• 제목/요약/키워드: XRD:DSC

검색결과 360건 처리시간 0.021초

기계적 합금화법으로 제조된 $MgH_x-Fe_2O_3$ 복합재료의 수소화 특성 평가 (The Evaluation of Hydrogenation Properties on $MgH_x-Fe_2O_3$ Composite by Mechanical Alloying)

  • 석송;조경원;홍태환
    • 한국수소및신에너지학회논문집
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    • 제18권1호
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    • pp.26-31
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    • 2007
  • Hydrogen has a high potential to be a renewable substitute for fossil fuels, because of its high gravimetric energy density and environment friendliness. In particular, Magnesium have attracted much interest since their hydrogen capacity exceeds that of known metal hydrides. One of the approaches to improve the kinetic is addition of metal oxide. In this paper, the effect of $Fe_2O_3$ concentration on the kinetics of Mg hydrogen absorption reaction was investigated. $MgH_x-Fe_2O_3$ composites have been synthesized by hydrogen induced mechanical alloying. The powder synthesized was characterized by XRD, SEM and simultaneous TG, DSC analysis. The hydrogenation behaviors were evaluated by using a sievert's type automatic PCT apparatus. Absorption and desorption kinetics of Mg catalyzed with 5,10 mass% $Fe_2O_3$ are determined at 423, 473, 523, 573, 623K.

Thermal Stability, Mechanical Properties and Magnetic Properties of Fe-based Amorphous Ribbons with the Addition of Mo and Nb

  • Han, Bo-Kyeong;Jo, Hye-In;Lee, Jin Kyu;Kim, Ki Buem;Yim, Haein
    • Journal of Magnetics
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    • 제18권4호
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    • pp.395-399
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    • 2013
  • The metallic glass ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) were obtained by melt spinning with 25-30 ${\mu}m$ thickness. The thermal stability, mechanical properties and magnetic properties of Fe-Co-B-Si based systems were investigated. The values of thermal stability were measured using differential scanning calorimetry (DSC), including glass transition temperature ($T_g$), crystallization temperature ($T_x$) and supercooled liquid region (${\Delta}T_x=T_x-T_g$). These amorphous ribbons were identified as fully amorphous, using X-ray diffraction (XRD). The mechanical properties of Febased samples were measured by nano-indentation. Magnetic properties of the amorphous ribbons were measured by a vibrating sample magnetometer (VSM). The amorphous ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) exhibited soft magnetic properties with low coercive force ($H_c$) and high saturation magnetization (Ms).

Spatial Distributions of Alloying Elements Obtained from Atom Probe Tomography of the Amorphous Ribbon Fe75C11Si2B8Cr4

  • Shin, Jinkyung;Yi, Seonghoon;Pradeep, Konda Gokuldoss;Choi, Pyuck-Pa;Raabe, Dierk
    • 한국재료학회지
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    • 제23권3호
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    • pp.190-193
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    • 2013
  • Spatial distributions of alloying elements of an Fe-based amorphous ribbon with a nominal composition of $Fe_{75}C_{11}Si_2B_8Cr_4$ were analyzed through the atom probe tomography method. The amorphous ribbon was prepared through the melt spinning method. The macroscopic amorphous natures were confirmed using an X-ray diffractometer (XRD) and a differential scanning calorimeter (DSC). Atom Probe (Cameca LEAP 3000X HR) analyses were carried out in pulsed voltage mode at a specimen base temperature of about 60 K, a pulse to base voltage ratio of 15 %, and a pulse frequency of 200 kHz. The target detection rate was set to 5 ions per 1000 pulses. Based on a statistical analyses of the data obtained from the volume of $59{\times}59{\times}33nm^3$, homogeneous distributions of alloying elements in nano-scales were concluded. Even with high carbon and strong carbide forming element contents, nano-scale segregation zones of alloying elements were not detected within the Fe-based amorphous ribbon. However, the existence of small sub-nanometer scale clusters due to short range ordering cannot be completely excluded.

BCNU 함유 PLGA 웨이퍼의 제조와 생체외 방출거동 (Preparation of BCNU-loaded PLGA Wafers and In Vitro Release Behavior)

  • 성하수;문대식;강길선;이정식;이해방
    • 폴리머
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    • 제26권1호
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    • pp.128-138
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    • 2002
  • 종양부위 또는 종양을 수술로 제거한 부위에 직접 이식하여 항암제를 투여함으로써 종양 또는 종양재발을 억제하는 악성뇌종양치료에 이용하기 위한 국소서방성 항암제제로서 항암제 1,3-bis(2-chloroethyl)-1-nitrosourea (BCNU, Carmustine)가 함유된 poly(D,L-lactide-co-glycolide) (PLGA, 락타이드와 글리콜라이드 몰비 75 : 25) 미분말을 제조하여 웨이퍼로 성형하였다. BCNU가 함유된 PLGA 미분말은 분사건조법에 의해 제조하였으며 주사전자현미경으로 관찰한 결과 제조된 미분말은 미립구의 형태를 나타내었다. XRD와 DSC를 통하여 PLGA에 포접된 BCNU의 결정성이 현저히 감소하였음을 확인하였다. 생체외 방출시험조건에서 BCNU의 방출경향은 PLGA의 분자량 및 농도, BCNU의 함량 등에 의존하였으며 초기 burst effect 이후 거의 0차 방출의 경향으로 8주 이상 지속적인 방출경향을 나타내었다. 방출시험기간 동안 웨이퍼의 형태변화를 관찰하고 방출시험액의 pH 변화를 측정함으로써 BCNU의 함량이 증가할수록 PLGA의 수화와 분해가 촉진됨을 확인하였다.

