• Title/Summary/Keyword: Solid-solid phase transition

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Compressibility of $FeS_{2}$ ($FeS_{2}$의 압축성 연구)

  • Kim, Young-Ho;Hwang, Gil-Chan;Cho, Hyen-Goo
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.3 s.49
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    • pp.189-195
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    • 2006
  • Compression work on a pyrite powder has been carried out using energy dispersive X-ray diffraction (EDXRD) with Mao-Bell type diamond anvil cell (DAC) and synchrotron radiation(SR) at room temperature. It has been reported the bulk moduli of pyrite show the large variations depending on the experimental conditions as well as the apparatus used. Thus, two kinds of sample in different pressure transmitting media of both NaCl and MgO powder emerged in alcoholic fluids were subjected to measure their compressibilities. Bulk moduli thus obtained are 138.9 GPa and 198.2 GPa, respectively, and this result contradicts to the anticipated values according to the hydrostaticity conditions of the sample chamber. This might be due to the alcoholic fluids phase transition mainly with the side effects from the difference of both solid state detector (SSD) used and E*d value applied. All experiments were performed at the Beam Line 1B2 of Pohang Light Source (PLS).

Size Tailored Nanoparticles of ZrN Prepared by Single-Step Exothermic Chemical Route

  • Lee, Sang-Ki;Park, Kyung-Tae;Ryu, Hong-Youl;Nersisyan, Hayk H.;Lee, Kap-Ho;Lee, Jong-Hyeon
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.243-248
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    • 2012
  • ZrN nanoparticles were prepared by an exothermic reduction of $ZrCl_4$ with $NaN_3$ in the presence of NaCl flux in a nitrogen atmosphere. Using a solid-state combustion approach, we have demonstrated that the zirconium nitride nanoparticles synthesis process can be completed in only several minutes compared with a few hours for previous synthesis approaches. The chemistry of the combustion process is not complex and is based on a metathesis reaction between $ZrCl_4$ and $NaN_3$. Because of the low melting and boiling points of the raw materials it was possible to synthesize the ZrN phase at low combustion temperatures. It was shown that the combustion temperature and the size of the particles can be readily controlled by tuning the concentration of the NaCl flux. The results show that an increase in the NaCl concentration (from 2 to 13 M) results in a temperature decrease from 1280 to $750^{\circ}C$. ZrN nanoparticles have a high surface area (50-70 $m^2/g$), narrow pore size distribution, and nano-particle size between 10 and 30 nm. The activation energy, which can be extracted from the experimental combustion temperature data, is: E = 20 kcal/mol. The method reported here is self-sustaining, rapid, and can be scaled up for a large scale production of a transition metal nitride nanoparticle system (TiN, TaN, HfN, etc.) with suitable halide salts and alkali metal azide.

In Situ Observation of Solidification Behavior in Undercooled $Pd_{40}Cu_{30}Ni_{10}P_{20}$ Alloy Melts during Linear Cooling (연속냉각 중 과냉 된 $Pd_{40}Cu_{30}Ni_{10}P_{20}$ 합금 용탕의 실시간 응고거동 관찰)

  • Kim, Ji-Hun
    • Journal of Korea Foundry Society
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    • v.23 no.5
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    • pp.276-285
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    • 2003
  • In the undercooled melt of $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy, the solidification behavior including nucleation and growth of crystals at the micrometer level has been observed in-situ by use of a confocal scanning laser microscope combined with an infrared image furnace. The $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy specimens were cooled from the liquid state to glass transition temperature. 575 K, at various cooling late under a helium gas flow. According to the cooling rate, the morphologies of the solidification front are changed among various types, irregular jog like front, columnar dendritic front, cellular grain, star like shape jog and fine grain, etc. The velocities of the solid-liquid interface are measured to be $10^{-5}{\sim}10^{-8}$ m/s which are at least two orders higher than the theoretical crystal growth rates. Combining the morphologies observed in terms of cooling rates and their solidification behaviors, we conclude that phase separation takes place in the undercooled molten $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy. The continuous cooling transformation (CCT) diagram was constructed from solidification onset time at various linear cooling conditions with different rate. The CCT diagram suggests that the critical cooling rate for glassy solidification is about 1.5 K/s, which is in agreement with the previous calorimetric findings.

