• Journal of Surface Science and Engineering
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• v.25 no.5
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• pp.235-252
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• 1992

(Ti, Al)N films were deposited on 304 stainless steel sheet by D.C. magnetron sputtering using Al target and Ti plate. The high temperature oxidation of (T, Al)N films with the variation of composition has been investigated. The chemical composition of (Ti, Al)N films with the variation of composition has been investigated. The chemical composition of (Ti, Al)N films was similar to the sputter area ratio of titanium to aluminum target by means of EDS and AES survey. The high temperature oxidation test of (Ti, Al)N showed that (Ti, Al)N has better high temperature resistance than TiN and TiC films. TiC films were cracked at 40$0^{\circ}C$ in air TiN films quickly were oxidised at $600^{\circ}C$, were spalled more than $700^{\circ}C$. But (Ti, Al)N films are relatively stable to$ 900^{\circ}C$. The good resistance to high temperature oxida-tion of (Ti, Al)N films are due to the formation of dense Al2O3 and TiO2 oxide layer. Especially, Al2O3 oxide layer is more important. The results obtained from this study show, it is believe that the (Ti, Al)N film by D.C. magnetron sputtering is promising for the use of high temperature and wear resistance mate-rials.

• Journal of Surface Science and Engineering
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• v.31 no.5
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• pp.251-260
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• 1998

Stainless Steel is being used widely for various purposes due to its good corrosion resistance. There have been many researches to produce colored stainless steel by several methods such as anodizing and ion-plating. In this experiment, we $Ti_XN$(C,O) on the films SUS304, aluminium, and glass substrates with DC magentron sputterinng system made by Leybold Hereus, and strdied the structur, corrsion and pit characture of the TiXN observed by TeM image was black and whink and white columnar hed a very fine(200$\AA$) dense sturcture,and the diffraction resistance at the $3{\times}10_6A/\textrm{cm}^2$ and $10_{10}\times{cm}^2$current density were obtained in the under-stoichiometry $Ti_xN$ compound of Ar/$N_2$(Ar:$N_2$=100:6, titanium-rich compound) and the over-stoichiometry compound of Ar/$N_2$((Ar:$N_2$=60:15) respectively. When the thiness was over 1.64$\mu\textrm{m}$, good pit resistance could be obtained and its improvement was especially affected by perfect surfaceface. Typical TiN anodic polarzation curves of very unstable corrosion were observed by $Ti_xN$ film on the glass and perfect film of 3.28$\mu\textrm{m}$ thickness.

• Korean Journal of Metals and Materials
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• v.50 no.1
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• pp.86-91
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• 2012

Ti-6Al-4V extra low interstitial (ELI) alloy has been widely used as an orthopedic implant material because of its excellent biocompatibility, corrosion resistance and mechanical properties. However, V-free titanium alloys such as Ti-6%Al-7%Nb and Ti-5%Al-2.5%Fe have recently been developed because of the toxicity of V. Hydroxyapatite (HA) is used as a coating material on Ti or Ti biomaterials due to its good biocompatibility. However, HA coated on Ti alloy causes a problem for tissue by peeling off during usage. Therefore, such peeling off during long time usage can be suppressed by adding HA in Ti or Ti alloy composites. The aim of this study was to manufacture an ultra fine grained (UFG) Ti-Nb-HA bulk alloy, which is usually difficult to fabricate using melting and casting technology, by rapid sintering process using high energy mechanical milled (HEMM) powder.

