• Title/Summary/Keyword: Al impurity

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A resistivity anomaly at 380 K in reproduced LK-99

  • Sangjin Kim;Kwang-Tak Kim;Jeonghun Kang;Dong-Hyeon Gim;Yoon Han Lee;Kee Hoon Kim
    • Progress in Superconductivity and Cryogenics
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    • v.25 no.4
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    • pp.10-13
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    • 2023
  • To confirm the room-temperature superconductivity at ambient pressure as claimed in recent arXiv preprints by Lee et al., we followed the original authors' systematic solid-state synthesis recipe to reproduce Cu-doped Pb-apatite, known as LK-99. Using X-ray diffraction and Raman spectroscopy, we identified inclusion of various impurities alongside the apatite phase in our sample. While the sample exhibited an overall semiconducting behavior in electrical transport, an intriguing resistivity anomaly at 380 K was observed, possibly originating from a structural phase transition of the Cu2-δS impurity. Based on the transport and magnetization measurements, we conclude that the sample is a non-magnetic semiconductor, with absence of superconductivity.

Hydrogen Reduction Behavior of NCM-based Lithium-ion Battery Cathode Materials (NCM계 리튬이온 배터리 양극재의 수소환원 거동)

  • So-Yeong Lee;So-Yeon Lee;Dae-Hyeon Lee;Ho-Sang Sohn
    • Journal of Powder Materials
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    • v.31 no.2
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    • pp.163-168
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    • 2024
  • As the demand for lithium-ion batteries for electric vehicles is increasing, it is important to recover valuable metals from waste lithium-ion batteries. In this study, the effects of gas flow rate and hydrogen partial pressure on hydrogen reduction of NCM-based lithium-ion battery cathode materials were investigated. As the gas flow rate and hydrogen partial pressure increased, the weight loss rate increased significantly from the beginning of the reaction due to the reduction of NiO and CoO by hydrogen. At 700 ℃ and hydrogen partial pressure above 0.5 atm, Ni and Li2O were produced by hydrogen reduction. From the reduction product and Li recovery rate, the hydrogen reduction of NCM-based cathode materials was significantly affected by hydrogen partial pressure. The Li compounds recovered from the solution after water leaching of the reduction products were LiOH, LiOH·H2O, and Li2CO3, with about 0.02 wt% Al as an impurity.

Investigation on the phonon behavior of MgB2 films via polarized Raman spectra

  • R. P. Putra;J. Y. Oh;G. H. An;H. S. Lee;B. Kang
    • Progress in Superconductivity and Cryogenics
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    • v.26 no.1
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    • pp.14-19
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    • 2024
  • In this study, we explore the anisotropy of electron-phonon coupling (EPC) constant in epitaxially grown MgB2 films on c-axis oriented Al2O3, examining its correlation with the critical temperature (Tc) and local structural disorder assessed through polarized Raman scattering. Analysis of the polarized Raman spectra reveals angle-dependent variations in the intensity of the phonon spectra. The Raman active mode originating from the boron plane, along with two additional phonon modes from the phonon density of states (PDOS) induced by lattice distortion, was distinctly observed. Persistent impurity scattering, likely attributed to oxygen diffusion, was noted at consistent frequencies across all measurement angles. The EPC values derived from the primary Raman active phonon do not significantly vary with changing observation angles, followed by that the Tc values calculated using the Allen and Dynes formula remain relatively constant across all polarization angles. Although the E2g phonon mode plays a crucial role in the EPC mechanism, the determination of Tc values in MgB2 involves not only electron-E2g coupling but also contributions from other phonon modes.

