• Title/Summary/Keyword: electron microscope analysis

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Analysis of Crushing/Classification Process for Recovery of Black Mass from Li-ion Battery and Mathematical Modeling of Mixed Materials (폐배터리 블랙 매스(black mass) 회수를 위한 파쇄/분급 공정 분석 및 2종 혼합물의 수학적 분쇄 모델링)

  • Kwanho Kim;Hoon Lee
    • Resources Recycling
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    • v.31 no.6
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    • pp.81-91
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    • 2022
  • The use of lithium-ion batteries increases significantly with the rapid spread of electronic devices and electric vehicle and thereby an increase in the amount of waste batteries is expected in the near future. Therefore, studies are continuously being conducted to recover various resources of cathode active material (Ni, Co, Mn, Li) from waste battery. In order to recover the cathode active material, black mass is generally recovered from waste battery. The general process of recovering black mass is a waste battery collection - discharge - dismantling - crushing - classification process. This study focus on the crushing/classification process among the processes. Specifically, the particle size distribution of various samples at each crushing/classification step were evaluated, and the particle shape of each particle fraction was analyzed with a microscope and SEM (Scanning Electron Microscopy)-EDS(Energy Dispersive Spectrometer). As a result, among the black mass particle, fine particle less than 74 ㎛ was the mixture of cathode and anode active material which are properly liberated from the current metals. However, coarse particle larger than 100 ㎛ was present in a form in which the current metal and active material were combined. In addition, this study developed a PBM(Population Balance Model) system that can simulate two-species mixture sample with two different crushing properties. Using developed model, the breakage parameters of two species was derived and predictive performance of breakage distribution was verified.

A Study on the Collection and Analysis of Tire and Road Wear Particles(TRWPs) as Fine Dust Generated on the Roadside (도로변에서 발생되는 미세먼지로써 타이어와 도로 마모입자 채집과 분석 연구)

  • Kang, Tae-Woo;Kim, Hyeok-Jung
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.10 no.3
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    • pp.293-299
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    • 2022
  • Recently, various stakeholder are interested in microplastic to cause pollution of the marine's ecosystem and effort to conduct study of product's life cycle to reduce pollution of marine's ecosystem. The micorplastic refer to materials of the nano- to micro- sized units and it can be classified into primary and secondary. The primary microplastic mean the manufactured for use in the specific field such as the microbead of the cosmetic or cleanser. also, secondary mean the unintentionally generated during use of the product such as the textile crumb by the doing the laundry. Tire and Road Wear Particles(TRWPs) are also defined as secondary microplastic. Typically, TRWPs are created by friction between the tread compound's rubber of the tire and the surface of the road du ring the driving cars. Most of the generated TRWPs exist on the roadside and some of them were carried to marine by the rainwater. In this study, we perform the quantitative analysis of the TRWPs existed in fine dust at the roadside. So, we collected the dust from the roadside in Chungcheongnam-do's C site with a movement of 1,300 cars per the hour. The collected samples were separated according to size and density. And shape analysis was performed using the Scanning Electron Microscope(SEM). We were possible to discover a lot of TRWPs at the fine dust of the 100 ± 20 ㎛. And we analysis it u sing the Thermo Gravimetric Analysis(TGA) and Gas Chromatography/Mass Spectrometer(GC/MS) for the quantitative components from the tire. As a result, it was confirmed that TRWPs generated from the roadside fine dust were included the 0.21 %, and the tire and road components in the generated TRWPs consisted of the 3:7 ratio.

