• Title/Summary/Keyword: XPS (X-ray Photoelectron Spectroscopy)

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Effect of Alkali and Heat Treatments of Ti-6Al-4V Alloy on the Precipitation of Calcium Phosphate (Ti-6Al-4V 합금의 알칼리 및 열처리가 인산칼슘 침착에 미치는 영향)

  • Park, Jae-Han;Lim, Ki-Jung;Kim, Sang-Mok;Kim, Byung-Ock;Han, Kyung-Yoon
    • Journal of Periodontal and Implant Science
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    • v.30 no.1
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    • pp.187-203
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    • 2000
  • The precipitation of calcium phosphate on implant surface has been known to accelerate osseointegration and to enhance osseous adaptation. The present study was performed to examine whether the precipitation of calcium phosphate on Ti-6Al-4V alloy could be affected by the immersion in NaOH solution and heat treatment. Ti-6Al-4V alloy plates of $15{\times}3.5{\times}1mm$ in dimension were polished sequentially from #240 to #2,000 emery paper and one surface of each specimen was additionally polished with $0.1{\mu}m$ alumina paste. Polished specimens were soaked in various concentrations of NaOH solution(0.1, 1.0, 3.0, 5.0, 7.0, 10.0 M) at $60^{\circ}C$ for 24 hours for alkali treatment, and 5.0 M NaOH treated specimens were heated for 1 hour at each temperature of 400, 500, 600, 700, $800^{\circ}C$. After the alkali and heat treatments, specimens were soaked in the Hank's solution with pH 7.4 at $36.5^{\circ}C$ for 30days.The surface ingredient change of Ti-6Al-4V alloy was evaluated by thin-film X-ray diffractometer(TF-XRD) and the surface microstructure was observed by scanning electron microscope(SEM), and the elements of surface were analyzed by X-ray photoelectron spectroscopy(XPS). The results were obtained as follows ; 1. The precipitation of calcium phosphate on Ti-6Al-4V alloy was accelerated by the immersion in NaOH solution and heat treatment. 2. In Alkali treatment for the precipitation of calcium phosphate on Ti-6Al-4V alloy, the optimal concentration of NaOH solution was 5.0 M. 3. In heat treatment after alkali treatment in 5.0 M NaOH solution, the crystal formation on alloy surface was enhanced by increasing temperature. In heat treated alloys at $600^{\circ}C$, latticed structure and prominences of calcium phosphate layer were most dense. On heat treated alloy surface at the higher temperature(${\geq}700^{\circ}C$), main crystal form was titanium oxide rather than apatite. The above results suggested that the precipitation of calcium phosphate on the surface of Ti-6Al-4V alloy could be induced by alkali treatment in 5.0 M-NaOH solution and by heat treatment at $600^{\circ}C$.

Facile Synthesis of In2S3 Modified Ag3PO4 Nanocomposites with Improved Photoelectrochemical Properties and Stabilities

  • Zeng, Yi-Kai;Bo, Shenyu;Wang, Jun-hui;Cui, Bin;Gu, Hao;Zhu, Lei;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.30 no.11
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    • pp.601-608
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    • 2020
  • In this work, Ag3PO4/In2S3 nanocomposites with low loading of In2S3 (5-15 wt %) are fabricated by two step chemical precipitation approach. The microstructure, composition and improved photoelectrochemical properties of the as-prepared composites are studied by X-ray diffraction pattern (XRD), field emission scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), photocurrent density, EIS and amperometric i-t curve analysis. It is found that most of In2S3 nanoparticles are deposited on the surfaces of Ag3PO4. The as-prepared Ag3PO4/In2S3 composite (10 wt%) is selected and investigated by SEM and TEM, which exhibits special morphology consisting of lager size substrate (Ag3PO4), particles and some nanosheets (In2S3). The introduction of In2S3 is effective at improving the charge separation and transfer efficiency of Ag3PO4/In2S3, resulting in an enhancement of photoelectric behavior. The origin of the enhanced photoelectrochemical activity of the In2S3-modified Ag3PO4 may be due to the improved charge separation, photocurrent stability and oriented electrons transport pathways in environment and energy applications.

