• Title/Summary/Keyword: Solid-State Synthesis

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Synthesis and Characterization of Methyltriphenylsilane for SiOC(-H) Thin Film (SiOC(-H) 박막 제조용 Methyltriphenylsilane 전구체 합성 및 특성분석)

  • Han, Doug-Young;Park Klepeis, Jae-Hyun;Lee, Yoon-Joo;Lee, Jung-Hyun;Kim, Soo-Ryong;Kim, Young-Hee
    • Korean Journal of Materials Research
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    • v.20 no.11
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    • pp.600-605
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    • 2010
  • In order to meet the requirements of faster speed and higher packing density for devices in the field of semiconductor manufacturing, the development of Cu/Low k device material is explored for use in multi-layer interconnection. SiOC(-H) thin films containing alkylgroup are considered the most promising among all the other low k candidate materials for Cu interconnection, which materials are intended to replace conventional Al wiring. Their promising character is due to their thermal and mechanical properties, which are superior to those of organic materials such as porous $SiO_2$, SiOF, polyimides, and poly (arylene ether). SiOC(-H) thin films containing alkylgroup are generally prepared by PECVD method using trimethoxysilane as precursor. Nano voids in the film originating from the sterichindrance of alkylgroup lower the dielectric constant of the film. In this study, methyltriphenylsilane containing bulky substitute was prepared and characterized by using NMR, single-crystal X-ray, GC-MS, GPC, FT-IR and TGA analyses. Solid-state NMR is utilized to investigate the insoluble samples and the chemical shift of $^{29}Si$. X-ray single crystal results confirm that methyltriphenylsilane is composed of one Si molecule, three phenyl rings and one methyl molecule. When methyltriphenylsilane decomposes, it produces radicals such as phenyl, diphenyl, phenylsilane, diphenylsilane, triphenylsilane, etc. From the analytical data, methyltriphenylsilane was found to be very efficient as a CVD or PECVD precursor.

Synthesis and Luminescent Characterization of Eu2+/Dy3+-Doped Sr2MgSi2O7 Powders (Eu2+/Dy3+ 이온이 도핑된 Sr2MgSi2O7 분말 합성 및 발광 특성)

  • Park, Jaehan;Kim, Young Jin
    • Korean Journal of Materials Research
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    • v.24 no.12
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    • pp.658-662
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    • 2014
  • $Eu^{2+}/Dy^{3+}$-doped $Sr_2MgSi_2O_7$ powders were synthesized using a solid-state reaction method with flux ($NH_4Cl$). The broad photoluminescence (PL) excitation spectra of $Sr_2MgSi_2O_7:Eu^{2+}$ were assigned to the $4f^7-4f^65d$ transition of the $Eu^{2+}$ ions, showing strong intensities in the range of 375 to 425 nm. A single emission band was observed at 470 nm, which was the result of two overlapping subbands at 468 and 507 nm owing to Eu(I) and Eu(II) sites. The strongest emission intensity of $Sr_2MgSi_2O_7:Eu^{2+}$ was obtained at the Eu concentration of 3 mol%. This concentration quenching mechanism was attributable to dipole-dipole interaction. The $Ba^{2+}$ substitution for $Sr^{2+}$ caused a blue-shift of the emission band; this behavior was discussed by considering the differences in ionic size and covalence between $Ba^{2+}$ and $Sr^{2+}$. The effects of the Eu/Dy ratios on the phosphorescence of $Sr_2MgSi_2O_7:Eu^{2+}/Dy^{3+}$ were investigated by measuring the decay time; the longest afterglow was obtained for $0.01Eu^{2+}/0.03Dy^{3+}$.

Piezoelectric Properties of 0.98(Na0.5K0.5)NbO3-0.02Li(Sb0.17Ta0.83)O3+0.01wt%ZnO Ceramics with a Sintering Temperature (소결 온도에 따른 0.98(Na0.5K0.5)NbO3-0.02Li(Sb0.17Ta0.83)O3+0.01wt%ZnO 세라믹스의 압전 특성)

