• Title/Summary/Keyword: diffraction parameter

Search Result 191, Processing Time 0.031 seconds

Understanding the Mechanism of Indomethacin-Saccharin Co-crystal Formation Using In-line Monitoring System based on PVM and FBRM (PVM 및 FBRM 기반 인라인 모니터링을 통한 indomethacin-saccharin 공결정의 생성 메커니즘이해)

  • Kim, Paul;Cho, Min-Yong;Choi, Guang J.
    • Korean Chemical Engineering Research
    • /
    • v.55 no.2
    • /
    • pp.180-189
    • /
    • 2017
  • Pharmaceutical co-crystals primarily to improve the solubility as well as stability of insoluble drug are to be investigated more intensively for IMDs as US FDA has reclassified co-crystal as a special case of solvates in August this year. In this study, we proposed a mechanism of indomethacin-saccharin co-crystal formation and the creation of transient indomethacin meta-stable form using in-line monitoring tools with the addition rate of anti-solvent as a critical process parameter. Among various instruments, we combined PVM (particle vision measurement) and FBRM (focused beam reflectance measurement) for the in-line monitoring of anti-solvent co-crystallization process. The off-line characterization of resulting powders was carried out employing the PXRD (powder x-ray diffraction) and DSC (differential scanning calorimeter). It was observed that the pathway to the final IMC-SAC co-crystal was significantly dependent upon the anti-solvent addition rate. The process conditions to obtain high quality co-crystal powder effectively were established. Consequently, we concluded that in-line monitoring combing the PVM and FBRM should be useful for the in-line monitoring of pharmaceutical co-crystallization processes.

Mössbauer Study of Crystallographic and Magnetic Properties in Vanadium Ferrite(VxFe3-xO4) Thin Films (바나듐 페라이트 박막의 결정구조 및 자기적 성질에 관한 뫼스바우어 분광학적 연구)

  • Park, Jae-Yun;Kim, Kwang-Joo
    • Journal of the Korean Magnetics Society
    • /
    • v.18 no.1
    • /
    • pp.19-23
    • /
    • 2008
  • The mixed ferrite $V_xFe_{3-x}O_4$(x=0.0, 0.15, 0.5, 1.0) thin films were prepared by sol-gel method. Their crystallographic and magnetic hyperfine properties have been studied using X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS) and conversion electron $M\"{o}ssbauer$ spectroscopy(CEMS). The crystal structure is found to be cubic spinel throughout the series($x{\leq}1.0$), and the lattice parameter $a_0$ increases linearly with increasing V content. XRD, XSP and CEMS indicate that $V^{3+}$ substitution for $Fe^{3+}$ in B-site is superior to $V^{2+}$ substitution for $Fe^{2+}$ in B-site. It is noticeable that both quadrupole shift and hyperfine field decreases with increasing V composition, suggesting the change of local symmetry and accompanying line-broadening. The line-broadening on CEMS spectra can be explained by the distribution of magnetic hyperfine fields.

Synthesis and Characterization of a Series of PtRu/C Catalysts for the Electrooxidation of CO (일산화탄소 산화를 위한 PtRu/C 시리즈 촉매의 합성 및 특성 연구)

  • Lee, Seonhwa;Choi, Sung Mook;Kim, Won Bae
    • Clean Technology
    • /
    • v.18 no.4
    • /
    • pp.432-439
    • /
    • 2012
  • The electrocatalytic oxidation of CO was studied using carbon-supported 20 wt% PtRu (PtRu/C) catalysts, which were prepared with different Pt : Ru atomic ratios from 7 : 3 to 3 : 7 using a colloidal method combined with a freeze-drying procedure. The bimetallic PtRu/C catalysts were characterized by various physicochemical analyses, including X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). CO stripping voltammetry measurements indicated that the addition of Ru with a Pt catalyst significantly improved the electrocatalytic activity for CO electrooxidation. Among the tested catalysts, the $Pt_5Ru_5/C$ catalyst had the lowest onset potential (vs.Ag/AgCl) and the largest CO EAS. Structural modification via lattice parameter change and electronic modification in the unfilled d band states for Pt atoms may facilitate the electrooxidation of CO.

