Tetsuhide Shimizu

Process stabilization by peak current regulation in reactive high-power impulse magnetron sputtering of hafnium nitride

A simple and cost effective approach to stabilize the sputtering process in the transition zone during reactive high-power impulse magnetron sputtering (HiPIMS) is proposed. The method is based on real-time monitoring and control of the discharge current waveforms. To stabilize the process conditions at a given set point, a feedback control system was implemented that automatically regulates the pulse frequency, and thereby the average sputtering power, to maintain a constant maximum discharge current. In the present study, the variation of the pulse current waveforms over a wide range of reactive gas flows and pulse frequencies during a reactive HiPIMS process of Hf-N in an Ar-N2 atmosphere illustrates that the discharge current waveform is a an excellent indicator of the process conditions. Activating the reactive HiPIMS peak current regulation, stable process conditions were maintained when varying the N2 flow from 2.1 to 3.5 sccm by an automatic adjustment of the pulse frequency from 600 Hz to 1150 Hz and consequently an increase of the average power from 110 to 270 W. Hf-N films deposited using peak current regulation exhibited a stable stoichiometry, a nearly constant power-normalized deposition rate, and a polycrystalline cubic phase Hf-N with (111)- preferred orientation over the entire reactive gas flow range investigated. The physical reasons for the change in the current pulse waveform for different process conditions are discussed in some detail.

Effect of Heating on Springback in Heat Assisted Microbending

A novel heat assisted microbending system was developed by applying the resistance heating technology. To clarify the effect of heating on springback for ultra-thin metal foils, high precision microbending test was carried out under the different temperature of room temperature (RT), 300oC and 600oC. As-received rolled and electrochemically polished pure titanium foils with thickness of 0.1, 0.05 and 0.02mm were used. To evaluate the springback in each thickness, springback angle of pure titanium foils with different thicknesses was measured under the same maximum bending strain. As results, the springback angle was decreased with increasing the process temperature for all materials and thickness conditions. Furthermore, the thinner the foil, the larger the springback angle, irrespective of the temperature conditions. The relationship between the heating temperature and the decreasing ratio of the springback angle was experimentally demonstrated.

High-Density Energy-Assisted Microforming for Fabrication of Metallic Devices

ABSTRACT A high-energy-assisted microforming system, which combines heating and vibration, was developed to improve the efficiency and accuracy of microscale metal parts. The system consists of a desktop servo-press system that can supply various motions including step and vibration motions and a resistance-heating system with contact electrode probes embedded in the dies that are capable of heating only the workpiece and of real-time control. Microdeep drawing and microforging was conducted to evaluate the performance of the high-energy assistance. The formability was found to improve significantly, and the surface roughness improves due to improved flowability and deformation uniformity.

Grain Refinement by Combined ECAE/Extrusion and Dieless Drawing Processes for AZ31 Magnesium Alloy Tubes

Grain refinement processing by severe deformation, combined equal-channel angular extrusion (ECAE) processing and conventional tube extrusion, is applied to AZ31 magnesium alloy. By a combination of ECAE processing and tube extrusion, a fabricated tube, with outer and inner diameters of 2 mm and 1 mm, respectively, has fine, homogeneous, and equiaxed grain structure with an average grain size of 1.5m. Tensile test results indicate that the fine-grained tubes exhibited a superplasticity potential m value of 0.55.The maximum elongation (688%) is obtained at a temperature of 673K. Furthermore, the tubes fabricated by combined ECAE/extrusion process is applied to dieless drawing process without using any tool and die.As a result, dieless drawing limit is enhanced due to high m value achieved by combined ECAE/Extrusion process. From these results, the effectiveness of new grain refinement processing for fabricating fine-grained tubes and its application for dieless drawing process to fabricate the fine tubes was demonstrated experimentally.

Deformation Behavior of Ultra-Thin Metal Foils in Strip Drawing Friction Test

This study focuses on the surface deformation of thin metal foils caused by friction. To clarify the effect of the relative ratio of surface plastic region to the foil thickness on global deformation behavior, strip drawing tests for ultra thin metal foil with 20μm and 100μm thickness were conducted As a result, different surface deformation and elongation behavior under the same friction condition were observed in different thicknesses. Aided by finite element analysis of the friction test, the contribution of the deformation caused by friction to the foil elongation was investigated and the importance of the friction on material deformation in metal foil forming was demonstrated.

Influence of structural dimensions of micro-pillar array in reaction field on sensitivity of enzyme-linked immunosorbent assay (ELISA)

ABSTRACT For high sensitivity and rapid reaction of enzyme-linked immunosorbent assay (ELISA), the film-stack reaction field with micro-pillars array was designed and developed. The film-stack reaction field was fabricated by a nanoimprint process and an automatic punch-press process. The films with different gaps between micro-pillars (5, 10 and 50 μm) were prepared. These reaction fields were evaluated by IgA ELISA using 96-well microtitre plates and the computational simulation analysis of the fluid flow and the particle trajectory. Compared with ELISA using only the microtitre plate, higher detection sensitivity and shorter incubation time were achieved using the film-stack reaction field due to the increased surface area and the circulating flow through the space between films in a well by the rotation of the film-stack reaction field. Furthermore, in the ELISA results obtained using the film-stack reaction fields, the fluorescence intensities in 10-μm and 50-μm pillar gaps were the minimum and maximum values, respectively. This trend was due to the flow rate between micro-pillars, and the number and the diffusion distance of supplied biomolecules to the inertial space in the film-stack reaction field. In simulation results, the trend of the number of adsorbed biomolecule particles with different gaps between micro-pillars was in agreement with the trend in the ELISA results. Hence, these simulation analyses were validated in the quantitative evaluation of this reaction field and could be applied in the design of this reaction field as an effective design tool.

