• Title/Summary/Keyword: x-ray diffraction(XRD)

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Development and Characterization of Horse Bone-derived Natural Calcium Phosphate Powders

  • Jang, Kyoung-Je;Cho, Woo Jae;Seonwoo, Hoon;Kim, Jangho;Lim, Ki Taek;Chung, Pill-Hoon;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.2
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    • pp.122-133
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    • 2014
  • Purpose: This study was to develop an effective process for fabricating biocompatible calcium phosphate powders (CPPs) using horse bones, and to investigate the characteristics of them. Methods: The characteristics of horse bone powders (HBPs) were investigated according to the different osseous tissue types (compact bone and cancellous bone), bone types (spine and tibia), pretreatment methods (cold water, $H_2O_2$, and hot water), sintering time (4, 8 and 12h), and sintering temperature (600, 900, 1100 and $1300^{\circ}C$). In addition, the grinding methods were compared based on the wet grinding (ball mill) and dry grinding (blade grinder) method to make it as powders. Finally, their cytotoxicity and cell viability were checked. Results: Regardless of the types of osseous tissues and bones, HBPs were well fabricated as biocompatible CPPs. It was also found that the pretreatment methods did not influence on the resultants, showing well-fabricated HBPs. Considering the processing time, the hot water method was the most suitable compared to other pretreatment methods. Further, 12h-sintering time was sufficient to remove residual organic compounds. The sintering temperatures greatly affected the properties of bone powders fabricated. The x-ray diffraction (XRD) peak of horse bone sintered at $600^{\circ}C$ was most closed to that of hydroxyapatite (HA). Our bioactivity study demonstrated that the HBPs fabricated by sintering horse bones at $1300^{\circ}C$ showed the best performance in terms of cell viability whereas the HBPs $1100^{\circ}C$ showed the cytotoxicity. Conclusions: Using various types of horse bone tissues, biocompatible CPPs were successfully developed. We conclude that the HBPs may have a great potential as biomaterials for various biological applications including bone tissue engineering.

Effects of Annealing on Ni/Au Ohmic Contact to Nonpolar p-type GaN

  • Lee, Dong-Min;Kim, Jae-Gwan;Yang, Su-Hwan;Kim, Jun-Yeong;Lee, Seong-Nam;Lee, Ji-Myeon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.358-359
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    • 2012
  • 최근 분극 특성이 상이한 무분극 GaN 에피성장에 관한 심도 있는 연구와 함께 전자-전공 캐리어의 주입 및 캐리어의 거동, 방출되는 편광 특성 및 다양한 물리적 특성들에 대해 보고되고 있으며, 광학적 특성 및 물리적 특성의 확보를 위한 많은 연구가 활발히 진행 중이다 [1]. GaN의 ohmic 접촉(ohmic contact)의 형성은 발광 다이오드(light emitting diode), 레이저 다이오드(Laser), 태양전지(solar cell)와 같은 고신뢰도, 고효율 광전자 소자를 제조하기 위해서는 매우 중요하다 [2]. 그러나 이와 함께 병행 되어야 할 무분극 p-GaN 의 ohmic contact에 관한 연구는 많이 이루어지고 있지 않는 실정이다. 따라서 본 논문에서는 r-plane 사파이어 기판 상에 성장된 p-GaN에서의 ohmic 접촉 형성 연구를 위하여 Ni/Au ohmic 전극의 접촉저항 특성을 연구하였다. 본 실험에서는 성장된 a-plane GaN의 Hole농도가 $3.09{\times}1017cm3$ 인 시편을 사용하였다. E-beam evaporation 장비를 이용하여 Ni/Au를 각각 20 nm 그리고80 nm 증착 하였으며 비접촉저항을 측정하기 위해 Circle-Transfer Length Method (C-TLM) 패턴을 사용하였다. 샘플은 RTA (Rapid Thermal Annealing)를 사용하여 $300^{\circ}C$에서 $700^{\circ}C$까지 온도를 변화시키며 전기적 특성을 비교하여 그림 1(a) 나타내었다. 그림에서 알 수 있듯이 $400^{\circ}C$에서 가장 낮은 비접촉저항 값인 $6.95{\times}10-3{\Omega}cm2$를 얻을 수 있음을 발견하였다. 이 때의 I-V curve 도 그림1(b)에 나타낸 바와 같이 열처리에 의해 크게 향상됨을 알 수 있다. 그러나, $500^{\circ}C$ 이상 온도를 증가시키면 다시 비접촉 저항이 증가하는 것을 관찰하였다. XRD (x-Ray Diffraction) 분석을 통하여 $400^{\circ}C$ 이상열처리 온도가 증가하면 금속 표면에 $NiO_2$가 형성되며, 이에 따라 오믹특성이 저하 된다고 사료된다. 또한 $Ni_3N$의 존재를 확인 하였으며 이는 nonpolar surface의 특성으로 인해 nitrogen out diffusion 현상이 동시에 발생하여 계면에는 dopant로 작용하는 질소 공공을 남기고 표면에 $Ni_3N$을 형성하여 ohmic contact의 특성이 저하되기 때문인 것으로 사료된다.