In Situ Monitoring of the MBE Growth of AlSb by Spectroscopic Ellipsometry

  • Kim, Jun-Yeong;Yun, Jae-Jin;Lee, Eun-Hye;Bae, Min-Hwan;Song, Jin-Dong;Kim, Yeong-Dong
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2013.02a
    • /
    • pp.342-343
    • /
    • 2013
  • AlSb is a promising material for optical devices, particularly for high-frequency and nonlinear-optical applications. And AlSb offers significant potential for devices such as quantum-well lasers, laser diodes, and heterojunction bipolar transistors. In this work we study molecular beam epitaxy (MBE) growth of an unstrained AISb film on a GaAs substrate and identify the real-time monitoring capabilities of in situ spectroscopic ellipsometry (SE). The samples were fabricated on semi-insulating (0 0 1) GaAs substrates using MBE system. A rotating sample stage ensured uniform film growth. The substrate was first heated to $620^{\circ}C$ under As2 to remove surface oxides. A GaAs buffer layer approximately 200 nm- thick was then grown at $580^{\circ}C$. During the temperature changing process from $580^{\circ}C$ to $530^{\circ}C$, As2 flux is maintained with the shutter for Ga being closed and the reflection high-energy electron diffraction (RHEED) pattern remaining at ($2{\times}4$). Upon reaching the preset temperature of $530^{\circ}C$, As shutter was promptly closed with Sb shutter open, resulting in the change of RHEED pattern from ($2{\times}4$) to ($1{\times}3$). This was followed by the growth of AlSb while using a rotating-compensator SE with a charge-coupled-device (CCD) detector to obtain real-time SE spectra from 0.74 to 6.48 eV. Fig. 1 shows the real time measured SE spectra of AlSb on GaAs in growth process. In the Fig. 1 (a), a change of ellipsometric parameter ${\Delta}$ is observed. The ${\Delta}$ is the parameter which contains thickness information of the sample, and it changes in a periodic from 0 to 180o with growth. The significant change of ${\Delta}$ at~0.4 min means that the growth of AlSb on GaAs has been started. Fig. 1b shows the changes of dielectric function with time over the range 0.74~6.48 eV. These changes mean phase transition from pseudodielectric function of GaAs to AlSb at~0.44 min. Fig. 2 shows the observed RHEED patterns in the growth process. The observed RHEED pattern of GaAs is ($2{\times}4$), and the pattern changes into ($1{\times}3$) with starting the growth of AlSb. This means that the RHEED pattern is in agreement with the result of SE measurements. These data show the importance and sensitivity of SE for real-time monitoring for materials growth by MBE. We performed the real-time monitoring of AlSb growth by using SE measurements, and it is good agreement with the results of RHEED pattern. This fact proves the importance and the sensitivity of SE technique for the real-time monitoring of film growth by using ellipsometry. We believe that these results will be useful in a number of contexts including more accurate optical properties for high speed device engineering.

  • PDF

A Study on the Numerical Simulation of the Seismic Sea Waves in the East Sea based on the Boussinesq Equation (Boussinesq 방정식을 이용한 동해지진해일 수치실험 연구)

  • Kim, Sung-Dae;Jung, Kyung-Tae;Park, Soo-Young
    • Ocean and Polar Research
    • /
    • v.29 no.1
    • /
    • pp.9-31
    • /
    • 2007
  • Most seismic sea waves in the East Sea originate from earthquakes occurring near the Japanese west coast. While the waves propagate in the East Sea, they are deformed by refraction, diffraction and scattering. Though the Boussinesq equation is most applicable for such wave phenomena, it was not used in numerical modelling of seismic sea waves in the East Sea. To examine characteristics of seismic sea waves in the East Sea, numerical models based on the Boussinesq equation are established and used to simulate recent tsunamis. By considering Ursell parameter and Kajiura parameter, it is proved that Boussinesq equation is a proper equation for seismic sea waves in the East Sea. Two models based on the Boussinesq equation and linear wave equation are executed with the same initial conditions and grid size ($1min{\times}1min$), and the results are compared in various respects. The Boussinesq equation model produced better results than the linear model in respect to wave propagation and concentration of wave energy. It is also certified that the Boussinesq equation model can be used for operational purpose if it is optimized. Another Boussinesq equation model whose grid size is $40sec{\times}30sec$ is set up to simulate the 1983 and 1993 tsunamis. As the result of simulation, new propagation charts of 2 seismic sea waves focused on the Korean east coast are proposed. Even though the 1983 and 1993 tsunamis started at different areas, the propagation paths near the Korean east coast are similar and they can be distinguished into 4 paths. Among these, total energy and propagating time of the waves passing over North Korea Plateau(NKP) and South Korea Plateau(SKP) determine wave height at the Korean east coast. In case of the 1993 tsunami, the wave passing over NKP has more energy than the wave over SKP. In case of the 1983 tsunami, the huge energy of the wave passing over SKP brought about great maximum wave heights at Mukho and Imwon. The Boussinesq equation model established in this study is more useful for simulation of seismic sea waves near the Korean east coast than it is the Japanese coast. To improve understanding of seismic sea waves in shallow water, a coastal area model based on the Boussinesq equation is also required.