  • Lee, Dong-Hyun;Lee, Seung-Hwan;Lee, Sung-Gap;Lee, Ku-Tak;Lee, Young-Hie
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.24 no.7
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    • pp.543-546
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    • 2011
  • We studied sintering temperature to enhance the piezoelectric properties of $0.98(Na_{0.5}K_{0.5})NbO_3-0.02Li(Sb_{0.17}Ta_{0.83})O_3$+0.01wt%ZnO (hereafter NKN-LST+ZnO) lead free piezoelectric ceramics. The synthesis and sintering method were the conventional solid state reaction method and sintering was executed at $1,080\sim1,120^{\circ}C$. We found that NKN-LST+ZnO ceramics at optimal sintering temperature showed the improved piezoelectric properties at the optimal sintering temperature. The NKN-LST+ZnO ceramics show good performance with piezoelectric constant $d_{33}$= 153 pC/N sintered at $1,090^{\circ}C$. The results reveal that NKN-LST+ZnO ceramics are promising candidate materials for lead-free piezoelectric application.

Synthesis and Characteristics of SrAl2O4: Eu2+, Dy3+ Long Afterglow Phosphors by Polymerized Complex Method (착체중합법을 이용한 SrAl2O4: Eu2+, Dy3+ 축광성 형광체의 합성)

  • Kim, Tae-Ho;Hwang, Hae-Jin;Kim, Jin-Ho;Hwang, Kwang-Taek;Han, Kyu-Sung
    • Korean Journal of Materials Research
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    • v.26 no.10
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    • pp.561-569
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    • 2016
  • $SrAl_2O_4$: $Eu^{2+}$ and $Dy^{3+}$ phosphorescent phosphors were synthesized using the polymerized complex method. Generally, phosphorescent phosphors synthesized by conventional solid state reaction show a micro-sized particle diameter; thus, this process is restricted to applications such as phosphorescent ink and paint. However, it is possible to synthesize homogeneous multi-component powders with fine particle diameter by wet process such as the polymerized complex method. The characteristics of $SrAl_2O_4$: $Eu^{2+}$ and $Dy^{3+}$ powders prepared by polymerized complex method with one and two step calcination processes were comparatively analyzed. Temperatures of organic material removal and crystallization were observed through TG-DTA analysis. The crystalline phase and crystallite size of the $SrAl_2O_4$: $Eu^{2+}$ and $Dy^{3+}$ phosphorescent phosphors were analyzed by XRD. Microstructures and afterglow characteristics of the $SrAl_2O_4$: $Eu^{2+}$ and $Dy^{3+}$ phosphors were measured by SEM and spectrofluorometry, respectively.

Selective Synthesis of a New Macropolycycle Containing One N-CH2-N Linkage and Its Reaction with Cu2+ and Ni2+ Ions in Methanol

  • Kang, Shin-Geol;Kweon, Jae-Keun;Jeong, Gyeong-Rok;Lee, Uk
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1905-1910
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    • 2008
  • The reaction of 3,14-dimethyl-2,6,13,17-tetraazatetracyclo[16.4.0$0^{1.18}.0^{7.12}$]docosane ($L^1$) with formaldehyde in warm methanol yielded 3,14-dimethyl-2,6,13,17-tetraazatetracyclo[16.4.$1^{2.6}.0^{1.18}.0^{7.12}$]tricosane ($L^7$) containing one 1,3-diazacyclohexane subunit. In methanol, $L^7$ readily reacts with $Cu^{2+}$ ion to form [$CuL^7(H_2O)$]$^{2+}$ which is extremely inert against methanolysis. In the solution containing $Ni^{2+}$ ion, however, $L^7$ reacts with methanol to yield [$NiL^3$]$^{2+}$ ($L^3$ = 2-(methoxymethyl)-5,16-dimethyl-2,6,13,17-tetraazatricyclo[16.4.$0^{1.18}.0^{7.12}$]- docosane), in which one N-$CH_2OCH_3$ pendant arm is appended. The copper(II) complex [$CuL^7(H_2O)$]- $(ClO_4)_2{\cdot}3H_2O\;(I{\cdot}3H_2O)$ has a severely distorted trigonal bipyramidal coordination geometry with a 4-5- 6-5 chelate ring sequence. The crystal structure of [$NiL^3$]$(PF_6)_2{\cdot}2H_2O$ (IIb) shows that the N-$CH_2OCH_3$ pendant arm is not coordinated to the metal ion in the solid state. In various solvents (S), however, the nickel(II) complex exists as a mixture of [$NiL^3$(S)]$^{2+}$, in which the N-$CH_2OCH_3$ group as well as S is coordinated to the metal ion, and [$NiL^3$]^{2+}.

