• 제목/요약/키워드: In situ X-ray diffraction

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Thermal behavior of groundwater-saturated Korean buffer under the elevated temperature conditions: In-situ synchrotron X-ray powder diffraction study for the montmorillonite in Korean bentonite

  • Park, Tae-Jin;Seoung, Donghoon
    • Nuclear Engineering and Technology
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    • 제53권5호
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    • pp.1511-1518
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    • 2021
  • In most countries, the thermal criteria for the engineered barrier system (EBS) is set to below 100 ℃ due to the possible illitization in the buffer, which will likely be detrimental to the performance and safety of the repository. On the other hand, if the thermal criteria for the EBS increases, the disposal density and the cost-effectiveness for the high-level radioactive wastes will dramatically increase. Thus, fundamentals on the thermal behavior of the buffer under the elevated temperatures is of crucial importance. Yet, the behaviors at the elevated temperatures of the bentonite under groundwater-saturated conditions have not been reported to-date. Here, we have developed an in-situ synchrotron-based method for the thermal behavior study of the buffer under the elevated temperatures (25-250 ℃), investigated dspacings of the montmorillonite in the Korean bentonite (i.e., Ca-type) at dry and KURT (KAERI Underground Research Tunnel) groundwater-saturated conditions (KJ-ii-dry and KJ-ii-wet), and compared the behaviors with that of MX-80 (i.e., Na-type, MX-80-wet). The hydration states analyzed show tri-, bi-, and mono-hydrated at 25, 120, and 250 ℃, respectively for KJ-ii-wet, whereas tri-, mono-, and de-hydrated at 25, 150, and 250 ℃, respectively for MX-80-wet. The Korean bentonite starts losing the interlayered water at lower temperatures; however, holds them better at higher temperatures as compared with MX-80.

Transmission Electron Microscopy Characterization of Early Pre-Transition Oxides Formed on ZIRLOTM

  • Bae, Hoyeon;Kim, Taeho;Kim, Ji Hyun;Bahn, Chi Bum
    • Corrosion Science and Technology
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    • 제14권6호
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    • pp.301-312
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    • 2015
  • Corrosion of zirconium fuel cladding is known to limit the lifetime and reloading cycles of fuel in nuclear reactors. Oxide layers formed on ZIRLO4^{TM}$ cladding samples, after immersion for 300-hour and 50-day in a simulated primary water chemistry condition ($360^{\circ}C$ and 20 MPa), were analyzed by using the scanning transmission electron microscopy (STEM), in-situ transmission electron microscopy (in-situ TEM) with the focused ion beam (FIB) technique, and X-ray diffraction (XRD). Both samples (immersion for 300 hours and 50 days) revealed the presence of the ZrO sub-oxide phase at the metal/oxide interface and columnar grains developed perpendicularly to the metal/oxide interface. Voids and micro-cracks were also detected near the water/oxide interface, while relatively large lateral cracks were found just above the less advanced metal/oxide interface. Equiaxed grains were mainly observed near the water/oxide interface.

In-situ 도핑된 다결정 3C-SiC 박막의 전기적 특성 (Electrical characteristics of In-situ doped polycrystalline 3C-SiC thin films)

  • 김강산;정귀상
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2008년도 추계학술대회 논문집 Vol.21
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    • pp.137-137
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    • 2008
  • In-situ doped polycrystalline 3C-SiC thin films were deposited by APCVD at $1200^{\circ}C$ using HMDS(hexamethyildisilane: $Si_2(CH_3)_6)$) as Si and C precursor, and 0 ~ 100 sccm $N_2$ as the dopant source gas. The peak of SiC is appeared in polycrystalline 3C-SiC thin films grown on $SiO_2$/Si substrates in XRD(X-ray diffraction) and FT-IR(Fourier transform infrared spectroscopy) analyses. The resistivity of polycrystalline 3C-SiC thin films decreased from 8.35 $\Omega{\cdot}cm$ with $N_2$ of 0 sccm to 0.014 $\Omega{\cdot}cm$ with 100 sccm. The carrier concentration of poly 3C-SiC films increased with doping from $3.0819\times10^{17}$ to $2.2994\times10^{19}cm^{-3}$ and their electronic mobilities increased from 2.433 to 29.299 $cm^2/V{\cdot}S$, respectively.

