• Title/Summary/Keyword: in-situ XRD

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Solvothermal Synthesis and Gas Permeation Properties of Nanoporous HKUST-1 Membranes (용매열합성법에 의한 나노기공 HKUST-1 막의 제조 및 기체투과 특성)

  • Noh, Seung-Jun;Kim, Jinsoo
    • Membrane Journal
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    • v.22 no.6
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    • pp.435-440
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    • 2012
  • In this study, nanoporous HKUST-1 membranes were synthesized by solvothermal method. It is very difficult to prepare uniform and crack-free HKUST-1 layer on macroporous alumina support by in-situ solvothermal method. In this study, continuous and crack-free HKUST-1 membranes could be obtained by spraying solvothermal precursor solution on the heated alumina support, followed by solvothermal synthesis. HKUST-1 membranes were characterized by XRD, FE-SEM and single gas permeation experiments.

Investigation of Electron Thermally Induced Phase Transition in MAPbI3 Perovskite Solar Cells Using In-Situ XRD and TEM (실시간 XRD와 TEM을 이용한 MAPbI3의 온도 변화에 따른 구조 분석)

  • Choi, Jin-Seok;Eom, Ji-Ho;Yoon, Soon-Gil
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.32 no.1
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    • pp.64-69
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    • 2019
  • Methylammonium lead triiodide ($MAPbI_3$)-based perovskite solar cells potentially have potential advantages such as high efficiency and low-cost manufacturing procedures. However, $MAPbI_3$ is structurally unstable and has low phase-change temperatures ($30^{\circ}C$ and $130^{\circ}C$); it is necessary to solve these problems. We investigated the crystal structure and phase separation using real-time temperature-change X-ray diffraction, transmission electron microscopy, and electron energy loss spectroscopy. $MAPbI_3$ has a tetragonal structure, and at about $35^{\circ}C$ the c-axis contracts, transforming $MAPbI_3$ into the related cubic crystal structure. In addition, at $130^{\circ}C$, phase separation occurs in which $CH_3NH_2$ and HI at the center of the unit cell of the perovskite structure are extracted by gas, leavingand only $PbI_2$ of the three-component structure, is produced as the final solid product.

Mechanical Properties of in-situ Doped Polycrystalline 3C-SiC Thin Films by APCVD (APCVD로 in-situ 도핑된 다결정 3C-SiC 박막의 기계적 특성)

  • Kim, Kang-San;Chung, Gwiy-Sang
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.22 no.3
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    • pp.235-238
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    • 2009
  • This paper describes the mechanical properties of poly (Polycrystalline) 3C-SiC thin films with $N_2$ in-situ doping. In this work, the poly 3C-SiC film was deposited by APCVD (Atmospheric Pressure Chemical Vapor Deposition) method using single-precursor HMDS (Hexamethyildisilane: $Si_2(CH_3)_6)$ at $1200^{\circ}C$. The mechanical properties of doped poly 3C-SiC thin films were measured by nono-indentation according to the various $N_2$ flow rate. In the case of 0 sccm $N_2$ flow rate, Young's Modulus and hardness were obtained as 285 GPa and 35 GPa, respectively. Young's Modulus and hardness were decreased according to increase of $N_2$ flow rate. The crystallinity and surface roughness was also measured by XRD (X-Ray Diffraction) and AFM (Atomic Force Microscopy), respectively.

A Study on the Structural and Electrochemical Properties of Li0.99Ni0.46Mn1.56O4 Cathode Material Using Synchrotron based in-situ X-ray Diffraction

  • Choi, Sol;Yoon, JeongBae;Muhammad, Shoaib;Yoon, Won-Sub
    • Journal of Electrochemical Science and Technology
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    • v.4 no.1
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    • pp.34-40
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    • 2013
  • The structural and electrochemical properties of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ ($Fd{\bar{3}}m$, disordered spinel) cathode material were studied and compared with stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$ ($P4_332$, ordered spinel). First cycle discharge capacity of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was similar to that of $LiNi_{0.5}Mn_{1.5}O_4$ at C/3 and 1C rate, but cycling performance of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was better than that of $LiNi_{0.5}Mn_{1.5}O_4$ especially at high rate of 1C. This can be explained by performing synchrotron based in-situ XRD and results of GITT measurements. It is considered that faster lithium ion diffusion in the $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ cathode results in the improvement of the rate capability. To study structural changes during cycling, synchrotron in-situ XRD patterns of both the samples were recorded at C/3 and 1C rate. Compared to stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$, disordered $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ spinel sample has pseudo one phase behavior and one step phase transition between two cubic phases. So, $LiNi_{0.5}Mn_{1.5}O_4$ would experience a much greater strain and stress, originating from the two phase transitions between three cubic phases and suffer from capacity loss during cycling especially at high rate.

A Comparison Method of Silver Nanoparticles Prepared by the Gamma Irradiation and in situ Reduction Methods

  • Lee, Chul-Jae;Karim, Mohammad Rezaul;Vasudevan, T.;Kim, Hee-Jin;Raushan, K.;Jung, Maeng-Joon;Kim, Dong-Yeub;Lee, Mu-Sang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1993-1996
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    • 2010
  • Silver nanoparticles has been prepared by the $\gamma$-irradiation and in situ reduction methods. Based on the Raman spectra, TEM images, X-ray Diffraction (XRD) patterns and UV-vis spectra, the in situ reduction method is more stable and the average size of the silver nanoparticles is also smaller than by the $\gamma$-irradiation reduction method. It is identified that the silver ions interacting with nonbonding electrons of oxygen atom in the carbonyl group of polyvinylpyrrolidone (PVP) by the in situ reduction method. It is also found advantages of the in situ reduction method including no additional reducing agents, without $\gamma$-irradiations treatment and the room temperature treatment suitability.

