Ultrasonic flexural vibration assisted chemical mechanical polishing for sapphire substrate

The sapphire substrates are polished by traditional chemical mechanical polishing (CMP) and ultrasonic flexural vibration (UFV) assisted CMP (UFV-CMP) respectively with different pressures. UFV-CMP combines the functions of traditional CMP and ultrasonic machining (USM) and has special characteristics, which is that ultrasonic vibrations of the rotating polishing head are in both horizontal and vertical directions. The material removal rates (MRRs) and the polished surface morphology of CMP and UFV-CMP are compared. The MRR of UFV-CMP is two times larger than that of traditional CMP. The surface roughness (root mean square, RMS) of the polished sapphire substrate of UFV-CMP is 0.83 Å measured by the atomic force microscopy (AFM), which is much better than 2.12 Å obtained using the traditional CMP. And the surface flatness of UFV-CMP is 0.12 μm, which is also better than 0.23 μm of the traditional CMP. The results show that UFV-CMP is able to improve the MRR and finished surface quality of the sapphire substrates greatly. The material removal and surface polishing mechanisms of sapphire in UFV-CMP are discussed too.     

Interaction behaviors at the interface between liquid Al–Si and solid Ti–6Al–4V in ultrasonic-assisted brazing in air

Power ultrasonic vibration (20 kHz, 6 μm) was applied to assist the interaction between a liquid Al–Si alloy and solid Ti–6Al–4V substrate in air. The interaction behaviors, including breakage of the oxide film on the Ti–6Al–4V surface, chemical dissolution of solid Ti–6Al–4V, and interfacial chemical reactions, were investigated. Experimental results showed that numerous 2–20 μm diameter-sized pits formed on the Ti–6Al–4V surface. Propagation of ultrasonic waves in the liquid Al–Si alloy resulted in ultrasonic cavitation. When this cavitation occurred at or near the liquid/solid interface, many complex effects were generated at the small zones during the bubble implosion, including micro-jets, hot spots, and acoustic streaming. The breakage behavior of oxide films on the solid Ti–6Al–4V substrate, excessive chemical dissolution of solid Ti–6Al–4V into liquid Al–Si, abnormal interfacial chemical reactions at the interface, and phase transformation between the intermetallic compounds could be wholly ascribed to these ultrasonic effects. An effective bond between Al–Si and Ti–6Al–4V can be produced by ultrasonic-assisted brazing in air.     

Fatigue properties of a S45C steel subjected to ultrasonic nanocrystal surface modification

An ultrasonic nanocrystal surface modification (UNSM) technique, at 3 different vibration strike numbers (34,000 times/mm², 45,000 times/mm², 68,000 times/mm²) was used to modify the surface structure and properties of S45C. These three process conditions respectively produced 2 μm, 12 μm and 30 μm nanocrystal layers. UNSM technique improves the following mechanical properties: microhardness, surface roughness, and compressive residual stress. Also, fatigue life increased with the vibration strike number. UNSM C3 (with the vibration strike number of 68,000 times/mm²) has improved the fatigue strength by as much as 33% for S45C. Optical microscope pictures show that cracks usually initiate from intergranular microcracks on the surface and then extend along the tip traces of UNSM which are considered as process defects. A simple math model (tearing adhesive plaster model) has been made to analyze the initiation and growth of cracks. Though most of the cracks initiate at the surface of specimens, surface nanocrystal layers can help to retard crack initiation. In S45C, the efficiency of crack resistance is more than 48%.the vibration strike number     

Characterization and structure study of the anodic oxide film on Zircaloy-4 synthesized using NaOH electrolytes at room temperature

Thick crystalline zirconium oxide films were synthesized on Zircaloy-4 substrates by anodic oxidation at room temperature in NaOH solution with a stable applied voltage (300 V). The film is approximately 4.7 μm in thickness. The XPS and SEM analysis shows that the film is a three-layer structure in water, hydroxide and oxide parts. The thickness of that order is ∼0.01 μm, ∼1 μm, ∼3.7 μm, respectively. The oxide layer is composed of tetragonal and monoclinic phases with the volume ratio about 0.2. Furthermore, the thick anodic film acts as a barrier to oxygen and zirconium migrations. It effectively protects zirconium alloys against the worse corrosion. An extremely low passive current density of ∼0.018 μA/cm² and a low oxidation weight gain of ∼0.411 mg/cm² were also observed in the films.     

