The behavior of hydrogen species on the surface of the catalyst during the Lewis acid transformation to form Brønsted acid sites over the spherical silica-supported WOx catalyst was investigated. To understand the structure-activity relationship of Lewis acid transformation and hydrogen bonding interactions, we explore the potential of using the in situ diffuse reflection infrared Fourier transform spectroscopy (DRIFTS) with adsorbed ammonia and hydrogen exposure. From the results of in situ DRIFTS measurements, Lewis acid sites on surface catalysts were transformed into new Brønsted acid sites upon hydrogen exposure. The adsorbed NH3 on Lewis acid sites migrated to Brønsted acid sites forming NH4+. The results show that the dissociated H atoms present on the catalyst surface formed new Si-OH hydroxyl species - the new Brønsted acid site. Besides, the isolated Si-O-W species is the key towards H-bond and Si-OH formation. Additionally, the H atoms adsorbed surrounding the Si-O-W species of mono-oxo O=WO4 and di-oxo (O=)2WO2 species, where the Si-O-W species are the main species presented on the Inc-SSP catalysts than that of the IWI-SSP catalysts.
We present the results of multi-epoch, multi-frequency monitoring of a blazar 4C +29.45, which was regularly monitored as part of the Interferometric Monitoring of GAmma-ray Bright AGNs program - a key science program of the Korean Very long baseline interferometry Network (KVN). Observations were conducted simultaneously at 22, 43, 86 and 129 GHz during the 4 years from December 2012 to December 2016. We also used additional data from the 15 GHz Owens Valley Radio Observatory (OVRO) monitoring program. From the 15 GHz light curve, we estimated the variability time scales of the source during several radio flux enhancements. We found that the source experiencesd 6 radio flux enhancements with variability time scales of 9-187 days during the observing period, yielding corresponding variability Doppler factors of 9-27. From the multi-frequency simultaneous KVN observations, we were able to obtain accurate radio spectra of the source and hence to more precisely measure the turnover frequencies 𝜈r of synchrotron self-absorbed (SSA) emission with a mean value of ${\bar{\nu}_r}=28.9GHz$. Using jet geometry assumptions, we estimated the size of the emitting region at the turnover frequency. Taking into account these results, we found that the equipartition magnetic field strength is up to two orders of magnitudes higher than the SSA magnetic field strength (0.6-99 mG). This is consistent with the source being particle dominated.
We present a study of the inexplicit connection between radio jet activity and ${\gamma}$-ray emission of BL Lacertae (BL Lac; 2200+420). We analyze the long-term millimeter activity of BL Lac via interferometric observations with the Korean VLBI Network (KVN) obtained at 22, 43, 86, and 129 GHz simultaneously over three years (from January 2013 to March 2016); during this time, two ${\gamma}$-ray outbursts (in November 2013 and March 2015) can be seen in ${\gamma}$-ray light curves obtained from Fermi observations. The KVN radio core is optically thick at least up to 86 GHz; there is indication that it might be optically thin at higher frequencies. To first order, the radio light curves decay exponentially over the time span covered by our observations, with decay timescales of $411{\pm}85$ days, $352{\pm}79$ days, $310{\pm}57$ days, and $283{\pm}55$ days at 22, 43, 86, and 129 GHz, respectively. Assuming synchrotron cooling, a cooling time of around one year is consistent with magnetic field strengths $B{\sim}2{\mu}T$ and electron Lorentz factors ${\gamma}$ ~ 10 000. Taking into account that our formal measurement errors include intrinsic variability and thus over-estimate the statistical uncertainties, we find that the decay timescale ${\tau}$ scales with frequency ${\nu}$ like ${\tau}{\propto}{\nu}^{-0.2}$. This relation is much shallower than the one expected from opacity effects (core shift), but in agreement with the (sub-)mm radio core being a standing recollimation shock. We do not find convincing radio flux counterparts to the ${\gamma}$-ray outbursts. The spectral evolution is consistent with the 'generalized shock model' of Valtaoja et al. (1992). A temporary increase in the core opacity and the emergence of a knot around the time of the second ${\gamma}$-ray event indicate that this ${\gamma}$-ray outburst might be an 'orphan' flare powered by the 'ring of fire' mechanism.
