• Title/Summary/Keyword: Bulk crystallization

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Micro-deformation behavior of Brittle Hf-based Metallic Glass during Mechanical Milling (기계적 합금화 공정에 의한 Hf계 비정질 분말의 미세변형거동 관찰)

  • Kim, Song-Yi;Lee, A-Young;Cha, Eun-Ji;Kwon, Do-Hun;Hong, Sung-Uk;Lee, Min-Woo;Kim, Hwi-Jun;Lee, Min-Ha
    • Journal of Powder Materials
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    • v.25 no.3
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    • pp.246-250
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    • 2018
  • In this study, we investigate the deformation behavior of $Hf_{44.5}Cu_{27}Ni_{13.5}Nb_5Al_{10}$ metallic glass powder under repeated compressive strain during mechanical milling. High-density (11.0 g/cc) Hf-based metallic glass powders are prepared using a gas atomization process. The relationship between the mechanical alloying time and microstructural change under phase transformation is evaluated for crystallization of the amorphous phase. Planetary mechanical milling is performed for 0, 40, or 90 h at 100 rpm. The amorphous structure of the Hf-based metallic glass powders during mechanical milling is analyzed using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Microstructural analysis of the Hf-based metallic glass powder deformed using mechanical milling reveals a layered structure with vein patterns at the fracture surface, which is observed in the fracture of bulk metallic glasses. We also study the crystallization behavior and the phase and microstructure transformations under isothermal heat treatment of the Hf-based metallic glass.

Effects of Zinc Stearates on the Thermal and Rheological Properties of Polystyrene Ionomers (폴리스티렌 이오노머의 열적·유변학적 성질에 미치는 스테아린산 아연의 영향)

  • Kim, Jong-sang;Doo, Jun Kil;Lee, Dai Soo
    • Applied Chemistry for Engineering
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    • v.10 no.8
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    • pp.1216-1220
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    • 1999
  • Different amounts of zinc stearate were incorporated as a plasticizer into poly(styrene-co-sodium methacrylate) ionomers prepared by bulk-suspension plymerization and neutralization with sodium hydroxide and effects of the zinc stearate on the thermal and rheological properties were investigated. It was obseved that the crystallization of zinc stearate in the ionomers were partially suppressed depending on the content of ionic moieties. It is postulated that the ionic moieties dissolved zinc stearate and suppressed crystallization of the zinc stearates. We speculated that 0.4~0.6 mole of zinc stearate was dissolved by one mole of the ionic moiety. Poly(styrene-co-sodium methacrylate) containing only the dissolved zinc stearates showed typical rheological properties of homogeneous systems in Cox-Mertz plots. However, poly(styrene-co-sodium methacrylate) containing crystallizable zinc stearates as well as dissolved ones showed typical rheological properties of heterogeneous systems.

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Synthesis and Physical Properties of Sm Doped Pb Free 3 Phase-Glasses (Sm 농도에 따른 무연 3상 유리계의 합성과 물리적 성질)

  • Park, Jong-Ho
    • Korean Journal of Materials Research
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    • v.22 no.7
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    • pp.368-373
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    • 2012
  • Glasses were prepared with compositions of $(13-x)BaO-80B2_O_3-7Li_2O{\cdot}xSm_2O_3$, BBLSx(x=0.5, 0.4, 0.3) by melting the starting materials of boron oxide(99.9%), lithium oxide(99.9%), barium carbon oxide(99.9%), and samarium oxide(99.9%) and then quenching the melt at $1350^{\circ}C$. This led to good-quality BBLSx(x=0.4, 0.3) and poor-quality BBLSx(x=0.5) glasses. The physical and structural properties of the BBLSx glasses were studied by means x-ray diffraction, scanning electron microscopy(SEM), differential scanning calorimetry(DSC), and dielectric spectroscopy. From the x-ray diffraction and SEM results, the quality of the BBLSx glasses significantly depends on the $Sm_2O_3$ concentration. The x-ray diffraction pattern showed that the crystallites in the BBLSx glasses after heat treatment at $700^{\circ}C$ may be $LiBaB_9O_{15}$. From the DSC results, the glass transition temperatures($T_g$), crystallization temperatures($T_c$), and the maximum temperatures of the crystallized($T_p$) BBLSx glasses all changed with the $Sm_2O_3$ concentration. According to the dielectric spectroscopy results, the values of the real dielectric constant and Tan ${\delta}$ of the BBLSx glasses depended on the $Sm_2O_3$ concentration. The values of the real dielectric constant and Tan ${\delta}$ were also shown to depend on the measuring temperature, possibly due to the ion migration in the bulk of the BBLSx glasses.