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Physical Property Change of the Gapless Semiconductor $PbPdO_2$ Thin Film by Ex-situ Annealing

  • Choo, S.M.;Park, S.M.;Lee, K.J.;Jo, Y.H.;Park, G.S.;Jung, M.H.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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    • pp.371-372
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    • 2012
  • We have studied lead-based gapless semiconductors, $PbPdO_2$, which is very sensitive to external parameters such as temperature, pressure, electric field, etc[1]. We have fabricated pure $PbPdO_2$, Co- and Mn-doped $PbPdO_2$ thin films using the pulsed laser deposition. Because of the volatile element of Pb, it is very difficult to grow the films. Note that in case of $MgB_2$, Mg is also volatile element. So in order to enhance the quality of $MgB_2$, some experiments are carried out in annealing with Mg-rich atmosphere [2]. This annealing process with volatile element plays an important role in making smooth surface. Thus, we applied such process to our studies of $PbPdO_2$ thin films. As a result, we found the optimal condition of ex-situ annealing temperature ${\sim}650^{\circ}C$ and time ~12 hrs. The ex-situ annealing brought the extreme change of surface morphology of thin films. After ex-situ annealing with PbO-rich atmosphere, the grain size of thin film was almost 100 times enlarged for all the thin films and also the PbO impurity phase was smeared out. And from X-ray diffraction measurements, we determined highly crystallized phases after annealing. So, we measured electrical and magnetic properties. Because of reduced grain boundary, the resistivity of ex-situ annealed samples changed smaller than no ex-situ sample. And the carrier densities of thin films were decreased with ex-situ annealing time. In this case, oxygen vacancies were removed by ex-situ annealing. Furthermore, we will discuss the transport and magnetic properties in pure $PbPdO_2$, Co- and Mn-doped $PbPdO_2$ thin films in detail.

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펄스레이저 증착법으로 제작된 $Bi_4Ti_3O_{12}/LaAlO_3$ 박막과 $Bi_4Ti_3O_{12}/YBa_2Cu_3O_{7-x}/LaAlO_3$ 복합구조의 에피 성장 (Epitaxial Growth of Pulsed-Laser Deposited Bi4Ti3O12/LaAlO3 Thin Films and Bi4Ti3O12/YBa2Cu3O7-x/LaAlO3 Heterostructure)

  • 조월렴;조학주;노태원
    • 한국결정학회지
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    • 제5권2호
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    • pp.85-92
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    • 1994
  • 펄스 레이저 증착법을 이용하여 강유전체 Bi4T13012 박막을 laA109(001) 위에 성장시켰다. 넓은 영역의 온도에서 증착한 박막의 상 형성과 구조적 성질을 X선 회절법을 이용하여 조사하였다. 740℃에서 증착한 박막은 박막의 c-축이 기판에 수직한 형태의 에피 성장의 경향을 보인다. 펄스 레이저 증착법을 이용하여 Bi4Ti3O12/YBa2Cu3O7-x/LaAlO3 복합구조를 in-situ 성장시켰다. Yba2Cu3O7-x의 a-, b-축이 LaAlO3와 완벽하게 평행하게 배열되어 있지 않음에도 불구하고, Bi4Ti3012 박막은 에피 성장의 경향을 보인다.

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Hot-wall epitaxy 방법에 의한 HgCdTe 박막 성장 (Growth of HgCdTe thin film by the hot-wall epitaxy method)

  • 최규상;정태수
    • 한국진공학회지
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    • 제9권4호
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    • pp.406-410
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    • 2000
  • Hot-wall epitaxy 방법으로 GaAs (100) 기판 위에 9 $\mu\textrm{m}$의 CdTe (111)을 완충층으로 성장하고 그 위에 in-situ로 $Hg_{1-x}Cd_x$/Te (MCT)박막을 성장하였다. 성장된 MCT박막의 2결정 x-선 요동곡선의 반치폭 값은 125 arcsec이었으며 표면 형상의 roughness는 10 nm의 작고 깨끗한 면을 나타내었다. 성장된 MCT 박막에 대한 광전류 측정으로부터 최대 peak 파장과 cut off 파장은 각각 1.1050 $\mu\textrm{m}$ (1.1220 eV)와 1.2632 $\mu\textrm{m}$ (0.9815 eV)임을 알았다 이 peak 파장은 광전도체의 intrinsic transition에 기인한 band gap에 대응하는 봉우리이다. 이로부터 MCT 박막은 1.0 $\mu\textrm{m}$에서 1.6 $\mu\textrm{m}$의 근적외선 파장 영역을 감지할 수 있는 광전도체용 검출기로 쓰일 수 있음을 알았다.

