• 제목/요약/키워드: stoichiometric analysis

검색결과 163건 처리시간 0.025초

In-situ Synchrotron Radiation Photoemission Spectroscopy Study of Atomic Layer Deposition of $Ta_2O_5$ film on Si Substrate with Ta(NtBu)(dmamp)$_2Me$ and $H_2O$

  • Lee, Seung Youb;Jung, Woosung;Kim, Yooseok;Kim, Seok Hwan;An, Ki-Seok;Park, Chong-Yun
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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    • pp.619-619
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    • 2013
  • The interfacial state between $Ta_2O_5$ and a Si substrate during the growth of $Ta_2O_5$ films by atomic layer deposition (ALD) was investigated using in-situ synchrotron radiation photoemission spectroscopy (SRPES). A newly synthesized liquid precursor Ta($N^tBu$) $(dmamp)_2Me$ was used as the metal precursor, with Ar as a purging gas and $H_2O$ as the oxidant source. After each half reaction cycle, samples were analyzed using in-situ SRPES under ultrahigh vacuum at room temperature. SRPES analysis revealed that Ta suboxide and Si dioxide were formed at the initial stages of $Ta_2O_5$ growth. However, the Ta suboxide states almostdisappeared as the ALD cycles progressed. Consequently, the $Ta^{5+}$ state, which corresponds with the stoichiometric $Ta_2O_5$, only appeared after 4.0 cycles. Additionally, tantalum silicate was not detected at the interfacial states between $Ta_2O_5$ and Si. The measured valence band offset between $Ta_2O_5$ and the Si substrate was 3.22 eV after 3.0 cycles.

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The Effect of the Oxygen Flow Rate on the Electronic Properties and the Local Structure of Amorphous Tantalum Oxide Thin Films

  • Denny, Yus Rama;Lee, Sunyoung;Lee, Kangil;Kang, Hee Jae;Yang, Dong-Seok;Heo, Sung;Chung, Jae Gwan;Lee, Jae Cheol
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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    • pp.398-398
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    • 2013
  • The electronic properties and the local structure of tantalum oxide thin film with variation of oxygen flow rate ranging from 9.5 to 16 sccm (standard cubic centimeters per minute) have been investigated by X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), and X-ray absorption spectroscopy (XAS). The XPS results show that the Ta4f spectrum for all films consist of the strong spin-orbit doublet $Ta4f_{7/2}$ and $Ta4f_{5/2}$ with splitting of 1.9 eV. The oxygen flow rate of the film results in the appearance of new features in the Ta4f at binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV, these peaks attribute to $Ta^{1+}$, $Ta^{2+}$, $Ta^{4+}$/$Ta^{2+}$, and $Ta^{5+}$, respectively. Thus, the presence of non-stoichiometric state from tantalum oxide ($TaO_x$) thin films could be generated by the oxygen vacancies. The REELS spectra suggest the decrease of band gap for tantalum oxide thin films with increasing the oxygen flow rate. The absorption coefficient ${\mu}$ and its fine structure were extracted from the fluorescence mode of extended X-ray absorption fine structure (EXAFS) spectra. In addition, bond distances (r), coordination numbers (N) and Debye-Waller factors (${\sigma}^2$) each film were determined by a detailed of EXAFS data analysis. EXAFS spectrapresent both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the increase of oxygen flow rate.

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바이칼린 함유 생약의 제제화 및 생체이용률 (제3보) : 황금 및 황련 공침물의 포접화합물 제조 및 생체이용률에 관한 연구 (Preparation and Bioavailability of Oriental Medicine Containing Baicalin (III) : Preparation of Inclusion Complex and Bioavailability of Coprecipitated Product of Scutellariae Radix and Coptidis Rhizoma)

  • 양재헌;신상철;류희두
    • Journal of Pharmaceutical Investigation
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    • 제27권1호
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    • pp.29-38
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    • 1997
  • Precipitation was formed during the preparation of decoction from a mixture of Scutellariae Radix and Coptidis Rhizoma. Baicalin and berberine were identified in this coprecipitated product (CPP) and these components were the active ingredients of two herbal medicine. We extracted respectively crude baicalin and berberine in Scutellariae Radix and Coptidis Rhizoma and prepared coprecipitate of crude baicalin-berberine. To increase the stability and bioavailability of coprecipitate of crude baicalin-berberine(CBB), which is slightly soluble drug, its inclusion complex was prepared and studied in this experiment. Inclusion complex of CBB with ${\beta}-cyclodextrin(CBB-{\beta}-CD)$ was prepared by freeze drying method and its characteristics were ascertained by means of solubility test, differential thermal analysis(DTA) and scanning electron microscope(SEM). The type of $CBB-{\beta}-CD$ is classified as $A_L-type$ on phase solubility diagram, and the stoichiometric ratio of CBB(baicalin in CBB) : ${\beta}-CD$ complex is 1:1 and formation constant is 151 $M^-1$. The solubility, dissolution, in situ absorption and serum concentration of $CBB-{\beta}-CD$ were significantly increased when compared to CBB. Therefore enhanced bioavailability of CBB by inclusion complexation with ${\beta}-cyclodextrin$ might be useful for dosage form design of active ingredients of two herbal medicine.