Synthesis and Defect-Structure Analysis of $ThO_2-Tm_2O_3$ Solid Solutions ($ThO_2-Tm_2O_3$ 고용체의 합성 및 결함구조해석)

  • Don Kim;Chang Kwon Kang;Keu Hong Kim;Jae Shi Choi
    • Journal of the Korean Chemical Society
    • /
    • v.31 no.6
    • /
    • pp.491-497
    • /
    • 1987
  • $ThO_2-Tm_2O_3$ (TDT) solid solutions containing 1,3,5,8,10, and 15 mol% $Tm_2O_3$ were synthesized from spectroscopically pure $ThO_2$ and $Tm_2O_3$ polycrystalline powders. The TDT solid solutions were indentified to the fluorite structure by the X-ray powder technique. The values of the lattice parameter were decreased with increasing amount of $Tm_2O_3$ incorporated. But, there was no linearity for the samples containing 8, 10, and 15 mol% $Tm_2O_3$. It was concluded that these samples became incomplete solid solutions. From the intensity analyses of X-ray diffraction patterns, the residual factor was found below 0.13 even for the 15 mol% TDT system. lt was confirmed from the DTA and TGA analyses that any phase transitions did not occur under the experimental condition executed. Comparing the pycnometric density with the lattice parameter obtained from XRD, it was suggested that the predominant defect model be an oxygen vacancy.

  • PDF

Colossal Magnetoresistance and Mossbauer Studies of La-Ca-Mn-O Compound Doped with $^{57}Fe$ ($^{57}Fe$를 미량 치환한 La-Ca-Mn-O의 초거대자기저항과 Mossbauer분광학연구)

  • 박승일;김성철
    • Journal of the Korean Magnetics Society
    • /
    • v.8 no.6
    • /
    • pp.335-340
    • /
    • 1998
  • Colossal magnetoresistance $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ material has been produced by a metal-salt routed sol-gel process method. Magnetic properties of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been studied with x-ray diffraction, Rutherford back-scattering spectroscopy(RBS), vibrating sample magnetometer, and Mossbauer spectroscopy. Crystalline $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was perovskite cubic structure with a lattice parameter $a_0=3.868$\AA$$. And there was no appreciable change in the value of the lattice parameter when a small amount (x=0.01) of iron was added. However, Mossbauer and VSM data indicate the Curie temperature of the $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ decreased from 282 to 270 k and also the saturation magnetization from 84 to 81 emu/g at 77 K. Mossbauer spectra of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been taken at various temperatures ranging form 4.2 K to room temperature. Analysis of $^{57}Fe$ Mossbauer data in terms of the local configurations of Mn atoms has permitted the influence of the magnetic hyperfine interactions to be monitored. The isomer shifts show that the charge state of all Fe ions are ferric. The magnetoresistance of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was about 33 % at semiconductor-metal transition temperature $T_{SC-M}=250K$.