Scaling up Hydrothermal Synthesis of Na-A Type Zeolite from Natural Siliceous Mudstone and Its Heavy Metal Adsorption Behavior (규질 이암으로부터 Na-A형 제올라이트의 scale-up 수열합성 및 중금속흡착)

  • Bae, In-Kook;Jang, Young-Nam;Shin, Hee-Young;Chae, Soo-Chun;Ryu, Kyoung-Won
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.4
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    • pp.341-347
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    • 2008
  • The feasibility of commercializing the hydrothermal synthesis of Na-A type zeolite from siliceous mudstone has been conducted using a 50-liter bench-scale autoclave and the application of the zeolite as an environmental remediation agent. Siliceous mudstone, which is widely distributed around the Pohang area, was adopted as a precursor. The siliceous mudstone is favorable for the synthesis of zeolite because it contains 70.7% $SiO_2$ and 10.0% $Al_2O_3$, which are major ingredient of zeolite formation. The synthesis of zeolite was carried out under the following conditions that had been obtained from the previous laboratory-scale tests: 10hr reaction time, $80^{\circ}C$ reaction temperature, $Na_2O/SiO_2$ ratio = 0.6, $SiO_2/Al_2O_3$ ratio = 2.0 and $H_2O/Na_2O$ ratio= 98.6. The crystallinity and morphology of the zeolite formed were similar to those obtained from the laboratory-scale tests. The recovery and cation exchange ion capacity were 95% and 215 cmol/kg, respectively, which are slightly higher than those obtained in laboratory scale tests. To examine the feasibility of the zeolite as an environmental remediation agent, experiments for heavy metal adsorption to zeolite were conducted. Its removal efficiencies of heavy metals in simulated waste solutions decreased in the following sequences: Pb > Cd > Cu = Zn > Mn. In a solution of 1500 mg/L total impurity metals, the removal efficiencies for these impurity metals were near completion (> 99%) except for Mn whose efficiency was 98%. Therefore, the synthetic Na-A type zeolite was proven to be a strong absorbent effective for removing heavy metals.

Microstructure and Strength of Class F Fly Ash based Geopolymer Containing Sodium Sulfate as an Additive (황산나트륨 첨가제에 따른 플라이애시 기반 지오폴리머의 미세구조 및 강도 특성)

  • Jun, Yubin;Oh, Jae-Eun
    • Journal of the Korea Concrete Institute
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    • v.27 no.4
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    • pp.443-450
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    • 2015
  • This paper presents an investigation of the mechanical and microstructural properties of Class F fly ash based geopolymer containing sodium sulfate as an additive. Sodium sulfate was used as an chemical additive at the dosage levels of 0, 2, 4, and 6wt% of fly ash. Sodium hydroxide and sodium silicate solutions were used to activate fly ash. The compressive strengths of geopolymer pastes were measured at the age of 28 days. The microstructures of the geopolymer pastes were examined using XRD, MIP and SEM tests. The additions of 2wt% and 4wt% sodium sulfate produced geopolymers with high strength, while increasing the dosage of levels to 6% resulted in almost no changes in strength, comparing with the control geopolymer. The optimum increase in strength was obtained with the addition of 4wt% sodium sulfate. As the amount of sodium sulfate is increased, no additional crystalline phase was detected and no change of amorphous phase indicated despite the change in the strength development. The increase in the strength was due to the change of pore size distribution in samples. As addition of sodium sulfate altered the morphologies of reactive productions and Si/Al ratios of the reaction products, the strengths were thus affected. It was found that the strengths of geopolymer were larger for lower Si/Al ratios of reaction products formed in samples. The optimal amount of sodium sulfate in the fly ash based geopolymer helps to improve mechanical properties of the geopolymer, on the other hand, the high percentage of sodium sulfate could exist as an impurity in the geopolymer and hinder the geopolymer reaction.

A Study on Types and Reasons of Engine Troubles Related to Fuel Oil (연료유에 의한 선박 디젤엔진 손상에 관한 연구)

  • Na, Eun-Young;Baik, Shin-Young
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.12 no.3
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    • pp.143-150
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    • 2009
  • Fuel oil mostly used for a ship is made from crude oil by refining process. In order to produce plenty of high-quality fuel oil, the Fluid catalytic cracking(FCC) method is widely adopted to many refinery factories during the decomposition process from high molecule into lower molecule. The major constituents in spent FCC catalysts are Si, Al, Fe, Ti, alkali metals and some others. The spent catalyst is also composed small amounts of rare metals such as Ce, Nd, Ni and V. The big problem in FCC oil is mixing the catalyst in the oil. This reason is unstable separation of FCC catalyst in separator. Such a FCC catalyst will become a reason of heavy wear down in moving parts of engine. The impurity in oil is ash and deposit compound, such as Al, Si, Ni, Fe and V, which will accelerate the wear down on fuel pump, fuel injection valve cylinder liner and piston ring. It is important to find a basic reason of an engine trouble for preventing similar troubles anymore. Insurance compensation will be different according to the reason of an engine trouble which might be natural abrasion or other external causes. In this study, types and reasons of engine troubles related to fuel oil will be covered.