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Copper Film Growth by Chemical Vapor Deposition: Influence of the Seeding Layer (ICB seeding에 의한 CVD Cu 박막의 증착 및 특성 분석)

  • Yoon, Kyoung-Ryul;Choi, Doo-Jin;Kim, Seok;Kim, Ki-Hwan;Koh, Seok-Keun
    • Korean Journal of Materials Research
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    • v.6 no.7
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    • pp.723-732
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    • 1996
  • Cu films were deposited by chemical wapor deposition on the as-received substrates (TiN/Si) and three kinds of Cu-seeded substrates (Cu/TiN/Si) which had seeding layer in the thick ness of 5 ${\AA}$ and 130 ${\AA}$ coated by ICB(Ionized Cluster Beam) method. The effect of Cu seeding layers on the growth rate, crystallinity, grain size uniformity and film adhesion strength of final CVD-Cu films was investigated by scanning eletron microscopy(SEM), X-ray diffractometry and scratch test. The growth rate was found to incresase somewhat in the case of ICB-seeding. The XRD patterns of the Cu films on the as-received substrate and ICB Cu-seeded substrates exhibited the diffraction peaks corresponding to FCC phase, but the peak intensity ratio($I_{111}/I_{200}$) of Cu films deposited on the ICB Cu-seeded substrates increased compared with that of Cu films on the as-received substrate. The resistivity of final Cu film on 40 ${\AA}$ seeded substrate was observed as the lowest value, 2.42 $\mu\Omega\cdot$cm compared with other Cu films. In adhesion test, as the seeding thickness increased from zero to 130 ${\AA}$, the adhesion strength increased from 21N to 27N.

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Fabrication and Mechanical Property of Fe-20Cu-1C Compacts by SPS process with Different Heating Rate (방전플라즈마소결법 적용 승온속도 변화에 따라 제조된 Fe-20Cu-1C 소결체 제조 및 특성평가)

  • Ryu, Jung-Han;Shin, Soo-Sik;Ryu, Byung-Rok;Kim, Kyung-Sik;Jang, Jun-Ho;Oh, Ik-Hyun;Kim, Kap-Tae;Park, Hyun-Kuk
    • Journal of Powder Materials
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    • v.24 no.4
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    • pp.302-307
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    • 2017
  • In this study, Fe-Cu-C alloy is sintered by spark plasma sintering (SPS). The sintering conditions are 60 MPa pressure with heating rates of 30, 60 and $9^{\circ}C/min$ to determine the influence of heating rate on the mechanical and microstructure properties of the sintered alloys. The microstructure and mechanical properties of the sintered Fe-Cu-C alloy is investigated by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The temperature of shrinkage displacement is changed at $450^{\circ}C$ with heating rates 30, 60, and $90^{\circ}C/min$. The temperature of the shrinkage displacement is finished at $650^{\circ}C$ when heating rate $30^{\circ}C/min$, at $700^{\circ}C$ when heating rate $60^{\circ}C/min$ and at $800^{\circ}C$ when heating rate $90^{\circ}C/min$. For the sintered alloy at heating rates of 30, 60, and $90^{\circ}C/min$, the apparent porosity is calculated to be 3.7%, 5.2%, and 7.7%, respectively. The hardness of the sintered alloys is investigated using Rockwell hardness measurements. The objective of this study is to investigate the densification behavior, porosity, and mechanical properties of the sintered Fe-Cu-C alloys depending on the heating rate.

