• Title/Summary/Keyword: interlayer spacing

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Calcium annealing approach to control of surface groups and formation of oxide in Ti3C2Tx MXene

  • Jung-Min Oh;Su Bin Choi;Taeheon Kim;Jikwang Chae;Hyeonsu Lim;Jae-Won Lim;In-Seok Seo;Jong-Woong Kim
    • Advances in nano research
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    • v.15 no.1
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    • pp.1-13
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    • 2023
  • Ti3C2Tx MXene, a 2D material, is known to exhibit unique characteristics that are strongly dependent on surface termination groups. Here, we developed a novel annealing approach with Ca as a reducing agent to simultaneously remove F and O groups from the surface of multilayered MXene powder. Unlike H2 annealing that removes F effectively but has difficulty in removing O, annealing with Ca effectively removed both O and F. X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy revealed that the proposed approach effectively removed F and O from the MXene powder. The results of O/N analyses showed that the O concentration decreased by 57.5% (from 2.66 to 1.13 wt%). In addition, XPS fitting showed that the volume fraction of metal oxides (TiO2 and Al2O3) decreased, while surface termination groups (-O and -OH) were enhanced, which could increase the hydrophilic and adsorption properties of the MXene. These findings suggest that when F and O are removed from the MXene powder, the interlayer spacing of its lattice structure increases. The proposed treatment also resulted in an increase in the specific surface area (from 5.17 to 10.98 m2/g), with an increase in oxidation resistance temperature in air from ~436 to ~667 ℃. The benefits of this novel technology were verified by demonstrating the significantly improved cyclic charge-discharge characteristics of a lithium-ion battery with a Ca-treated MXene electrode.

Structures and Double Layer Performances of Carbons Pyrolized from Carbon Oxides (산화탄소로부터 열분해한 탄소의 구조 및 전기이중층 거동)

  • Kim, Ick-Jun;Yang, Sunhye;Jeon, Min-Je;Moon, Seong-In;Kim, Hyun-Soo;An, Kye-Hyeok
    • Applied Chemistry for Engineering
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    • v.18 no.5
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    • pp.522-526
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    • 2007
  • Structural features and electrochemical performances of cokes pyrolized from oxidized cokes were examined, and compared with KOH-activated coke. Needle cokes ($d_{002}=3.5{\AA} $), having a graphene layer structure, were changed to a single phase of graphite oxide after oxidation treatment with an acidic solution having an $NaCLO_3$/needle coke composition ratio of above 7.5, and the inter-layer distance of the oxidized coke was expanded to $6.9{\AA} $ with increasing oxygen content. After heating at $200^{\circ}C$, the oxidized coke was pyrolized to the graphene layer structure with inter-layer distance of $3.6{\AA} $. However, the change of the inter-layer distance of the needle coke was not observed in the KOH activation process. On the other hand, an intercalation of electrolyte ions into the pyrolized coke, observed at first charge, occurred at 1.0 V, in which the value was lower than that of KOH-activation coke. The cell capacitor using pyrolized coke exhibited a lower internal resistance of $0.57{\Omega}$ in 1 kHz, and a larger capacitance per weight and volume of 30.3 F/g and 26.9 F/ml at the two-electrode system in the potential range 0~2.5 V than those of the cell capacitor using KOH-activation of coke. This better electrochemical performance may be associated with structure defects in the graphene layer derived from the process of the inter-layer expansion and shrinkage.

