A study of fused silica micro/nano patterning by focused-ion-beam

A dual-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system was used to pattern fused silica substrates coated with a 15 nm thin Cr layer. The dimensions of fabricated features together with their surface morphology and profiles were investigated by SEM and atomic force microscopy (AFM). The study demonstrated that with the increase of the ion beam fluence the sputtering rate of the fused silica decreased non-linearly. Also, it was found that initially the sputtering rate increased with the increase of the beam current, after reaching a maximum value, it started decreasing when further beam current increment was performed. Compared with unprocessed areas, the surface finish of the features fabricated by FIB exhibited a significant improvement, and the ion fluence influence on the surface roughness of trenches with low aspect ratios could be considered as negligible. Using a fine beam probe, nano-gratings in the form of grooves with a width down to 54 nm and an aspect ratio higher than three were fabricated. The study showed that FIB machining could be an alternative technology to e-beam lithography for producing fused silica templates for UV nanoimprinting.     

Accurate detection of interface between SiO2 film and Si substrate

Accurate end point detection of interface for multilayers using focused ion beam (FIB) is important in nanofabrication and IC modification. Real-time end point graph shows sample absorbed current as a function of sputtering time during FIB milling process. It is found that sample absorbed current increases linearly with ion beam current for the same material and changes when ion beam is milling through a different material. Investigation by atomic force microscope (AFM) and FIB cross-sectioning shows that accurate SiO₂/Si interface occurs to where the maximum sample absorbed current occurs. Since sample absorbed current can be real-time monitored in focused ion beam machine, the paper provides a viable and simple method for accurately determining the interface during FIB milling process for widely used SiO₂/Si system.     

Femtosecond laser patterning of Ta0.1W0.9Ox/ITO thin film stack

Selective laser patterning of thin films in a multilayered structure is an emerging technology for process development and fabrication of optoelectronics and microelectronics devices. In this work, femtosecond laser patterning of electrochromic Ta_0.1W_0.9O_x film coated on ITO glass has been studied to understand the selective removal mechanism and to determine the optimal parameters for patterning process. A 775 nm Ti:sapphire laser with a pulse duration of 150 fs operating at 1 kHz was used to irradiate the thin film stacks with variations in process parameters such as laser fluence, feedrate and numerical aperture of objective lens. The surface morphologies of the laser irradiated regions have been examined using a scanning electron microscopy and an optical surface profiler. Morphological analysis indicates that the mechanism responsible for the removal of Ta_0.1W_0.9O_x thin films from the ITO glass is a combination of blistering and explosive fracture induced by abrupt thermal expansion. Although the pattern quality is divided into partial removal, complete removal, and ITO film damage, the ITO film surface is slightly melted even at the complete removal condition. Optimal process window, which results in complete removal of Ta_0.1W_0.9O_x thin film without ablation damage in the ITO layer, have been established. From this study, it is found that focusing lens with longer focal length is preferable for damage-free pattern generation and shorter machining time.     

Microstructure evolution in the rapidly quenched Fe78Si9B13 ribbons

We report microstructure evolution in as-spun Fe₇₈Si₉B₁₃ ribbons under various wheel speeds (s), which was investigated by X-ray diffraction (XRD), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). With decreasing s, the volume fraction of the residual amorphous phase (V_a) in the as-spun ribbons decreases gradually, and the total exothermic heat of the crystallization in the DSC curves also decreases, but the ratio of the exothermic heat of the second crystallization to the first one is on the contrary. α-Fe is found in the ribbon with s of 32.9 m/s, while α-Fe, eutectic α-Fe+Fe₂B, and Fe₃Si phases are found in ribbons with s of 25.6 and 18.3 m/s. The phase precipitating behavior in cooling processes is well consistent with the annealing process in the literatures.     