Microstructural analyses of the nanoparticles obtained after laser irradiation of Ti and W in ethanol

The laser ablation technique has been employed to prepare titanium (Ti) and tungsten (W) colloids from the elemental solids in ethanol using a copper-hydrogen bromide (CuHBr) vapour laser. The obtained nanoparticles were spherical with most diameters ranging from 0.05 to 0.5 μm. Some particles, notably when using Ti targets, are bigger than 0.9 μm, indicating resolidification of liquid droplets. The mechanism of material removal was characterized by photo-ablation where some particles were generated by rapid solidification from the melt. The W particles had tendency to coalescence, since small clusters merge to larger spheres. On the other hand, the Ti particles were coalescence-free, perhaps due to the thin high-resistant oxide layer at their surface.     

Novel device to measure critical point "Onset" of capillary wave and interpretation of Faraday instability wave by numerical analysis

A capillary wave was created on a surface by vibrating from the bottom of a container. When the amplitude of the container vibration approached the critical point, called the onset state, the surface broke up and bursted into very small drops on the air. The numerical analysis was used to determine the amplitude of the onset. The onset point was found to be 0.349 μm at f = 500 kHz. The critical amplitude h_cr was determined by using a multi-Fourier horn nozzle (MFHN) device. The onset point was measured to be 0.37 μm using a laser Doppler vibrometer (LDV) with the MFHN at f = 486 kHz. These drops indicate that particle size distributions of 10.8 μm and 7.0 μm were produced by the MFHN at f = 289 kHz and f = 486 kHz, respectively. These results agreed with those obtained using Kelvin’s equation, which predicted D = 0.34λ.     

Magnetic binary nanofillers

Magnetic binary nanofillers containing multiwall carbon nanotubes (MWCNT) and hercynite were synthesized by Chemical Vapor Deposition (CVD) on Fe/AlOOH prepared by the sol–gel method. The catalyst precursor was fired at 450 °C, ground and sifted through different meshes. Two powders were obtained with different particle sizes: sample A (50–75 μm) and sample B (smaller than 50 μm). These powders are composed of iron oxide particles widely dispersed in the non-crystalline matrix of aluminum oxide and they are not ferromagnetic. After reduction process the powders are composed of α-Fe nanoparticles inside hercynite matrix. These nanofillers are composed of hercynite containing α-Fe nanoparticles and MWCNT. The binary magnetic nanofillers were slightly ferromagnetic. The saturation magnetization of the nanofillers depended on the powder particle size. The nanofiller obtained from powder particles in the range 50–75 μm showed a saturation magnetization 36% higher than the one formed from powder particles smaller than 50 μm. The phenomenon is explained in terms of changes in the magnetic environment of the particles as consequence of the presence of MWCNT.     

Plate-shaped non-contact ultrasonic transporter using flexural vibration

We developed a plate-shaped non-contact transporter based on ultrasonic vibration, exploiting a phenomenon that a plate can be statically levitated at the place where its gravity and the acoustic radiation force are balanced. In the experiment, four piezoelectric zirconate titanate elements were attached to aluminum plates, on which lattice flexural vibration was excited at 22.3 kHz. The vibrating plates were connected to a loading plate via flexible posts that can minimize the influence of the flexure induced by heavy loads. The distribution of the vibration displacement on the plate was predicted through finite-element analysis to find the appropriate positions of the posts. The maximum levitation height of this transporter was 256 μm with no load. When two vibrating plates were connected to a loading plate, the maximum transportable load was 4.0 kgf.     

Simulation analysis of the aluminum thin film thickness measurement by using low energy electron beam

This paper indicates a simulation analysis for estimating the aluminum (Al) thin film thickness measurements by using the low energy electron beam. In order to calculate the Al thickness estimation, the energy of the incident electron beams was varied from 10 to 30 keV, while the thickness of the Al film was varied between 6 and 14 μm. From the simulation results it was found that electron transmittance fraction in 14 μm sample is about nine orders of magnitude more than 6 μm sample at the same incident electron beam energy. Simulation results show that maximum transmitted electrons versus Al layer thickness has a parabolic relation and by using the obtained equation, it is possible to estimate unknown thickness of the thin film Al layer. All calculations here were done by CASINO numerical simulation package.     

