Comparison of microstructures and tensile properties of pulse electrodeposited Ni on polycrystalline and amorphous substrates

Abstract

Ultrafine grained nickel (UFG Ni) and microcrystalline nickel (MC Ni) were fabricated on two types of substrates, i.e. the amorphous (Ni–P) and polycrystalline (stainless steel) substrates by pulse electrodeposition without additives. This study demonstrates that when inhibiting the epitaxial growth by first depositing a thin amorphous layer on the polycrystalline substrates, the grain size of the subsequent Ni deposit decreases dramatically from microscale to the UFG regime, which depends on the deposition conditions. Compared with MC Ni, which has an ultimate tensile strength σ_UTS of 397 MPa and an elongation to failure ε_TEF of 11·98%, UFG Ni with an average grain size of 120·72 nm exhibits an enhanced σ_UTS of 807 MPa and a comparable ε_TEF of 10·44%. The electrodeposited method used in this study provides an effective and low cost way to produce UFG materials with both high strength and ductility, which can meet the demands for practical application as structural materials.     

Synthesis of Silver Nanoparticles by a Laser–Liquid–Solid Interaction Technique

Silver nanoparticles of high chemical homogeneity have been synthesized by a novel laser–liquid–solid interaction technique from a solution composed of silver nitrate, distilled water, ethylene glycol, and diethylene glycol. Rotating nickel, niobium, stainless steel, and ceramic Al₂O₃ substrates were irradiated using a continuous-wave CO₂ laser and Q-switched Nd–YAG laser ( = 1064 and 532 nm). The silver nanoparticles were characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM), and electron probe x-ray microanalysis (EPMA). The shape of silver particles was dependent on the chemical composition and laser parameters. The synthesis mechanism of silver nanoparticles has been proposed to occur primarily at the laser–liquid–substrate interface by a nucleation and growth mechanism.     

The growth and physical properties of low pressure chemically vapour-deposited films of tantalum silicide on n+-type polycrystalline silicon

Bilayer films of tantalum silicide on n⁺-type polycrystalline silicon prepared by low pressure chemical vapour deposition (LPCVD) were fabricated from SiH₄ and TaCl₅ in a single standard hot-wall LPCVD reactor. The main advantages over conventional co-sputtered films are reduced wafer handling, improved conformal deposition, increased wafer throughput and the use of only one piece of process equipment. Both films of the bilayer structure are deposited at 575°C and annealing is carried out in the deposition reactor at 900°C. The amorphous deposited silicon films were doped in situ with PH₃. The stoichiometry of the as-deposited tantalumrich Ta₅Si₃ films is shifted to the desired low resistivity TaSi₂ during the annealing process, in which the additional silicon required is supplied from the underlying polycrystalline silicon. The resistivity of annealed LPCVD tantalum silicide films is 60–70μΩ cm which is comparable with that of films prepared by co-sputtering. The peak-to-valley surface roughness of 30 nm is at present typically a factor of 2 larger than that for co-sputtered films. Wet oxidation experiments indicate that there is no large difference in the thermal SiO₂ formation between LPCVD and co-sputtered tantalum silicide.     

Thin film growth of epitaxial, polycrystalline and amorphous SrRuO3

The SrRuO₃ thin films were grown on amorphous fused silica and (100) single crystal LaAlO₃ substrates by pulsed laser deposition method. On fused silica substrates, polycrystalline SrRuO₃ thin film was obtained and below the crystallization temperature, SrRuO₃ thin films show an amorphous phase. For the case of epitaxial growth on (100) single crystal LaAlO₃ substrate, the crystallization temperature of SrRuO₃ thin film was increased by ∼ 100 °C indicating that additional energy is necessary in order to obtain the epitaxial thin film. By using the eclipse method and the control of substrate temperature, the variations of surface morphologies and grain size were observed by atomic force microscope. Below the crystallization temperature, amorphous SrRuO₃ thin film shows hopping transport property of an insulator.     