Structural characterization and ferromagnetic behavior of Fe-doped TiO2 powder by high-energy ball milling

Fe-doped TiO₂ powder was prepared by high-energy ball milling, using TiO₂ Degussa P-25 and α-Fe powders as the starting materials. The structure and magnetic properties of the Fe-doped TiO₂ powder were studied by X-ray diffraction, ⁵⁷Fe Mossbauer spectroscopy and vibrating sample magnetometer. The Reitveld refinement of XRD revealed that ball milling not only triggered incorporation of Fe in TiO₂ lattice but also induced the phase transformation from anatase to rutile in TiO₂ and consequently the milled Fe-doped TiO₂ powder contained only rutile.⁵⁷Fe Mössbauer effect measure showed that Fe atoms existed in Fe²⁺ and Fe³⁺ state, which were assigned to the solid solution Fe_xTi_1−xO₂. The magnetization measurements indicated that the milled Fe-doped TiO₂ powder was ferromagnetic above room temperature. The ferromagnetism in our milled Fe-doped TiO₂ powder seemingly does not come from Fe and iron oxides particles/clusters but from the Fe-doped TiO₂ powder matrices.     

金属玻璃(Fe0.8Ni0.15Cr0.05)78Si8B14的起始磁导率减落现象

在77—553K范围内的不同温度下测量了金属玻璃(Fe_0.8Ni_0.15,Cr_0.05)₇₈Si₈B₁₄的起始磁导率减落。测量结果表明,减落的温度关系表现为一个具有单一弛豫峰的不对称谱。在273K下考察了减落的动力学行为。用Hesse-Rubartsch方法拟合动力学曲线得到一个左右不对称的单峰激活能谱,最可几激活能大约为1.40eV。考察了减落的退火效应及退火动力学行为,结果表明,在宽的温度范围内,减落呈现明显的退火效应,而且退火动力学行为近似服从lnt动力学。 关键词：     

Superhydrophobicity of LaMnO3 Coatings with Hierarchical Microstructures

As proposed by Herminghaus, a hierarchical structure could render any surface nonwettable as long as the roughness amplitude at small scales is sufficient to suspend a free liquid surface. Recently we reported that the wettability of La0.7Sr0.3MnO3, an intrinsic hydrophilic oxide, can be tuned from superhydrophilicity to superhydrophobicity by hierarchical microstructures generated by annealing the coatings of La0.7Sr0.3MnO3 powder in nanometric scale at different temperatures. Here we further demonstrate the similar phenomenon observed on LaMaO3 coatings, which conforms THAT the surface geometrical structure is a key factor to determine the wettability.     

Femtosecond laser ablation of crystals SiO2 and YAG

Damage threshold of crystals SiO₂ and YAG against 60-900 fs, 800 nm laser pulses are reported. The breakdown mechanisms were discussed based on the double-flux model and Keldysh theory. We found that impact ionization plays the important role in the femtosecond laser-induced damage in crystalline SiO₂, while the roles of photoionization and impact ionization in YAG crystals depend on the laser pulse durations.     

Laser (a pulsed Nd:YAG) cladding of AZ91D magnesium alloy with Al and Al2O3 powders

The laser surface cladding of an AZ91D magnesium alloy with Al and Al₂O₃ powders was investigated using a pulsed Nd:YAG laser. The optimum ratio of Al to Al₂O₃ and the suitable range of laser processing parameters were identified. The resulting microstructure in the modified surface layer was examined and the wear resistance property was evaluated. The results show that the wear resistance of the laser treated samples was much superior to that of the untreated samples.     

Structural evolution of nanocrystalline/amorphous Fe/Ni75B25 multilayers: temperature dependence of electrical resistivity

X-ray specular-reflectivity measurements have been carried out on nanocrystalline/amorphous Fe/Ni₇₅B₂₅ multilayer films which were sputter-deposited on Si substrates, to investigate the evolution of interface roughness and the correlation between structure and transport properties. A significant interface roughness correlation with increasing Fe/NiB layer repetition was observed. The investigated films indicated a temperature dependent high electrical resistivity—10⁴ μΩ-cm at 10 K and 10³ μΩ-cm at 300 K—with a semiconductor-metal transition like behavior. Selected area electron diffraction revealed the presence of crystalline bcc Fe phase and NiB in amorphous state. The structural and transport properties of the multilayers are discussed.     