The Change in Geotechnical Properties of Clay Liner and the Contamination Behavior of Groundwater Due to Contaminant (오염물질에 의한 점토 차수재의 역학적 특성변화 및 지하수 오염거동)

  • Ha, Kwang-Hyun;Lee, Sang-Eun;Chung, Sung-Rae;Chun, Byung-Sik
    • Journal of Soil and Groundwater Environment
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    • v.13 no.1
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    • pp.13-23
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    • 2008
  • The triaxial compression tests and consolidation tests using NaCl solution and leachates as substitute pore (or saturated) water in samples were carried out to find out the behavior characteristics of strength, deformation and permeability coefficient of contaminated clay. Also, the chemical property analysis on the clay samples using scanning electron microscope and energy dispersive x-ray spectrometer were involved. The magnitudes of composition ratio were shown in the order of O, C, Si, Al, and Fe as a result of chemical composition analysis for clay samples. Besides, as the results of triaxial compression tests and consolidation tests, the shear strength, compression and permeability properties were increased with increasing in the concentration of contaminant (NaCl). It may be considered that these circumstances be caused by the changes of soil structure to flocculent structure due to the decrease in the thickness of diffuse double layer with increasing in the concentration of electrolyte. MT3D model was also using to grasp the procedures that the groundwater may be contaminated by the leachates permeated through the clay liner. The results of contaminant transport analysis showed a tendency that the predicted concentration of groundwater was higher with increasing in the initial concentration of $Cl^-$ ion and increased as a nonlinear curves with time. The transportation distance calculated by the use of regression equation between the distance from contaminant source and the concentration of $Cl^-$ ion was increased with increasing the initial concentration.

Modification of Silica Nanoparticles with Bis[3-(triethoxysilylpropyl)]tetrasulfide and Their Application for SBR Nanocomposite (Bis[3-(triethoxysilylpropyl)]tetrasulfide에 의한 실리카 입자의 표면개질 반응과 SBR 나노 복합체 응용)

  • Ryu, Hyun Soo;Lee, Young Seok;Lee, Jong Cheol;Ha, KiRyong
    • Polymer(Korea)
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    • v.37 no.3
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    • pp.308-315
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    • 2013
  • In this study, we performed surface modification of silica nanoparticles with bis[3-(triethoxysilylpropyl)]tetrasulfide (TESPT) silane coupling agent to study the effects of treatment temperature, treatment time, and amount of TESPT used on the silanization degree with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), elemental analysis (EA) and solid state $^{13}C$ and $^{29}Si$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR). We found peak area of isolated silanol groups at $3747cm^{-1}$ decreased, but peak area of $-CH_2$ asymmetric stretching of TESPT at $2938cm^{-1}$ increased with the amount of TESPT from FTIR measurements. We also used universal testing machine (UTM) to study mechanical properties of styrene butadiene rubber (SBR) nanocomposites with 20 phr (parts per hundred of rubber) of pristine and TESPT modified silicas, respectively. The tensile strength and 100% modulus of modified silica/SBR nanocomposite were enhanced from 5.65 to 9.38MPa, from 1.62 to 2.73 MPa, respectively, compared to those of pristine silica/SBR nanocomposite.

The effect of low temperature aging on the mechanical property & phase stability of Y-TZP ceramics

  • Kim, Hyung-Tae;Han, Jung-Suk;Yang, Jae-Ho;Lee, Jai-Bong;Kim, Sung-Hun
    • The Journal of Advanced Prosthodontics
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    • v.1 no.3
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    • pp.113-117
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    • 2009
  • STATEMENT OF PROBLEM. Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported. PURPOSE. The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM). MATERIAL AND METHODS. Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad $S\ddot{a}ckingen$, Germany) were prepared in 40 mm (length) $\times$ 4 mm (width) $\times$ 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and $225^{\circ}C$ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences ($\alpha$= .05). RESULTS. The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below $125^{\circ}C$ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above $150^{\circ}C$, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa. CONCLUSION. The monoclinic phase started to appear after aging treatment above $100^{\circ}C$. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above $175^{\circ}C$. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

Expansion Behavior of Aggregate of Korea due to Alkali-Silica Reaction by ASTM C 1260 Method (ASTM C 1260 실험에 의한 국내 골재의 알칼리-실리카 반응 팽창 특성)

