• Title/Summary/Keyword: Physical Vapor Deposition(PVD)

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Effects of HA and TiN Coating on the Electrochemical Characteristics of Ti-6Al-4 V Alloys for Bone Plates

  • Oh, Jae-Wook;Choe, Han-Cheol;Ko, Yeong-Mu
    • Journal of the Korean institute of surface engineering
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    • v.37 no.5
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    • pp.249-252
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    • 2004
  • Effects of HA and TiN coating on the electrochemical characteristics of Ti-6AI-4V alloys for bone plates were investigated using various test methods. Ti-6AI-4V alloys were fabricated by using a vacuum induction furnace and bone plates were made by laser cutting and polishing. HA was made of extracted tooth sintered and then tooth ash was used as HA coating target. The TiN and HA film coating on the surface were carried on using electron-beam physical vapor deposition (EB-PVD) method. The corrosion behaviors of the samples were examined through potentiodynamic method in 0.9% NaCI solutions at $36.5\pm$$1^{\circ}C$ and corrosion surface was observed using SEM and XPS. The surface roughness of TiN coated bone plates was lower than that of tooth ash coated plates. The structure of TiN coated layer showed the columnar structure and tooth ash coated layer showed equiaxed and anisotrophic structure. The corrosion potential of the TiN coated specimen is comparatively high. The active current density of TiN and tooth ash coated alloy showed the range of about $1.0xl0^{-5}$ $A\textrm{cm}^2$, whereas that of the non-coated alloy was$ 1.0xl0^{-4}$ $A\textrm{cm}^2$. The active current densities of HA and TiN coated bone plates were smaller than that of non-coated bone plates in 0.9% NaCl solution. The pitting potential of TiN and HA coated alloy is more drastically increased than that of the non-coated alloy. The pit number and pit size of TiN and HA coated alloy decreased in compared with those of non-coated alloy. For the coated samples, corrosion resistance increased in the order of TiN coated, tooth ash coated, and non-coated alloy.

High temperature properties of surface-modified Hastelloy X alloy (표면처리에 따른 Hastelloy X 합금의 고온물성)

  • Cho, Hyun;Lee, Byeong-Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.4
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    • pp.183-189
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    • 2012
  • Surface treatments and their effects on high temperature properties for the Hastelloy X, which is a promising candidate alloy for high temperature heat-transport system, have been evaluated. For TiAlN and $Al_2O_3$ overlay coatings, the two different PVD (physical vapor deposition) methods using an arc discharge and a sputtering, were applied, respectively. In addition, a different surface treatment method of the diffusion coating by a pack cementation of Al (aluminiding) was also adopted in this study. To achieve enhanced thermal oxidation resistance at $1000^{\circ}C$ by suppressing the inhomogeneous formation of thick $Cr_2O_3$ crust at the surface region, a study for the surface modification methods on the morphological and structural properties of Hastelloy X substrates has been conducted. The structural and compositional properties of each sample were characterized before and after heat-treatment at $1000^{\circ}C$ under air and He environment. The results showed that the Al diffusion coating showed the more enhanced high temperature properties than the overlay coatings such as the suppressed thick $Cr_2O_3$ crust formation and lower wear loss.

Thermal stability of surface modified Ni-Cr-alloys in molten FLiNaK salt (표면처리된 Ni-Cr계 합금의 FLiNaK 용융염 하에서의 고온 안정성)

  • Kwang, Hyun Cho;Bang, Hyun;Lee, Tae Suk;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.5
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    • pp.227-232
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    • 2012
  • Inconel 617 and Hastelloy X are the most promising candidate materials for the heat exchanger of next generation nuclear reactor. Surface coating and its effects on high temperature properties for the Inconel 617 and Hastelloy X under molten FLiNaK (LiF-NaF-KF) salt environment have been investigated. For TiAlN and $Al_2O_3$ overlay coatings, the two different PVD (physical vapor deposition) methods of an arc discharge and a sputtering were applied, respectively. A study for the thermal stability of the surface modified Ni-Cr alloy substrates has been conducted. To evaluate the corrosion mechanism of Ni-Cr alloys in the molten salt, a ruptured Inconel pipe used for the molten salt transportation has been analyzed. The thermal properties of morphological and structural properties each sample were characterized before and after heat-treatment at $600^{\circ}C$ in molten FLiNaK salt. The results showed that the TiAlN and $Al_2O_3$ overlay coated specimens had the enhanced high temperature stability.

