• Title/Summary/Keyword: in situ spectroscopy

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In-situ measurement of Ce concentration in high-temperature molten salts using acoustic-assisted laser-induced breakdown spectroscopy with gas protective layer

  • Yunu Lee;Seokjoo Yoon;Nayoung Kim;Dokyu Kang;Hyeongbin Kim;Wonseok Yang;Milos Burger;Igor Jovanovic;Sungyeol Choi
    • Nuclear Engineering and Technology
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    • v.54 no.12
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    • pp.4431-4440
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    • 2022
  • An advanced nuclear reactor based on molten salts including a molten salt reactor and pyroprocessing needs a sensitive monitoring system suitable for operation in harsh environments with limited access. Multi-element detection is challenging with the conventional technologies that are compatible with the in-situ operation; hence laser-induced breakdown spectroscopy (LIBS) has been investigated as a potential alternative. However, limited precision is a chronic problem with LIBS. We increased the precision of LIBS under high temperature by protecting optics using a gas protective layer and correcting for shotto-shot variance and lens-to-sample distance using a laser-induced acoustic signal. This study investigates cerium as a surrogate for uranium and corrosion products for simulating corrosive environments in LiCl-KCl. While the un-corrected limit of detection (LOD) range is 425-513 ppm, the acoustic-corrected LOD range is 360-397 ppm. The typical cerium concentrations in pyroprocessing are about two orders of magnitude higher than the LOD found in this study. A LIBS monitoring system that adopts these methods could have a significant impact on the ability to monitor and provide early detection of the transient behavior of salt composition in advanced molten salt-based nuclear reactors.

Interfacial Electronic Structure of Bathocuproine and Al: Theoretical Study and Photoemission Spectroscopy

  • Lee, Jeihyun;Kim, Hyein;Shin, Dongguen;Lee, Younjoo;Park, Soohyung;Yoo, Jisu;Jeong, Junkyeong;Hyun, Gyeongho;Jeong, Kwangho;Yi, Yeonjin
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.169-169
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    • 2014
  • Interfacial electronic structure of bathocuproine and Al was investigated using in-situ photoemission spectroscopy and density functional theory (DFT) calculations. Bathocuproine is used for exciton blocking and electron transport material in organic photovoltaics and Al is typical cathode material. When thin thickness of Al was thermally evaporated on BCP, gap states were observed by ultraviolet photoemission spectroscopy. The closest gap state yielded below 0.3 eV from Fermi level. By x-ray photoemission spectroscopy, interaction of Al with nitrogen of BCP was observed. To understand the origin of gap states, DFT calculation was carried out and gap states was verified with successive calculation of interaction of Al and nitrogen of BCP. Furthermore, emergency of another state above Fermi level was observed. Remarkable reduction of electron injection barrier between Al and BCP, therefore, is possible.

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Study on Stabilization of Arsenic in Soil through in situ Formation of Amorphous Fe Oxides and use of X-ray Absorption Spectroscopy (비결정질철산화물 원위치 형성을 통한 비소오염토양 안정화 및 X선 분광분석법의 활용에 대한 연구)

  • Park, Jinhee;Chung, Hyeonyong;Kim, Sang Hyun;An, Jinsung;Nam, Kyoungphile
    • Journal of Soil and Groundwater Environment
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    • v.25 no.2
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    • pp.9-15
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    • 2020
  • This study was conducted to investigate the in situ formation of amorphous Fe oxides as a stabilization technology in As-contaminated soil. After addition of ferric nitrate and the neutralizing agent, most of extractable fractions of As in soil (i.e., SO42- and PO43--extractable As) was converted into As bound to amorphous Fe oxides. In addition, results of solubility bioavailability research consortium (SBRC) test indicated that a significant amount of As in untreated soil changed to a non-bioaccessible form after stabilization. The reason was attributed to the newly formed amorphous Fe oxides in the stabilized soil, which was confirmed by linear combination of fitting (LCF) using X-ray absorption spectroscopy (XAS) analysis. Interestingly, after five months of aging of the stabilized soil, ferrihydrite and schwertmannite newly formed in the soil were transformed to crystalline Fe oxides such as goethite, and further decrease in SBRC extractable fraction of As was observed. The results suggest that co-precipitated As with amorphous Fe oxides can be further immobilized with time, due to the crystallization of amorphous Fe oxides.