On the Properties of TLCP/PBT Blends Prepared by In Situ Polymerization in PBT Solution (In situ 중합에 의해서 제조된 TLCP/PBT 블렌드의 특성 연구)

  • Choi, Jae-Kon;Park, Il-Soo;Kim, Sun;Choi, Yoo-Sung;Lee, Eung-Jae;Jo, Byung-Wook
    • Elastomers and Composites
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    • v.39 no.3
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    • pp.217-227
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    • 2004
  • A new thermotropic liquid crystalline polymer(TLCP) containing a triad aromatic ester type mesogenic unit and butylene terephthalate unit(BT) in the main chain was synthesized by polycondensation reaction. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature from solid to mesophase was $260^{\circ}C$. The TLCP/PBT blends were prepared by in-situ polymerization in PBT solution and characterized by differential scanning calorimeter(DSC), thermogavimetric analyzer(TGA), scanning electron microscope(SEM), x-ray diffractometer(XRD), and dynamic mechanical thermal analyze, (DMTA). The blends showed well dispersed TLCP phases with domain sizes $0.05{\sim}0.2{\mu}m$ in the PBT matrix. As the increasing TLCP content from 5 to 20 wt%, ${\Delta}Hm$ values of pure PBT in the blend were increased because TLCP acts as a nucleating agent in the PBT matrix. The mechanical properties of the blends depended on the TLCP contents because the TLCP acted effectively as a reinforcing material in the PBT matrix. The blends showed good interfacial adhesion between the TLCP phase and PBT matrix.The blends prepared by in-situ polymerization showed higher mechanical properties and well dispersed TLCP domains than those of the blends prepared by melt blending.

Neutron irradiation impact on structural and electrical properties of polycrystalline Al2O3

  • Sunil Kumar;Sejal Shah;S. Vala;M. Abhangi;A. Chakraborty
    • Nuclear Engineering and Technology
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    • v.56 no.2
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    • pp.402-409
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    • 2024
  • High energy neutron irradiations impact on structural and electrical properties of alumina are studied with particular emphasis on real time in-situ radiation induced conductivity measurement in low flux region. Polycrystalline Al2O3 samples are subjected to high energy neutrons produced from D-T neutron generator and Am-Be neutron source. 14 MeV neutrons from D-T generator are chosen to study the role of fast neutron irradiation in the structural modification of samples. Real time in-situ electrical measurement is performed to investigate the change in insulation resistance of Al2O3 due to radiation induced conductivity at low flux regime. During neutron irradiation, a significant transient decrease in insulation resistance is observed which recovers relative higher value just after neutron exposure is switched off. XRD results of 14 MeV neutron irradiated samples suggest annealing effect. Impact of relatively low energy neutrons on the structural properties is also studied using Am-Be neutrons. In this case, clustering is observed on the sample surface after prolonged neutron exposure. The structural characterizations of pristine and irradiated Al2O3 samples are performed using XRD, SEM, and EDX. The results from these characterizations are analysed and interpreted in the manuscript.

Analysis of the Structural Properties for ZnO/Sapphire(0001) Thin Films by In-situ Atmosphere Annealing (In-situ 분위기 Annealing에 따른 ZnO/Sapphire(0001) 박막의 구조적 특성 분석)

  • Wang Min-Sung;Yoo In-Sung;Park Choon-Bae
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.19 no.8
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    • pp.769-774
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    • 2006
  • In this paper the ZnO thin films, which has used spotlight of next generation short wavelength LEDs and semiconductor laser were deposited based on RF magnetron sputtering is described. The temperature at substrate and work pressure, which has implemented in sputtering process of ZnO thin films were settle down at $100^{\circ}C$ and 15 mTorr respectively. The ZnO 5N has used target. The thickness of ZnO thin films was about $1.6{\mu}m$ which was measured by SEM analysis after the sputtering process. Structural properties of ZnO thin films by in-situ and atmosphere annealing were analyzed by XRD. Transformation of grain size and surface roughness were observed by AFM. XPS spectra showed that ZnO thin film had a peak positions corresponding to the $Zn_{2p}$ and the $O_{1s}$. As form above XPS, we confirmed that post-annealing condition changed the atom ratio of Zn/O and microstructure in ZnO thin films.

Indium Tin Oxide (ITO) Coatings Fabricated Using Mixed ITO Sols

  • Cheong, Deock-Soo;Yun, Dong-Hun;Park, Sang-Hwan;Kim, Chang-Sam
    • Journal of the Korean Ceramic Society
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    • v.46 no.6
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    • pp.708-712
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    • 2009
  • ITO films were achieved by sintering at $500{\sim}550{^{\circ}C}$. This was possible by inducing a seeding effect on an ITO sol by producing crystalline ITO nanoparticles in situ during heat treatment. Two kinds of ITO sols (named ITO-A and ITO-B) were prepared at 2.0 wt% from indium acetate and tin(IV) chloride in different mixed solvents. The ITO-A sol showed a high degree of crystallinity of ITO without any detectable Sn$O_2$ on XRD at $350{^{\circ}C}$/1 h, but the ITO-B sol showed a small amount of Sn$O_2$ even after annealing at $600{^{\circ}C}$/1 h. The 10 wt% ITO-A//ITO-B showed the sheet resistance of 3600$\Omega$/□, while the ITO-B sol alone showed 5200 $\Omega$/□ by sintering at $550{^{\circ}C}$ for 30 min. Processing parameters were studied by TG/DSC, XRD, SEM, sheet resistance, and visible transmittance.