• Title/Summary/Keyword: Polymorphs

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Materials Characterization Using A Novel Simultaneous Near-Infrared/X-ray Diffraction Instrument

  • Yeboah, S.Agyare;Blanton, Thomas;Switalski, Steve;Schuler, Julie;Analytical, Craig Barnes
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1288-1288
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    • 2001
  • X-ray powder diffraction (XRD) is utilized for determination of polymorphism in crystalline organic materials. Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications. Near-Infrared spectroscopy (NIR) can be adapted to in situ manufacturing schemes by use of a source/detector probe. Conversely, NIR is unable to conclusively define the existence of polymorphism in crystalline materials. By combining the two techniques, a novel simultaneous NIR/XRD instrument has been developed. During material's analysis, results from XRD allow for defining the polymorphic phase present, and NIR data are collected as a fingerprint for each of the observed polymorphs. These NIR fingerprints will allow for the development of a library, which can be referenced during the use of a NIR probe in manufacturing settings.

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Applications of metal-semiconductor phase transition in 2D layered transition metal dichalcogenides (2차원 층상구조 전이금속칼코젠의 반도체-도체 구조상전이 기반 응용 기술)

  • Cho, Suyeon;Kim, Sera;Seok, Jinbong;Yang, Heejun
    • Vacuum Magazine
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    • v.3 no.1
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    • pp.4-8
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    • 2016
  • Motivated by two dimensional graphene, layered transition metal dichalcogenides (TMDs) have attracted scientific interests by their diverse electronic, optical and catalytic properties. In particular, group 6 TMDs such as $MoS_2$ and $MoTe_2$ have polymorphs (with metallic octahedral and semiconducting hexagonal phases) which are not present in graphene. Here, we introduce a new concept in 2D materials' studies, structural phase transition, with group 6 TMDs and its current research trend and applications for electric device and electrochemical catalyst.

Study on the Polymorphism of Sulfa Drugs (설파제의 다형(多形)에 관한 연구)

  • Sohn, Young-Taek
    • Journal of Pharmaceutical Investigation
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    • v.20 no.1
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    • pp.35-42
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    • 1990
  • A new form of sulfabenzamide was characterized using X-ray diffraction patterns and differential scanning calorimetry. Solubility studies demonstrated that, of the sulfabenzamide polymorphs, the new form was more soluble than form I. Compression of the new form at compression force of 1000 $kg/cm{^2}$ didn't induce polymorphic change in the crystal. Similar patterns were also produced through grinding. The effects of some diluents on the polymorphic transformation from the new form into form I by grinding and compression were also studied. Three diluents, $Avicel^{\circledR}$, lactose and starch showed no influence on the polymorphic transformation. The new form seemed to be more suitable for the pharmaceutical preparation.

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Thermal Decomposition and Sintering Characteristics of Cr-Deficient $(La,Ca)CrO_3$ (크롬부족 (란탄, 칼슘)크로마이트의 열분해과정 및 소결특성)

  • 이상기;조성걸
    • Journal of the Korean Ceramic Society
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    • v.34 no.11
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    • pp.1182-1186
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    • 1997
  • La0.8Ca0.2Cr0.98O3 powder was prepared using the modified Pechini process. Various crystalline phases formed during thermal decomposition were investigated. (La,Ca)CrO4 phase, first formed from the precursor, was transformed to (La,Ca)CrO3 and CaCrO4 above 80$0^{\circ}C$, which remained up to 110$0^{\circ}C$. However, only (La,Ca)CrO3 phase consisting of orthorhombic and intermediate rhombohedral polymorphs was observed after sintering at 125$0^{\circ}C$. The specimens sintered at 140$0^{\circ}C$ exhibited 98% of relative density and rather wide grain size distribution with average grain size of 3-4 ${\mu}{\textrm}{m}$. Densification and grain growth of the specimens observed above 125$0^{\circ}C$ were presumably attributed to liquid phase sintering resulted from melting of Ca3(CrO4)2 phase.

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Precipitated Calcium Carbonate Synthesis by Simultaneous Injection to Produce Nano Whisker Aragonite

  • Ramakrishna, Chilakala;Thenepalli, Thriveni;Huh, Jae-Hoon;Ahn, Ji Whan
    • Journal of the Korean Ceramic Society
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    • v.53 no.2
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    • pp.222-226
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    • 2016
  • The synthesis of pure calcium carbonate nanocrystals was achieved using a simultaneous injection method to produce nano particles of uniform size. These were characterized using scanning electron microscopy and powder X-ray diffraction. The nano particles were needle-shaped aragonite polymorphs, approximately 100-200 nm in length. The aragonite polymorph of calcium carbonate was prepared using aqueous solutions of $CaCl_2$ and $Na_2CO_3$, which were injected simultaneously into double distilled water at $50^{\circ}C$ and then allowed to react for 1.5 h. The resulting whisker-type nano aragonite with high aspect ratio (30) is biocompatible and potentially suitable for applications in light weight plastics, as well as in the medical, pharmaceutical, cosmetic and paint industries.