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고온가스로용 핵연료 제조에서 열처리 조건이 우라늄산화물 입자 특성에 미치는 영향 (Effects of Thermal Treatment Conditions on the Powder Characteristics of Uranium Oxide in HTGR Fuel Preparation)

  • 김연구;정경채;오승철;서동수;조문성
    • 한국분말재료학회지
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    • 제16권2호
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    • pp.115-121
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    • 2009
  • The effects of thermal treatment conditions on ADU (ammonium diuranate) prepared by SOL-GEL method, so-called GSP (Gel supported precipitation) process, were investigated for $UO_2$ kernel preparation. In this study, ADU compound particles were calcined to $UO_3$ particles in air and Ar atmospheres, and these $UO_3$ particles were reduced and sintered in 4%-$H_2$/Ar. During the thermal calcining treatment in air, ADU compound was slightly decomposed, and then converted to $UO_3$ phases at $500^{\circ}C$. At $600^{\circ}C$, the $U_3O_8$ phase appeared together with $UO_3$. After sintering of theses particles, the uranium oxide phases were reduced to a stoichiometric $UO_2$. As a result of the calcining treatment in Ar, more reduced-form of uranium oxide was observed than that treated in air atmosphere by XRD analysis. The final phases of these particles were estimated as a mixture of $U_3O_7$ and $U_4O_9$.

$SiO_x(x{\le}2)$ 플레이트의 표면 결함 분포가 화학 소염에 미치는 영향 (Effects of Surface Defect Distribution of $SiO_x(x{\le}2)$ Plates on Chemical Quenching)

  • 김규태;권세진
    • 한국연소학회:학술대회논문집
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    • 한국연소학회 2005년도 제31회 KOSCO SYMPOSIUM 논문집
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    • pp.328-336
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    • 2005
  • Effects of surface defect distribution on flame instability during flame-surface interaction are experimentally investigated. To examine the chemical quenching phenomenon, we prepared thermally grown silicon oxide plates with well-defined defect density. Ion implantation was used to control the number of defects, i.e. oxygen vacancies. In an attempt to preferentially remove the oxygen atoms from silicon dioxide surface, argon ions with low energy level from 3keV to 5keV were irradiated at the incident angle of $60^{\circ}C$. Compositional and structural modification of $SiO_2$ induced by low-energy $Ar^+$ ion irradiation has been characterized by Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS). The analysis shows that as the ion energy increases, the number of structural defect also increases and non-stoichiometric condition of $SiO_x(x{\le}2)$ plates is enhanced. From the quenching distance measurements, we found out that when the surface temperature is under $300^{\circ}C$, the quenching distance decreases on account of reduced heat loss; as the surface temperature increases over $300^{\circ}C$, however, quenching distance increases despite reduced heat loss effect. Such aberrant behavior is caused by heterogeneous chemical reaction between active radicals and surface defect sites. The higher defect density, the larger quenching distance. This results means that chemical quenching is governed by radical adsorption and can be parameterized by the oxygen vacancy density on the surface.

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혼합원자가 $La_{1-x}Ca_xFeO_{3-y}$의 비화학양론에 관한 연구 (Nonstoichiometric Studies of the Mixed Valency $La_{1-x}Ca_xFeO_{3-y}$)

  • 여철현;편웅범;이은석;이성주
    • 대한화학회지
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    • 제32권1호
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    • pp.9-14
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    • 1988
  • $La_{1-x}Ca_xFeO_{3-y}$ 계의 perovskite 형의 화합물은 La_2O_3,\;CaCO_3$, 및 Fe(NO-3)_3{\cdot}9H_2O$의 정량적 혼합물은 1100$^{\circ}C$에서 24시간 동안 가열하여 제조하였다. 이 고용체의 결정구조는 모든 조성에서 사방정계였다. X-선 회절분석과 Mohr 염 분석을 통하여 y값이 증가하면 공위배열에 의한 상전이가 일어나며 격자체적은 x값이 증가함에 따라 감소한다는 것을 확인하였다. 비화학양론적 조성 y는 0.0에서 0.5사이의 값을 나타내었다. Mossbauer 분광분석을 298K에서 수행하여 x = 0.75 조성이 높은 닐온도를 갖는다는 것을 확인하였다. 시료의 전기전도도는 $-100{\sim}100^{\circ}C$ 온도범위에서 측정하였다. 활성화 에너지로부터 공위 배열에 기인한 열린 통로를 갖고 있는 시료들은 이온성 전기전도에 의한 기여가 어느 정도 존재하는 것으로 밝혀졌다.

