Hyun S. Myung;Lee, Hyuk M.;Kim, Sang S.;Jeon G. Han
한국표면공학회:학술대회논문집
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한국표면공학회 2001년도 추계학술발표회 초록집
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pp.37-37
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2001
TiN coatings were applied for VarIOUS application fields, because of a good wear-resistance and a high hardness. Typically, TiN thin films show the hardness of 25GPa and friction coefficient of 0.6. However, in many field, one is looking for a more improved tool which has low friction coefficient and high wear resistance. The main motivation of this study is to characterize the influence of copper dopant content on TiN thin films. Ti-Cu-N thin films were deposited onto D2 steel substrates by PVD processing with various magnetron current densities (Cu contents). In this work, we synthesized titanium nitride films similar with reported typical titanium nitride films and synthesized Ti-Cu-N thin films with the addition of elemental copper which is measured improved hardness more than pure TiN films with copper content variables. This films has preferred oriented films of (111) direction. In addition, It was found that there is a strong correlation between content of various metal and film characteristics such as preferred orientation, grain size, hardness and friction coefficient and so, in future study, improved mechanical properties of TiN films can be controlled by change in target current density. The Ti-Cu-N film will show apparent hardness improvement and mechanical properties enhancement, when doping element is added onto TiN thin films. Film structure, chemical composition, mechanical properties were investigated by means of X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy(EDS), wear resistance tester and nanohardness tester.
Recently, thin film capacitors used for vehicle inverters are small size, high capacitance, fast response, and large capacitance. But its applications were made up of liquid as electrolyte, so its capacitors are limited to low operating temperature range and the polarity. This research proposes using Ni-P alloys by electroless plating as the electrode instead of liquid electrode. Our substrate has a high aspect ratio and complicated shape because of anodic aluminum oxide (AAO). We used AAO because film thickness and effective surface area are depended on for high capacitance. As the metal electrode instead of electrolyte is injected into AAO, the film capacitor has advantages high voltage, wide operating temperature, and excellent frequency property. However, thin film capacitor made by electroless-plated Ni on AAO for full-filling into etched tunnel was limited from optimizing the deposition process so as to prevent open-through pore structures at the electroless plating owing to complicated morphological structure. In this paper, the electroless plating parameters are controlled by temperature in electroless Ni plating for reducing reaction rate. The Electrical properties with I-V and capacitance density were measured. By using nickel electrode, the capacitance density for the etched and Ni electroless plated films was 100 nFcm-2 while that for a film without any etch tunnel was 12.5 nFcm-2. Breakdown voltage and leakage current are improved, as the properties of metal deposition by electroless plating. The synthesized final nanostructures were characterized by scanning electron microscopy (SEM).
Some applications of carbon nanotubes (CNTs) as field emitters, such as x-ray tubes and microwave amplifiers, require high current emission from a small emitter area. To emit the high current density, CNT emitters should be optimally fabricated in terms of material properties and morphological aspects including high crystallinity, aspect ratio, distribution density, height uniformity, adhesion on a substrate, low outgassing rate during electron emission in vacuum, etc. In particular, adhesion of emitters on the substrate is one of the most important parameters to be secured for high current field emission from CNTs. So, we attempted a novel approach to improve the adhesion of CNT emitters by incorporating metal oxide layers between CNT emitters. In our previous study, CNT emitters were fabricated on a metal mesh by filtrating the aqueous suspensions containing both highly crystalline thin multiwalled CNTs and thick entangled multiwalled CNTs. However, the adhesion of CNT film was not enough to produce a high emission current for an extended period of time even after adopting the metal mesh as a fixing substrate of the CNT film. While a high current was emitted, some part of the film was shown to delaminate. In order to strengthen the CNT networks, cobalt-nickel oxides were incorporated into the film. After coating the oxide layer, the CNT tips seemed to be more strongly adhered on the CNT bush. Without the oxide layer, the field emission voltage-current curve moved fast to a high voltage side as increasing the number of voltage sweeps. With the cobalt-nickel oxide incorporated, however, the curve does not move after the second voltage sweep. Such improvement of emission properties seemed to be attributed to stronger adhesion of the CNT film which was imparted by the cobalt-nickel oxide layer between CNT networks. Observed after field emission for an extended period of time, the CNT film with the oxide layer showed less damage on the surface caused by high current emission.