Proceedings of the Materials Research Society of Korea Conference
/
2011.10a
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pp.7-7
/
2011
Quantum beam technology has been expected to develop breakthroughs for nanotechnology during the third basic plan of science and technology (2006~2010). Recently, Green- or Life Innovations has taken over the national interests in the fourth basic science and technology plan (2011~2015). The NIMS (National Institute for Materials Science) has been conducting the corresponding mid-term research plans, as well as other national projects, such as nano-Green project (Global Research for Environment and Energy based on Nanomaterials science). In this lecture, the research trends in Japan and NIMS are firstly reviewed, and the typical achievements are highlighted over key nanotechnology fields. As one of the key nanotechnologies, the quantum beam research in NIMS focused on synchrotron radiation, neutron beams and ion/atom beams, having complementary attributes. The facilities used are SPring-8, nuclear reactor JRR-3, pulsed neutron source J-PARC and ion-laser-combined beams as well as excited atomic beams. Materials studied are typically fuel cell materials, superconducting/magnetic/multi-ferroic materials, quasicrystals, thermoelectric materials, precipitation-hardened steels, nanoparticle-dispersed materials. Here, we introduce a few topics of neutron scattering and ion beam nanofabrication. For neutron powder diffraction, the NIMS has developed multi-purpose pattern fitting software, post RIETAN2000. An ionic conductor, doped Pr2NiO4, which is a candidate for fuel-cell material, was analyzed by neutron powder diffraction with the software developed. The nuclear-density distribution derived revealed the two-dimensional network of the diffusion paths of oxygen ions at high temperatures. Using the high sensitivity of neutron beams for light elements, hydrogen states in a precipitation-strengthened steel were successfully evaluated. The small-angle neutron scattering (SANS) demonstrated the sensitive detection of hydrogen atoms trapped at the interfaces of nano-sized NbC. This result provides evidence for hydrogen embrittlement due to trapped hydrogen at precipitates. The ion beam technology can give novel functionality on a nano-scale and is targeting applications in plasmonics, ultra-fast optical communications, high-density recording and bio-patterning. The technologies developed are an ion-and-laser combined irradiation method for spatial control of nanoparticles, and a nano-masked ion irradiation method for patterning. Furthermore, we succeeded in implanting a wide-area nanopattern using nano-masks of anodic porous alumina. The patterning of ion implantation will be further applied for controlling protein adhesivity of biopolymers. It has thus been demonstrated that the quantum beam-based nanotechnology will lead the innovations both for nano-characterization and nano-fabrication.
Proceedings of the Korean Vacuum Society Conference
/
2012.02a
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pp.312-312
/
2012
Magnesium oxide has become focus for research activities due to its use in magnetic tunnel junctions and for understanding of do ferromagnetism. Theoretical investigations on such type of system indicate that the presence of defects greater than a threshold value is responsible for the magnetic behaviour. It has also been shown experimentally that by decreasing the film thickness and size of nanoparticles, enhancement/increase in magnetization can be achieved. Apart from the change in dimension, swift heavy ions (SHI) are well known for creating defects and modifying the properties of the materials. In the present work, we have studied the irradiation induced effects in magnesium oxide thin film deposited on quartz substrate via X-ray absorption spectroscopy (XAS). Magnesium oxide thin films of thickness 50nm were deposited on quartz substrate by using e-beam evaporation method. These films were irradiated by 200 MeV Ag15+ ion beam at fluence of $1{\times}10^{11}$, $5{\times}10^{11}$, $1{\times}10^{12}$, $3{\times}10^{12}$ and $5{\times}10^{12}ions/cm^2$ at Nuclear Science Centre, IUAC, New Delhi (India). The grain size was observed (as studied by AFM) to be decreased from 37 nm (pristine film) to 23 nm ($1{\times}10^{12}ions/cm^2$) and thereafter it increases upto a fluence of $5{\times}10^{12}ions/cm^2$. The electronic structure of the system has been investigated by X-ray absorption spectroscopy (XAS) measurements performed at the high energy spherical grating monochromator 20A1 XAS (HSGM) beamline in the National Synchrotron Radiation Research Center (NSRRC), Taiwan. Oxides of light elements like MgO/ZnO possess many unique physical properties with potentials for novel application in various fields. These irradiated thin films are also studied with different polarization (left and right circularly polarized) of incident x-ray beam at 05B3 EPU- Soft x-ray scattering beamline of NSRRC. The detailed analysis of observed results in the wake of existing theories is discussed.