• Archives of Metallurgy and Materials
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• v.65 no.4
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• pp.1357-1360
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• 2020

The low adherence of diamond-like carbon (DLC) films on titanium (Ti) alloys can be improved by using interlayer coatings. In this study, DLC (a-C:H) films were deposited using radio-frequency plasma-enhanced chemical vapor deposition (rf-PECVD), and a TiCN interlayer was applied between the extra low interstitial (ELI) grade of Ti-6Al-4V alloy and a-C:H film. The characteristics of the a-C:H-coated Ti-6Al-4V ELI alloy were investigated using field emission scanning electron microscopy, Vickers hardness, and scratch and wear tests. The DLC (a-C:H) films deposited by rf-PECVD had a thickness of 1.7 ㎛, and the TiCN interlayer had a thickness of 1.1 ㎛. Vickers hardness of the DLC (a-C:H) films were increased as a result of the influence of the TiCN interlayer. The resulting friction coefficient of the a-C:H-coated Ti-6Al-4V with the TiCN interlayer had an extremely low value of 0.07.

• Korean Journal of Dental Materials
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• v.44 no.3
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• pp.263-272
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• 2017

In this study, antibacterial chlorhexidine (CHX)-containing hydroxyapatite (HAp) was coated on titanium and investigated its characteristics. Ti-mSBF-CHX group was prepared by soaking titanium disks in the modified simulated body fluid (mSBF) mixed with CHX. Ti-mSBF group was coated using mSBF without CHX. Ti-mSBF-adCHX group was prepared by soaking Ti-mSBF specimen in CHX-containing solution. The crystallines clusters composed with nano-shaped crystallites were coated on the surface of the Ti-mSBF specimen. The ribbon-shaped crystallites were observed with the crystalline clusters on the Ti-mSBF-CHX specimen. The content of CHX chemical compositions was high in ribbon-shaped crystallites. HAp crystalline structure was dominant for all prepared specimens, and ${\beta}-TCP$ (tricalcium phosphate) and OCP (octacalcium phosphate) crystalline structures were observed in the Ti-mSBF-CHX specimen. FT-IR spectra showed the strong peaks of CHX in Ti-mSBF-adCHX and Ti-mSBF-CHX groups. However, after immersing in a phosphate buffered saline (PBS), CHX was rapidly released in Ti-mSBF-adCHX group, while it was slowly released in Ti-mSBF-CHX. We expect that the coating method of Ti-mSBF-CHX group could be used for protecting inflammation of titanium implant by incorporating antibacterial agent CHX into HAp layer.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.195-195
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• 2016

Titanium and its alloys are widely used as implants in orthopedics, dentistry and cardiology due to their outstanding properties, such as high strength, high level of hemocompatibility and enhanced biocompatibility. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element, such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}-stabilizer$ and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. The aim of this study is to research Si and Mg doped hydroxyapatite film formation by plasma electrolytic oxidation. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. Each alloy was anodized in solution containing typically 0.15 M calcium acetate monohydrate + 0.02 M calcium glycerophosphate at room temperature. A direct current power source was used for the process of anodization. Anodized alloys was prepared using 270V~300V anodization voltage at room. A Si and Mg coating was produced by RF-magnetron sputtering system. RF power of 100W was applied to the target for 1h at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.199-199
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• 2016

Commercially pure titanium (cp-Ti) and Ti alloys (typically Ti-6Al-4V) display excellent corrosion resistance and biocompatibility. Although the chemical composition and topography are considered important, the mechanical properties of the material and the loading conditions in the host have, conventionally. Ti and its alloys are not bioactive. Therefore, they do not chemically bond to the bone, whereas they physically bond with bone tissue. The electrochemical deposition process provides an effective surface for biocompatibility because large surface area can be served to cell proliferation. Electrochemical deposition method is an attractive technique for the deposition of hydroxyapatite (HAp). However, the adhesions of these coatings to the Ti surface needs to be improved for clinical used. Plasma electrolyte oxidation (PEO) enables control in the chemical com position, porous structure, and thickness of the $TiO_2$ layer on Ti surface. In addition, previous studies h ave concluded that the presence of $Ca^{+2}$ and ${PO_4}^{3-}$ ion coating on porous $TiO_2$ surface induced adhesion strength between HAp and Ti surface during electrochemical deposition. Silicon (Si) in particular has been found to be essential for normal bone and cartilage growth and development. Zinc (Zn) plays very important roles in bone formation and immune system regulation, and is also the most abundant trace element in bone. The objective of this work was to study electrochemical characteristcs of Zn and Si coating on Ti-6Al-4V by PEO treatment. The coating process involves two steps: 1) formation of porous $TiO_2$ on Ti-6Al-4V at high potential. A pulsed DC power supply was employed. 2) Electrochemical tests were carried out using potentiodynamic and AC impedance methoeds. The morphology, the chemical composition, and the micro-structure an alysis of the sample were examined using FE-SEM, EDS, and XRD. The enhancements of the HAp forming ability arise from $Si/Zn-TiO_2$ surface, which has formed the reduction of the Si/Zn ions. The promising results successfully demonstrate the immense potential of $Si/Zn-TiO_2$ coatings in dental and biomaterials applications.

