivalent oxide thickness (EOT) of the layers shows a decrease in physical thickness obtained by using the silicon oxynitride layer instead of the classical silicon dioxide. These findings are important for the consideration of chances of PECVD oxynitride layer application for CMOS technology.     

Growth of 3C-SiC on 150-mm Si(100) substrates by alternating supply epitaxy at 1000 °C

To lower deposition temperature and reduce thermal mismatch induced stress, heteroepitaxial growth of single-crystalline 3C-SiC on 150 mm Si wafers was investigated at 1000 °C using alternating supply epitaxy. The growth was performed in a hot-wall low-pressure chemical vapor deposition reactor, with silane and acetylene being employed as precursors. To avoid contamination of Si substrate, the reactor was filled in with oxygen to grow silicon dioxide, and then this thin oxide layer was etched away by silane, followed by a carbonization step performed at 750 °C before the temperature was ramped up to 1000 °C to start the growth of SiC. Microstructure analyses demonstrated that single-crystalline 3C-SiC is epitaxially grown on Si substrate and the film quality is improved as thickness increases. The growth rate varied from 0.44 to 0.76 ± 0.02 nm/cycle by adjusting the supply volume of SiH₄ and C₂H₂. The thickness nonuniformity across wafer was controlled with ± 1%. For a prime grade 150 mm virgin Si(100) wafer, the bow increased from 2.1 to 3.1 μm after 960 nm SiC film was deposited. The SiC films are naturally n type conductivity as characterized by the hot-probe technique.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

Effect of laser shock processing on fatigue crack growth of duplex stainless steel

Duplex stainless steels have wide application in different fields like the ship, petrochemical and chemical industries that is due to their high strength and excellent toughness properties as well as their high corrosion resistance. In this work an investigation is performed to evaluate the effect of laser shock processing on some mechanical properties of 2205 duplex stainless steel. Laser shock processing (LSP) or laser shock peening is a new technique for strengthening metals. This process induces a compressive residual stress field which increases fatigue crack initiation life and reduces fatigue crack growth rate. A convergent lens is used to deliver 2.5 J, 8 ns laser pulses by a Q-switched Nd:YAG laser, operating at 10 Hz with infrared (1064 nm) radiation. The pulses are focused to a diameter of 1.5 mm. Effect of pulse density in the residual stress field is evaluated. Residual stress distribution as a function of depth is determined by the contour method. It is observed that the higher the pulse density the greater the compressive residual stress. Pulse densities of 900, 1600 and 2500 pul/cm² are used. Pre-cracked compact tension specimens were subjected to LSP process and then tested under cyclic loading with R = 0.1. Fatigue crack growth rate is determined and the effect of LSP process parameters is evaluated. In addition fracture toughness is determined in specimens with and without LSP treatment. It is observed that LSP reduces fatigue crack growth and increases fracture toughness if this steel.     

Size effect on fracture toughness of freestanding copper nano-films

We conducted fracture toughness experiments on freestanding copper films with thicknesses ranging from about 800 to 100 nm deposited by electron beam evaporation to elucidate the size effect on fracture toughness in the nano- or submicron-scale. It was found that initially, the crack propagated stably under loading, and then the crack propagation rate rapidly increased, resulting in unstable fracture. The fracture toughness K_C was estimated on the basis of the R-curve concept to be 7.81 ± 1.22 MPa m^1/2 for the 800-nm-thick film, 6.63 ± 1.05 MPa m^1/2 for the 500-nm-thick film and 2.34 ± 0.54 MPa m^1/2 for the 100-nm-thick film. Thus, a clear size effect was observed. The fracture surface suggested that the crack underwent large plastic deformation in the thicker 800-nm and 500-nm films, whereas it propagated with highly localized plastic deformation in the thinner 100-nm film. This size effect in fracture toughness might be related to a transition in deformation and fracture morphology near the crack tip.     

Development of analytical model for strained silicon relaxation on (100) fully relaxed Si0.8Ge0.2 pseudo-substrates

Early stages of strained silicon (sSi) relaxation during the growth on (100) Si_0.8Ge_0.2 pseudo-substrates with low threading dislocation density (3 · 10^+ 4/cm²) have been studied. Threading dislocations are only observed in sSi layers at early stages of growth whereas Shockley partial dislocations appear at thicknesses of sSi above 18 nm. By analyzing the dislocation types in different sSi layers we observed three different regimes of relaxation:

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for sSi thickness below 15 nm, no dislocation generation is observed,

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for sSi thickness between 15 nm and 18 nm, threading dislocation density increases but no stacking faults are generated,

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for sSi thickness above 18 nm, threading dislocation density decreases as well as Shockley partial dislocation density increases due to the splitting of threading dislocations into partial dislocations. In this regime the stacking fault linear density has a logarithmic dependence with sSi thickness.

We developed an analytical model to describe stacking fault linear density evolution with sSi thickness and we showed that 18 nm threshold thickness for dislocation splitting corresponds to an intrinsic stacking fault energy of 90 mJ/m² in sSi.     

Ellipsometric characterization of SiOx films with embedded Si nanoparticles

In this work we present results on the ellipsometric study of SiO_x films in the spectral range of 280-820 nm. The films were deposited by vacuum thermal evaporation of SiO onto Si substrates heated at 150 °C. To stimulate the formation of silicon clusters in the oxide matrix the films were annealed at temperatures 700, 1000 and 1100 °C in argon for 5, 15 and 30 min. By applying the Bruggeman effective-medium approximation theory and using multiple-layer optical models, from the ellipsometric data analysis the thickness, complex refractive index and composition of the films, as well as the size of the embedded Si nanocrystallites have been determined. Atomic-force microscopy imaging showed a very smooth surface, the roughness value of which correlated well with the top-layer thickness, determined from the ellipsometric data analysis.     

An X-ray photoelectron spectroscopy study of ultra-thin oxynitride films

Oxynitrides prepared by nitridation of 2 to 5 nm SiO₂ films on silicon, were studied by X-ray photoelectron spectroscopy at two analyser exit angles. An iterative procedure was applied to obtain simultaneously the average nitrogen content and the thickness of the nitrided layer, mutually dependent via the electron transport properties of the layer matrix. Inelastic mean free paths and elastic corrections thereof were determined in accordance with ISO18118:2004(E), whereas a set of empirical relative sensitivity factors was used. The results reveal a significant increase of the 2 nm film thickness upon nitrogen incorporation of the order of 50 at.%, whereas the 5 nm films retain their thickness upon comparable extent of nitridation.     

Low refractive index silicon oxide coatings at room temperature using atmospheric-pressure very high-frequency plasma

Low refractive index silicon oxide films were deposited using atmospheric-pressure He/SiH₄/CO₂ plasma excited by a 150-MHz very high-frequency power. Significant increase in deposition rate at room temperature could prevent the formation of dense SiO₂ network, decreasing refractive index of the resulting film effectively. As a result, a silicon oxide film with the lowest refractive index, n = 1.24 at 632.8 nm, was obtained with a very high deposition rate of 235 nm/s. The reflectance and transmittance spectra showed that the low refractive index film functioned as a quarter-wave anti-reflection coating of a glass substrate.