Hydroxyapatite-silicon film deposited on Ti–Nb–10Zr by electrochemical and magnetron sputtering method

Jeong, Yong-Hoon,Choe, Han-Cheol,Brantley, William A Elsevier 2016 THIN SOLID FILMS - Vol.620 No.-

<P><B>Abstract</B></P> <P>The purpose of this study was to investigate silicon-doped hydroxyapatite (HA) films deposited on Ti–35Nb–10Zr by an electrochemical and magnetron sputtering method. The Ti–35Nb–10Zr alloy was manufactured in an arc-melting furnace. Electrochemical deposition of HA was performed by pulsing the potential, using cyclic voltammetry, in the electrolyte composed of 5mM·Ca(NO<SUB>3</SUB>)<SUB>2</SUB>·4H<SUB>2</SUB>O+6.0mM·NH<SUB>4</SUB>H<SUB>2</SUB>PO<SUB>4</SUB> at 85°C. The silicon doping was performed with a pure Si target by radio-frequency (RF) magnetron sputtering with variable deposition time. The surface characteristics were investigated by field-emission scanning electron microscopy, X-ray diffraction, and electrochemical corrosion testing. It was found that the Si particles on the electrochemically deposited HA layer became thicker with increased sputtering time. The composition of the Si-HA coating surface showed a decrease of the Ca/P ratio with increased sputtering time. The intensity of X-ray diffraction peaks for the HA coating was increased by annealing, and there were no phase changes or appearance of other peaks from the annealing treatment. From the corrosion test, an increase in Si sputtering time could cause higher corrosion potential and lower corrosion current density. Increasing the Si sputtering time increased the corrosion resistance in the passivation region.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Si sputtering was performed on the HA layer electrochemically deposited on the titanium alloy. </LI> <LI> The Si layer was deposited onto HA particles with a plate-like morphology. </LI> <LI> The Si particles in the layer became thicker with longer sputtering times. </LI> <LI> The crystallinity of the HA layer was not changed by Si sputtering. </LI> <LI> Corrosion resistance of the titanium alloy was increased with longer Si sputtering times. </LI> </UL> </P>

RF reactive magnetron sputtering으로 제조한 TiO₂ 박막의 구조 및 광학적 특성

강계원,이영훈,곽재천,이동구,정봉교,박성호,최병호,Gang, Gye-Won,Lee, Yeong-Hun,Gwak, Jae-Cheon,Lee, Dong-Gu,Jeong, Bong-Gyo,Park, Seong-Ho,Choe, Byeong-Ho 한국재료학회 2002 한국재료학회지 Vol.12 No.6

Titanium oxide films were prepared by RF reactive magnetron sputtering. The effect of sputtering conditions on structural and optical properties was investigated systemically as a function of sputtering pressure(5~20 mTorr) and $O_2/Ar$ flow ratio(0.08~0.4). The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. At low sputtering pressure and $O_2/Ar$ flow ratio, the films had preferred orientations along [101] and [200] directions. As the sputtering pressure and $O_2/Ar$ flow ratio increased, the intensity of the 101 and 200 diffraction peaks decreased gradually. The microstructure of the sputtered films showed the fine grain size (20nm~50nm) and columnar microcrystals perpendicular to the substrate. With increasing the sputtering pressure and decreasing $O_2/Ar$ flow ratio, the sputtered films showed the more porous columnar structure. XPS analysis showed that stoichiometric $TiO_2$ films were deposited at 7 mTorr sputtering pressure and 0.2 $O_2/Ar$ flow ratio. The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. Ellipsometeric analysis showed that the refractive index increased from 2.32 to 2.46 as the sputtering pressure decreased. The packing density calculated using the refractive index varied from 0.923 to 0.976, indicating that $TiO_2$films became denser as the sputtering pressure decreased.