대면적 플라즈마 공정에서 자장이 내장형 선형 유도결합형 플라즈마 특성에 미치는 영향에 관한 연구

  • 경세진;이영준;김경남;염근영
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2003.05a
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    • pp.55-55
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    • 2003
  • 최근 높은 해상도의 평판 디스플레이 장치 특히 차세대 TFT-LCD를 개발하기 위해서는 건식식각공정의 개발이 필수 불가결하며 이는 플라즈마 공정장치의 대면적화가 가능해야 한다. 따라서 산업계는 이러한 제조 조건에 알맞는 대면적 플라즈마 반응기 개발을 추구하고 있다. 이를 위해서는 건식식각공정의 개발이 필수 불가결하며 이를 위해선 플라즈마 공정장 치의 대면적화가 가능해야 한다. 이러한 대면적 공정을 위해서는 낮은 공정압력, 고밀도, 높은 플라즈마 균일도가 요구된다. 또한 이러한 대면적 고밀도 플라즈마에의 적용을 위하여 새로운 유도결합형 플라즈마 소오스의 개발이 진행되고 있으며, 안정적인 300mm웨이퍼 공정을 위하여 여러 형태의 안테나가 연구되어지고 있다. 그러나 차세대 TFT-LCD에 적용 가 능하게끔 기존의 ICP 소오스를 직접적으로 대면적화 하는데 있어서는 안테나의 인덕턴스의 값이 키지며, 유전물질의 두께 증가 및 그에 따른 재료비의 상슴에 의해 그 한계점을 나타 내었다. 본 연구에서는 차세대 TFT-LCD 및 POP 대면적 공정에 적용 가능한 고밀도 플라즈마를 발생시키기 위해서 내장형 유도결합형 선형 안테나를 사용하였다. 내장형 유도결합형 선형 안테나가 가지고 있는 고유의 정전기적 결합효과를 최소화시키기 위해 직사각형모양의 플라즈마 챔버(830mm*1,020mm)에서 영구자석을 사용하였다. 영구자석을 사용하여 외부자 장을 인가하였을 때가, 그럴지 않은 때보다 RF 안테나에 걸리는 코일의 전압을 낮춰주었으며, 영구자석의 배열에 따라 코일의 인덕턴스의 값이 크게 변함을 알 수 있었다. 그리고, 최적화된 자장의 배열은 플라즈마의 이온밀도를 증가시켰으며, 플라즈마 균일도 또한 10% 이 내로 유지됨을 알 수 있었다. 따른 식각 메커니즘에 대하여 알아보고자 하였다. $CF_4/Cl_2$ gas chemistry 에 첨 가 가스로 $N_2$와 Ar을 첨 가할 경 우 텅 스텐 박막과 하부 layer 간의 etch selectivity 증가는 관찰되지 않았으며, 반면에 첨가 가스로 $O_2$를 사용할 경우, $O_2$의 첨가량이 증가함에 따라 etch s selectivity 는 계속적으로 증가렴을 관찰할 수 있었다. 이는 $O_2$ 첨가에 따라 형성되는 WOF4 에 의한 텅스텐의 etch rates 의 감소에 비하여, $Si0_2$ 등의 형성에 의한 poly-Si etch rates 이 더욱 크게 감소하였기 때문으로 사료된다. W 과 poly-Si 의 식각 특성을 이해하기 위하여 X -ray photoelectron spectroscopy (XPS)를 사용하였으며, 식각 전후의 etch depth 를 측정하기 위하여 stylus p pmfilometeT 를 이용하였다.X> 피막이 열처리 전후에 보아는 기계적 특성의 변화 양상은 열역학적으로 안정한 Wurzite-AlN의 석출에 따른 것으로 AlN 석출상의 크기에 의존하며, 또한 이러한 영향은 $(Ti_{1-x}AI_{x})N$ 피막에 존재하는 AI의 함량이 높고, 초기에 증착된 막의 업자 크기가 작을 수록 클 것으로 여겨진다. 그리고 환경의 의미의 차이에 따라 경관의 미학적 평가가 달라진 것으로 나타났다.corner$적 의도에 의한 경관구성의 일면을 확인할수 있지만 엄밀히 생각하여 보면 이러한 예의 경우도 최락의 총체적인 외형은 마찬가지로

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Study on the Melting Point Depression of Tin Nanoparticles Manufactured by Modified Evaporation Method (수정된 증발법을 이용하여 제작된 주석 나노입자의 녹는점 강하에 관한 연구)

  • Kim, Hyun Jin;Beak, Il Kwon;Kim, Kyu Han;Jang, Seok Pil
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.38 no.8
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    • pp.695-700
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    • 2014
  • In the present study, the melting temperature depression of Sn nanoparticles manufactured using the modified evaporation method was investigated. For this purpose, a modified evaporation method with mass productivity was developed. Using the manufacturing process, Sn nanoparticles of 10 nm size was manufactured in benzyl alcohol solution to prevent oxidation. To examine the morphology and size distribution of the nanonoparticles, a transmission electron microscope was used. The melting temperature of the Sn nanoparticles was measured using a Differential scanning calorimetry (DSC) which can calculate the endothermic energy during the phase changing process and an X-ray photoelectron spectroscopy (XPS) used for observing the manufactured Sn nanoparticle compound. The melting temperature of the Sn nanoparticles was observed to be $129^{\circ}C$, which is $44^{\circ}C$ lower than that of the bulk material. Finally, the melting temperature was compared with the Gibbs Thomson and Lai's equations, which can predict the melting temperature according to the particle size. Based on the experimental results, the melting temperature of the Sn nanoparticles was found to match well with those recommended by the Lai's equation.