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Impurity analysis and acid leaching purification of silica minerals (실리카광물의 산침출 정제와 불순물 분석법 연구)

  • Lee, Kil Yong;Yoon, Yoon Yeol;Cho, Soo Young;Chae, Young-Bae
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.516-523
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    • 2007
  • Purification of silica mineral has been investigated by acid leaching of pulverized silica. A series of studies has been carried out on the effect of leaching silica powder as a function of the leaching time at the constant temperature of $80^{\circ}C$ in oxalic acid, aqua regia, and two mixed acids of HF/HCl, $HF/HNO_3$. The impurities of silica and leachantes were measured by neutron activation analysis (NAA), inductively coupled plasma atomic emission spectrometry (ICP-AES), atomic absorption spectrometry, x-ray fluorescence (XRF) method and wet analysis (WA). Certain metals, such as sodium, calcium, iron, aluminium and titanium, have been found in concentrations of hundreds or even thousands of mg/kg. Comparison of purification processes of silica and analytical methods of impurities in the silica was conducted in this study.

Chemical and TEM Studies of Chklorites in the Talc Deposites of the Chungnam Area, Korea (우리나라 충남지역 활석광상에서 산출되는 녹니석의 화학적 및 투과전자현미경 연구)

  • Geon-Young Kim;Soo Jin Kim
    • Journal of the Mineralogical Society of Korea
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    • v.13 no.2
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    • pp.53-64
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    • 2000
  • Chlorite from the talc deposits in the Chungnam area, Korea, has been studied using electron microprobe analysis and high resolution transmission electron microscopy (HRTEM), Talc orea are hydrothermal alteration products of serpentinite which was originated from ultramafic rocks. Chlorite occurs in close association with talc ores of with the black alteration zone between talc ore bodies and granitic gneiss. It is the most abundant impurity mineral of talc ores. Chlorite in association with talc is characterized by very high but narrow variation in Mg/(Mg+Fe) ratios (0.784~0.951), significant octahedral substitution (-0.200~0.692), wide variation in Al contents (1.085~3.160 / 14 oxygens), and high Cr and Ni contents. It was formed under a very limited but high Mg/(Mg+Fe) condition in close connection with serpentinite. Chlorite in the black alteration zone is characterized by a high Fe content, wide variation in Mg/(Mg+Fe) ratios (0.378~0.852), narrow octahedral substitution (-0.035~0.525), high narrow Al contents (1.468~2.959), and low Cr and Ni contents. It was formed under a low Mg/(Mg+Fe) and relatively Al-rich condition in close connection with county rocks. Two different chemical modes for chlorite suggest two different origins for two different chlorites. Although most of chlorites show typical 14-$\AA$ lattice fringe images under HRTEM, some chlorites show fringe images of 21-$\AA$ (14$\AA$+7$\AA$) spacings within (001) lattice-fringe images of chlorite (14$\AA$). But brown chlorite from the black zone has high Ti and K contents suggesting that mica was the precursor of brown chlorite. Such possibility is also supported by the fact that lattice-fringe images of brown chlorite show 14-$\AA$ chlorite layers in which 10-$\AA$ mica single layer or packets are interlayered. Partial terminations from 3 mica layers to 2 chlorite layers are often observed. It, therefore, is suggested that the chlorite associated with talc ores is a hydrothermal alteration products of serpentinite, whereas the chlorites in the black alteration zone is a hydrothermal alteration product of granitic gnesis under a partial influence of serpentinite.