Performance Evaluation of Magnesium Bipolar Plate in Lightweight PEM Fuel Cell Stack for UAV (무인기용 경량 PEM 연료전지 스택용 마그네슘 분리판의 성능평가)

  • Park, To-Soon;Oh, Ji-Hyun;Ryu, Tae-Kyu;Kwon, Se-Jin
    • Journal of the Korean Society for Aeronautical & Space Sciences
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    • v.41 no.10
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    • pp.788-795
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    • 2013
  • A magnesium bipolar plate whose surface was protected by thinly deposited silver layer was investigated as an alternative to existing graphite bipolar plate of PEM fuel cells. Thin silver layer of $3{\mu}m$ was deposited on a magnesium alloy substrate by physical vapor deposition (PVD) method in an environment of $180^{\circ}C$. A number of tests were conducted on the fabricated magnesium based bipolar plates to determine their suitability for use in PEM fuel cell stacks. The test on corrosion resistance in the same pH condition as in a PEM operation demonstrated the layer protected the magnesium alloy substrate, while unprotected substrate suffered from severe corrosion. The contact resistance of the fabricated bipolar plate was less than $20m{\Omega}-cm^2$ which was superior to the conventional bipolar plates. A single cell was constructed using the fabricated bipolar plates and power output was measured. Due to the enhanced conductivity caused by low contact resistance, slight increase was observed in current density and output voltage. With low density of the magnesium substrate and ease on machining, the weight reduction of the stack of 30~40 % is possible to produce the same power output.

A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.239-240
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    • 2008
  • As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

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Process technology and the formation of the TiN barrier metal by physical vapor deposition (PVD 방법에 의한 TiN barrier metal 형성과 공정개발)

  • 최치규;강민성;박형호;염병렬;서경수;이종덕;김건호;이정용
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.255-262
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    • 1997
  • Titanium nitride (TiN) films were prepared by reactive sputter deposition in mixed gas of Ar+$N_2$. The volume percentage of $N_2$ in the working gas was chosen so as to grow stoichiometric TiN films and the substrate temperature during film growth was set from room temperature to $700^{\circ}C$. Stoichiometric $Ti_{0.5}N){0.5}$ films with (111) texture were grown at temperatures over $600^{\circ}C$, while films prepared at temperatures below $600^{\circ}C$ showed N-rich TiN. The composition X and y in the $Ti_xN_y$ films determined by XPS and RBS varied within 5% with the substrate temperature. The sheet resistance of the TiN films decreases as the substrate temperature increased. TiN film prepared at $600^{\circ}C$ showed 14.5$\Omega\Box$, and it decreased to 8.9$\Omega\Box$ after the sample was annealed at $700^{\circ}C$, 30 sec in Ar-gas ambient by RTA. By far, high quality stoichiometric TiN films by reactive sputtering in the mixed gas ambient could be prepared at substrate temperature over $600^{\circ}C$.

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A STUDY ON MECHANICAL PROPERTIES OF TiN, ZrN AND WC COATED FILM ON THE TITANIUM ALLOY SURFACE