High frequency ultrasonic detection of C-crack defects in silicon nitride bearing balls

A non-destructive testing method for silicon nitride bearing balls based on ultrasonic resonance spectroscopy is proposed here. Through the theoretical study of their elastic vibrations, it is possible to characterize the balls using a vibration mode that is similar to surface wave propagation. The study of the influence of C-crack defects on the resonances of Rayleigh modes is presented here. These C-cracks are typically formed by impacts between balls during finishing or handling. They are frequently found on the surface of silicon nitride bearing balls and these C-cracks decrease the rolling contact fatigue life considerably. This kind of defect is difficult to detect because the C-shaped surface crack is very small and narrow (500 μm × 5 μm), and its depth does not exceed 50 μm. The proposed methodology can both excite spheroidal vibrations in the ceramic balls and detect such vibrations over a large frequency range. In particular, high frequency vibrations are considered because these are similar to the surface waves propagating in the cortical zone of the ceramic balls and consequently they can be used to detect C-crack defects.     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Long-period fiber-gratings produced by exposure with a low-pressure mercury lamp and their sensing characteristics

A new production method of long-period fiber-gratings using neither a laser nor a fine-positioning system was proposed. A low-pressure mercury lamp emitting 254 nm ultraviolet light was used as a light source. Hydrogen-loaded Ge-B co-doped fiber was exposed to the emission of the lamp through an amplitude mask. A coupling loss up to 23 dB was obtained for a grating period of 212 μm. The maximum coupling loss for a grating period of 460 μm was 18 dB. The growth rate of the refractive index change by mercury-lamp exposure was 1.3 × 10⁻⁴/h. The temperature and strain characteristics were measured and compared with those fabricated by excimer-laser exposure. The temperature and strain sensitivities of long-period gratings with a period of 212 μm were higher than those of 460 μm. The temperature and strain sensitivities of those by mercury-lamp exposure were almost equal to those by excimer-laser exposure of the same fiber. The sensitivities of those by excimer-laser exposure of non-loaded fiber were higher than those of hydrogen-loaded fiber by mercury-lamp or excimer-laser exposures except for the temperature sensitivity of a grating period of 460 μm.     

Low temperature ITO thin film deposition on PES substrate using pulse magnetron sputtering

Experiments were conducted using pulse magnetron sputtering (PMS) to deposit transparent conducting indium tin oxide (ITO) thin film onto flexible polyethersulfone (PES) plastic substrates. The thin film microstructure, optoelectronic and residual stress were analyzed using the modulating PMS power, work pressure, pulse frequency, duty cycle and cycle time process parameters. The residual stress of the thin film was determined by scanning electron microscopy (SEM) combined with the Sony equation. The experimental results show that PMS has a lower process temperature, higher deposition rate and lower resistivity compared with the radio frequency process at the same output power. The duty cycle increase produces the optimum optoelectronic characteristics. When the pressure, power, duty cycle and sputter time are increased, the thin film stress will also increase, causing flexural distortion in the PES plastic substrate. When the deposition thickness reaches 1.5 μm, ITO thin film will appear with a distinct split. Under 5 mtorr work pressure, 60 W power, 33 μs duty time and 2 μs pulse reverse time at duty cycle 95%, thin film with an optimized electrical 3.0 × 10⁻⁴ Ω-cm, RMS surface roughness of 0.85 nm and visible region optical transmittance will be achieved with acquisition of over 85%.     

Dynamic ultrasonic contact detection using acoustic emissions

For a non-contact ultrasonic material removal process, the control of the standoff position can be crucial to process performance; particularly where the requirement is for a standoff of the order of <20 μm. The standoff distance relative to the surface to be machined can be set by first contacting the ultrasonic tool tip with the surface and then withdrawing the tool to the required position. Determination of this contact point in a dynamic system at ultrasonic frequencies (>20 kHz) is achieved by force measurement or by detection of acoustic emissions (AE). However, where detection of distance from a surface must be determined without contact taking place, an alternative method must be sought.     

Dielectric properties of anodic films on sputter-deposited Ti-Si porous columnar films

For electrolytic capacitor application of the single-phase Ti alloys containing supersaturated silicon, which form anodic oxide films with superior dielectric properties, porous Ti-7 at% Si columnar films, as well as Ti columnar films, have been prepared by oblique angle magnetron sputtering on to aluminum substrate with a concave cell structure to enhance the surface area and hence capacitance. The deposited films of both Ti and Ti-7 at% Si have isolated columnar morphology with each column revealing nanogranular texture. The distances between columns are ∼500 nm, corresponding to the cell size of the textured substrate and the gaps between columns are 100-200 nm. When the porous Ti-7 at% Si film is anodized at a constant current density in ammonium pentaborate electrolyte, the growth of a uniform amorphous oxide film continues to ∼35 V, while it is limited to less than 6 V on the porous Ti film. The maximum voltage of the growth of uniform amorphous oxide films on the Ti-7 at% Si films is similar for both the flat and porous columnar films, suggesting little influence of surface roughness on the amorphous-to-crystalline transition of growing anodic oxide under the high electric field. Due to the suppression of crystallization to sufficiently high voltages, the anodic oxide films formed on the porous Ti-7 at% Si film shows markedly improved dielectric properties, in comparison with those on the porous Ti film.     