Effect of Electropolishing on Surface Quality of Stamped Leadframe (Stamped Leadframe의 표면 품질에 미치는 전해연마 효과)

  • 남형곤;박진구
    • Journal of the Microelectronics and Packaging Society
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    • v.7 no.3
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    • pp.45-54
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    • 2000
  • The effect of electropolishing far stamped leadframe on the removal of the edge burr and residual stress relief was examined. The present study showed that the electropolishing could be used for enhanced surface quality of stamped leadframes. The electropolishing was performed at the condition of 60% phosphoric acid electrolyte, 5 ampere of current and 3 cm electrode gap at $70^{\circ}C$ for 2 minutes for Alloy42 type leadframe, and $50^{\circ}C$ for 1.5 minutes for C-194 type leadframe. The FWHM values from X-ray diffraction showed that residual stress of electropolished leadframe recovered to the level of as-received raw materials and surface roughness measured by using AFM tuned out to be improved by 0.079 $\mu\textrm{m}$ and 0.014 $\mu\textrm{m}$ ($R_{rms}$) far alloy 42 and C-194 type leadframes, respectively. The plated thickness using XRF showed the improved uniformity in thickness variation by 0.4~0.5 $\mu\textrm{m}$ and grain growth, which is favorable for interface adhesion, was also observed from the bake test samples. We could certify dimensional stability of leadframe with inspection by means of 3D-topography and hardness measurements.

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Effect of Solubilizing and Microemulsifying Excipients in Polyethylene Glycol 6000 Solid Dispersion on Enhanced Dissolution and Bioavailability of Ketoconazole

  • Heo, Min-Young;Piao, Zong-Zhu;Kim, Tae-Wan;Cao, Qing-Ri;Kim, Ae-Ra;Lee, Beom-Jin
    • Archives of Pharmacal Research
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    • v.28 no.5
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    • pp.604-611
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    • 2005
  • Polyethylene glycol (PEG) 6000-based solid dispersions (SDs), by incorporating various pharmaceutical excipients or microemulsion systems, were prepared using a fusion method, t o compare the dissolution rates and bioavailabilities in rats. The amorphous structure of the drug in SDs was also characterized by powder X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). The ketoconazole (KT), as an antifungal agent, was selected as a model drug. The dissolution rate of KT increased when solubilizing excipients were incorporated into the PEG-based SDs. When hydrophilic and lipophilic excipients were combined and incorporated into PEG-based SDs, a remarkable enhancement of the dissolution rate was observed. The PEG-based SDs, incorporating a self microemulsifying drug delivery system (SMEDDS) or microemulsion (ME), were also useful at improving the dissolution rate by forming a microemulsion or dispersible particles within the aqueous medium. However, due to the limited solubilization capacity, these PEG-based SDs showed dissolution rates, below 50% in this study, under sink conditions. The PEG-based SD, with no pharmaceutical excipients incorporated, increased the maximum plasma concentration (C$_{max}$) and area under the plasma concentration curve (AUC$_{0-6h}$) two-fold compared to the drug only. The bioavailability was more pronounced in the cases of solubilizing and microemulsifying PEG-based SDs. The thermograms of the PEG-based SDs showed the characteristic peak of the carrier matrix around 60$^{\circ}C$, without a drug peak, indicating that the drug had changed into an amorphous structure. The diffraction pattern of the pure drug showed the drug to be highly crystalline in nature, as indicated by numerous distinctive peaks. The lack of the numerous distinctive peaks of the drug in the PEG-based SDs demonstrated that a high concentration of the drug molecules was dissolved in the solid-state carrier matrix of the amorphous structure. The utilization of oils, fatty acid and surfactant, or their mixtures, in PEG-based SD could be a useful tool to enhance the dissolution and bioavailability of poorly water-soluble drugs by forming solubilizing and microemulsifying systems when exposed to gastrointestinal fluid.