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Synthesis of Nano-Sized Y3Al5O12:Ce3+ Phosphors Prepared by High Energy Beads Milling Process and Their Luminescence Properties

  • Song, Hee-Jo;Kim, Dong-Hoe;Park, Jong-Hoon;Han, Byung-Suh;Hong, Kug-Sun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.386-386
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    • 2012
  • For white light emitting diode (LED) applications, it has been reported that Y3Al5O12:Ce3+ (YAG:Ce) in nano-sized phosphor performs better than it does in micro-sized particles. This is because nano-sized YAG:Ce can reduce internal light scattering when coated onto a blue LED surface. Recently, there have been many reports on the synthesis of nano-sized YAG particles using bottom-up method, such as co-precipitation method, sol-gel process, hydrothermal method, solvothermal method, and glycothermal method. However, there has been no report using top-down method. Top-down method has advantages than bottom-up method, such as large scale production and easy control of doping concentration and particle size. Therefore, in this study, nano-sized YAG:Ce phosphors were synthesized by a high energy beads milling process with varying beads size, milling time and milling steps. The beads milling process was performed by Laboratory Mill MINICER with ZrO2 beads. The phase identity and morphology of nano-sized YAG:Ce were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM), respectively. By controlling beads size, milling time and milling steps, we synthesized a size-tunable and uniform nano-sized YAG:Ce phosphors which average diameters were 100, 85 and 40 nm, respectively. After milling, there was no impurity and all of the peaks were in good agreement with YAG (JCPDS No. 33-0040). Luminescence and quantum efficiency (QE) of nano-sized YAG:Ce phosphors were measured by fluorescence spectrometer and QE measuring instrument, respectively. The synthesized YAG:Ce absorbed light efficiently in the visible region of 400-500 nm, and showed single broadband emission peaked at 550 nm with 50% of QE. As a result, by considering above results, high energy beads milling process could be a facile and reproducible synthesis method for nano-sized YAG:Ce phosphors.

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Plasma Etching Characteristics of Sapphire Substrate using $BCl_3$-based Inductively Coupled Plasma ($BCl_3$ 계열 유도결합 플라즈마를 이용한 사파이어 기판의 식각 특성)

  • Kim, Dong-Pyo;Woo, Jong-Chang;Um, Doo-Seng;Yang, Xue;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.363-363
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    • 2008
  • The development of dry etching process for sapphire wafer with plasma has been key issues for the opto-electric devices. The challenges are increasing control and obtaining low plasma induced-damage because an unwanted scattering of radiation is caused by the spatial disorder of pattern and variation of surface roughness. The plasma-induced damages during plasma etching process can be classified as impurity contamination of residual etch products or bonding disruption in lattice due to charged particle bombardment. Therefor, fine pattern technology with low damaged etching process and high etch rate are urgently needed. Until now, there are a lot of reports on the etching of sapphire wafer with using $Cl_2$/Ar, $BCl_3$/Ar, HBr/Ar and so on [1]. However, the etch behavior of sapphire wafer have investigated with variation of only one parameter while other parameters are fixed. In this study, we investigated the effect of pressure and other parameters on the etch rate and the selectivity. We selected $BCl_3$ as an etch ant because $BCl_3$ plasmas are widely used in etching process of oxide materials. In plasma, the $BCl_3$ molecule can be dissociated into B radical, $B^+$ ion, Cl radical and $Cl^+$ ion. However, the $BCl_3$ molecule can be dissociated into B radical or $B^+$ ion easier than Cl radical or $Cl^+$ ion. First, we evaluated the etch behaviors of sapphire wafer in $BCl_3$/additive gases (Ar, $N_2,Cl_2$) gases. The behavior of etch rate of sapphire substrate was monitored as a function of additive gas ratio to $BCl_3$ based plasma, total flow rate, r.f. power, d.c. bias under different pressures of 5 mTorr, 10 mTorr, 20 mTorr and 30 mTorr. The etch rates of sapphire wafer, $SiO_2$ and PR were measured with using alpha step surface profiler. In order to understand the changes of radicals, volume density of Cl, B radical and BCl molecule were investigated with optical emission spectroscopy (OES). The chemical states of $Al_2O_3$ thin films were studied with energy dispersive X-ray (EDX) and depth profile anlysis of auger electron spectroscopy (AES). The enhancement of sapphire substrate can be explained by the reactive ion etching mechanism with the competition of the formation of volatile $AlCl_3$, $Al_2Cl_6$ or $BOCl_3$ and the sputter effect by energetic ions.

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