High-Temperature Behavior of Ba-Doped Boehmite Hydrothermally Prepared from $Al(OH)_3$ and $Ba(OH)_2$

  • Fujiyohi, Kaichi;Ishida, Shingo
    • The Korean Journal of Ceramics
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    • v.5 no.4
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    • pp.379-385
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    • 1999
  • Minute boehmite crystals with high aspect rations, which were hydrothermally synthesized from gibbsite in $Ba(OH)_2$ solution, occluded Ba with the Ba/Al molar ratio of about 0.03 in their interlayers. Their surface areas were about 14$\m^2$/g. The Ba-intercalated bohemite samples were partly used for producing $BaAl_{12}O){19}$ with low sinterability by externally supplementing $Ba(OH)_2$, and for forming transient aluminas. The surface area of $BaAl_{12}O){19}$ obtained by firing at $1500^{\circ}C$ for 3 h was 5.3$\m^2$/g, which was significantly lower than 12$\m^2$/g of the sol-gel origin. While a mixture ${\gamma}$-alumina and BaO is known to from $BaAl_{12}O){19}$ at $1200^{\circ}C$, solid state reaction between η-alumina transformed from the Ba-intercalated boehmite and BaO formed from $Ba(OH)_2$ deposited on the boehmite started above $1300^{\circ}C$. This suggests that large sized $Ba^{2+}$ ion occluded in η-alumina considerably suppresses the diffusion of $Al^{3+}$ ion. The surface area of the Ba-intercalated boehmite fired at $1400^{\circ}C$ for 3h was as high as 14$\m^2$/g indicative of its potential applicability to combustion catalysts. But it was decreased to 5.0$\m^2$/g after firing at $1500^{\circ}C$ for 3 h, accompanied by abrupt formations of $\alpha$-alumina and $BaAl_{12}O){19}$ as main products. The suppression of $\alpha$-alumina formation up to $1400^{\circ}C$ also suggests the significant blocking effect of $Ba^{2+}$ ion on the diffusion of the component ions.

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Immobilization of Metal lons Using Low-Temperature Calcination Techniques of Spinel-ferrites

  • Yen, Fu-Su;Kao, Hsiao-Chiun;Chen, Wei-Chien
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.106-110
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    • 2001
  • Formation of stoichiometric lithium-, nickel-, and zinc- ferrites by calcining organo-metallic precursors a temperature below 40$0^{\circ}C$ is examined using DTA/TG, and XRD techniques. It attempts to simulate th immobilization of metal ions in industrial liquid influents (waste) through the synthesis of stoichiometric spinel ferrites (SSF). Two steps of the SSF formation during thermal treatments are noted. The transformation of magnetite to ${\gamma}$ - Fe$_2$O$_3$and subsequent first formation of SSF were observed at temperatures ranging from 200 to 45$0^{\circ}C$. Th formation of cation-containing ${\gamma}$-Fe$_2$O$_3$and subsequent second formation of the ferrite occurred at temperature ranges of < 45$0^{\circ}C$ and 500 to $650^{\circ}C$, depending on the heating rate used. Then the temperature range of 200t 45$0^{\circ}C$ is critical to the performance of the technique, because a calcination at the range would lead to a complete formation of SSF, avoiding the occurrences of ${\gamma}$-Fe$_2$O$_3$and ion-containing ${\gamma}$-Fe$_2$O$_3$. If not, so $\alpha$-Fe$_2$O$_3$would occur. And annealing at temperature above $650^{\circ}C$ must be employed by which solid-state reactio of $\alpha$-Fe$_2$O$_3$with metal ions (possibly metal oxides) to form SSF can be conducted.

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Synthesis and Structural Studies of an Organic Complex and its Association with BSA