지속적인 국소마취를 위한 생분해성 PLGA 미립구의 제조와 생체외 방출 거동 (Preparation of Biodegradable PLGA Microspheres for Sustained Local Anesthesia and Their in vitro Release Behavior)

  • 조진철;강길선;최학수;이종문;이해방
    • 폴리머
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    • 제24권5호
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    • pp.728-735
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    • 2000
  • 지속적인 국소 마취의 가능성을 연구하기 위하여 펜타닐이 함유된 생분해성 poly(L-lactide-glycolide) (75 : 25 락타이드와 글리콜라이드의 몰 비, PLGA) 미립구를 제조하였다. 펜타닐 베이스가 함유된 PLGA 미립구는 일반적인 O/W 용매 증발법으로 제조하였으며 미립구의 크기는 10에서 150 $\mu\textrm{m}$의 범위에 있었다. 미립구의 표면과 단면 형태를 전자현미경으로 관찰하였고 생체외 펜타닐 베이스 방출량은 HPLC로 분석하였다. 젤라틴 유화제의 사용으로 가장 낮은 다공성 단면의 형태와 가장 높은 포접율을 가질 수 있었다. 펜타닐의 방출 패턴은 유화제의 종류, PLGA의 분자량 및 농도, 초기 약물 loading양 등과 같은 제조 조건들의 영향이 미치는 것으로 관찰되었다. 생체외에서 펜타닐 베이스의 방출은 제조 조건을 조절함으로써 거의 zero-order 형태로 25일 이상으로 지속적이었다. 또한 XRD와 DSC로 펜타닐이 함유된 PLGA 미립구의 물리화학적인 성질을 조사하였다.

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Effect of Calcination Temperature of Size Controlled Microstructure of LiNi0.8Co0.15Al0.05O2 Cathode for Rechargeable Lithium Battery

  • Park, Tae-Jun;Lim, Jung-Bin;Son, Jong-Tae
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.357-364
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    • 2014
  • Size controlled, $LiNi_{0.8}Co_{0.15}Al_{0.05}O_2$ cathode powders were prepared by co-precipitation method followed by heat treatment at temperatures between 750 and $850^{\circ}C$. The synthesized samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and electrochemical performance. The synthesized $LiNi_{0.8}Co_{0.15}Al_{0.05}O_2$ after calcined at $750^{\circ}C$ has a good electrochemical performance with an initial discharge capacity of $190mAhg^{-1}$ and good capacity retention of 100% after 30 cycles at 0.1C ($17mAg^{-1}$). The capacity retention of $LiNi_{0.8}Co_{0.15}Al_{0.05}O_2$ after calcined at $750^{\circ}C$ is better than that at 800 and $850^{\circ}C$ without capacity loss at various high C rates. This is ascribed to the minimized cation disorder, a higher conductivity, and higher lithium ion diffusion coefficient ($D_{Li}$) observed in this material. In the differential scanning calorimetry DSC profile of the charged sample, the generation of heat by exothermic reaction was decreased by calcined at high temperature, and this decrease is especially at $850^{\circ}C$. This behavior implies that the high temperature calcinations of $LiNi_{0.8}Co_{0.15}Al_{0.05}O_2$ prevent phase transitions with the release of oxygen.

티타늄이 도핑된 이산화 바나듐의 열변색 특성에 관한 연구 (A Study on the Thermochromic properties of Ti-doped Vanadium Dioxide)

  • 박진욱;박성수;안병현;홍성수;이근대
    • 청정기술
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    • 제21권4호
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    • pp.235-240
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    • 2015
  • 본 연구에서는 열변색 물성을 향상시키기 위한 방안의 하나로 0~0.5 at % 범위의 티타늄을 도핑한 이산화 바나듐(Ti-VO2)을 제조하였다. Ti-VO2 입자들은 바나딜설페이트, 중탄산암모늄, 사염화 티타늄 등을 사용하여 바나듐 화합물 전구체를 제조한 후 열분해법을 이용하여 제조하였다. 제조된 시료들의 결정 구조, 형상, 화학적 구조 및 열변색 특성은 X-선 회절분석기, 전계방사 주사전자현미경, X-선 광전자 분광기, 시차주사열량분석기, 자외선-가시광선-근적외선 분광기 등을 이용하여 분석하였다. 제조된 Ti-VO2 입자들은 단사 결정계를 지니고 있고, 또한 티타늄이 이산화 바나듐 결정내에 잘 도핑되어 있음을 확인할 수 있었다. 티타늄 도핑량이 증가함에 따라 최종 Ti-VO2 입자들의 크기가 작아지고 상전이 온도가 낮아졌으며, 또한 NIR switching efficiency는 증가하였다.