Proceedings of the Materials Research Society of Korea Conference
/
2011.05a
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pp.5-5
/
2011
The research and development of hybrid electric vehicle (HEV), plug-in hybrid electric vehicle (PHEV) and electric vehicle (EV) are intensified due to the energy crisis and environmental concerns. In order to meet the challenging requirements of powering HEV, PHEV and EV, the current lithium battery technology needs to be significantly improved in terms of the cost, safety, power and energy density, as well as the calendar and cycle life. One new technology being developed is the utilization of composite cathode by mixing two different types of insertion compounds [e.g., spinel $LiMn_2O_4$ and layered $LiMO_2$ (M=Ni, Co, and Mn)]. Recently, some studies on mixing two different types of cathode materials to make a composite cathode have been reported, which were aimed at reducing cost and improving self-discharge. Numata et al. reported that when stored in a sealed can together with electrolyte at $80^{\circ}C$ for 10 days, the concentrations of both HF and $Mn^{2+}$ were lower in the can containing $LiMn_2O_4$ blended with $LiNi_{0.8}Co_{0.2}O_2$ than that containing $LiMn_2O_4$ only. That reports clearly showed that this blending technique can prevent the decline in capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and related structural phase transitions for these composite cathodes. In this presentation, we will report our in situ x-ray diffraction studies on this mixed composite cathode material during charge-discharge cycling. The mixed cathodes were incorporated into in situ XRD cells with a Li foil anode, a Celgard separator, and a 1M $LiPF_6$ electrolyte in a 1 : 1 EC : DMC solvent (LP 30 from EM Industries, Inc.). For in situ XRD cell, Mylar windows were used as has been described in detail elsewhere. All of these in situ XRD spectra were collected on beam line X18A at National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory using two different detectors. One is a conventional scintillation detector with data collection at 0.02 degree in two theta angle for each step. The other is a wide angle position sensitive detector (PSD). The wavelengths used were 1.1950 ${\AA}$ for the scintillation detector and 0.9999 A for the PSD. The newly installed PSD at beam line X18A of NSLS can collect XRD patterns as short as a few minutes covering $90^{\circ}$ of two theta angles simultaneously with good signal to noise ratio. It significantly reduced the data collection time for each scan, giving us a great advantage in studying the phase transition in real time. The two theta angles of all the XRD spectra presented in this paper have been recalculated and converted to corresponding angles for ${\lambda}=1.54\;{\AA}$, which is the wavelength of conventional x-ray tube source with Cu-$k{\alpha}$ radiation, for easy comparison with data in other literatures. The structural changes of the composite cathode made by mixing spinel $LiMn_2O_4$ and layered $Li-Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ in 1 : 1 wt% in both Li-half and Li-ion cells during charge/discharge are studied by in situ XRD. During the first charge up to ~5.2 V vs. $Li/Li^+$, the in situ XRD spectra for the composite cathode in the Li-half cell track the structural changes of each component. At the early stage of charge, the lithium extraction takes place in the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component only. When the cell voltage reaches at ~4.0 V vs. $Li/Li^+$, lithium extraction from the spinel $LiMn_2O_4$ component starts and becomes the major contributor for the cell capacity due to the higher rate capability of $LiMn_2O_4$. When the voltage passed 4.3 V, the major structural changes are from the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, while the $LiMn_2O_4$ component is almost unchanged. In the Li-ion cell using a MCMB anode and a composite cathode cycled between 2.5 V and 4.2 V, the structural changes are dominated by the spinel $LiMn_2O_4$ component, with much less changes in the layered $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, comparing with the Li-half cell results. These results give us valuable information about the structural changes relating to the contributions of each individual component to the cell capacity at certain charge/discharge state, which are helpful in designing and optimizing the composite cathode using spinel- and layered-type materials for Li-ion battery research. More detailed discussion will be presented at the meeting.