  • Yun, Kyong-Ku;Hong, Seung-Ho;Han, Seung-Hwan
    • Journal of the Korea Concrete Institute
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    • v.20 no.4
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    • pp.431-437
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    • 2008
  • The concrete pavement at Seohae Expressway in Korea has suffered from serious distress, only after four to seven years of construction. The deterioration of ASR has seldom been reported per se in Korea, because the aggregate used for the cement concrete has been considered safe against alkali-silica reaction so far. The purpose of this study is to examine the expansion behavior of aggregates of Korea due to alkali-silica reaction by ASTM C 1260 standard method of the accelerated mortar bar test (AMBT), stereo microscopic analysis, scanning electronic microscope (SEM) analysis, and electron dispersive X-ray spectrometer (EDX) analysis. The results are presented as it follows. The accelerated mortar bar test (AMBT) showed that mica granite and felsite of igneous rocks, aroke, red sandstone and shale of sedimentary rocks, slate of metamorphic rock, and dendrite and quartz of mineral rock showed more expansion than 0.1% at 14 days. But, some sedimentary rocks and metamorphic rocks expanded more than 0.1% at 28 days even though they were less than 0.1% at 14 days. The mortar bars, which showed more than occurred 0.1% expansion, resulted in cracking on surface. SEM and EDX analysis confirmed that the white gel was a typical reaction product of ASR. The ASR gel in Korea mainly consisted of Silicate (Si) and Potassium (K) from the cement. The crack in the concrete pavement was caused by ASR. It seems that Korea is no longer safe zone against alkali-silica reaction.

CO2 Sequestration and Utilization of Calcium-extracted Slag Using Air-cooled Blast Furnace Slag and Convert Slag (괴재 및 전로슬래그를 이용한 CO2 저감 및 칼슘 추출 후 슬래그 활용)

  • Yoo, Yeongsuk;Choi, Hongbeom;Bang, Jun-Hwan;Chae, Soochun;Kim, Ji-Whan;Kim, Jin-Man;Lee, Seung-Woo
    • Applied Chemistry for Engineering
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    • v.28 no.1
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    • pp.101-111
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    • 2017
  • Mineral carbonation is a technology in which carbonates are synthesized from minerals including serpentine and olivine, and industrial wastes such as slag and cement, of which all contain calcium or magnesium when reacted with carbon dioxide. This study aims to develop the mineral carbonation technology for commercialization, which can reduce environmental burden and process cost through the reduction of carbon dioxide using steel slag and the slag reuse after calcium extraction. Calcium extraction was conducted using NH4Cl solution for air-cooled slag and convert slag, and ${\geq}98%$ purity calcium carbonate was synthesized by reaction with calcium-extracted solution and carbon dioxide. And we conducted experimentally to minimize the quantity of by-product, the slag residue after calcium extraction, which has occupied large amount of weight ratio (about 80-90%) at the point of mineral carbonation process using slag. The slag residue was used to replace silica sand in the manufacture of cement panel, and physical properties including compressive strength and flexible strength of panel using the slag residue and normal cement panel, respectively, were analyzed. The calcium concentration in extraction solution was analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES). Field-emission scanning electron microscope (FE-SEM) was also used to identify the surface morphology of calcium carbonate, and XRD was used to analyze the crystallinity and the quantitative analysis of calcium carbonate. In addition, the cement panel evaluation was carried out according to KS L ISO 679, and the compressive strength and flexural strength of the panels were measured.

Microstructure of ZnO Thin Film on Nano-Scale Diamond Powder Using ALD (나노급 다이아몬드 파우더에 ALD로 제조된 ZnO 박막 연구)