Recent Development in Polymer Ferroelectric Field Effect Transistor Memory

  • Park, Youn-Jung;Jeong, Hee-June;Chang, Ji-Youn;Kang, Seok-Ju;Park, Cheol-Min
    • JSTS:Journal of Semiconductor Technology and Science
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    • v.8 no.1
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    • pp.51-65
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    • 2008
  • The article presents the recent research development in polymer ferroelectric non-volatile memory. A brief overview is given of the history of ferroelectric memory and device architectures based on inorganic ferroelectric materials. Particular emphasis is made on device elements such as metal/ferroelectric/metal type capacitor, metal-ferroelectric-insulator-semiconductor (MFIS) and ferroelectric field effect transistor (FeFET) with ferroelectric poly(vinylidene fluoride) (PVDF) and its copolymers with trifluoroethylene (TrFE). In addition, various material and process issues for realization of polymer ferroelectric non-volatile memory are discussed, including the control of crystal polymorphs, film thickness, crystallization and crystal orientation and the unconventional patterning techniques.

Crystal Forms of Ketorolac

  • Sohn, Young-Taek;Seo, Hyun-Ok
    • Archives of Pharmacal Research
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    • v.27 no.3
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    • pp.357-360
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    • 2004
  • Four crystal forms of ketorolac have been obtained by recrystallization in organic solvents under variable conditions. Different ketorolac polymorphs and pseudo polymorph were characterized by X-ray powder diffraction crystallography (XRD), Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In the dissolution studies in water at $37{\pm}0.5^{\circ}C$ four crystal forms showed different patterns. The solubility of Form I were the highest. The solubility decreased in rank order: Form I> Form II > Form III > Form IV. Form land Form III were shown to have a good physical stability at room temperature for 60 days. However, Form II is converted to Form III and Form IV is converted to Form I after 60 days storage. Therefore, these observations indicate that crystalline polymorphism for ketorolac is readily inter-convertible and the relationship may have to taken into consideration in the formulation of the drug.

Fine Needle Aspiration Cytology of Collecting Duct Carcinoma of the Kidney - A Case Report - (신장 집합관 암종의 세침흡인 세포학적 소견 - 1예 보고 -)

  • Yi, Sang-Yeop;Lee, Kwang-Gil
    • The Korean Journal of Cytopathology
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    • v.5 no.2
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    • pp.160-166
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    • 1994
  • Collecting duct carcinoma of the kidney is an unusual variety of renal carcinoma considered to arise from the epithelium of the collecting ducts. We recently experienced a case of fine needle aspiration cytology of collecting duct carcinoma of the kidney in a 17 year-old girl. The smear revealed many cellular clusters of ordinary papillary pattern, characterized by clumping of cells with nuclear overlapping, in a slightly necrotic background. The tumor cells had abundant delicate granular cytoplasm with some having vacuolation. The nuclei were only slightly pleomorphic with somewhat coarse chromatin and one or more small nucleoli Some nuclei showed irregular nuclear membrane and nuclear groove. A few polymorphs were also present.

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Crystal Form of Olmutinib

  • Lee, Chang-Yeob;Sohn, Young-Taek
    • Journal of the Korean Chemical Society
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    • v.63 no.1
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    • pp.7-11
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    • 2019
  • Olmutinib, N-[3-({2-[4-(4-methylpiperazine-1-yl)aniline]thieno[3,2-d]Pyrimidin-4-yl}oxy)phenyl]prop-2-enamide dihydrochloride monohydrate, $Olita^{TM}$ is an oral, third-generation epidermal growth factor receptor tyrosine kinase inhibitor (EGFR TKI) that was developed by Boehringer Ingelheim and Hanmi Pharmaceutical Co. Ltd for the treatment of non-small cell lung cancer (NSCLC). The aim of this work was to investigate the existence of polymorphs and pseudopolymorphs of olmutinib. Three crystal forms of olmutinib have been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). From the DSC and TG data it was confirmed that Form 1 is monohydrate, Form 2 is dihydrate, Form 3 is 1.5 hydrate. The PXRD patterns of three crystal forms were different respectively. After storage of 1 month at $2^{\circ}C$, 24% RH (Relative Humidity), Form 1, Form 2, and Form 3 were not transformed.

Electronic Structure and Si L2,3-edge X-ray Raman Scattering Spectra for SiO2 Polymorphs: Insights from Quantum Chemical Calculations (양자화학계산을 이용한 SiO2 동질이상의 전자 구조와 Si L2,3-edge X-선 라만 산란 스펙트럼 분석)

  • Kim, Yong-Hyun;Yi, Yoo Soo;Lee, Sung Keun
    • Korean Journal of Mineralogy and Petrology
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    • v.33 no.1
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    • pp.1-10
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    • 2020
  • The atomic structures of silicate liquids at high pressure provide insights into the transport properties including thermal conductivities or elemental partitioning behavior between rocks and magmas in Earth's interior. Whereas the local electronic structure around silicon may vary with the arrangement of the nearby oxygens, the detailed nature of such relationship remains to be established. Here, we explored the atomic origin of the pressure-induced changes in the electronic structure around silicon by calculating the partial electronic density of states and L3-edge X-ray absorption spectra of SiO2 polymorphs. The result showed that the Si PDOS at the conduction band varies with the crystal structure and local atomic environments. Particularly, d-orbital showed the distinct features at 108 and 130 eV upon the changes in the coordination number of Si. Calculated Si XAS spectra showed features due to the s,d-orbitals at the conduction band and varied similarly with those observed in s,d-orbitals upon changes in the crystal structures. The calculated Si XAS spectrum for α-quartz was analogous to the experimental Si XRS spectrum for SiO2 glass, implying the overall similarities in the local atomic environments around the Si. The edge energies at the center of gravity of XAS spectra were closely related to the Si-O distance, thus showing the systematic changes upon densification. Current results suggest that the Si L2,3-edge XRS, sensitive probe of the Si-O distance, would be useful in unveiling the densification mechanism of silicate glasses and melts at high pressure.