Structure and magnetic properties of nanocrystalline Fe75Si25 powders prepared by mechanical alloying

Nanocrystalline Fe₇₅Si₂₅ powders were prepared by mechanical alloying in a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling process were studied by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer measurements. The evolution of non-equilibrium solid solution Fe (Si) during milling was accompanied by refinement of crystallite size down to 10 nm and the introduction of high density of dislocations of the order of 10¹⁷ m⁻². During the milling process, Fe sites get substituted by Si. This structural change and the resulting disorder are reflected in the lattice parameters and average magnetic moment of the powders milled for various time periods. A progressive increase of coercivity was also observed with increasing milling time. The increase of coercivity could be attributed to the introduction of dislocations and reduction of powder particle size as a function of milling time.     

Electrical resistivity of amorphous metallic glasses Fe80B80 and Fe78Mo2B20 between 78 and 1000 K

Electrical resistivity (ρ) of amorphous Fe₈₀B₂₀ and Fe₇₈Mo₂B₂₀ have been studied as a function of temperature (T) between 78 and 1000 K. The ρ vs T curves, obtained with specified warming and cooling rates, show that such curves are sensitive probes of the crystallization process. Within the experimental error, no anomalies in the ρ behavior can be seen at the Curie temperature of each amorphous alloy.     

Co-relation between pre-exponential factor and activation energy of non-isothermal crystallization for virgin and irradiated Fe78B13Si9 metallic glass

The present work shows the applicability of Meyer-Neldel relation between the pre-exponential factor and activation energy of non-isothermal crystallization of Fe₇₈B₁₃Si₉ metallic glass. Differential scanning calorimeter (DSC) technique is used to observe the variation in the above two kinetic parameters of the non-isothermal crystallization due to ionic irradiation at three different fluences with high-energy heavy ion Ni¹¹⁺ having energy 150 MeV.     

Characterization of ultra-fast deposited polycrystalline graphite by a CO2 laser-assisted combustion-flame method

High deposition rate, 750 μm/min, crystalline graphite was deposited on WC substrates by a CO₂ laser-assisted combustion-flame method at laser powers between 300 and 800 W. The structures, which were identified as pillars, were characterized by various methods. The pillars were cylindrical in shape and grew to a size of approximately 3 mm in length and in a few minutes. The laser power did not affect the overall length of the pillar, but caused changes in the physical shape. X-ray and electron diffraction results revealed the pillars to be crystalline graphite regardless of the laser power. Investigation of the pillars by scanning electron microscopy showed two distinct microstructural areas: an inner core of dense material surrounded by an outer shell of lamellar-like material. The core/shell microstructure was unaffected by the level of CO₂ laser power.     

Low temperature electrical conductivity and magnetoconductivity of Fe39Ni39Mo4Si6B12 and Co58Ni10Fe5Si11B16 metallic glass alloys

A detailed study on the weak localization phenomenon vis-a-vis electron-electron interaction effects in magnetic metallic glasses has been carried out. We measured the electrical conductivity and magnetoconductivity within the temperature range 1.8≤T≤300K. A maximum on the conductivity versus temperature curve exists atT=T _m. The conductivity was observed to follow aT ^1/2 law forT<T _m andT ² law forT>T _m. Magnetoconductivity data of these alloys indicate the prominence of electron-electron interaction at low temperatures. The authors have determined the inelastic scattering field and spin-orbit scattering field from the magnetoconductivity data. The inelastic scattering field obeys aT ^p law (p=2) at low temperatures.     