The Characteristics of Mesophase Pitch Prepared by Heterogeneous Fluorination Process from Pyrolysis Fuel Oil (열분해잔사유로부터 불균일계 불소화공정에 의해 제조된 메조페이스 피치의 특성)

  • Kim, Do Young;Kim, Ji-Hyun;Lee, Hyung-Ik;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.27 no.5
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    • pp.537-542
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    • 2016
  • In this study, we have prepared mesophase pitch from pyrolysis fuel oil (PFO) by heterogeneous reforming process. This process was conducted by direct fluorination at various temperature and followed by the heat treatment at $390^{\circ}C$. The reformed pitch was then investigated by softening point analysis, elemental analysis, fourier-transform infrared spectroscopy, high resolution X-ray diffraction and polarization microscope analysis. Carbon contents of reformed pitch increased according to increasing the reaction temperature of fluorination, while oxygen, nitrogen and sulfur contents were completely eliminated. As the fluorination temperature increased, the creation, growth, coalescence and alignment process of mesophase spheres were observed. Also the interlayer spacing of carbon hexagonal planar structure decreased, while its crystalline size increased. In addition, aromatic ring compound contents increased by the condensation polymerization of aliphatic compound. These results can be attributed to the radical reactivity of the fluorine increased as the reaction temperature increased. It was considered that the fluorination reaction could help PFO to generate aromatic compounds, via promoting polymerization by radical reaction.

Synthesis of Nanoporous NiO-SiO2 Pillared Clays and Surface Modification of the Pillaring Species (나노다공성 NiO-SiO2 가교화 점토의 합성 및 가교물질의 표면개질 연구)

  • Yoon, Joo-Young;Shim, Kwang-Bo;Moon, Ji-Woong;Oh, You-Keun
    • Journal of the Korean Ceramic Society
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    • v.41 no.1
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    • pp.81-85
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    • 2004
  • Nanoporous materials with nanometer-sized pores, are of great interest in the various applications such as selective adsorbents, heterogeneous catalysts and catalyst supports because of their high porosity, surface area, and size selective adsorption properties. This study is aimed to prepare nanoporous catalytic materials on the basis of two-dimersional clay by pillaring of $SiO_2$ sol particles. $SiO_2$ Pillared Montmorillonite (Si-PILM) was prepared by ion exchanging the interlayer $Ni^{2+}$ ions of clay with $SiO_2$ nano-sized particles of which the surface was modified with nicked polyhydroxy cations sach as $Ni_4(OH)_4^{4+}$. Nano-sized $SiO_2$ particles were formed by the controlled hydrolysis of tetraethyl orthosilicate (TEOS). Upon pillaring of $Ni^+$-modified $SiO_2$ nano particles between the clay layers, the basal spacing was expanded largely to $45{\AA}$ and the extremely large specific surface area ($S_{BET}$) of $760m^2/g$ was obtained.

Behavior Evaluation of Thin Bonded Continuously Reinforced Concrete Overlay on Aged Jointed Concrete Pavement(2) (노후 줄눈 콘크리트 포장 보수를 위한 얇은 연속 철근 콘크리트 덧씌우기 포장의 거동 평가(2))

  • Ryu, Sung-Woo;Cho, Yoon-Ho
    • International Journal of Highway Engineering
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    • v.12 no.4
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    • pp.101-110
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    • 2010
  • In this paper, it has been studied about the CRCO to maintain or rehabilitate the aged JCP. The CRCO and JCO was constructed at useless section of Seo-Hae-Ahn express highway in South Korea. The performance evaluation was conducted. Especially, it was focused on the roll of longitudinal reinforced steels inserted into the CRCO. On crack survey results from field construction section, the reflection cracks at joint of the existing pavement occurred in CRCO. However, due to the constraints of longitudinal reinforced steels, crack width was small. Total crack length and quantity in the CRCO more than that in the JCO. And crack spacing in the CRCO was narrower than it in the CRCP. Through the bonding strength test results, if the cold milling and cleaning as well as surface treatment is applied, there will be no debonding problem at interlayer in the early age. From analysis of the horizontal behavior at the joint, the longitudinal reinforced steels constrained crack width which became wider than initial state over time. Also, that steel in the CRCO reduced the horizontal movement due to temperature variation(4 times than that in the JCO). But, if interface is debonded, the roll decreased. Vertical VWG data showed that CRCO did not occur debonding problem at steel location, but there was some problem in JCO. It was confirmed by field coring. The tensile strain appeared in the CRCO, But the compressive strain occurred in the JCO in early age. Through the FWD test result, deflection in the CRCO was less than that in the JCO. And K value in the CRCO was greater than it in the JCO.