In nitride and oxide film deposition, sputtered metals react with nitrogen or oxygen gas in a vacuum chamber to form metal nitride or oxide films on a substrate. The physical properties of sputtered films (metals, oxides, and nitrides) are strongly influenced by magnetron plasma density during the deposition process. Typical target power densities on the magnetron during the deposition process are ~ (5-30) W/cm2, which gives a relatively low plasma density. The main challenge in reactive sputtering is the ability to generate a stable, arc free discharge at high plasma densities. Arcs occur due to formation of an insulating layer on the target surface caused by the re-deposition effect. One current method of generating an arc free discharge is to use the commercially available Pinnacle Plus+ Pulsed DC plasma generator manufactured by Advanced Energy Inc. This plasma generator uses a positive voltage pulse between negative pulses to attract electrons and discharge the target surface, thus preventing arc formation. However, this method can only generate low density plasma and therefore cannot allow full control of film properties. Also, after long runs ~ (1-3) hours, depends on duty cycle the stability of the reactive process is reduced due to increased probability of arc formation. Between 1995 and 1999, a new way of magnetron sputtering called HIPIMS (highly ionized pulse impulse magnetron sputtering) was developed. The main idea of this approach is to apply short ${\sim}(50-100){\mu}s$ high power pulses with a target power densities during the pulse between ~ (1-3) kW/cm2. These high power pulses generate high-density magnetron plasma that can significantly improve and control film properties. From the beginning, HIPIMS method has been applied to reactive sputtering processes for deposition of conductive and nonconductive films. However, commercially available HIPIMS plasma generators have not been able to create a stable, arc-free discharge in most reactive magnetron sputtering processes. HIPIMS plasma generators have been successfully used in reactive sputtering of nitrides for hard coating applications and for Al2O3 films. But until now there has been no HIPIMS data presented on reactive sputtering in cluster tools for semiconductors and MEMs applications. In this presentation, a new method of generating an arc free discharge for reactive HIPIMS using the new Cyprium plasma generator from Zpulser LLC will be introduced. Data (or evidence) will be presented showing that arc formation in reactive HIPIMS can be controlled without applying a positive voltage pulse between high power pulses. Arc-free reactive HIPIMS processes for sputtering AlN, TiO2, TiN and Si3N4 on the Applied Materials ENDURA 200 mm cluster tool will be presented. A direct comparison of the properties of films sputtered with the Advanced Energy Pinnacle Plus + plasma generator and the Zpulser Cyprium plasma generator will be presented.
Because collagen is inherently piezoelectric, research is being actively conducted to utilize it to harvest energy. In this study, a collagen solution was prepared using edible low-molecular-weight peptide collagen powder, and collagen films were fabricated using a dip coating method. The collagen films prepared by dip coating showed a smooth surface without defects such as pinholes or cracks. Dehydrothermal treatment of the collagen films was performed to induce a stable molecular structure through cross-linking. The collagen film subjected to dehydrothermal treatment at 110 ℃ for 24 h showed a thickness reduction rate of 19 %. Analysis of the collagen films showed that the crystallinity of the collagen film improved by about 7.9 % after dehydrothermal treatment. A collagen film-based piezoelectric nanogenerator showed output characteristics of approximately 13.7 V and 1.4 ㎂ in a pressure test of 120 N. The generator showed a maximum power density of about 2.91 mW/m2 and an output voltage of about 8~19 V during various human body movements such as finger tapping. The collagen film-based piezoelectric generator showed improved output performance with improved crystallinity and piezoelectricity after dehydrothermal treatment.
Flexible $TiO_2$ films were deposited as dielectric materials for high-energy-density capacitors on polyethylene terephthalate (PET) substrates using a roll-to-roll sputtering method. Both the growth behavior and electrical properties of the flexible $TiO_2$ films were dependent on the sputtering pressure and $O_2$/Ar gas ratio during the sputtering process. All $TiO_2$ films had an amorphous structure regardless of the sputtering conditions due to the low substrate temperature. Microstructural characteristics such as the surface morphology and roughness of the films degraded with an increase in the sputtering pressure and $O_2$ gas concentration. The $TiO_2$ films deposited at a low pressure showed better electrical properties than those of films deposited at a high pressure. The $TiO_2$ films prepared at 10 mTorr exhibited a dielectric constant of approximately 90 at 1 kHz and a leakage current density of $5{\sim}6{\times}10^{-7}A/cm^2$ at 3 MV/cm.