Physicochemical Characterization of Extrudate Solid Formulation of Angelica gigas Nakai Prepared by Hot Melt Extrusion Process

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Koo, Ja Seong;Park, Cheol Ho;Kang, Wie Soo
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2018년도 춘계학술발표회
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    • pp.72-72
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    • 2018
  • The root of Angelica gigas Nakai (AGN) is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, a major challenge associated with the usage of the active compounds from AGN is their poor water solubility. Therefore, this work aimed to enhance the solubility of active compounds by a chemical (viz. surfactant) and physical (hot melt extrusion) crosslinking method (CPC). Infrared Fourier transform spectroscopy (FT-IR) revealed multiple peaks in extrudate solids representing new functional groups including carboxylic acid, alkynes and benzene derivatives. Differential scanning calorimetry (DSC) analysis of the extrudate showed lower glass transition temperature (Tg) and lower enthalpy (${\Delta}H$) (Tg: $43^{\circ}C$; ${\Delta}H$: <6 (J/g)) compared to the non-extrudate (Tg $68.5^{\circ}C$; ${\Delta}H$: 123.2) formulations. X-ray powder diffraction (XRD) analysis revealed amorphization of crystal materials in extrudate solid. In addition, nanonization, enhanced solubility and higher extraction of phenolic compounds were achieved in the extrudate solid. Among the different extrudates, acetic acid- and Span 80-mediated formulations showed superior extractions. We conclude that the CPC method successfully enhanced the production of amorphous nano dispersions from extrudate solid formulations.

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수경성석회 종류에 따른 수황 및 탄산화 특성 (Hydration and Carbonation Properties of Different Hydraulic Lime)

  • 문기연;최문관;조계홍;조진상;안지환;연규석
    • 한국세라믹학회지
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    • 제51권2호
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    • pp.72-81
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    • 2014
  • The main mineral phases of natural hydraulic lime (NHL) as a hydraulic lime binderare $Ca(OH)_2$, $C_2S$, $C_3S$, $C_3A$, and $SiO_2$ residues. Also, NHL has the characteristic of setting and hardening by a hydration reaction with water and by carbonation reactions with carbon dioxide from the air. In this study, in an effort to investigate changes of the mineral phases by NHL hydration and carbonation reactions, transitions of mineral phases and the microstructures of hardened pastes were analyzed by XRD, DSC, SEM, and by pore size distributions using domestic and foreign-sourced NHL pastes after curing at 1, 3, 7, and 28 days. On the basis of the analysis results, it was confirmed that domestic low-grade limestone can be used for the manufacturing of NHL. The main hydration mineral phases were $Ca(OH)_2$, $CaCO_3$, $C_2S$, and $SiO_2$ residues, while in the case of foreign-sourced NHL, a small amount of an aluminium hydration phase formed. Also, the $CaCO_3$ content after the carbonation reaction increased with an increase in the curing time. After hydration for 28 days, NHL containing considerable amounts of $C_2S$ and $C_3S$ showed higher carbonation ratios than others types.

기계적 합금화법으로 제조한 MgHx-Graphene 복합재료의 수소화 거동 특성 (Evaluation of Hydrogenation Behavior of MgHx-Graphene Composites by Mechanical Alloying)

  • 이수선;이나리;김경일;홍태환
    • 한국수소및신에너지학회논문집
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    • 제22권6호
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    • pp.780-786
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    • 2011
  • Mg hydride had high hydrogen capacity (7.6%), lightweight and low cost materials and it was promising hydrogen storage material at high temperature. However, commercial applications of the Mg hydride are currently hindered by its high absorption/desorption temperature, and very slow reaction kinetics. one of the approaches to improve the kinetic is $MgH_x$ intermixed with carbon. And it shows that carbon and carbon allotropes have a beneficial effect on hydrogen sorption in Mg. The graphene is a kind of carbon allotropes which is easily desorbed reaction at low temperatures because its reaction is exothermic. In this work, the effect of graphene concentration on the kinetics of Mg hydrogen absorption reaction was investigated. The $MgH_x$-Graphene composites has been prepared by hydrogen induced mechanical alloy (HIMA). The synthesized powder was characterized by XRD and simultaneous TG, DSC analysis. The hydrogenation behaviors were evaluated by using a sievert's type automatic PCT apparatus. In this research, results of kinetic profiles exhibit hydrogen absorption rate of $MgH_x$-5wt.% and 10wt.% graphene composite, as 1.25wt.%/ms, 10.33wt.%/ms against 0.88wt.%/ms for $MgH_x$ alone at 473K.