Computer simulation of intrinsic defects in YAlO3 single crystal

Computer simulation techniques were used to investigate intrinsic defects in YAlO₃ single crystal. A set of short-range potential parameters were derived using a relaxed fitting procedure incorporating with the known crystal properties. These parameters were then applied within the framework of the shell model. The simulation results reveal that oxygen Frenkel disorder and the antisite defect of Al ion substituting the Y ion dominate the intrinsic defects in YAlO₃. An analysis of redox reactions corroborate that the oxidation is most likely to occur via forming interstitial oxygen, while the oxidation via filling oxygen vacancies and reduction reaction may predominate at high temperature. The activation energy of oxygen vacancy migration on conduction was also studied.     

Chemical and microstructural study of the oxygen passivation behaviour of nanocrystalline Mg and MgH2

Nanocrystalline Mg and MgH₂ samples have been prepared by high-energy ball milling and gas phase condensation methods. Starting from these materials in their “as received” state without air exposure, a study of the oxygen and air passivation behaviour was carried out by “in situ” analysis of the samples by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The binding energy and photoemission Auger parameters have been determined for metallic magnesium as well as for magnesium hydride, oxide and hydroxide species. Values of the MgH₂ material were reported for the first time. The study clearly shows the formation of an oxide passivation layer of ca. 3-4 nm in thickness for all the nanocrystalline magnesium samples handled under controlled inert gas atmospheres. A hydroxide like amorphous layer is formed at the topmost surface layers of the nanocrystalline Mg and MgH₂ samples. The implication of these studies for H₂ storage and transport applications of nanocrystalline magnesium is discussed.     

Studies of the relaxed amorphous phase in the Fe80Nb6B14 alloy

The paper presents measurements of magnetic permeability, magnetic after-effects, magnetostriction, DSC and XPS for the Fe₈₀Nb₆B₁₄ amorphous alloys preliminary annealed for 1 h at temperatures ranging from 300 to 770 K. It was shown that annealing out of free volume and internal stresses causes a decrease of magnetostriction coefficient and leads to the formation of the energetically stable relaxed amorphous state. The XPS spectra show local fluctuation of boron density. This effect was attributed to the formation of small iron clusters—the characteristic feature for the relaxed amorphous phase.     

Superhydrophilic stability enhancement of RF co-sputtered TixSi1−xO2 thin films in dark

Ti_xSi_1−xO₂ compound thin-film systems were deposited by reactive RF magnetron co-sputtering technique. The effect of Ti concentration on the hydrophilicity of Ti_xSi_1−xO₂ compound thin films was studied and it was shown that the films with Ti_0.6Si_0.4O₂ composition possess the best hydrophilic property among all the grown samples. Surface ratio and average roughness of the thin films were measured by atomic force microscopy (AFM). Surface chemical states and stoichiometry of the films were determined by X-ray photoelectron spectroscopy (XPS). In addition, XPS revealed that the amount of Ti-O-Si bonds in nanometer depth from the surface of the Ti_0.6Si_0.4O₂ films was the maximum, which resulted in the most stable superhydrophilic property. According to XRD data analysis for the pure TiO₂ films, the polycrystalline anatase phase was formed with an average grain size of about 15 nm. Moreover, amorphous phase was also formed for the Ti_xSi_1−xO₂ compound systems due to presence of silicon in the films. Finally, optical properties of the films such as transmission, reflection and band gap energy were investigated using UV-vis spectrophotometry. It was found that the transmittance of the films was decreased with increasing Ti concentration in the films.     

Deposition and characterization of La2Ti2O7 thin films via spray pyrolysis process

Thin films of La₂Ti₂O₇ have been deposited on fused silica and Si substrates by a spray pyrolysis method using ethylene glycol solution of La(III)-Ti(IV)-citrate complexes as starting material and O₂ as a carrier gas. The composition, crystal structure and morphology of the films are studied.