Synthesis of Micron and Submicron Nickel and Nickel Oxide Particles by a Novel Laser–Liquid Interaction Process

The laser–liquid–solid interaction is a new technique for synthesis of nickel and nickel oxide particles. The process uses a continuous-wave CO₂ laser beam as the source of thermal energy required to induce precipitation reactions in solution. The uniqueness of the process is the synthesis reaction taking place in a localized region, which allows better control of the chemical reaction. Porous nickel and nickel oxide powders have been synthesized by laser-induced reactions between a nickel nitrate hexahydrate [Ni(NO₃)₂·6H₂O] precursor and 2-ethoxyethanol-based mixtures. Nickel powders were produced after irradiating a solution of the precursor salt and a 2-ethoxyethanol and d-sorbitol mixture. Crystalline nickel oxide (NiO) powders were isolated after irradiating a solution containing the precursor salt and a 2-ethoxyethanol and water mixture. Powders containing both nickel and nickel oxide crystalline phases were produced after irradiating a solution of the precursor salt and 2-ethoxyethanol. The mean particle diameter is found to be sensitive to irradiation time, substrate thermal conductivity, irradiation power density, and solution concentration. It is hypothesized that nucleation and growth of crystalline phases occurring in irradiated solutions are thermal driven.     

In situ electrical conductivity and amorphous-crystalline transition in vacuum-deposited thin films of Se20Te80 alloy

In situ electrical conductivity measurements have been carried out on vacuum-deposited thin films of Se₂₀Te₈₀ alloy during heating and cooling cycles. The electrical conductivity and X-ray diffraction studies show that the as-grown Se₂₀Te₈₀ films are amorphous and, upon heating, undergo an irreversible amorphous-crystalline transition between 315 and 350 K. The observation that the as-grown thin films (deposited at room temperature on glass substrates) are amorphous is in contrast to earlier observations by other workers who find that they are polycrystalline. Above the transition temperature, the electrical conductivity of the polycrystalline Se₂₀Te₈₀ films changes as an exponential function of reciprocal temperature. The amorphous-crystalline transition in Se₂₀Te₈₀ thin films is broad, with films of high initial resistance having lower transition temperatures and low-resistance films having higher transition temperatures. The observation of a broad transition in the case of the present Se₂₀Te₈₀ thin films has to be contrasted with our earlier observations of sharp transitions in the case of Se₈₀Te₂₀ and Se₅₀Te₅₀ thin films.     

Laser surface melting and alloying of type 304L stainless steel

Microstructures of laser surface melted (LSM) and alloyed (molybdenum and tantalum) type 304L stainless steel have been studied. -ferrite was found to be the primary solidification phase for these alloys. Chemical analysis of the laser-processed layers indicated no compositional variation between the as-received and laser-processed layers in terms of major alloying elements, i.e. chromium and nickel. However, laser processing resulted in a lowered manganese content, by about 15%. Furthermore, TEM studies showed laser processing to introduce extensive amorphous Mn-Si precipitation into the microstructure.     

X-ray photoemission study of Fe40Ni40B20 metallic glass

X-ray photoelectron spectroscopic (XPS) study of the valence band and the core levels of amorphous Fe₄₀Ni₄₀B₂₀ are presented. The oxides which formed at the surface of as-received sample are due to oxidation of iron and boron. For etched samples, the presence of oxide is not discernible, and the chemical environment is predominantly iron-boron-like, while nickel remains unassociated. The valence band has a high density of states at Fermi levels of amorphous Fe₄₀Ni₄₀B₂₀ are presented. The oxides which formed at the surface of B2s and Fe3d states, and metalloids-states respectively.     