  • Meng, Fa-Yan;Yu, Sheng-Rong;Liang, Li-Xi;Zhong, Xue-Ping;Wang, Li;Zhu, Jin-Mei;Lin, Cui-Wu
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2253-2259
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    • 2011
  • The self-assembly of one novel organic complex based on chlorogenic acid (HCA) and 2,2'-bipyridine (2,2'-bipy) has been synthesized and characterized. The complex achieved by hydrogen-bonding interactions, adopted a 1:1 stoichiometry in a solid state. The proton transfer occurred from the carboxyl oxygen to the aromatic nitrogen atom to form salts CA${\cdot}$(2,2'-Hbipy), the 2,2'-Hbipy molecule individually occupies the pseudo-tetragonum that is formed with CA. In this paper, the interactions of CA${\cdot}$(2,2'-Hbipy) with bovine serum albumin (BSA) were studied by fluorescence spectrometry. For CA${\cdot}$(2,2'-Hbipy), HCA and 2,2'-bipy, the average quenching constants for BSA were $2.4384{\times}10^4$, $4.653{\times}10^3$, and $3.059{\times}10^3\;L{\cdot}mol^{-1}$, respectively. The mechanism for protein fluorescence quenching is apparently governed by a static quenching process. The Stern-Volmer quenching constants and corresponding thermodynamic parameters ${\Delta}$H, ${\Delta}$G and ${\Delta}$S were calculated. The binding constants and the number of binding sites were also investigated. The conformational changes of BSA were observed from synchronous fluorescence spectra.

Synthesis and Photoluminescence of the Sr1-xBaxAl2O4:Eu2+, Dy3+ Long Phosphorescence Phosphor (Sr1-xBaxAl2O4:Eu2+, Dy3+계 축광성 형광체의 합성과 그의 발광특성)

  • Park, Jin-Woo;Kim, Jung-Sik
    • Journal of the Korean Ceramic Society
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    • v.43 no.6 s.289
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    • pp.333-337
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    • 2006
  • In this study, the $Sr_{1-x}Ba_{x}Al_{2}O_{4}:Eu^{2+},Dy^{3+}$ phosphor were prepared by the solid-state reaction method and its photoluminescence properties were investigated. Starting powders of $SrCO_3,\;BaCO_3,\;and\;Al_{2}O_3$ were mixed with $Eu_{2}O_3$ as activator, $Dy_{2}O_3$ as co-activator and $B_{2}O_3$ as flux. Then, the mixed powders were heated at the temperature of $1100{\sim}1400^{\circ}C$ for 3 h under the reducing ambient atmosphere of $95%Ar+5%H_2$. The effect of Ba addition from 0.0 to 1.0 mol on photoluminescence was investigated. As the amount of Ba increased, the intensity of emission increased and the optimum long phosphorescence occurred at the amount of 0.1 mol Ba. The optimum sintering condition for long phosphorescent phosphor of $Sr_{1-x}Ba_{x}Al_{2}O_{4}:Eu^{2+},Dy^{3+}$($x=0{\sim}1.0mol$) was found at $1400^{\circ}C$. The excitation spectra showed a broad band of $250{\sim}450nm$ with maximum peak at 360 nm. The maximum peak intensity of emission spectra occurred at the range of $480{\sim}520nm$, depending on Ba content.

Synthesis and Formation Mechanism of ZrTiO4 Gray Pigment (ZrTiO4계 Gray 안료 합성과 형성기구)

  • Hwang, Dong-Ha;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.84-89
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    • 2012
  • Attempts were made to develop a stable gray pigment at reducing atmosphere, substituting Ti in $ZrTiO_4$ with Mn, Fe, Co and Cu The pigment synthesized at $1300~1500^{\circ}C$ by solid state method with the composition of $ZrTi_{1-x-y}A_xB_yO_4$ (x = y = 0.005, 0.015, 0.035, 0.055, 0.075, 0.095, 0.115, 0.135, 0.155, 0.175 and 0.195 mole, A = Mn(III), Fe(III), Co(II, III) and Cu(II) (chromophores), B = Sb (counterion). The pigments were fired at $1400^{\circ}C$ for 3 h with substitute amount changes of Mn, Fe, Co and Cu to $ZrTiO_4$ crystals, and analyzed by Raman spectroscopy to figure out substitute limits. Results indicated 0.035 mole for Mn, 0.115 mole for Fe, 0.015 mole for Co and 0.015 mole for Cu as substitute limits, respectively. Figs. 1, 2, 3, and 4 represent each substitute pigments of Mn, Fe, Co and Cu. Synthesized pigment was applied to a lime and a lime-magnesia glaze at 7 wt% each, and fired at reducing atmosphere of $1240^{\circ}C$, soaking time 1h. Gray color was obtained with CIE-$L^*a^*b^*$ values at 44.55, -0.65, 1.19(Mn), 40.36, -0.90, 0.30(Fe), 42.63, -0.03, -1.49(Cu) and -40.79, -0.28, -0.91(Co), respectively.