• The Journal of Korean Academy of Prosthodontics
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• v.48 no.2
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• pp.122-127
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• 2010

Purpose: The objective of this study was to investigate the effects of calcium phosphate coated titanium implant surface on bone response and implant stability at early stage of healing period of 3 weeks and later healing period of 6 weeks. Material and methods: A total of 24 machined, screw-shaped implants (Dentium Co., Ltd., Seoul, Korea) which dimensions were 3.3 mm in diameter and 5.0 mm in length, were used in this research. All implants (n = 24), made of commercially pure (grade IV) titanium, were divided into 2 groups. Twelve implants (n = 12) were machined without any surface modification (control). The test implants (n = 12) were anodized and coated with thin film (150nm) of calcium phosphate by electron-beam deposition. The implants were placed on the proximal surface of the rabbit tibiae. The bone to implant contact (BIC) ratios was evaluated after 3 and 6 weeks of implant insertion. Results: The BIC percentage of calcium phosphate coated implants ($70.8{\pm}18.9%$) was significantly higher than that of machined implants ($44.1{\pm}16.5%$) 3 weeks after implant insertion (P = 0.0264). However, there was no significant difference between the groups after 6 weeks of healing (P > .05). Conclusion: The histomorphometric evaluation of implant surface revealed that; 1. After 3 weeks early healing period, bone to implant contact (BIC) percentage of calcium phosphate coated implants (70.8%) was much greater than that of surface untreated machined implants (44.1%) with P = 0.0264. 2. After 6 weeks healing period, however, BIC percentage of calcium phosphate coated implants group (79.0%) was similar to the machined only implant group (78.6%). There was no statistical difference between two groups (P = 0.8074). 3. We found the significant deference between the control group and experimental group during the early healing period of 3 weeks. But no statistical difference was found between two groups during the later of 6 weeks.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.4
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• pp.167-172
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• 2013

Titanium dioxides nanoparticles coated aluminum oxide powders were fabricated by pulsed laser deposition (PLD) with Nd : YAG laser at 266 nm. The Pulse laser energy is 100 mJ/pulse. During the irradiation of the focused laser on the $TiO_2$ target, Ar gas is supplied into the chamber. The gas pressure is varied in a range of $1{\times}10^{-2}$ to 100 Pa. Titanium dioxides nanoparticles deposited aluminum oxide powders were characterized by using energy dispersive X-ray spectroscopy (EDX), high resolution transmission electron microscopy (HR-TEM), in order to understand the effect of Ar background gas on surface morphology and properties of the powders. The coated $TiO_2$ nanoparticles had nanosized spherical shape and the crystallite sizes of 10~30 nm. The morphology of coated $TiO_2$ nanoparticles is not affected by gas pressure. However, the particle size and crystallinity slightly increased with the increase of gas pressure. According to this technique, the size and crystallinity of nanoparticles can be easily controlled by controlling pressure during the laser irradiation.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1999.10a
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• pp.3-4
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• 1999