Comparison study of the effect of blending method on PVDF/PPTA blend membrane structure and performance

  • Li, Hongbin;Shi, Wenying;Zhang, Yufeng;Zhou, Rong
    • Membrane and Water Treatment
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    • v.6 no.3
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    • pp.205-224
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    • 2015
  • A novel hydrophilic poly (vinylidene fluoride)/poly (p-phenylene terephthalamide) (PVDF/PPTA) blend membrane was prepared by in situ polycondensation of p-phenylene diamine (PPD) and terephthaloyl chloride (TPC) in PVDF solution with subsequent nonsolvent induced phase separation (NIPS) process. For comparison, conventional solution blend membrane was prepared directly by adding PVDF powder into PPTA polycondensation solution. Blend membranes were characterized by means of viscometry, X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM). The effects of different blending methods on membrane performance including water contact angle (WCA), mechanical strength, anti-fouling and anti-compression properties were investigated and compared. Stronger interactions between PVDF and PPTA in in situ blend membranes were verified by viscosity and XPS analysis. The incorporation of PPTA accelerated the demixing rate and caused the formation of a more porous structure in blend membranes. In situ blend membranes exhibited better hydrophilicity and higher tensile strength. The optimal values of WCA and tensile strength were $65^{\circ}$ and 34.1 MPa, which were reduced by 26.1% and increased by 26.3% compared with pure PVDF membrane. Additionally, antifouling properties of in situ blend membranes were greatly improved than pure PVDF membrane with an increasing of flux recovery ratio by 25%. Excellent anti-compression properties were obtained in in situ blend membranes with a stable pore morphology. The correlations among membrane formation mechanism, structure and performance were also discussed.

Initial Reactions of Ti on the Atomically Clean Si Substrates (초청정한 Si 기판 위에서 Ti의 초기 반응)

  • Jeon, Hyeongtag;Nemanich, R.J.
    • Analytical Science and Technology
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    • v.5 no.3
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    • pp.303-308
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    • 1992
  • Initial reactions of Ti and Si have been studied to examine the surface roughness of titanium silicide. Formation mechanism has been explored with in-situ measurement tools such as AES(Auger electron spectroscopy) and LEED (low energy electron diffraction). One or two monolayers of Ti films have been deposited in ultrahigh vacuum on atomically clean Si(111) substrates. Atomically clean Si substrates which are reconstructed $7{\times}7$ Si(111) have been obtained after in-situ heat cleaning in ultrahigh vacuum. Deposition of the films were monitored by a quartz cuystal oscillator and the Ti films were analyzed with in-situ AES and LEED. The in-situ measurements show that the initial reactions of Ti and Si occur at room temperature and form a disordered layer. At low temperatures($200^{\circ}C{\sim}300^{\circ}C$) intermixing of Ti and Si is detected by AES. Substrate $1{\times}1$ LEED patterns are displayed after $400^{\circ}C$ anneal. This indicates that the disordered layer has transformed to form an ordered surface. The reappearance of the $7{\times}7$ LEED pattern in observed with further high temperature anneals and indicates three dimensional titanium silicide island formation.

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In-situ magnetization measurements and ex-situ morphological analysis of electrodeposited cobalt onto chemical vapor deposition graphene/SiO2/Si

  • Franco, Vinicius C. De;Castro, Gustavo M.B.;Corredor, Jeaneth;Mendes, Daniel;Schmidt, Joao E.
    • Carbon letters
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    • v.21
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    • pp.16-22
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    • 2017
  • Cobalt was electrodeposited onto chemical vapor deposition (CVD) graphene/Si/$SiO_2$ substrates, during different time intervals, using an electrolyte solution containing a low concentration of cobalt sulfate. The intention was to investigate the details of the deposition process (and the dissolution process) and the resulting magnetic properties of the Co deposits on graphene. During and after electrodeposition, in-situ magnetic measurements were performed using an (AGFM). These were followed by ex situ morphological analysis of the samples with ${\Delta}t_{DEP}$ 30 and 100 s by atomic force microscopy in the non-contact mode on pristine CVD graphene/$SiO_2$/Si. We demonstrate that it is possible to electrodeposit Co onto graphene, and that in-situ magnetic measurements can also help in understanding details of the deposition process itself. The results show that the Co deposits are ferromagnetic with decreasing coercivity ($H_C$) and demonstrate increasing magnetization on saturation ($M_{SAT}$) and electric signal proportional to remanence ($M_r$), as a function of the amount of the electrodeposited Co. It was also found that, after the end of the dissolution process, a certain amount of cobalt remains on the graphene in oxide form (this was confirmed by X-ray photoelectron spectroscopy), as suggested by the magnetic measurements. This oxide tends to exhibit a limited asymptotic amount when cycling through the deposition/dissolution process for increasing deposition times, possibly indicating that the oxidation process is similar to the graphene surface chemistry.