  • Oh, Dong-Joon;Kim, Hee-Jung;Chung, Chae-Heon
    • The Journal of Korean Academy of Prosthodontics
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    • v.44 no.6
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    • pp.740-750
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    • 2006
  • Statement of problems. In an attempt to reduce screw loosening, dry lubricant coatings such as pure gold or tefron have been applied to the abutment screw. However, under repeated tightening and loosening procedures, low wear resistance and adhesion strength of coating material produced free particles on the surface of abutment screw and increased frictional resistance resulting in screw tightening problems. Purpose. The aim of this study was to compare friction coefficient, adhesion strength, vickers hardness and evaluate coating surface of titanium alloy specimens coated with TiN(titanium nitride), ZrN(zirconium nitride) and WC(tungsten carbide). Material and method. Titanium alloy(Ti-6Al-4V) discs of 12mm in diameter and 1mm in thickness divided into 4 groups. TiN, ZrN and WC was coated for the specimens of 3 groups respectively, and those of 1 group were not coated. Each group was made up of 4 specimens. In this study, sputtering method was used among the PVD(Physical Vapor Deposition) techniques available for TiN, ZrN and WC coatings. Friction coefficient, adhesion strength, vickers hardness and coating surface of 4 groups were measured. Results. 1. For all three coating conditions, friction coefficient was significantly decreased. Especially, ZrN coated surface showed the lowest value. $TiN(0.39{\pm}0.02)$, $ZrN(0.24{\pm}0.01)$, $WC(0.31{\pm}0.03)$. 2. TiN coating showed the highest adhesion strength, however ZrN coating had the lowest value. $TiN(25.3N{\pm}1.6)$, $ZrN(14.8N{\pm}0.6)$, $ WC(18.4N{\pm}0.7)$. 3. Vickers hardness of all three coatings was remarkably increased as compared with that of none coated specimen. TiN coating had the highest Vickers hardness, however WC coating showed the lowest value. $TiN(1865.2{\pm}33.8)$, $ZrN(1814.4{\pm}18.6)$, $WC(1008.5{\pm}35.9)$. 4. The ZrN or WC coated specimen showed a homogeneous and smooth surface, however the rough surface with defects was observed for TiN coating. Conclusions. When TiN, ZrN and WC coating applied to the abutment screw, frictional resistance would be reduced, as a result, the greater preload and prevention of the screw loosening could be expected.

HIGH HEAT FLUX TEST WITH HIP BONDED 35X35X3 BE/CU MOCKUPS FOR THE ITER BLANKET FIRST WALL

  • Lee, Dong-Won;Bae, Young-Dug;Kim, Suk-Kwon;Jung, Hyun-Kyu;Park, Jeong-Yong;Jeong, Yong-Hwan;Choi, Byung-Kwon;Kim, Byoung-Yoon
    • Nuclear Engineering and Technology
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    • v.42 no.6
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    • pp.662-669
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    • 2010
  • To develop the manufacturing methods for the blanket first wall (FW) of the International Thermonuclear Experimental Reactor (ITER) and to verify the integrity of the joint, Be/Cu mockups were fabricated and tested at the KoHLT-1 (Korea Heat Load Test facility), a graphite heater facility located at the Korea Atomic Energy Research Institute (KAERI). Since Be and Cu joining is the focus of the present study, the fabricated mockups had a CuCrZr heat sink joined with three Be tiles as an armor material, unlike the original ITER blanket FW, which has a stainless steel structure and coolant tubes. Hot isostatic pressing (HIP) was carried out at $580^{\circ}C$ and 100 MPa for 2 hours as the method for Be/Cu joining. Three interlayers, namely, $1{\mu}mCr/10{\mu}mCu$, $1{\mu}mTi/0.5{\mu}mCr/10{\mu}mCu$, and $5{\mu}mTi/10{\mu}mCu$ were applied as a coating to the Be tiles by a physical vapor deposition (PVD) method. A shear test was performed with the specimens, which were fabricated by the same methods as those used to fabricate the mockups. The average values were 125 MPa to 180 MPa, and the samples with the $1{\mu}mCr/10{\mu}mCu$ interlayer showed the lowest value. No defect or delamination was found in the joints of the mockups by the developed ultrasonic test using a flat-type probe with a 10 MHz frequency and a 0.25 inch diameter. High heat flux (HHF) tests were performed at $1.0\;MW/m^2$ heat flux for each mockup using the given conditions, and the results were analyzed by ANSYS-CFX code. For the test criteria, an expected fatigue lifetime about 1,000 cycles was obtained by analysis with ANSYS-mechanical code. Mockups using the interlayers of $1{\mu}mTi/0.5{\mu}mCr/10{\mu}mCu$ and $5{\mu}mTi/10{\mu}mCu$ survived up to 1,100 cycles over the required number of cycles. However, one of the Be tiles in the other two mockups using the $1{\mu}mCr/10{\mu}mCu$ interlayer was detached during the screening test, and others were detached by discharge after 862 cycles. The integrity of the joints using the proposed interlayers was proven by the HHF test, but the other interlayer requires more study before it can be used for the joining of Be to Cu. Moreover, it was confirmed that the measured temperatures agreed well with the analysis temperatures, which were used to estimate the lifetime and that the developed facility showed its capability of the long time operation.