Simultaneous recrystallization, phosphorous diffusion and antireflection coating of silicon films using laser treatment

Laser technique application to polycrystalline silicon thin-film solar cell fabrication on glass substrates has received appreciable attention. In this paper, a laser-doping technique is developed for plasma-deposited amorphous silicon film. A process involving recrystallization, phosphorous diffusion and antireflection coating can be achieved simultaneously using the laser annealing process. The doping precursor, a phosphorous-doped titanium dioxide (TiO₂) solution, is synthesized using a sol-gel method and spin-coated onto the sample. After laser irradiation, the polycrystalline silicon grain size was about 0.5∼1.0 μm with a carrier concentration of 2 × 10¹⁹ cm^− 3 and electron mobility of 92.6 cm²/V s. The average polycrystalline silicon reflectance can be reduced to a value of 4.65% at wavelengths between 400 and 700 nm, indicating the upper TiO₂ film of antireflection coating.     

A.c. photoconductivity and optical properties of bulk polycrystalline and amorphous In x Se1−x thin films

The a.c. photoconductivity of bulk polycrystalline In _x Se_1–x and the optical properties of amorphous In _x Se_1–x thin films were investigated. The effect of heat treatment on the absorption coefficient of InSe thin films was also studied. The spectral response of the photoconductivity of polycrystalline In _x Se_1–x related to the near-edge absorption spectrum, shows a well-defined maximum corresponding to the width of the forbidden gap. Polycrystalline In _x Se_1–x realizes the behaviour of photoconductors which are sensitive in a spectral range between 400 and 1700 nm. Optical absorption of amorphous In _x Se_1–x thin films was recorded as a function of photon energy and the data were used to deduce the value of optical energy gap of the films. It was found that the optical energy gap decreased with increasing indium content in both bulk polycrystalline and amorphous thin films. The effect of heat treatment on the optical gap of the film has been interpreted in terms of the density of states model of Mott and Davis.     

Plate-shaped Yb:LuPO4 crystal for efficient CW and passively Q-switched microchip lasers

It is demonstrated that plate-shaped crystals of Yb:LuPO₄, which are grown from spontaneous nucleation by high-temperature solution method, can be utilized to make microchip lasers operating in continuous-wave (CW) or passively Q-switched mode. Efficient operation of such a microchip laser, which is built with a 0.3 mm thick crystal plate in a 2 mm long plane-parallel cavity, is realized at room temperature. With 2.37 W of pump power absorbed, 1.45 W of CW output power is generated with a slope efficiency of 73%. When passively Q-switched with a Cr⁴⁺:YAG crystal plate as saturable absorber, the laser produces a maximum pulsed output power of 0.53 W at 1013.3 nm, at a pulse repetition rate of 23.8 kHz, the resulting pulse energy, duration, and peak power are 22.3 μJ, 4.0 ns, and 5.6 kW, respectively.     

Fabrication and Transport Properties of MgB2 Thin Films and Tunnel Junctions

We report on fabrication and characterization of MgB₂ thin films and tunnel junction structures. The MgB₂ films were prepared on Al₂O₃, Si, glass, and plastic foil substrates by either vacuum codeposition of boron and magnesium, or high-temperature magnesium annealing of boron films. The crystalline structure of our films depended directly on the method of preparation. The films prepared by codeposition and postannealed in Ar atmosphere were amorphous with nanocrystal inclusions and were characterized by very smooth surfaces. On the other hand, the boron-precursor films annealed in magnesium vapor were rough, polycrystalline with approximately 1-m-diameter single-crystal blocks. Because of their surface quality, the amorphous films were used for preparation of point contact junctions and for optical characterization. The point-contact spectra of tested junctions exhibited a two-gap structure. The MgB₂ polycrystalline films was used for bulk transport studies. The best films were characterized by the critical temperature T _c of up to 39 K and the current density j _c at 4.2 K of about 10⁷ A/cm².     