Measurement of combustion gas temperature using laser-induced breakdown spectroscopy (레이저 유도 플라즈마 분광분석법을 이용한 연소 가스 온도 측정 기술)

  • Lee, Seok Hwan;Kim, Yong-Gyoo;Kang, Woong;Joung, Wukchul;Lee, Joo Hyun;Kim, Sunghun;Yang, Inyoung
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2017.05a
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    • pp.285-289
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    • 2017
  • Laser-induced breakdown spesctroscopy (LIBS) is a technique that complements the disadvantages of conventional laser-based combustion diagnosis techniques such as weak signal strength, complex equipment configuration, and low accuracy. In this study, basic research was carried out to measure the combustion gas temperature of scramjet engines using LIBS. Spray flames were generated from Jet A-1 fuel used in scramjet engines and gas temperatures were measured at the top of the flames with a calibrated thermocouple. The LIBS signals were acquired at the same points as the temperature measurement positions of the thermocouple. The LIBS spectra were analyzed to obtained a calibration curve between the LIBS signal and the reference temperature measured at the thermocouple. Therefore, it was confirmed that the combustion gas temperature can be measured in-situ using LIBS.

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Numerical Simulation on Self-heating for Interlayer Tunneling Spectroscopy in $Bi_2Sr_2CaCu_2O_{8+x}$

  • Park, Jae-Hyun;Lee, Hu-Jong
    • Progress in Superconductivity
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    • v.9 no.1
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    • pp.18-22
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    • 2007
  • For interlayer tunneling spectroscopy using a small stack of $Bi_2Sr_2CaCu_2O_{8+x}$ (Bi-2212) intrinsic junctions in a high-bias range, large self-heating takes place due to the poor thermal conductivity of Bi-2212. In this study, we numerically estimate the self-heating around a Bi-2212 sample stack for I-V or dI/dV-V measurements. Our results show that the temperature discrepancy between the Bi-2212 sample stack and top Au electrodes due to bias-induced self-heating is small enough along the c-axis direction of Bi-2212. On the other hand, the lateral temperature discrepancy between the sample stack and the Bi-2212 on-chip thermometer stack can be as large as ${\sim}20\;K$ for the highest bias required to observe the pseudogap hump structure. We thus suggest a new in-situ ac thermometry, employing the Au current-bias electrode itself deposited on top of the sample stack as the resistive thermometer layer, which is supposed to allow safe temperature measurements for the interlayer tunneling spectroscopy.

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X-Ray Photoelectron Spectroscopy Studies of Pd Supported MgO/Mg (X-선 광전자분광법을 이용한 MgO/Mg 표면에 증착된 Pd의 분석)

  • Tai, Wei-Sheng;Seo, Hyun-Ook;Kim, Kwang-Dae;Kim, Young-Dok
    • Journal of the Korean Vacuum Society
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    • v.18 no.4
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    • pp.281-287
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    • 2009
  • Pd was deposited on magnesium-oxide-covered magnesium ribon substrate by metal thermal evaporation method in high vacuum. The electronic and chemical properties of Pd samples with different coverages were studied using in-situ X-ray Photoelctron Spectroscopy (XPS) and Field Emission Scanning Electron Microscopy (SEM). For relatively lower amounts of Pd deposited(< 1nm), separate Pd particles could be observed, whereas at higher Pd coverages, Pd thin films caused by agglomeration of Pd nanoparticles was found. The metal support interaction with Pd-support was observed. The Pd atoms on the metal oxide/metal interface were partially negative charged by charge transfer.

In-situ Synchrotron Radiation Photoemission Spectroscopy Study of Properties Variation of Ta2O5 Film during the Atomic Layer Deposition

  • Lee, Seung Youb;Jeon, Cheolho;Jung, Woosung;Kim, Yooseok;Kim, Seok Hwan;An, Ki-Seok;Park, Chong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.283.2-283.2
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    • 2013
  • The variation of chemical and interfacial state during the growth of Ta2O5 films on the Si substrate by atomic layer deposition (ALD) was investigated using in-situ synchrotron radiation photoemission spectroscopy. A newly synthesized liquid precursor Ta(NtBu)(dmamp)2Me was used as the metal precursor, with Ar as a purging gas and H2O as the oxidant source. The core-level spectra of Si 2p, Ta 4f, and O 1s revealed that Ta suboxide and Si dioxide were formed at the initial stages of Ta2O5 growth. However, the Ta suboxide states almost disappeared as the ALD cycles progressed. Consequently, the Ta5+ state, which corresponds with the stoichiometric Ta2O5, only appeared after 4.0 cycles. Additionally, tantalum silicate was not detected at the interfacial states between Ta2O5 and Si. The measured valence band offset value between Ta2O5 and the Si substrate was 3.08 eV after 2.5 cycles.

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