Preparation of AgCl/Ag3PO4/Diatomite Composite by Microemulsion Method for Rapid Photo-Degradation of Rhodamine B with Stability under Visible Light

  • Zhu, Hai-Tao;Ren, Qi-Fang;Jin, Zhen;Ding, Yi;Liu, Xin-Yu;Ni, Xi-Hui;Han, Meng-Li;Ma, Shi-Yu;Ye, Qing;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.30 no.8
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    • pp.383-392
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    • 2020
  • In this paper, AgCl/Ag3PO4/diatomite photocatalyst is successfully synthesized by microemulsion method and anion in situ substitution method. X-ray diffraction (XRD), photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) are used to study the structural and physicochemical characteristics of the AgCl/Ag3PO4/diatomite composite. Using rhodamine B (RhB) as a simulated pollutant, the photocatalytic activity and stability of the AgCl/Ag3PO4/diatomite composite under visible light are evaluated. In the AgCl/Ag3PO4/diatomite visible light system, RhB is nearly 100 % degraded within 15 minutes. And, after five cycles of operation, the photocatalytic activity of AgCl/Ag3PO4/diatomite remains at 95 % of the original level, much higher than that of pure Ag3PO4 (40 %). In addition, the mechanism of enhanced catalytic performance is discussed. The high photocatalytic performance of AgCl/Ag3PO4/diatomite composites can be attributed to the synergistic effect of Ag3PO4, diatomite and AgCl nanoparticles. Free radical trapping experiments are used to show that holes and oxygen are the main active species. This material can quickly react with dye molecules adsorbed on the surface of diatomite to degrade RhB dye to CO2 and H2O. Even more remarkably, AgCl/Ag3PO4/diatomite can maintain above 95 % photo-degradation activity after five cycles.

Preparation and Release Behavior of Atorvastatin Calcuim - Encapsulated Polyoxalate Microspheres (아토르바스타틴 칼슘을 함유한 폴리옥살레이트 미립구의 제조 및 방출거동)

  • Lee, Cheon Jung;Kim, Su Young;Lee, Hyun Gu;Yang, Jaewon;Park, Jin Young;Cha, Se Rom;Lim, Dong-Kwon;Lee, Dongwon;Khang, Gilson
    • Polymer(Korea)
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    • v.38 no.5
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    • pp.656-663
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    • 2014
  • Atorvastatin calcium-loaded polyoxalate (POX) microspheres were prepared by an emulsion solvent-evaporation/ extraction method of oil-in-oil-in-water ($O_1/O_2/W$) for sustained release. We investigated the release behavior according to initial drug ratio, molecular weight ($M_w$) and concentration of POX and concentration of emulsifier. The microsphere was characterized on the surface, the cross-section morphology and the behavior of atorvastatin calcium release for 10 days by scanning electron microscopy (SEM) and high performance liquid chromatography (HPLC). The analysis of crystallization was analyzed to use X-ray diffraction (XRD), differential scanning calorimeter (DSC) and Fourier transform infrared (FTIR). These results showed that the release behaviors can be controlled by preparation conditions.

Material Characteristics of Forge Welded Bar and By-product through Reproduction Experiment to the Refining and Forge Welding Process (정련·단접 공정 재현 실험을 통해 생산된 소재 및 부산물의 재료학적 특성)

  • Oh, Min Jee;Cho, Hyun Kyung;Cho, Nam Chul;Han, Jung Uk
    • Journal of Conservation Science
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    • v.34 no.2
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    • pp.87-96
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    • 2018
  • This study analyzed the influence of folding time on the forge welded bar and hammer scale produced using the traditional refining and forge welding reproduction experiment. In the case of the forge welded bar, increasing the forging time decreased the percentage of impurities and porosity from 26.09% to 1.8%. Additionally, the hardness increased by an average of 36.88 HV. In other words, the microstructure gradually became more precise. For the hammer scale, the amount of T Fe increased with forging time. X-ray diffraction analysis revealed the presence of quartz, fayalite, $w{\ddot{u}stite$, and magnetite. The amount of quartz decreased as the forging time increased. In addition, as the forging time increased, the granular $w{\ddot{u}stite$ changed into a cohesive, long, white band. The results provide information on the characteristics of the forge welded bar and hammer scale produced in the refining and forging process. This information can be used as technical data for ancient steel making processes as well as for future technological systems.