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MOCVD법으로 제조한 $AL_2O_3$ 박막의 열처리에 의한 특성 평가 (Characterization of the heat treatment of $AL_2O_3$ thin films by MOCVD)

  • 이상화;김종국;박병옥
    • 한국결정성장학회지
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    • 제7권2호
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    • pp.216-223
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    • 1997
  • 출발물질로 aluminum iso-propoxide ($Al(OC_3H_7)_3$, AIP)를 사용하여 화학증착법으로 Si-wafer(100)위에 알루미나 박막을 증착하였다. 증착된 박막의 조성을 알아보기 위해 ESCA를 이용하였으며, SEM을 이용하여 박막의 형상 및 두께를 평가하였다. 그리고 굴절율 및 C-V 특성은 각각 ellipsometry와 HP4192A를 사용하였다. ESCA와 SEM의 분석결과에서 상압보다는 저압에서 막이 균일하고 조성이 잘 맞는 것을 알 수 있었으며 열처리를 통해 굴절율의 변화를 볼 수 있었다. 그리고 NMOS소자에서의 C-V특성을 개선하기 위해, $Al_2O_3$와 Si사이에 $SiO_2$층을 형성하는 것이 좋음을 알 수 있었다.

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다양한 Ball Mill Method에 의해 제조된 V/TiO2 촉매의 NH3-SCR 활성 증진연구 (Enhanced NH3-SCR Activity of V/TiO2 Catalyst Prepared by Various Ball Mill Method)

  • 김동호;서필원;홍성창
    • 청정기술
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    • 제23권1호
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    • pp.64-72
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    • 2017
  • 본 연구에서는, $150{\sim}400^{\circ}C$ 영역에서 $NO_x$를 제어하기 위한 ball mill 기법을 사용한 선택적 환원촉매(SCR)의 연구를 수행하였다. 제조된 촉매들의 구조적 특성 및 산화가 특성을 확인하기 위하여 XRD, BET, XPS 분석을 수행하였다. 다양한 ball mill 기법에 의해 제조된 촉매는 $250^{\circ}C$ 이하의 온도구간에서의 활성의 차이를 보였다. 이중 가장 우수한 탈질효율을 갖는 촉매를 기준으로, ball mill 시간이 3시간일 때 가장 높은 활성을 나타내었다. XPS 분석 결과, vanadium의 비 화학양론종의 존재 및 원자 수 증가가 활성증진에 유리하게 작용한 것으로 나타났다. 또한 $O_2$ on-off 실험을 통해 격자산소량의 양과 탈질 효율과의 상관관계를 나타내었고, 이는 서로 비례관계에 있음을 확인하였다.

고 에너지 볼 밀링을 통한 Co-ferrite 제조 및 열적 환원에 대한 연구 (A Study on the Synthesis of Co-ferrite by High-energy Ball Milling and Thermal Reduction Characteristics)

  • 조미선;김우진;김창희;강경수;김영호;박주식
    • 한국수소및신에너지학회논문집
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    • 제17권3호
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    • pp.309-316
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    • 2006
  • Co-ferrite was synthesized by HEBM (High Energy Ball Milling) with a stoichiometric (Co/Fe=0.5/2.5) mixture of CoO and $Fe_2O_3$ powders. The effect of milling time on the phase transformation of the mixture was investigated by XRD. Mono-phase solid solution of Co-ferrite, which was milled for 4 h and then calcined at $900^{\circ}C$ in the Ar atmosphere, was confirmed by XRD analysis. The composition and thermal reduction behavior of Co-ferrite were analyzed by TGA and XRF. As a result, oxygen deficient Co-ferrite was synthesized by HEBM and the weight decrease of the Co-ferrite, which was oxidized at $600^{\circ}C$ for 10h by $H_2O$ vapor, was 2.41 wt% during thermal reduction at $1300^{\circ}C$.

Synthesis and Characteristic of Novel Soluble Triazoleimide Oligomers with Terminated Arylacetylene

  • Zhou, Xiao'an;Du, Lei;Wan, Liqiang;Wang, Xiaofei;E, Yanpeng;Huang, Farong
    • Bulletin of the Korean Chemical Society
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    • 제31권9호
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    • pp.2603-2606
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    • 2010
  • Novel soluble triazoleimide oligomers terminated with arylacetylene terminated were synthesized by the Cu(I)-catalysed 1,3-dipolar cycloaddition polymerization of diazides and imide-containing dialkyne. Several molecular weight triazoleimide oligomers were prepared from diazide and dialkyne monomers with different stoichiometric combinations. The curing behaviors of the oligomers were tested by differential scanning calorimetry (DSC). The thermal properties of the cured products were evaluated by DSC and thermogravimetric analysis (TGA). These cured oligomers showed the glass transition temperature of about $225-235^{\circ}C$ and the decomposition temperature (at 5% weight loss) of about $385-393^{\circ}C$ in nitrogen.