알루미늄 스퍼터링 처리 의류소재의 스텔스 특성과 전자파 차단 및 전기적 특성에 관한 연구- 밀도 변화를 중심으로 -

한혜리 복식문화학회 2022 服飾文化硏究 Vol.30 No.4

This study examines the surface characteristics, electrical conductivity, electromagnetic wave blocking characteristics, infrared (IR) transmittance, stealth function, thermal characteristics, and moisture characteristics of IR thermal imaging cameras. Nylon film (NFi), nylon fabric (NFa), and 5 types of nylon mesh were selected as the base materials for aluminum sputtering, and aluminum sputtering was performed to study IR thermal imaging, color difference, temperature change, and so on, and the relationship with infrared transmittance was assessed. The electrical conductivity was measured and the aluminum-sputtered nylon film demonstrated 25.6kΩ of surface resistance and high electrical conductivity. In addition, the electromagnetic wave shielding characteristics of the sputtering-treated nylon film samples were noticeably increased as a result of aluminum sputtering treatment as measured by the electromagnetic wave blocking characteristics. When NFi and NFa samples with single-sided sputtering were placed on the human body (sputtering layer faced the outside air) and imaged using IR thermographic cameras, the sputtering layer displayed a color similar to the surroundings, showing a stealth effect. Moreover, the tighter the sample density, the better the stealth function. According to the L, a, b measurements, when the sputtering layer of NFi and NFa samples faced the outside air, the value of a was generally high, thereby demonstrating a concealing effect, and the △E value was also high at 124.2 and 93.9, revealing a significant difference between the treated and untreated samples. This research may be applicable to various fields, such as the military wear, conductive sensors, electromagnetic wave shielding film, and others.

DC 및 RF 스퍼터링법으로 증착한 Cr 박막의 특성 비교

박민우,이종무,Park, Min-Woo,Lee, Chong-Mu 한국재료학회 2006 한국재료학회지 Vol.16 No.8

Chromium (Cr) films were deposited on plain carbon steel sheets by DC and RF magnetron sputtering as well as by electroplating. Effects of DC or RF sputtering power on the deposition rate and properties such as, hardness, surface roughness and corrosion-resistance of the Cr films were investigated. X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microcopy (SEM) analyses were performed to investigate the crystal structure, surface roughness, thickness of the Cr films. Salt fog tests were used to evaluate the corrosion resistance of the samples. The deposition rate, hardness, and surface roughness of the Cr film deposited by either DC or RF sputtering increase with the increase of sputtering power but the adhesion strength is nearly independent of the sputtering power. The deposition rate, hardness, and adhesion strength of the Cr film deposited by DC sputtering are higher than those of the Cr film deposited by RF sputtering, but RF sputtering offers smoother surface and higher corrosion-resistance. The sputter-deposited Cr film is harder and has a smoother surface than the electroplated one. The sputter-deposited Cr film also has higher corrosion-resistance than the electroplated one, which may be attributed to the smoother surface of the sputter-deposited film.

The transient sputtering yield change of an amorphous Si layer by low energy $O_2^{+}$ and $Ar^{+}$ ion bombardment

Shin, Hye-Chung,Kang, Hee-Jae,Lee, Hyung-Ik,Moon, Dae-Won The Korean Vacuum Society 2003 Applied Science and Convergence Technology Vol.12 No.1

The sputtering yield change of an amorphous Si layer on Si(100) was measured quantitatively for 0.5 keV $O_2^{+}$ and $Ar^{+}$ ion bombardment with in suit MEIS. In the case of 0.5 keV $O_2^{+}$ ion bombardment, at the initial stage of sputtering before surface oxidation, the sputtering yield of Si was 1.4 (Si atoms/$O_2^{+}$) and then decreased down to 0.06 at the ion dose of $3\times10^{16}O_2\;^{+}\textrm{/cm}^2$. In the case of 0.5 keV $Ar^{+}$ ion bombardment, the sputtering yield of Si for the surface normal incidence was 0.56 at the ion dose of 2.5 ${\times}$ 10$^{15}$ $Ar^{+}\textrm{cm}^2$, and rapidly saturated to 1.2 at dose of $7.5\times10^{15}Ar^+\textrm{cm}^2$. For the incidence angle of 80 from surface normal, the sputtering yield of Si was saturated to about 1.4 at the initial stage of sputtering. The surface transient effects, caused by change in sputtering yield at the initial stage of sputtering can be negligible when 0.5 keV $Ar^{+}$ ion at extremely grazing angle was used for sputter depth profiling.g.