A Study on the Electromigration Characteristics in Ag, Cu, Au, Al Thin Films (Ag, Cu, Au, Al 박막에서 엘렉트로마이그레이션 특성에 관한 연구)

  • Kim, Jin-Young
    • Journal of the Korean Vacuum Society
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    • v.15 no.1
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    • pp.89-96
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    • 2006
  • Recent ULSI and multilevel structure trends in microelectronic devices minimize the line width down to less than $0.25{\mu}m$, which results in high current densities in thin film interconnections. Under high current densities, an EM(electromigration) induced failure becomes one of the critical problems in a microelectronic device. This study is to improve thin film interconnection materials by investigating the EM characteristics in Ag, Cu, Au, and Al thin films, etc. EM resistance characteristics of Ag, Cu, Au, and Al thin films with high electrical conductivities were investigated by measuring the activation energies from the TTF (Time-to-Failure) analysis. Optical microscope and XPS (X-ray photoelectron spectroscopy) analysis were used for the failure analysis in thin films. Cu thin films showed relatively high activation energy for the electromigration. Thus Cu thin films may be potentially good candidate for the next choice of advanced thin film interconnection materials where high current density and good EM resitance are required. Passivated Al thin films showed the increased MTF(Mean-time-to-Failure) values, that is, the increased EM resistance characteristics due to the dielectric passivation effects at the interface between the dielectric overlayer and the thin film interconnection materials.

Hydrogeneted Amorphous Carbon Nitride Films on Si(100) Deposited by DC Saddle Field Plasma Enhanced Chemical Vapor Deposition ($N_2/CH_4$가스비에 따른 Hydrogenated Amorphous Carbon Nitride 박막의 특성)

  • 장홍규;김근식;황보상우;이연승;황정남;유영조;김효근
    • Journal of the Korean Vacuum Society
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    • v.7 no.3
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    • pp.242-247
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    • 1998
  • Hydrogenated amorphous carbon nitride[a-C:H(N)] films were deposited on p-type Si(100) at room temperature with bias voltage of 200 V by DC saddle-field plasma-enhanced chemical vapor deposition. Effects of the ratio of $N_2$ to $CH_4$($N_2/CH_4$), in the range of 0 and 4 on such properties as optical properties, microstucture, relative fraction of nitrogen and carbon, etc. of the films have been investigated. The thickness of the a-C:H(N) film was abruptly decreased with the addition of nitrogen, but at $N_2/CH_4$>0.5, the thickness of the film gradually decreased with the increase of the $N_2/CH_4$. The ratio of N to C(N/C) of the films was saturated at 0.25 with the increase of $N_2CH_4$. N-H, C≡N bonds of the films increased but C-H bond decreased with the increase of $N_2CH_4$.Optical band gap energy of the film decreased from 2.53 eV at the ratio of $N_2CH_4$=4.

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Adhesion Properties between Polyimide Film and Copper by Ion Beam Treatment and Imidazole-Silane Compound (이온빔 및 이미다졸-실란 화합물에 의한 폴리이미드 필름과 구리의 접착 특성)

  • Kang, Hyung Dae;Kim, Hwa Jin;Lee, Jae Heung;Suh, Dong Hack;Hong, Young Taik
    • Journal of Adhesion and Interface
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    • v.8 no.1
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    • pp.15-27
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    • 2007
  • Polyimide (PI) surface modification was carried out by ion-beam treatment and silane-imidazole coupling agent to improve the adhesion between polyimide film and copper. Silane-imidazole coupling agent contains imidazole functional groups for the formation of a complex with copper metal through a coordination bonding and methoxy silane groups for the formation of siloxane polymers. The PI film surface was first treated by argon (Ar)/oxygen ($O_2$) ion-beam, followed by dipping it into a modified silane-imidazole coupling agent solution. The results of X-ray photoelectron spectroscopy (XPS) spectra revealed that the $Ar/O_2$ plasma treatment formed oxygen functional groups such as hydroxyl and carbonyl groups on the polyimide film surface and confirmed that the PI surface was modified by a coupling reaction with imidazole-silane coupling agent. Adhesion between copper and the treated PI film by ion-beam and coupling agent was superior to that with untreated PI film. In addition, adhesion of PI film treated by an $Ar/O_2$ plasma to copper was better than that of PI film treated by a coupling agent. The peeled-off layers from the copper-PI film joint were completely different in chemical composition each other. The layer of PI film side showed similar C1s, N1s, O1s spectra to the original Upilex-S and no Si and Cu atoms appeared. On the other hand the layer of copper side showed different C1s and N1s spectra from the original PI film and many Si and Cu atoms appeared. This indicates that the failure occurs at an interface between the imidazole-silane and PI film layers rather than within the PI layers.