  • PDF

CIGS 박막태양전지용 Cd free형 ZnS(O, OH) 버퍼층 제조 및 특성평가

  • Kim, Hye-Jin;Kim, Jae-Ung;Kim, Gi-Rim;Jeong, Deok-Yeong;Jeong, Chae-Hwan
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2015.08a
    • /
    • pp.257.1-257.1
    • /
    • 2015
  • Cu(In,Ga)Se2 (CIGS) 박막 태양 전지에서 buffer layer는 CIGS 흡수층과 TCO 사이의 밴드갭 차이에 대한 문제점과 lattice mismatch를 해결하기 위해 필수적이다. 흔히 buffer layer 물질로는 CdS가 가장 많이 사용되고 있으나 Cd의 독성에 관한 문제가 야기되고 있다. 따라서 ZnS(O, OH) buffer layer가 친환경 물질로 기존의 CdS 버퍼 층의 대체 물질로 각광 받고 있으며, 단파장 범위에서 높은 투과율로 인해 wide band gap의 Chalcopyrite 태양 전지에 응용되는 buffer layer로 많은 연구가 이루어지고 있다. 또한 buffer layer를 최적화 하여 carrier lifetime과 양자 효율이 증가시킬 수 있는 특성을 가지고 있다. 이 연구에서는 Cu(In,Ga)Se2 (CIGS) 박막에 화학습식공정 (CBD) 방법을 이용하여 최적화된 ZnS(O, OH)의 증착 조건을 찾고, 고품질의 buffer layer를 제조하기 위한 실험에 초점을 맞췄다. 또한, buffer layer의 막질을 개선하고 균일한 막을 제조하기 위해 processing parameters인 시약의 농도, 제조 시간 및 온도 등의 다양한 변화를 통해 실험을 진행하였다. 그 후 최적화된 ZnS(O, OH) buffer layer의 특성 분석을 위해 X-ray diffraction(XRD), photoluminescence (PL), scanning electron microscope (SEM) and GD-OES을 이용하였고, 이를 통해 제조된 CIGS 박막 태양전지는 light induced current-voltage (LIV) and external quantum efficiency (EQE)를 통해 특성 분석을 실시 하였다. 결과적으로, 제조된 ZnS(O, OH) buffer layer의 $ZnSO4{\cdot}7H2O$의 농도는 0.16 M, Thiourea는 0.5 M, NH4OH는 7.5 M, 그리고 반응 온도는 77.5 oC의 조건 하에 CIGS 기판 위에 균일하고 균열이 없는 ZnS(O, OH) 박막을 제조하였으며 이때 제조된 태양전지의 소자 특성은 Voc = 0.478 V, Jsc = 35.79 mA/cm2, FF = 47.77%, ${\eta}=8,18 %$이다.

  • PDF

Crystallization Behavior of poly(trimethylene terephthalate) in a Confined Geometry (제한공간에서의 폴리(트리메틸렌 테레프탈레이트)의 결정화 거동)

  • 임정은;이종관;이광희
    • Polymer(Korea)
    • /
    • v.27 no.4
    • /
    • pp.293-298
    • /
    • 2003
  • The development of the crystalline structure of poly(trimethylene terephthalate) (PTT) in a confined geometry was investigated with optical microscope, small angle light scattering, and X-ray diffraction. The rejected distance, which was represented in terms of the parameter $\delta$, played an important role in determining the morphological patterns of poly (ethylene terethphalate) (PET/PTT) blend. In case of stepwise crystallization, the crystallization of PTT commenced in the interspherulitic region between the grown PET crystals and proceeded until the interspherulitic space was filled with the PTT crystals. The spherulitic surface of the PET crtstals acted as the nucleation sites where the PTT molecules preferentially crystallized, leading to the formation of transcrystalline structure. As a result, a mixed morphological pattern was observed in the PTT-rich phase: one was a typical spherulitic texture and the other was a transcrystalline texture. Some of the molecular conformations of PTT, which could adopt in the absence of the space limitation, were probably forbidden in the interlamellar and/or interfibrillar regions of the PET spherulite. This constraint was responsible for difference in the crystallization and melting behavior of PTT between the intra and interspheulitic regions of PET.

Gaussian apodization for annular pupil (윤대 동구에 대한 Gaussian Apodization)

  • 송영란;이민희;이상수
    • Korean Journal of Optics and Photonics
    • /
    • v.7 no.3
    • /
    • pp.196-199
    • /
    • 1996
  • The amplitude LSF(Line spread function, $C_1e^{{o^2}{x^2}}$ or amplitude impulse) of the Gaussian apodized annular pupil is found to be same to that of the full aperture LSF($C_0e^{{o^2}{x^2}}$). $C_0$ and $C_1$ depending on $\sigma$, ${\omega}_0=\frac{2{\pi}}{\lambda}\;\frac{a_0}{l}$ and ${\omega}_0'=\frac{2{\pi}}{\lambda}\;\frac{a_0'}{l}$ which are the geometric parameter and pupil coordinates of the annular pupil. The important inequality relation among ${\omega}_0,\;{\omega}_0'$, a (fraction of diffraction amplitude) and $\sigma$ is obtained. It is $\frac{{\omega}_0}{\sqrt{2}}<{\sigma}{\le}(\frac{1-a}{2a})^{1/2}\;{\omega}_0$, and in the case of $a=e^{-1},\;a_0'{\le}0.34a_0$. The case of λ=0.013${\mu}{\textrm}{m}$, l=20 cm, $a_0=5cm$ and $a_0=0.34a_0=1.7cm$ give a Gaussian apodized superresolution ${\Delta}=\frac{\sqrt{log2}}{\sigma}=0.008{\mu}m$ annular pupil with the intensity signal equal to $e_{-2}$ times the signal obtainable by using the full aperture system(a=1)

  • PDF