Synthesis and luminescent properties of $Er^{3+}$ doped $CaZrO_3$ long persistent phosphors ($Er^{3+}$를 첨가한 $CaZrO_3$ 축광성 형광체의 합성 및 발광 특성 분석)

  • Park, Byeong-Seok;Choi, Jong-Koen
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.1
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    • pp.27-32
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    • 2008
  • Novel long persistent phosphors of $CaZrO_3:Er^{3+}$ have been synthesized by traditional solid state reaction method. The long persistent phosphor crystalline particles were characterized by the X-ray diffraction (XRD), photoluminescence spectrophotometer, thermoluminescence (TL) and luminance meter. The results reveal that the samples are composed of single $CaZrO_3$ phase. The broadband emission spectra of 446 nm peak and 550 nm peak was revealed by synthesized at high temperature in $N_2$ gas. Green long persistent phosphors have been observed in the sys_em for over 6 h after UV irradiation (254 nm). The main emission peak was ascribed to $Er^{3+}$ ions transition from $^5D_{5/2}{\rightarrow}^4F_{9/2},\;^2H_{12/2},\;^4S_{3/2}{\rightarrow}^4I_{13/2}\;and\;^2G_{9/2}{\rightarrow}^4I_{13/2}$, and the afterglow may be ascribed to the suitable trap centers in the $CaZrO_3$ host lattice.

CeO2-Promoted Highly Active Catalyst, NiSO4/CeO2-ZrO2 for Ethylene Dimerization

  • Pae, Young-Il;Shin, Dong-Cheol;Sohn, Jong-Rack
    • Bulletin of the Korean Chemical Society
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    • v.27 no.12
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    • pp.1989-1996
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    • 2006
  • The $NiSO_4/CeO_2-ZrO_2 $catalysts containing different nickel sulfate and $CeO_2$ contents were prepared by the impregnation method, where support, $CeO_2-ZrO_2$was prepared by the coprecipitation method using a mixed aqueous solution of zirconium oxychloride and cerium nitrate solution followed by adding an aqueous ammonia solution. No diffraction line of nickel sulfate was observed up to 20 wt %, indicating good dispersion of nickel sulfate on the surface of $CeO_2-ZrO_2$. The addition of nickel sulfate (or $CeO_2$) to $ZrO_2$ shifted the phase transition of $ZrO_2$ from amorphous to tetragonal to higher temperatures because of the interaction between nickel sulfate (or $CeO_2$) and $ZrO_2$. A catalyst (10-$NiSO_4/1-CeO_2-ZrO_2$) containing 10 wt % $NiSO_4$ and 1 mole % $CeO_2$, and calcined at $600{^{\circ}C}$ exhibited a maximum catalytic activity for ethylene dimerization. The catalytic activities were correlated with the acidity of catalysts measured by the ammonia chemisorption method. The role of $CeO_2$was to form a thermally stable solid solution with zirconia and consequently to give high surface area, thermal stability and acidity of the sample.

Improvement of the Figure of Merit in Pb[(Mg1/3Ta2/3)0.7Ti0.3]O3 Systems

  • Kim, Yeon Jung
    • Applied Science and Convergence Technology
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    • v.25 no.5
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    • pp.88-91
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    • 2016
  • The $Pb[(Mg_{1/3}Ta_{2/3})_{0.7}Ti_{0.3}]O_3$+xwt%PbO systems at temperature of $1250^{\circ}C$ for 4 hours was successful synthesized. In this study, PbO-doped $Pb[(Mg_{1/3}Ta_{2/3})_{0.7}Ti_{0.3}]O_3$ systems with non-linear behaviors showed ordering-degree dependence at the low temperature range were prepared using the columbite precursor method. And the characteristic of remnant polarization vs. electric field were analyzed. The pyroelectric, dielectric and piezoelectric properties of partially disordered $Pb[(Mg_{1/3}Ta_{2/3})_{0.7}Ti_{0.3}]O_3$+xwt%PbO solid solutions were studied as a function of temperature, frequency, and electric field. It showed distinct features of temperature dependent of pyroelectric coefficient, spontaneous polarization and dielectric constant at about $50^{\circ}C$. The figure of merit was calculated as pyroelectric coefficient, dielectric constant and dissipation factor. It was found that the high voltage responsivity FV, high detectivity FD were $0.0373m^2/C$ and $0.6735{\times}10^{-4}Pa{-1/2}$, respectively, in the $Pb[(Mg_{1/3}Ta_{2/3})_{0.7}Ti_{0.3}]O_3$+3.0 wt%PbO system.

Analysis of the Dual Promoters and the $H_2O$$_2$-responsive Element of the cats Gene Encoding Catalase A in Streptomyces coelicolor

  • Cho, You-Hee;Hahn, Ji-Sook;Roe, Jung-Hye
    • Journal of Microbiology
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    • v.38 no.4
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    • pp.239-244
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    • 2000
  • The cats gene encodes the major catalase in Sreptomyces coelicolor, whose production increases upon H$_2$O$_2$treatment. Besides the previously identified primary promoter (catApl), a minor promoter (catAp2) was newly assigned by S1 nuclease mapping. The catAp2 transcript was observed transiently upon entry into the stationary phase in liquid culture and upon differentiation on solid plates, whereas the level of catApl transcription did not chance significantly during this growth transition. ThecatApl promoter was transcribed by the major vegetative RNA polymerase holoenzyme containing $\sigma$$\^$HrdB/, whereas the catAp2 was transcribed in vitro by the holoenzyme containing $\sigma$$\^$R/ that is activated under oxidative conditions. The cia-element regulating the H$_2$O$_2$-inducibility of catApl was identified within the 23 bp inverted repeat sequence located between -65 and -43 of the catApl promoter. We roamed this sequence HRE (H$_2$O$_2$-responsive Element). The distal half of the inverted repeat was more crucial for H$_2$O$_2$-dependent induction of the catApl transcript than the proximal half. HRE most likely serves as a binding site for the H$_2$O$_2$-responsive repressor CatR.