Investigation on Dynamic Impact Effect of Ultrasonic-Assisted Compression Test

Ultrasonic-assisted metal forming have been studied numerously in conventional macro scale. However, ultrasonic dynamic impact effect, occurring in micro scale, has never been studied thoroughly, which makes the characteristics of material deformation more unpredictable in ultrasonic-assisted micro forming. The purpose of this study is to confirm the critical condition for occurrence of ultrasonic dynamic impact effect and to investigate the dimensional height dependency of ultrasonic dynamic impact effect on material deformation. In this paper, commercially pure aluminum 1100 with varying height (φ2×2mm, φ2×1.5mm, φ2×1mm) were selected for conventional static (without ultrasonic vibration) and ultrasonic-assisted compression tests. Ultrasonic-induced stress reduction was evaluated and the contour shape of deformed specimens was compared to investigate the ultrasonic dynamic impact effect on material deformation. The results showed that, as dimensional height of specimen decreased, ultrasonic vibration can reduce forming stress more effectively. In addition, a surprising anti-barreling shape and a significant contact surface area expansion were observed near contact surfaces in every specimen compressed with ultrasonic-assistance, indicating that additional plastic deformation can be produced by ultrasonic dynamic impact effect. An ultrasonic dynamic impact factor (y) is proposed and estimated by an exponential type trend line as y = 2.42e-1.48x for different dimensional specimen height (x) to quantify the ultrasonic dynamic impact effect. The promising prospect of ultrasonic vibration in micro-forming was demonstrated by the findings above, which helped to provide a basis to understand the underlying mechanism of ultrasonic-assisted micro forming and design the process in the future.

Novel processes and related technologies for micro metal forming

Processes with high energy assistance, such as ultrasonic vibration or local heating, and automatic assembly system in a progressive die were developed for micro metal forming in order to improve process accuracy of micro product due to some size effects in this study. Furthermore, application of textured diamond like carbon (DLC) coating on die surface was attempted to improve the tribological performance for dry micro forming operations.

Deposition of Boron Nitride Films by Filament-Assisted CVD Using Tris(Bimethylamino)Borane Precursor

Boron nitride films were deposited on silicon substrate by a hot filament assisted chemical vapor deposition (HFCVD) system. The tris (dimethylamino) borane (B[N(CH3)2]3) was used as the single source precursor which has both the boron and nitrogen source, ammonia gas was used as the assisted gas to increase the nitrogen concentration in the films. The films deposited by different ratios of precursor to ammonia gas flow rate and filament temperatures were investigated. The boron-carbon-nitrogen (BCN) compound films were deposited under lower filament temperature. With increasing the ammonia gas flow rate, the carbon concentration in the films decreased. Fourier transform infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM) image reveal that hexagonal boron nitride (hBN) films were deposited at the higher filament temperature of 2000°C. Moreover, the crystallization degree of the films became better with the filament temperature increased.

Investigation on ultrasonic volume effects: Stress superposition, acoustic softening and dynamic impact

Conventional high power ultrasonic vibration has been widely used to improve manufacturing processes like surface treatment and metal forming. Ultrasonic vibration affects material properties, leading to a flow stress reduction, which is called ultrasonic volume effect. The volume effect contains multi-mechanisms such as stress superposition due to oscillatory stress, acoustic softening by easier dislocation motion and dynamic impact leading to extra surface plastic deformation. However, most researches ignored the stress superposition for the convenience of measurement, and few studies considered ultrasonic dynamic impact since the relatively low ultrasonic energy in macro scale. The purpose of this study is to investigate the characteristics and mechanisms of different ultrasonic volume effects in micro-forming. A 60 kHz longitudinal ultrasonic-assisted compression test system was developed and a series of ultrasonic-assisted compression tests at different amplitudes on commercially pure aluminum A1100 in micro-scale were carried out combining the surface analysis by SEM, EDX and micro-hardness test. Three different ultrasonic volume effects, stress superposition, acoustic softening and dynamic impact, were confirmed in the ultrasonic-assisted compression tests. In order to quantitatively predict stress superposition, a hybrid model for stress superposition is developed considering the elastic deformation of experimental apparatus in practice, the evolution of the modeling results fitted well with the experimental results. With low ultrasonic amplitude, stress superposition and acoustic softening occurred because vibrated punch contacted with the specimen all the time during compression. However, with higher amplitude, due to the extra surface plastic deformation by larger ultrasonic energy, forming stress was further reduced by the ultrasonic dynamic impact. A possible method to distinguish the effects of dynamic impact and acoustic softening is to analyze the waveform of the oscillatory stress in the process. In the case of ultrasonic dynamic impact effect, a higher amount of oxidation was observed on the specimen surface, which could be the result of local heating by surface plastic deformation and surface friction when the vibrated punch detached from the specimen. The findings of this study provide an instructive understanding of the underlying mechanisms of volume effects in ultrasonic-assisted micro-forming.