Real-time monitoring of structural vibration using spectral-domain optical coherence tomography

We report in this paper the development of a spectral-domain optical coherence vibration tomography (OCVT) using a broadband CCD-based spectrometer and a short-coherence white light source. We demonstrate that both the vibration amplitude and frequency can be quantified, in the frequency range 0-250 Hz, with an axial resolution of 1 μm. Furthermore, the inner structure (layer thickness) of a vibrating sample can also be quantified simultaneously. The developed OCVT is non-contact and noninvasive in nature, thus is ideal for real time and in situ monitoring of low-frequency micro-vibrations that have critical impacts on many high-precision manufacturing and engineering processes.     

A study on the biological detection chip through the use of PDMS lens for the reinforcement of fluorescence receiving signal

In this study, MEMS process technology is adopted to produce microfluidic chip and PDMS lens. SU-8 thick film photo resist is coated onto silicon wafer surface in two times of spin coating, then through lithography and mold transfer technology, PDMS chip of minimal line width 100 μm and thickness 200 μm is printed. In fluorescence detection aspect, we use objective lens to couple laser optical source to optical fiber, and then have it incident to excite fluorescence sample, the excited fluorescence then passes through filter and detected by optical detector of experiment group and spectrophotometer of reference group. From the experiment result, the Hex fluorescence detection limit of the system is verified to be 1 pmol/5 μl. In addition, we have integrated PDMS lens into microfluidic chip to make generalized detection experiment, it was found that the signal measured by optical embedded type is higher than that of non-embedded type. Meanwhile, the microfluidic chip with double concave lens (135°) and10 mm PDMS focusing lens can be utilized to obtain optimal fluorescence receiving effect. The fluorescence intensity is raised by 2–3 times, and the measurement limit is lowered to 100 fmol/5 μl.     

Fabrication and magnetic properties of Ni-Zn nanowire arrays

Ni-Zn nanowire arrays, with diameters of approximately 60 nm and lengths of around 40 μm, were fabricated by electrodeposition in porous anodic aluminum oxide templates at different electric potentials. X-ray diffraction observations demonstrated that the isolated nanowires had polycrystalline structure and that their phases changed with the deposition potential. The amount of deposited zinc in the nanowires increased with the deposition potential, whereas the amount of nickel decreased. Magnetic measurements showed that there was a gradual change of magnetism from isotropic to anistropic with increasing potential amplitude and that the coercivity reached a maximum value in the nanowire deposited at −1.35 V.     

Effect of nitrogen doping on the properties of AlSiO film for wide bandgap semiconductors

A gate insulator film with a wide bandgap and a high dielectric constant is required to achieve high-power field effect transistors (FET) using wide bandgap semiconductors such as SiC, GaN, and diamond. It is observed that an aluminum silicon oxide (AlSiO) film containing 11% nitrogen has a high resistivity of 5 × 10¹⁵ Ω cm, and the leakage current of a nitrogen-doped aluminum silicon oxide (AlSiON) film is also suppressed at high temperature, as compared to the AlSiO film. For example, the leakage current at 240 °C is four orders of magnitude smaller than that of the AlSiO film, suggesting that the AlSiON film is applicable to high temperature operation of wide bandgap semiconductor devices.     

Synthesis and characterization of (h 0 h)-oriented silicalite-1 films on α-Al2O3 substrates

A simple and well-designed synthesis procedure is proposed to fabricate silicalite-1 films on porous α-Al₂O₃ substrates on purpose of preventing the aluminum leaching. The continuous and 2 μm thick seed layer of silicalite-1 crystals is fabricated by using a spin coater. The first-time seeded growth is performed to synthesize a thin layer of intergrown ZSM-5 crystals on the silicalite-1 seed layer, where the use of low alkalinity and short synthesis time is to reduce the aluminum leaching. The intergrown layer of ZSM-5 crystals serves as a barrier to block the aluminum leaching from porous α-Al₂O₃ substrates in the second-time seeded growth, leading to the formation of ca. 11 μm thick intergrown and oriented silicalite-1 films with an extremely high Si/Al ratio. According to SEM images and XRD measurements, the as-synthesized silicalite-1 film is dense, continuous, and (1 0 1)-oriented. The electron probe microanalysis (EPMA) of the resulting film demonstrates that there is no aluminum leaching in the second-time seeded growth. The leaking tests confirm that non-zeolitic pores in the silicalite-1 film are negligible.