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The conversion of ammonium uranate prepared via sol-gel synthesis into uranium oxides

  • Schreinemachers, Christian;Leinders, Gregory;Modolo, Giuseppe;Verwerft, Marc;Binnemans, Koen;Cardinaels, Thomas
    • Nuclear Engineering and Technology
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    • v.52 no.5
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    • pp.1013-1021
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    • 2020
  • A combination of simultaneous thermal analysis, evolved gas analysis and non-ambient XRD techniques was used to characterise and investigate the conversion reactions of ammonium uranates into uranium oxides. Two solid phases of the ternary system NH3 - UO3 - H2O were synthesised under specified conditions. Microspheres prepared by the sol-gel method via internal gelation were identified as 3UO3·2NH3·4H2O, whereas the product of a typical ammonium diuranate precipitation reaction was associated to the composition 3UO3·NH3·5H2O. The thermal decomposition profile of both compounds in air feature distinct reaction steps towards the conversion to U3O8, owing to the successive release of water and ammonia molecules. Both compounds are converted into α-U3O8 above 550 ℃, but the crystallographic transition occurs differently. In compound 3UO3·NH3·5H2O (ADU) the transformation occurs via the crystalline β-UO3 phase, whereas in compound 3UO3·2NH3·4H2O (microspheres) an amorphous UO3 intermediate was observed. The new insights obtained on these uranate systems improve the information base for designing and synthesising minor actinide-containing target materials in future applications.

Synthesis and Comparative Analysis of Crystallite Size and Lattice Strain of Pb2Ba1.7Sr0.3Ca2Cu3O10+δ Superconductor

  • Hasan, Maher Abd Ali;Jasim, Kareem Ali;Miran, Hussein Ali Jan
    • Korean Journal of Materials Research
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    • v.32 no.2
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    • pp.66-71
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    • 2022
  • In this article, Pb2Ba1.7Sr0.3Ca2Cu3O10+δ superconductor material was synthesized using conventional solid-state reaction method. X-ray diffraction (XRD) analysis demonstrated one dominant phase 2223 and some impurities in the product powder. The strongest peaks in the XRD pattern were successfully indexed assuming a pseudo-tetragonal cell with lattice constants of a = 3.732, b = 3.733 and c = 14.75 Å for a Pb-Based compound. The crystallite size and lattice strain between the layers of the studied compound were estimated using several methods, namely the Scherrer, Williamson-Hall (W.H), size-strain plot (SSP) and Halder Wagner (H.W) approach. The values of crystallite size, calculated by Scherrer, W.H, SSP and H.W methods, were 89.4540774, 86.658638, 87.7555823 and 85.470086 Å, respectively. Moreover, the lattice strain values obtained by W.H, SSP and H.W methods were 0.0063240, 0.006325 and 0.006, respectively. It was noted that all crystallite size results are consistent; however, the best method is the size-strain plot because it gave a value of R2 approaching one. Furthermore, degree of crystallites was calculated and found to be 59.003321%. Resistivity analysis suggests zero-resistance, which is typical of superconducting materials at critical temperature. Four-probe technique was utilized to measure the critical temperature at onset Tc(onset), zero resistivity Tc(off set), and transition (width ΔT), corresponding to temperatures of 128 K, 116 K, and 12 K, respectively.

Microstructure and dielectric properties in the La2O3-doped BaTiO3 system (La2O3 첨가에 따른 BaTiO3의 미세구조 및 유전특성)

  • Choi, Woo-Jin;Moon, Kyoung-Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.3
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    • pp.103-109
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    • 2020
  • The effect of La2O3 addition on the crystalline phase, microstructure, and dielectric properties of BaTiO3 has been studied as a function of the amounts of La2O3. 0.3 mol% TiO2-excess BaTiO3 powder was synthesized by solid-state reaction, and then the powder compacts with various amounts of La2O3 were sintered at 1250℃ for 2 hours. Room temperature XRD showed changes in the lattice parameters and a decrease of tetragonality (c/a) as the amounts of La2O3 increased. It can be explained that the phase transition from tetragonal to cubic phase occurred because La3+ replaced Ba2+ site, which increased the instability of the tetragonal phase. As La2O3 was added over 0.1 mol%, the critical driving force for growth (Δgc) increased over maximum driving force (Δgmax). As the result, the grain size decreased with La2O3 addition. Dielectric constant decreased as the amounts of La2O3 increased, which was analyzed with crystal structure and microstructure.