Mechanical Properties of Bulk Amorphous Ti50Cu20Ni20Al10 Fabricated by High-energy Ball Milling and Spark-plasma Sintering

  • Nguyen, H.V.;Kim, J.C.;Kim, J.S.;Kwon, Y.J.;Kwon, Y.S.
    • Journal of Powder Materials
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    • v.16 no.5
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    • pp.358-362
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    • 2009
  • Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ quaternary amorphous alloy was prepared by high-energy ball milling process. A complete amorphization was confirmed for the composition of Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ after milling for 30hrs. Differential scanning calorimetry showed a large super-cooled liquid region ($\Delta$T$_x$ = T$_x$ T$_g$, T$_g$ and T$_x$: glass transition and crystallization onset temperatures, respectively) of 80 K. Prepared amorphous powders of Ti$_{50}$Cu$_{20}$Ni$_{20}$Al$_{10}$ were consolidated by spark-plasma sintering. Densification behavior and microstructure changes were investigated. Samples sintered at higher temperature of 713 K had a nearly full density. With increasing the sintering temperature, the compressive strength increased to fracture strength of 756 MPa in the case of sintering at 733 K, which showed a 'transparticle' fracture. The samples sintered at above 693 K showed the elongation maximum above 2%.

Surface Segregation of Hydroniums and Chlorides in a Thick Ice Film at Higher Temperatures

  • Lee, Du Hyeong;Bang, Jaehyeock;Kang, Heon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.263-263
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    • 2013
  • This work examines the dynamic properties of ice surfaces in vacuum for the temperature range of 140~180 K, which extends over the onset temperatures for ice sublimation and the phase transition from amorphous to crystallization ice. In particular, the study focuses on the transport processes of excess protons and chloride ions in ice and their segregative behavior to the ice surface. These phenomena were studied by conducting experiments with a relatively thick (~100 BL) ice film constructed with a bottom $H_2O$ layer and an upper $D_2O$ layer, with excess hydronium and chloride ions trapped at the $H_2O$/$D_2O$ interface as they were generated by the ionization of hydrogen chloride. The migration of protons, chloride ions, and water molecules to the ice film surface and their H/D exchange reactions were measured as a function of temperature using the methods of low energy sputtering (LES) and Cs+ reactive ion scattering (RIS). Temperature programmed desorption (TPD) experiments monitored the desorption of water and hydrogen chloride from the surface. Our observations indicated that both hydronium and chloride ions migrated from the interfacial layer to segregate to the surface at high temperature. Hydrogen chloride gas desorbs via recombination reaction of hydronium and chloride ions floating on the surface. Surface segregation of these species is driven by thermodynamic potential gradient present near the ice surface, whereas in the bulk, their transport is facilitated by thermal diffusion process. The finding suggests that chlorine activation reactions of hydrogen chloride for polar stratospheric ice particles occur at the surface of ice within a depth of at most a few molecular layers, rather than in the bulk phase.

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Fabrication and Characterization of Cu-based Amorphous Coatings by Cold Spray Process (저온 분사를 이용한 Cu계 비정질 코팅층의 제조 및 특성 연구)

  • Jung, Dong-jin;Park, Dong-Yong;Lee, Jin Kyu;Kim, Hyung Jun;Lee, Kee-Ahn
    • Korean Journal of Metals and Materials
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    • v.46 no.5
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    • pp.321-327
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    • 2008
  • Cu based amorphous ($Cu_{54}Zr_{22}Ti_{18}Ni_6$) coating was produced by cold spraying as a new fabrication process. The microstructure and macroscopic properties of amorphous coating layer was investigated and compared with those of cold sprayed pure Cu coating. Amorphous powders were prepared by gas atomization and Al 6061 was used as the substrate plate. X-ray diffraction results showed that Cu based amorphous powder could be successfully deposited by cold spraying without any crystallization. The Cu based amorphous coating layer ($300{\sim}400{\mu}m$ thickness) contained 4.87% porosity. The hardness of Cu based amorphous coating represented $412.8H_v$, which was correspond to 68% of the hardness of injection casted bulk amorphous material. The wear resistance of Cu based amorphous coating was found to be three times higher than that of pure Cu coating. The 3-point bending test results showed that the adhesion strength of Cu based amorphous coating layer was higher than that pure Cu coating. It was also observed that hard Cu base amorphous particle could easily deform soft substrate by particle collisions and thus generated strong adhesion between coating and substrate. However, the amorphous coating layer unexpectedly represented lower corrosion resistance than pure Cu coating, which might be resulted from the higher content of porosity in the cold sprayed amorphous coating.