  • Park, S.J.;Song, S.O.
    • Journal of the Korean Vacuum Society
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    • v.17 no.6
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    • pp.538-543
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    • 2008
  • Recently a nano-scale diamond is possible to manufacture forms of powder(below 100 nm) by new processing of explosion or deposition method. Using a sintering of nano-scale diamond is possible to manufacture of grinding tools. We have need of a processing development of coated uniformly inorganic to prevent an abnormal grain growth of nano-crystal and bonding obstacle caused by sintering process. This paper, in order to improve the sintering property of nano-scale diamond, we coated ZnO thin films(thickness: $20{\sim}30\;nm$) in a vacuum by ALD(atomic layer deposition) Economically, in order to deposit ZnO all over the surface of nano-scale diamond powder, we used a new modified fluidized bed processing replaced mechanical vibration effect or fluidized bed reactor which utilized diamond floating owing to pressure of pulse(or purge) processing after inserted diamond powders in quartz tube(L: 20 mm) then closed quartz tube by porosity glass filter. We deposited ZnO thin films by ALD in closed both sides of quartz tube by porosity glass filter by ALD(precursor: DEZn($C_4H_{10}Zn$), reaction gas: $H_2O$) at $10^{\circ}C$(in canister). Processing procedure and injection time of reaction materials set up DEZn pulse-0.1 sec, DEZn purge-20 sec, $H_2O$ pulse-0.1 sec, $H_2O$ purge-40 sec and we put in operation repetitive 100 cycles(1 cycle is 4 steps) We confirmed microstructure of diamond powder and diamond powder doped ZnO thin film by TEM(transmission electron microscope) Through TEM analysis, we confirmed that diamond powder diameter was some $70{\sim}120\;nm$ and shape was tetragonal, hexagonal, etc before ALD. We confirmed that diameter of diamond powders doped ZnO thin film was some $70{\sim}120\;nm$ and uniform ZnO(thickness: $20{\sim}30\;nm$) thin film was successfully deposited on diamond powder surface according to brightness difference between diamond powder and ZnO.

The Characterization of Spherical Perticles in Steam Generator Sludge (증기발생기 슬러지 중 구형입자의 특성 조사)

  • Pyo, Hyung-Yeal;Park, Yang-Soon;Park, Sun-Dal;Park, Kyoung-Kyun;Song, Byung-Chul;Park, Yong-Joon;Jee, Kwang-Yong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.4 no.1
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    • pp.59-64
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    • 2006
  • Ion exchange resin particles should not be found in steam generator(S/G) sludge. The suspicious spherical resin particles observed in S/G sludge sample were characterized for particle size distribution under optical microscope using the micro-technique, for element analysis by the electron probe micro analysis (EPMA), and for molecular identification by the IR spectroscopy. The particle sizes are distributed from 1 to $200{\mu}m$ for the sludge, while 40 to $500{\mu}m$ for the spherical resin particles. The results of the elemental analysis showed different major impurities: Si, Al, Mn, Cr, Ni, Zn and Ti for the sludge particles, while Si, Cu, Zn for the spherical resin particles. However, both particles contain Fe as a matrix of magnetite $(Fe_3O_4)$. IR spectrum of the spherical particles was not quite similar to the IR spectrum of ion exchange resins used in S/G system. These results indicate that the spherical particles are not related to ion exchange resin particles and may be formed by the process of the sludge formation.

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Determination of stoichiometric Ca/P ratio in biphasic calcium phosphates using X-ray diffraction analysis (X-선 회절분석을 이용한 biphasic calcium phosphate 분말의 화학양론적 Ca/P 비율 확인)

  • Song, Yong-Keun;Kim, Dong-Hyun;Kim, Tae-Wan;Kim, Yang-Do;Park, Hong-Chae;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.2
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    • pp.93-100
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    • 2010
  • The calcium to phosphate ratio (Ca/P) in biphasic calcium phosphates powders using X-ray diffraction analysis (XRD) was characterized. The BCP powders with various stoichiometric Ca/P molar ratio were synthesized with coprecipitation process and calcination. Compositions of the powders with Ca/P molar ratio between 1.5 and 1.67 were subjected to starting Ca/P molar ratio, pH = 10, and thermal treatment up to $900^{\circ}C$. The structural, morphological and chemical characterizations for BCP powders with stoichiometric Ca/P ratio were carried out with scanning electron microscope (SEM) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) and a phase quantification was investigated by XRD. The solubility of HAp, $\beta$-TCP, and BCP powders was tested in the phosphate buffer solution (PBS) at $36.5^{\circ}C$ and pH = 7.4.