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기계적 합금화과정에서의 in situ 열분석에 의한 Ti-25.0~37.5at%Si 분말의 합성거동 (Synthesis Behavior of Ti-25.0~37.5at%Si Powders by In situ Thermal Analysis during Mechanical Alloying)

  • 변창섭;현창용;김동관
    • 한국재료학회지
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    • 제14권5호
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    • pp.305-309
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    • 2004
  • Mechanical alloying (MA) of Ti-25.0~37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0~26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1~37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1~37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

기계적 합금화과정에서의 in situ 열분석에 의한 Ti-50.0~66.7at%Si 분말의 합성거동 (Synthesis Behavior of Ti-50.0 ~ 66.7at%Si Powders by In situ Thermal Analysis during Mechanical Alloying)

  • 변창섭;이상호;이원희;현창용;김동관
    • 한국재료학회지
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    • 제14권5호
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    • pp.310-314
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    • 2004
  • Mechanical alloying (MA) of Ti-50.0~66.7at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-50.0~59.6at%Si powders showed that there were exothermic peaks during MA, indicating TiSi, $TiS_2$, and $Ti_{5}$ $Si_4$ phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). Those of Ti-59.8~66.7 at%Si powders, however, showed that there were no peaks during MA, indicating any Ti silicide was not synthesised until MA 240 min. For Ti-50.0~59.6at%Si powders, the critical milling times for SHS increased from 34.5 min to 89.5 min and the temperature rise, $\Delta$T (=peak temperature-onset temperature) decreased form $26.2^{\circ}C$ to $17.1^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 59.6at% and the critical value of the negative heat of formation of Ti-59.6at%Si to be -1.48 kJ/g.

Heat Treatment of Carbonized Photoresist Mask with Ammonia for Epitaxial Lateral Overgrowth of a-plane GaN on R-plane Sapphire

  • Kim, Dae-sik;Kwon, Jun-hyuck;Jhin, Junggeun;Byun, Dongjin
    • 한국재료학회지
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    • 제28권4호
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    • pp.208-213
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    • 2018
  • Epitaxial ($11{\bar{2}}0$) a-plane GaN films were grown on a ($1{\bar{1}}02$) R-plane sapphire substrate with photoresist (PR) masks using metal organic chemical vapor deposition (MOCVD). The PR mask with striped patterns was prepared using an ex-situ lithography process, whereas carbonization and heat treatment of the PR mask were carried out using an in-situ MOCVD. The heat treatment of the PR mask was continuously conducted in ambient $H_2/NH_3$ mixture gas at $1140^{\circ}C$ after carbonization by the pyrolysis in ambient $H_2$ at $1100^{\circ}C$. As the time of the heat treatment progressed, the striped patterns of the carbonized PR mask shrank. The heat treatment of the carbonized PR mask facilitated epitaxial lateral overgrowth (ELO) of a-plane GaN films without carbon contamination on the R-plane sapphire substrate. Thhe surface morphology of a-plane GaN films was investigated by scanning electron microscopy and atomic force microscopy. The structural characteristics of a-plane GaN films on an R-plane sapphire substrate were evaluated by ${\omega}-2{\theta}$ high-resolution X-ray diffraction. The a-plane GaN films were characterized by X-ray photoelectron spectroscopy (XPS) to determine carbon contamination from carbonized PR masks in the GaN film bulk. After $Ar^+$ ion etching, XPS spectra indicated that carbon contamination exists only in the surface region. Finally, the heat treatment of carbonized PR masks was used to grow high-quality a-plane GaN films without carbon contamination. This approach showed the promising potential of the ELO process by using a PR mask.

Maximizing TPBs through Ni-self-exsolution on GDC based composite anode in solid oxide fuel cells

  • 탄제완;이대희;김보경;김주선;문주호
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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    • pp.402.1-402.1
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    • 2016
  • The performance of solid oxide fuel cells (SOFCs) is directly related to the electrocatalytic activity of composite electrodes in which triple phase boundaries (TPBs) of metallic catalyst, oxygen ion conducting support, and gas should be three-dimensionally maximized. The distribution morphology of catalytic nanoparticle dispersed on external surfaces is of key importance for maximized TPBs. Herein in situ grown nickel nanoparticle onto the surface of fluorite oxide is demonstrated employing gadolium-nickel co-doped ceria ($Gd0.2-xNixCe0.8O2-{\delta}$, GNDC) by reductive annealing. GNDC powders were synthesized via a Pechini-type sol-gel process while maximum doping ratio of Ni into the cerium oxide was defined by X-ray diffraction. Subsequently, NiO-GNDC composite were screen printed on the both sides of yttrium-stabilized zirconia (YSZ) pellet to fabricate the symmetrical half cells. Electrochemical impedance spectroscopy (EIS) showed that the polarization resistance was decreased when it was compared to conventional Ni-GDC anode and this effect became greater at lower temperature. Ex situ microstructural analysis using scanning electron microscopy after the reductive annealing exhibited the exsolution of Ni nanoparticles on the fluorite phases. The influence of Ni contents in GNDC on polarization characteristics of anodes were examined by EIS under H2/H2O atmosphere. Finally, the addition of optimized GNDC into the anode functional layer (AFL) dramatically enhanced cell performance of anode-supported coin cells.

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