Effect of modifiers on the properties of glass-ceramics containing coal bottom ash (석탄 바닥재가 포함된 결정화 유리의 특성에 미치는 수식제의 영향)

  • Kang, Seung-Gu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.1
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    • pp.53-57
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    • 2010
  • The influence of CaO addition on the crystallization temperature, crystal types, and microstructure of L-A-S ($Li_2O-Al_2O_3-SiO_2$) glass-ceramics system fabricated from a coal bottom ash, produced at thermal power plant, was studied. The glass transition and crystallization temperatures were shifted to the higher temperature position with increasing CaO content in a non-isothermal analysis using a DTA. The major crystalline phases of L-A-S glass-ceramics system produced were identified as ${\beta}$-spodumene ($LiAlSi_2O_6$) and eucryptite ($LiAlSiO_4$). The glass-ceramics showed a bulk and surface crystallization behavior at a time. With increasing CaO content, the ${\beta}$-spodumene peak in XRD increased and some CaO-related phases were formed. The surface crystal grown from the exterior to the center in glass-ceramics showed various shapes by amount of CaO added. Some cracks were generated at the glass-ceramics containing CaO above 9 wt% due to the mismatch of thermal expansion coefficients between a ${\beta}$-spodumene and CaO-related crystal phases.

Effect of $TiO_2$ in the Lead-Zinc-Borosilicate Solder Glass ($TiO_2$ 의 첨가가 Lead-Zinc-Borosilicate 봉착 유리에 미치는 영향)

  • 채수철;김철영
    • Journal of the Korean Ceramic Society
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    • v.21 no.4
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    • pp.349-354
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    • 1984
  • The purpose of present study is to find the structure crystallization mechanism and physical properties in $TiO_2$ containing lead zinc borosilicate glass system. The experiments such as differential thermal analysis infrared spectral analysis. X-ray diffraction analysis and thermal expansion measurements have been done. Differential thermal analysis of coarse and fine glass powder showed bulk nucleating mechanism for high $TiO_2$ containing glasses and surface nucleation mechanism for low $TiO_2$ containing glasses. The prepared glasses crystallized to crystalline mixture of PbO.2ZnO. $B_2O_3$ .4PbO.2ZnO.$5B_2O_3$and 2PbO.ZnO.$B_2O_3$ when heat-treated in the range of 480 and 51$0^{\circ}C$ and crystallized to PbTiO3 when heat-treated at $600^{\circ}C$. Obtained crystalline phase of $PbTiO_3$ in glass matrix strongly affects to thermal expansion coefficient and the value of crystallized glass varied 68.0 to $107.1{\times}10-7$/$^{\circ}C$ depending on the amount of $TiO_2$added. Infrared spectral analysis showed that [$BO_3$] triangle and [$BO_3$] tetrahedral units were coexisted in the glass with high content of PbO.

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On the Possibility of Bulk Large Diamond Single Crystal Synthesis with Hydrothermal Process

  • Andrzej M. Szymanski
    • Journal of the Mineralogical Society of Korea
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    • v.10 no.1
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    • pp.18-32
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    • 1997
  • Analysis of geological data, relating to occurrence and formation of diamonds as well as host rocks, inclined author to have different outlook on the diamond genesis and to establish a proposition on their formation at pneumatolytic-hydrothermal conditions near superficial Earth zones. Based on that theoretical foundations and experimental works, the first low-pressure and low-temperature hydrothermal diamond synthesis from water solution in pressure autoclave was executed. As a result, the natural diamond seed crystal grew bigger ad coupling of the synthetic diamond single-crystalline grains were obtained. SEM documentation proofs that parallely paragenetic crystallization of quartz and diamond, and nucleation of new octahedral diamond crystals brush take place on the seed crystal surface. Forecast of none times growth of diamond industrial application at 2000 and seventeen times at 2010 with reference to 1995, needs technology of large and pure single-crystals diamond synthesis. Growth of the stable and destressed diamond single-crystals in the pseudo-metastable diamond plot, may be realized with processes going through the long time and with participation of free radicals catalysts admixtures only. Sol-gel colloidal processes are an example of environment which form stable crystals in thermodynamically unstable conditions through a long time. Paper critically discusses a whole way of studies on the diamond synthesis, from high-pressure and high-temperature processes through chemical vapour deposition up to hydrothermal experiments.

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The properties of glass ceramics of Li2O-Al2O3-SiO2 system according to nucleation agent (조핵제 원료에 따른 Li2O-Al2O3-SiO2계 결정화 유리 특성)

  • Park, Hyun-Wook;Lee, Ji-Sun;Lim, Tae-Young;Hwang, Jonghee;Ra, Yong-Ho;Noh, Myoung-Rae;Seo, Kwan-Hee;Kim, Jin-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.28 no.6
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    • pp.229-234
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    • 2018
  • The glass-ceramic of $Li_2O-Al_2O_3-SiO_2$ system was synthesized by using $ZrO_2$, $ZrSiO_4$, $ZrOCl_2$ and $Zr(SO_4)_2$, which is a raw material of Zr serving as a nucleation agent. It was confirmed that Avrami parameter of these four glasses is over 3 for bulk crystallization. The glass synthesized by $ZrOCl_2$, and $Zr(SO_4)_2$ showed high melting quality during the melting process. It is also observed that the Zr component is uniformly distributed in the glass. Various characterizations was evaluated, including composition analysis and bending strength.