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The Oxidation Study of Lead-Free Solder Alloys Using Electrochemical Reduction Analysis (전기화학적 환원 분석을 통한 무연 솔더 합금의 산화에 대한 연구)

  • Cho Sungil;Yu Jin;Kang Sung K.;Shih Da-Yuan
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.1 s.34
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    • pp.35-40
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    • 2005
  • The oxidation of pure Sn and Sn-0.7Cu, Sn-3.5Ag, Sn-lZn, and Sn-9Zn alloys at $150^{\circ}C$ was investigated. Both the chemical nature and the amount of oxides were characterized using electrochemical reduction analysis by measuring the electrolytic reduction potential and total transferred electrical charges. X-ray photoelectron spectroscopy (XPS) was also conducted to support the results of reduction analysis. The effect of Cu, Ag and Zn addition on surface oxidation of Sn alloys is reported. For Sn, Sn-0.7Cu and Sn-3.5Ag, SnO grew first and then the mixture of SnO and $SnO_2$ was found. $SnO_2$ grew predominantly for a long-time aging. For Zn containing Sn alloys, both ZnO and $SnO_2$ were formed. Zn promotes the formation of $SnO_2$. Sn oxide growth rate of Pb-free solder alloys was also discussed in terms of alloying elements.

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Microstructure and Electrical Properties of the Pt/Pb1.1Zr0.53Ti0.47O3/PbO/Si (MFIS) Using the PbO Buffer Layer (PbO 완충층을 이용한 Pt/Pb1.1Zr0.53Ti0.47O3/PbO/Si (MFIS)의 미세구조와 전기적 특성)

  • Park, Chul-Ho;Song, Kyoung-Hwan;Son, Young-Guk
    • Journal of the Korean Ceramic Society
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    • v.42 no.2 s.273
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    • pp.104-109
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    • 2005
  • To study the role of PbO as the buffer layer, Pt/PZT/PbO/Si with the MFIS structure was deposited on the p-type (100) Si substrate by the r.f. magnetron sputtering with $Pb_{1.1}Zr_{0.53}Ti_{0.47}O_3$ and PbO targets. When PbO buffer layer was inserted between the PZT thin film and the Si substrate, the crystallization of the PZT thin films was considerably improved and the processing temperature was lowered. From the result of an X-ray Photoelectron Spectroscopy (XPS) depth profile result, we could confirm that the substrate temperature for the layer of PbO affects the chemical states of the interface between the PbO buffer layer and the Si substrate, which results in the inter-diffusion of Pb. The MFIS with the PbO buffer layer show the improved electric properties including the high memory window and low leakage current density. In particular, the maximum value of the memory window is 2.0V under the applied voltage of 9V for the Pt/PZT(200 nm, $400^{\circ}C)/PbO(80 nm)/Si$ structures with the PbO buffer layer deposited at the substrate temperature of $300^{\circ}C$.

Surface Modification of Polymethylmethacrylate(PMMA) by Ion-assisted reaction (이온 보조 반응법(Ion-assisted-reaction)을 이용한 Polymethylmethacrylate (PMMA)의 표면개질)

  • Jung, Sun;Cho, Jun-Sik;Choi, Sung-Chang;Koh, Seok-Keun
    • Korean Journal of Materials Research
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    • v.9 no.5
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    • pp.446-451
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    • 1999
  • Surface of Polymethylmethacrylate (PMMA) was modified by ion assisted reaction in which ion beam of Ar or$ O_2$is irradiated on polymer in reaction gas environment. Ion beam energy was changed from 600 to 1000eV, and ion doses were varied from $5\times10^{14} ions/cm^2 to 1\times10^{17} ions/cm^2$. Contact angle and surface energy of modified PMMA were measured by contact angle micrometer using distilled water and formamide. In the case of $Ar^+$ ion irradiation only, the contact angle reduced from $68^{\circ} to $35^{\circ}$ and the surface energy was changed from 46 dyne/cm to 60 dyne/cm. The contact angle significantly decreased to $14^{\circ}$and the surface energy increased to 72 dyne/cm when the surface of PMMA was modified by oxygen ion irradiation in oxygen gas environment. Improvement of wettability results from the formation of new hydrophilic group which is identified as C-O chain by XPS analysis. Recovery of wettability in dry air and maintenance of it in water condition were explained in view of the formation of hydrophilic group.

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