The plasma damage free and room temperature processedthin film deposition technology is essential for realization of various next generation organic microelectronic devices such as flexible AMOLED display, flexible OLED lighting, and organic photovoltaic cells because characteristics of fragile organic materials in the plasma process and low glass transition temperatures (Tg) of polymer substrate. In case of directly deposition of metal oxide thin films (including transparent conductive oxide (TCO) and amorphous oxide semiconductor (AOS)) on the organic layers, plasma damages against to the organic materials is fatal. This damage is believed to be originated mainly from high energy energetic particles during the sputtering process such as negative oxygen ions, reflected neutrals by reflection of plasma background gas at the target surface, sputtered atoms, bulk plasma ions, and secondary electrons. To solve this problem, we developed the NBAS (Neutral Beam Assisted Sputtering) process as a plasma damage free and room temperature processed sputtering technology. As a result, electro-optical properties of NBAS processed ITO thin film showed resistivity of $4.0{\times}10^{-4}{\Omega}{\cdot}m$ and high transmittance (>90% at 550 nm) with nano- crystalline structure at room temperature process. Furthermore, in the experiment result of directly deposition of TCO top anode on the inverted structure OLED cell, it is verified that NBAS TCO deposition process does not damages to the underlying organic layers. In case of deposition of transparent conductive oxide (TCO) thin film on the plastic polymer substrate, the room temperature processed sputtering coating of high quality TCO thin film is required. During the sputtering process with higher density plasma, the energetic particles contribute self supplying of activation & crystallization energy without any additional heating and post-annealing and forminga high quality TCO thin film. However, negative oxygen ions which generated from sputteringtarget surface by electron attachment are accelerated to high energy by induced cathode self-bias. Thus the high energy negative oxygen ions can lead to critical physical bombardment damages to forming oxide thin film and this effect does not recover in room temperature process without post thermal annealing. To salve the inherent limitation of plasma sputtering, we have been developed the Magnetic Field Shielded Sputtering (MFSS) process as the high quality oxide thin film deposition process at room temperature. The MFSS process is effectively eliminate or suppress the negative oxygen ions bombardment damage by the plasma limiter which composed permanent magnet array. As a result, electro-optical properties of MFSS processed ITO thin film (resistivity $3.9{\times}10^{-4}{\Omega}{\cdot}cm$, transmittance 95% at 550 nm) have approachedthose of a high temperature DC magnetron sputtering (DMS) ITO thin film were. Also, AOS (a-IGZO) TFTs fabricated by MFSS process without higher temperature post annealing showed very comparable electrical performance with those by DMS process with $400^{\circ}C$ post annealing. They are important to note that the bombardment of a negative oxygen ion which is accelerated by dc self-bias during rf sputtering could degrade the electrical performance of ITO electrodes and a-IGZO TFTs. Finally, we found that reduction of damage from the high energy negative oxygen ions bombardment drives improvement of crystalline structure in the ITO thin film and suppression of the sub-gab states in a-IGZO semiconductor thin film. For realization of organic flexible electronic devices based on plastic substrates, gas barrier coatings are required to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency flexible AMOLEDs needs an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}gm^{-2}day^{-1}$. The key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required (under ${\sim}10^{-6}gm^{-2}day^{-1}$) is the suppression of nano-sized defect sites and gas diffusion pathways among the grain boundaries. For formation of high quality single inorganic gas barrier layer, we developed high density nano-structured Al2O3 single gas barrier layer usinga NBAS process. The NBAS process can continuously change crystalline structures from an amorphous phase to a nano- crystalline phase with various grain sizes in a single inorganic thin film. As a result, the water vapor transmission rates (WVTR) of the NBAS processed $Al_2O_3$ gas barrier film have improved order of magnitude compared with that of conventional $Al_2O_3$ layers made by the RF magnetron sputteringprocess under the same sputtering conditions; the WVTR of the NBAS processed $Al_2O_3$ gas barrier film was about $5{\times}10^{-6}g/m^2/day$ by just single layer.
Hard disk drive(HDD) consists of a head/slider system which flies over the magnetic disk at an extremely low height. As the density of HDD increases the flying height of the head needs to be decreased. This increases the chance for contact between the slider and the disk. This paper addresses some key issues related to surface failure characteristics of HDD. It is shown that flying behavior of the slider during contact-start-stop cycle can be analyzed based on different regimes of air film lubrication, experimental methods for identifying the underlying mechanisms and improving the reliability of HDD are discussed.
Mg alloys have been developed for automobile and mobile equipments because of their low density of $1.7g/cm^3$. One of the main problems of Mg alloys is their poor corrosion resistance which has limited their wide applications. Plasma electrolytic oxidation (PEO) method is one of the promising surface treatment methods for Mg alloys. In this presentation, experimental data about the effects of solution composition and form of current are presented and discussed in view of dielectric breakdown and reformation of PEO films The role of various anions of phosphate, silicate, fluoride, carbonate and hydroxide ions is discussed in view of film breakdown and reformation of PEO films.
Anodization techniques are widely used in the area of surface treatment of aluminum alloys because of its simplicity, low-cost and good corrosion resistance. In this study, we investigated the relationship between the properties (porosity and thickness) of anodic aluminum oxide (AAO) and its corrosion behavior. Aluminum 5052 alloy was anodized in 0.3 M oxalic acid at $0^{\circ}C$. The anodizing of aluminum 5052 was performed at 20 V, 40 V and 60 V for various durations. The corrosion behavior was studied in 3.5 wt % NaCl using potentiodynamic polarization method. Results showed that the pore diameter and thickness increased as voltage and anodization time increased. The relatively thick oxide film revealed a lower corrosion current density and a higher corrosion potential value.
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