Properties on the Strength of Polymer Concrete Using Nano MMT-UP Composite (나노 MMT-폴리머 복합체를 이용한 폴리머 콘크리트의 강도 특성)

  • Jo, Byung-Wan;Moon, Rin-Gon;Park, Seung-Kook
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.4A
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    • pp.761-766
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    • 2006
  • Polymer composite are increasingly considered as structural components for use in civil engineering, on account of their enhanced strength-to-weight ratios. Unsaturated polyester (UP) resin have been widely used for the matrix of composites such as FRP and polymer composite, due to its excellent adhesive. Polymer nanocomposites are new class of composites derived from the nano scale inorganic particles with dimensions typically in the range of 1 to 1000 nm that are dispersed in the polymer matrix homogeneously. Owing to the high aspect ratio of the fillers, mechanical, thermal, flame, retardant and barrier properties are enhanced without significant loss of clarity, toughness or impact strength. To prepare the MMT (Montmorillonite)-UP exfoliated nanocomposites, UP was mixed with MMT at $60^{\circ}C$ for 3 hours by using pan mixer. XRD (X-ray diffraction) pattern of the composites and TEM (Transmission Electron Micrographs) showed that the interlayer spacing of the modified MMT were exfoliated in polymer matrix. The mechanical properties also supported these findings, since in general, tensile strength, modulus with modified MMT were higher than those of the composites with unmodified MMT. The thermal stability of MMT-UP nanocomposite is better than that of pure UP, and its glass transition temperature is higher than that of pure UP. The polymer concrete made with MMT-UP nanocomposite has better mechanical properties than of pure UP. Therefore, it is suggested that strength and elastic modulus of polymer concrete was found to be positively tensile strength and tensile modulus of the MMT-UP nanocomposites.

Study of Iodide Adsorption on Organobentonite using X-ray Absorption Spectroscopy (X-선 흡수분광기를 이용한 유기벤토나이트의 요오드 흡착연구)

  • Yoon, Ji-Hae;Ha, Ju-Young;Hwang, Jin-Yeon;Hwang, Byoung-Hoon;Gordon E. Brown, Jr.
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.1
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    • pp.23-34
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    • 2009
  • The adsorption of iodide on untreated bentonite and bentonites modified with organic cation (i.e., hexadecylpyridinium chloride monohydrate ($HDP^+$)) was investigated, and the organobentonites were characterized using uptake measurements, ${\mu}$-XRD, and electrophoretic mobilities measurement. Uptake measurements indicate that bentonite has a high affinity for $HDP^+$. Our ${\mu}$-XRD study indicates that organobentonites significantly expanded in basal spacing and organic cations were substantially intercalated into the interlayer spaces of bentonite. The electrophoretic mobility indicates that organobentonite tht is modified with organic cations in excess of the CEC of bentonite is completely different from untreated bentonite in the surface charge distribution. We found significant differences in adsorption capacities of iodide depending on the bentonite properties as follows: iodide adsorption capacities were 439 mmol/kg for the bentonite modified with $HDP^+$ at an equivalent amount corresponding to 200% of the CEC of bentonite whereas no adsorption of iodide was observed for the untreated bentonite. The molecular environments of iodine adsorbed on organobentonites were further studied using I K-edge and $L_{III}$-edge x-ray absorption spectroscopy (XAS). The X-ray absorption near-edge structure (XANES) of iodine spectra from organobentonites was similar to that of KI reference solution. Linear combination fitting of EXAFS data suggests the fraction of iodine reacted with the organic compound increased with increasing loading of the organic compound on organobentonites. In this study, we observed significant differences in the adsorption environments of iodide depending on the modified property of bentonite and suggest that an organobentonite has potential as reactive barrier material around a nuclear waste repository containing anionic radioactive iodide.