Formation of Magnesium Films on Galvanized Steel Substrates by PVD Method at Nitrogen Gas Pressures and Their Corrosion Resistances (질소가스 중 PVD법에 의해 용융아연도금 강판 상에 형성한 마그네슘 막의 내식특성)

  • Eom, Jin-Hwan;Park, Jae-Hyeok;Hwang, Seong-Hwa;Park, Jun-Mu;Yun, Yong-Seop;Lee, Myeong-Hun
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.182-182
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    • 2016
  • 철강은 기본적으로 강도가 우수하고 그 매장량이 풍부할 뿐만 아니라 대량생산이 가능하다 또한 다른 금속과 합금을 구성하여 또 다른 특성을 부여할 수 있기 때문에 현재 전 세계 금속 생산량의 95%를 차지할 정도로 많이 사용되며, 각종 산업과 기술이 발달함에 따라 그 중요도는 점점 더 커져가고 있다. 하지만 철강은 사용 환경 중 부식에 의해 그 수명과 성능이 급격히 저하되기 때문에 내식성을 향상시키기 위하여 도장이나 도금 등의 표면처리를 포함한 다양한 방법이 적용되고 있다. 그 중 철강재의 도금 표면처리방법은 주로 아연을 이용한 용융도금이나 전기도금 등과 같은 습식 프로세스가 널리 사용되고 있다. 여기서 아연은 철보다 이온화 경향은 크나 대기 환경 중 산소와 물과 반응하여 Zn(OH)2와 같은 화합물을 형성함으로써 철강재 표면상 부식인자를 차단(Barrier)함은 물론 사용 중 철 모재가 노출되는 결함이 발생하는 경우에는 철을 대신하여 희생양극(Sacrificial Anode) 역할을 하기 때문에 철의 부식방식용 금속으로 가장 많이 사용되고 있다. 한편 최근에는 철강의 사용 환경이 다양해짐은 물론 가혹해지고 있어서 이에 따른 내식성 향상이 계속해서 요구되고 있는 추세이다. 따라서 본 연구에서는 철강재의 내식성을 향상시키기 위한 일환으로 현재 많이 사용되고 있는 용융아연도금 강판 상에 아연보다 활성이 높은 마그네슘(Mg)을 건식 프로세스 방법 중에 하나인 PVD(Physical Vapour Deposition)법에 의해 코팅하는 것을 시도하였다. 일반적으로 PVD법에 의해 진공증착하는 경우에는 그 도입가스로써 불활성가스인 아르곤(Ar)을 사용하는 경우가 대부분이나 여기서는 상대적으로 비활성이면서 그 크기가 작은 질소(N2)가스를 도입하여 그 증착 막의 몰포로지는 물론 결정구조도 제어하여 그 내식특성을 향상시키고자 하였다. 본 연구에서는 철강재의 내식성을 향상시키기 위한 방법으로 마그네슘(Mg)를 PVD(Physical Vapor Deposition)법 중 진공증착법(Vacuum Deposition)을 사용하여 용융아연도금 강판 상에 마그네슘 증착 막을 형성하였다. 즉, 여기서는 진공증착 중 질소(Nitrogen, N2)가스를 도입하여 진공챔버(Vacuum Chamber)내의 진공도를 $1{\times}10^{-1}$, $1{\times}10^{-2}$, $1{\times}10^{-3}$, $1{\times}10^{-4}$로 조절하며 제작하였다. 또한 제작된 시편에 대해서는 SEM(Scanning Electron Microscope) 및 XRD(X-Ray Diffraction)을 사용하여 형성된 아연도금상 마그네슘 막의 표면 몰포로지 및 결정구조의 변화를 분석함은 물론 침지시험, 염수분무시험, 분극시험을 통해 이 막들에 대한 내식특성을 분석 평가하였다. 상기 실험결과에 의하면, 진공 가스압이 증가됨에 따라 마그네슘 막의 두께는 감소하였으며, 그 몰포로지의 단면은 주상정(Columnar)에서 입상정(Granular) 구조로 변화하며 표면의 결정립은 점점 미세화 되는 경향을 나타냈다. 이때의 표면의 결정배향성(Crystal orientation)은 표면에너지가 상대적으로 큰 면이 우세하게 나타나는 경향이 있었다. 또한 본 실험에서 형성한 진공증착 막은 비교재인 용융아연도금강판보다 우수한 내식성을 나타냈고, 본 형성 막 중에는 마그네슘 막 두께가 작음에도 불구하고 질소 가스압이 가장 큰 조건일수록 내식성이 우수한 경향을 나타냈다. 이상의 결과는 철강재의 내식성 향상을 위한 응용표면처리설계에 기초적인 지침을 제공할 수 있을 것으로 기대된다.

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