최근 산업이 고속도화, 고능률화 및 고정멸화의 추세로 발전함에 따라 우수한 내마모성, 인성, 고온 안정성 및 내구성을 갖는 공구 및 금형을 요구하게 되었다. 그러나 이와같은 성질들은 어떤 단일 재료에서는 얻을 수 없으며 적당한 기판공구나 금혈위에 내마모성 보호피막을 coating함으로 비교적 저렴하게 얻을 수 있다. 화학증착법으로 TiC, TiN등을 증착시킬때에는 $1000^{\circ}C$정도의 반응온도가 필요하며 이러한 증착온도는 모재가 초경합금일때는 문제가 안되나 강재일 경우 모재의 연화와 칫수변화의 문제를 야기시킨다. 최근에는 플라즈마를 사용하여 증착반응온도를 $550^{\circ}C$ 이하로 낮추는 플라즈마 화학 증착볍(PACVD)이 대두되고 있다. 그러나 이 방법어서 는 뚱착하려는 금속원소가 TiCl4의 형태로 공급되고 있으므로 생성된 층이 염소를 포함하고 있다. 이 층에 잔존하는 염소는 층의 기계적 성질을 저하시키고 층내의 stress를 유발시킨다. 또한 HCI개스의 생성으로 인하여 펌프 및 장비의 부식이 촉진 된다 이러한 결점을 극복하기 위하여 금속유기화합물 전구체(metallo-organic precursor)로 $TiCl_4$를 대체하고자 하는 연구가 활발하게 진행되고 있으며 본 연구실에서 이에 대하여 연구한 결과를 소개하고자 한다. diethylamino titanium을 전구체로 사용하여 $H_2,\;N_2,\;Ar$분위기하에서 pulsed d.c.를 사용하는 MO-PACVD에 의하여 $150~250^{\circ}C$의 저온에서 Al 2024 기판에 TiCN층 형 성을 하였다. 전구체 증발온도는 $74~78^{\circ}C$의 온도범위어야 하며 고경도의 코탱층은 54% duty, 14.2kHz, 450V의 조건에서 얻어졌으며 duty, 주파수, 전압이 증가함에 따라 경도는 저하되었다. 이때의 표면 morphology를 SEM으로 조사한바 dome structure가 크게 발달되었음을 알 수 있었다. 본 실험의 온도 범위내에서 얻은 TiCN 증착반응의 활성화에너지는 7.5Kcal/mol이었다. 증착된 TiCN층은 우수한 내마모섣을 나타내었으며 스크래치테스트 결과 17N의 엄계하중을 나타내었다. 본 연구에서 변화 시킨 duty, 주파수, 전압의 범위에서는 층의 밀착력은 크게 변화하지 않았다. titanium isopropoxide를 전구체로 사용하여 Hz, Nz 분위기하에서 d.c.를 사용하는 MO-PACVD에 의하여 Ti(NCO) 코팅층을 SKDll, SKD61, SKH9 공구강에 형성시키는 공정을 개발하였다. 최적의 Ti(NCO) 코탱층을 얻기 위해 유입전구체 부피%의 양은 향착압력의 5%를 넘지 않아야 되고 수소와 젤소 가스비가 1:1일 때 가장 높은 코팅층의 경도값을 나타내었다. 수소와 질소 가스비가 3:7일 때 TiFeCr(NCO)의 복화합물 코팅층이 형성됨을 알 수 있었고 500t의 증착온도에서 얻은 Ti(NCO) 코팅층이 높은 경도값과 좋은 내식성을 나타내었다. 또한 이와같은 Ti(NCO) 코팅공정과 본 실험실에서 개발한 확산층만 형성시키는 plsma nitriding 공정을 결합하여 복합코탱층을 형성하였는데 이 복합코팅층은 고경도와 우수한 내마모성, 내식성 뿐만 아니라 10)N 이상의 뛰어난 밀착력을 나타내었다. 현재 많이 사용되고 있는 PVD법은 step coverage가 좋지 않은 점과 cost intensive p process라는 단점이 있다. MO-PACVD법은 이러한 문제를 해결할 수 있는 방법으로서 앞으로 지속적인 도전이 요구되는 분야이다.