Effect of Sputtering Power on the Nucleation and Growth of Cu Films Deposited by Magnetron Sputtering

Le, Minh-Tung,Sohn, Yong-Un,Lim, Jae-Won,Choi, Good-Sun The Japan Institute of Metals 2010 Materials Transactions Vol.51 No.1

<P>Cu thin films were deposited on Si(100) substrates using direct current (DC) magnetron sputtering. We focused on the effect of sputtering DC power on the electrical, structural properties, and the nucleation and growth of Cu films during the initial stage of sputtering. The Cu films deposited at higher sputtering power showed strong crystallinity, low electrical resistivity in comparison with the Cu films deposited at lower sputtering power. Concerning the nucleation and growth of Cu films during initial stage of magnetron sputtering, it was found that the progress of the nucleation and growth of the Cu films at higher sputtering is much faster than those of the Cu films at lower sputtering power even though they have a similar nucleation and growth mechanism, and their relation to resultant microstructure was confirmed by atomic force microscopy.</P>

RF sputtering을 이용한 BaTiO_3 세라믹 박막의 제조 및 특성에 관한 연구

이영희,류기원 광운대학교 신기술연구소 1997 신기술연구소논문집 Vol.26 No.-

본 연구에서는 RF sputtering을 이용하여 Pt/SiO_2/Si(100) 기판 위에 BaTiO_3 박막을 제조하였으며, 박막의 구조적, 결정학적 특성을 증착조건과 열처리온도에 따라 조사하였다. 최적의 Ar/O_2 gas 비, sputtering 압력, RF power, 그리고 열처리온도는 각각 4/1, 12[mTorr], 120[W] 그리고, 650℃ 1시간이었다. 이때 박막의 증착율은 0.75[Å/sec]였다. X선 회절분석의 결과로부터 최적조건에서 증착된 BaTiO_3 박막은 강유전상을 나타내었으며 유전상수와 유전손실은 각각 683, 0.05였다. In this paper, BaTiO_3 thin film on Pt/SiO_2/Si(100) substrates were prepared by RF sputtering, whose structural, crystallographic properties were examined according to the deposition conditions and annealing temperatures. The optimum Ar/O_2 gas flow rate, sputtering pressure, RF power and annealing temperature were 4/1, 12[mTorr], 120[W] and 650[℃] for 1[hr], respectively. The growth rate of deposition film was about 0.75[A /sec]. From the results of X-ray diffraction pattern, BaTiO_3 thin film deposited at the optimum conditions was a ferroelectric phase. The dielectric constant and loss were about 683 and 0.05, respectively.

직류 마그네트론 스퍼터링 공정 중 타겟 오염에 따른 박막 및 계면 형성 특성

이진영,허민,이재옥,강우석 한국반도체디스플레이기술학회 2019 반도체디스플레이기술학회지 Vol.18 No.1

Reactive sputtering is widely used because of its high deposition rate and high step coverage. The deposition layer is often affected by target poisoning because the target conditions are changed, as well, by reactive gases during the initial stage of sputtering process. The reactive gas affects the deposition rate and process stability (target poisoning), and it also leads unintended oxide interlayer formation. Although the target poisoning mechanism has been well known, little attention has been paid on understanding the interlayer formation during the reactive sputtering. In this research, we studied the interlayer formation during the reactive sputtering. A DC magnetron sputtering process is carried out to deposit an aluminum oxide film on a silicon wafer. From the real-time process monitoring and material analysis, the target poisoning phenomena changes the reactive gas balance at the initial stage, and affects the interlayer formation during the reactive sputtering process.