Enhancement of stability and peak power in a diode-pumped doubly QML YVO4/Nd:YVO4 laser with EO and Cr:YAG saturable absorber

A diode-pumped doubly Q-switched and mode-locked (QML) YVO₄/NdYVO₄ laser is realized with the electro-optic (EO) modulator and Cr⁴⁺:YAG saturable absorber, in which the repetition rate of the Q-switched envelope is controlled by the active EO modulation while the mode-locked pulses inside the Q-switched envelope depend on both the actively modulated loss and the passive saturable absorption. The experimental results show that the doubly QML laser can generate more stable and shorter pulses with higher peak power when compared with the singly passively QML laser with Cr⁴⁺:YAG. At the pump power of 20 W and the repetition rate 1 kHz, a 21 ns Q-switched pulse envelope with a average mode-locked peak power of 544 kW is obtained, which is the shortest Q-switched pulse envelope to my knowledge. In comparison to the singly passively QML laser with Cr⁴⁺:YAG, the doubly QML laser has compressed the Q-switched envelope pulse width 70% and improved the mode-locked pulsed peak power 27 times. By using a hyperbolic secant square function and considering the Gaussian distribution of the intracavity photon density, the coupled equations for diode-pumped dual-loss-modulated QML laser is given and the numerical solutions of the equations are in good agreement with the experimental results.     

Investigation of continuous-wave and Q-switched microchip laser characteristics of Yb:YAG ceramics and crystals

Continuous-wave and passively Q-switched microchip laser performance of Yb:YAG ceramics and single-crystals was investigated. Highly efficient continuous-wave Yb:YAG laser performance was observed at 1030 nm and 1049 nm for both Yb:YAG ceramics and crystals with different transmissions of output couplers. The laser performance of Yb:YAG ceramic is comparable to that of Yb:YAG single crystal. Meanwhile, the laser performance of laser-diode pumped Yb:YAG/Cr⁴⁺:YAG all-ceramics- and all-crystals-combination passively Q-switched microchip lasers were investigated. Sub-nanosecond laser pulses with peak power over 150 kW were obtained with different Yb:YAG/Cr⁴⁺:YAG combinations. Linearly polarized laser was observed in Yb:YAG/Cr⁴⁺:YAG all-crystals combination and circular polarized laser was obtained in Yb:YAG/Cr⁴⁺:YAG all-ceramics combination. The best laser performance was obtained with Yb:YAG/Cr⁴⁺:YAG all-crystals combination.     

Temperature effect on structure and surface morphology of indium tin oxide films deposited by reactive ion-beam sputtering

Indium tin oxide (ITO) films were deposited by reactive ion-beam sputtering. The relationship among the surface morphology, the resistivity ρ of the films, the substrate temperature T_S and the film thickness t_F was investigated. The heat power from the ion source during the sputtering was 265 W. T_S increased from 30 to 145 °C with an increase of t_F. The films thinner than 187 nm at T_S lower than 120 °C were amorphous, the film surface was as smooth as the substrate. The films deposited at T_S in the range between 135 and 145 °C were polycrystalline. So, the films thicker than 375 nm were in a multilayer structure of a polycrystalline layer on an amorphous layer. The surface of the polycrystalline films became rough. ρ of the films suddenly decreased at t_F of 375 nm, where the structure of the films changed. Next, the amorphous films with t_F of 39 nm were annealed in the atmosphere. The film structure changed to a polycrystalline structure at annealing temperature T_A of 350 °C. However, the surface roughness of all the films was almost same. As a result, the substrate temperature during the sputtering was important for the deposition of the films with a very smooth surface.     

Er,Yb:YVO4 waveguides deposited on amorphous SiO2 by PLD and UVPLD

In this work, erbium, and erbium and ytterbium co-doped YVO₄ waveguiding thin films were deposited on amorphous SiO₂ substrates by pulsed laser deposition (PLD) and ultraviolet-assisted pulsed laser deposition (UVPLD). The influence of the deposition technique on the structure, morphology, and optical properties of the films was investigated. At lower dopant concentrations the films prepared by UVPLD show better crystallinity and optical properties. All the samples show preferred orientation of the (001) zone axes parallel to the substrate surface. The polycrystalline samples show difference in the refractive indexes ?n (?n = n_TE − n_TM) for the TE and TM polarizations.     