There are two beamlines (BLs), 4C1 and 4C2, at the Pohang Accelerator Laboratory that are dedicated to small angle X-ray scattering (SAXS). The 4C1 BL was constructed in early 2000 and is open to public users, including both domestic and foreign researchers. In 2003, construction of the second SAXS BL, 4C2, was complete and commissioning and user support were started. The 4C2 BL uses the same bending magnet as its light source as the 4C1 BL. The 4C1 BL uses a synthetic double multilayer monochromator, whereas the 4C2 BL uses a Si(111) double crystal monochromator for both small angle and wide angle X-ray scattering. In the 4C2 BL, the collimating mirror is positioned behind the monochromator in order to enhance the beam flux and energy resolution. A toroidal focusing mirror is positioned in front of the monochromator to increase the beam flux and eliminate higher harmonics. The 4C2 BL also contains a digital cooled charge coupled detector, which has a wide dynamic range and good sensitivity to weak scattering, thereby making it suitable for a range of SAXS and wide angle X-ray scattering experiments. The general performance of the 4C2 BL was initially tested using standard samples and further confirmed by the experience of users during three years of operation. In addition, several grazing incidence X-ray scattering measurements were carried out at the 4C2 BL.
This study aimed to fundamentally understand structural changes of zeolite under pressure and in the presence of different pressure-transmitting media (PTM) for application studies such as immobilization of heavy metal cation or CO2 storage using pressure. High-pressure X-ray powder diffraction study was conducted on the zeolite-W (K6.4Al6.5Si25.8O64× 15.3H2O, K-MER) to understand linear compressibility and the bulk moduli in different PTM conditions. Zeolite-w is a synthetic material having the same framework as natural zeolite merlinoite ((K, Ca0.5, Ba0.5, Na)10 Al10Si22O64× 22H2O). The space group of the sample was identified as I4/mmm belonging to the tetragonal crystal system. Water, carbon dioxide, and silicone-oil were used as pressure-transmitting media. The mixture of sample and each PTM was mounted in a diamond anvil cell (DAC) and then pressurized up to 3 GPa with an increment of ca. 0.5 GPa. Pressure-induced changes of powder diffraction patterns were measured using a synchrotron X-ray light source. Lattice constants, and bulk moduli were calculated using the Le-Bail method and the Birch-Murnaghan equation. In all PTM conditions, linear compressibility of c-axis (𝛽c) was 0.006(1) GPa-1 or 0.007(1) GPa-1. On the other hand, the linear compressibility of a(b)-axis (𝛽a) was 0.013(1) GPa-1 in silicone-oil run, which is twice more compressible than the a(b)-axis in water and carbon dioxide runs, 𝛽a = 0.006(1) GPa-1. The bulk moduli were measured as 50(3) GPa, 52(3) GPa, and 29(2) GPa in water, carbon dioxide, and silicone-oil run, respectively. The orthorhombicities of ac-plane in the water, and carbon dioxide runs were comparatively constant, near 0.350~0.353, whereas the value decreased abruptly in the silicone-oil run following formula, y = -0.005(1)x + 0.351(1) by non-penetrating pressure fluid condition.
Hyo-Im Kim;Sangmi Lee;Hyo-Jin Koo;Yoon Ji;Hyen-Goo Cho
Korean Journal of Mineralogy and Petrology
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v.36
no.4
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pp.303-312
/
2023
The determination of the oxidation states of metal elements in manganese nodules sheds light on the understanding of the formation mechanism of nodules, providing insights into the paleo-environmental conditions such as the redox potential of the aqueous system. This study aims to reveal the oxidation states and chemical bonding of manganese in the natural polymetallic nodules, utilizing conventional X-ray photoelectron spectroscopy (XPS). Specifically, shallow manganese nodules from the Siberian Arctic Sea, effectively recording mineralogical variations, were used in this study. Detailed analysis of XPS Mn 2p spectra showed changes in the manganese oxidation state from the center to the outer parts of the nodules. The central part of the nodules showed a higher Mn4+ content, approximately 67.9%, while the outermost part showed about 63% of Mn4+ due to an increase in the Mn3++Mn2+. The decrease in the Mn oxidation state with the growth is consistent with the previously reported mineralogical variations from todorokite to birnessite with growth. Additionally, the O 1s spectra presented a predominance of Mn-O-H bonds in the outer layers compared to the center, suggesting hydration by water in the layered manganates of outer layers. The results of this study demonstrate that XPS can be directly applied to understand changes in paleo-environmental conditions such as the redox states during the growth of manganese nodules. Finally, future studies using high-resolution synchrotron-based XPS experiments could achieve details in oxidation states of manganese and trace metal elements.
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