안경렌즈코팅용 소형 sputter coating system 설계 및 제작에 관한 연구

박문찬,이종근,주경복,정부영,김응순,문희성 한국안광학회 2008 한국안광학회지 Vol.13 No.1

목적: 안경렌즈용 소형 suptter coating system을 설계하고 제작하고자 한다. 방법: sputter system의 target 설계에 있어서 Essential Macleod thinfilm design software를 이용해 AR 코팅과 mirror 코팅이 동시에 설계 가능한 Si target 을 결정하였으며. 그 후 sputtering 장비를 제작하였다. 결과: SiO2와 Si3N4의 5층 박막으로 구성되는 AR 코팅의 최 적조건은 [air|SiO2(81.3)|Si3N4(102)|SiO2(19.21)|Si3N4(15.95)| SiO2(102)|glass] 이였다. Mirror 코팅의 경우, blue color 코 팅의 최적조건은 [air|SiO2(56.61)|Si3N4(135.86)|SiO2(67.64)| Si3N4(55.4)|SiO2 (53.53)|Si3N4(51.28)|glass] 이고, green color 코 팅의 최적조건은 [air|SiO2(66.2)|Si3N4(22.76)|SiO2(56.58)| Si3N4(140.35) |SiO2(152.35)|Si3N4(70.16)|SiO2(121.87)|glass] 이였으며, gold color 코팅의 최적조건은 [air|SiO2(83.59)|Si3N4(144.86) |SiO2(11.82)|Si3N4(129.93)|SiO2(90.01)|Si3N4 (88.37)|glass] 이였다. 결론: 코팅 시간을 줄여 안경단가를 줄이기 위하여 안경렌즈 코팅 시 렌즈의 전·후면을 동시 에 코팅을 해야 하기 때문에 sputtering장비 설계를 할 때 안경렌즈 전면과 후면에 동일하게 Si target을 갖춘 cathode 를 사용하였고, 렌즈의 곡률을 고려하여 각 층이 동일하게 코팅이 되어야 하기 때문에 target-substrate 간의 간격은 12.5cm에서 20cm로 가변할 수 있도록 설계하고 제작하였다. 고품질의 안경렌즈 코팅을 위하여 고진공 펌프로 turbo pump를 이용하였으며, 코팅박막의 균일함을 얻기 위해서 치구를 회전할 수 있도록 설계하고 제작하였다. Purpose: To design and fabricate the small sputter coating system for the Ophthalmic lens. Methods: The design of sputter target was done using macleod program for AR coating and mirror coating of Ophthalmic lens with Si target and then the sputter system was fabricated. Results: The optimum condition of AR coating with Si target was [air|SiO2(81.3)|Si3N4 (102)|SiO2(19.21)|Si3N4(15.95)|SiO2(102)|glass], for blue color mirror coating [air|SiO2(56.61)|Si3N4(135.86)|SiO2(67.64)|Si3N4(55.4)|SiO2(53.53)|Si3N4(51.28)|glass], for green color coating [air|SiO2(66.2)|Si3N4(22.76)|SiO2(56.58)|Si3N4(140.35)|SiO2(152.35)|Si3N4(70.16)|SiO2(121.87)|glass], for gold color [air|SiO2(83.59)|Si3N4(144.86)|SiO2(11.82)|Si3N4(129.93)|SiO2(90.01)|Si3N4(88.37)|glass]. Conclusions: In the fabrication of sputtering coating apparatus, Dual cathode with same Ti target were coated at the same time on both sides of Ophthalmic lens to lessen the time of coating on Ophthalmic Lens and save the cost of the lens. The distance of target-substrate of cathode was variable from 12.5cm to 20 cm. Turbo pump was used to take the whole coating process about 15 min. instead of diffusion pump. The lens holder was made to coat 2 pairs lens every coating and was rotated to get the uniformity of thin film.

RF-DC magnetron co-sputtering법에 의한 p-ZnO 박막의 성장

강승민,Kang Seung Min 한국결정성장학회 2004 한국결정성장학회지 Vol.14 No.6

p형 ZnO 에피 박막을 사파이어 기판의 (0001)면 상에 RF-DC magnet co-sputtering 법으로 성장시켰다. 약 120nm두께의 단결정상 박막을 성공적으로 얻어내었다. p형 ZnO를 만들기 위해서 Al 금속 타켓을 이용하여 DC 스퍼터링으로 $400^{\circ}C$와 $600^{\circ}C$에서 ZnO를 rf magnetron sputtering으로 증착하고, 동시에 Al의 doping을 행하였으며, 성장된 박막의 결정성과 광특성에 대하여 고찰하였다. p-ZnO films have been grown on (0001) sapphire substrates by RF-DC magnetron co-sputtering. The p-ZnO single crystalline thin films of the thickness about 120 nm were grown successfully. The dopant (Aluminum) was sputtered simultaneously from Al metal target by DC sputtering during rf-magnetron sputtering of ZnO at the substrate temperatures of $400^{\circ}C$ and $600^{\circ}C$ respectively. The crystallinity and optical properties of as-grown P-ZnO films have been characterized.