A Facile Molecular Approach to Amorphous Nickel Pnictides and Their Reconstruction to Crystalline Potassium-Intercalated γ-NiOOHx Enabling High-Performance Electrocatalytic Water Oxidation and Selective Oxidation of 5-Hydroxymethylfurfural

The low-temperature molecular precursor approach can be beneficial to conventional solid-state methods, which require high temperatures and lead to relatively large crystalline particles. Herein, a novel, single-step, room-temperature preparation of amorphous nickel pnictide (NiE; EP, As) nanomaterials is reported, starting from NaOCE(dioxane)_n and NiBr₂(thf)_1.5. During application for the oxygen evolution reaction (OER), the pnictide anions leach, and both materials fully reconstruct into nickel(III/IV) oxide phases (similar to γ-NiOOH) comprising edge-sharing (NiO₆) layers with intercalated potassium ions and a d-spacing of 7.27 Å. Remarkably, the intercalated γ-NiOOH_x phases are nanocrystalline, unlike the amorphous nickel pnictide precatalysts. This unconventional reconstruction is fast and complete, which is ascribed to the amorphous nature of the nanostructured NiE precatalysts. The obtained γ-NiOOH_x can effectively catalyse the OER for 100 h at a high current density (400 mA cm⁻²) and achieves outstandingly high current densities (>600 mA cm⁻²) for the selective, value-added oxidation of 5-hydroxymethylfurfural (HMF). The NiP-derived γ-NiOOH_x shows a higher activity for both processes due to more available active sites. It is anticipated that the herein developed, effective, room-temperature molecular synthesis of amorphous nickel pnictide nanomaterials can be applied to other functional transition-metal pnictides.     

The parameters of laser plasmas formed using polycrystalline CuInS<Subscript>2</Subscript>, copper,and indium targets

We have studied the electron temperature (T _e) and density (N _e) of laser plasmas formed under the action of a neodymium laser in a polycrystalline CuInS₂ target, as well as in pure copper and indium targets. At a laser beam power density of ∼10⁸ W/cm², the average electron temperature of a laser plasma at a distance of r=1 mm from the CuInS₂ target falls within 0.55–0.77 eV, while the laser plasmas of copper and indium are characterized by T _e(Cu)=0.4–1.8 eV and T _e(In)=0.58–2.4 eV, respectively. The average electron density at the core of the laser torch (r=1 mm) at the CuInS₂ target reaches N _e=2.2×10¹⁶ cm⁻³. The results obtained for the polycrystalline target can be used in microelectronics for optimization of the process of laser deposition of thin films for solar cell elements.     

Comparison of structure and properties of alloys in amorphous,nanocrystalline and coarse-grained polycrystalline states

Some properties, including the microhardness, H _v, and electrical resistivity of a nanocrystalline, two coarse-grained polycrystalline and one amorphous alloys of Fe-Mo-Si-B of the same composition, were measured experimentally and compared. The structures of amorphous, nanocrystalline and coarse-grained Fe-Mo-Si-B alloys are also compared and discussed.     

Effect of laser irradiation on the superconducting properties of high-T c SmBa2Cu3O x

Studies of the effect of high power laser (Q-switched Ruby laser, 694 nm, 30 ns) irradiation on the critical current density (J _c ) and magnetic hysteresis at 77K and temperature variation of microwave induced d.c. voltage on SmBa₂Cu₃O _x ceramic samples have been performed. Irradiation did not substantially changeT _c but caused a strong increase inJ _c and magnetic hysteresis at 77K. The microwave-induced d.c. voltage at 77K showed appreciable decrease after irradiation. SEM studies showed grain growth due to sintering which improves the interconnectivity among the superconducting grains. These are attributed to physical densification and consequent reduction in the number of weak links. The increase of magnetic hysteresis after laser irradiation is presumably connected with the creation of defects which act as pinning centres. Thermal modelling suggests that on irradiation the surface melts up to a depth of 1μ and laser-induced evaporation occurs at energy density of 2·5 J/cm².