• Title/Summary/Keyword: Solid-phase synthesis

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Preparation and Characterization of Ta-substituted Li7La3Zr2-xO12 Garnet Solid Electrolyte by Sol-Gel Processing

  • Yoon, Sang A;Oh, Nu Ri;Yoo, Ae Ri;Lee, Hee Gyun;Lee, Hee Chul
    • Journal of the Korean Ceramic Society
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    • v.54 no.4
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    • pp.278-284
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    • 2017
  • In this work, Ta-substituted $Li_7La_3Zr_{2-x}O_{12}$ (LLZTO) powder and pellets with garnet cubic structure were fabricated and characterized by modified and optimized sol-gel synthesis. Ta-substituted LLZO powder with the smallest grain size and pure cubic structure with little pyrochlore phase was obtained by synthesis method in which Li and La sources in propanol solvent were mixed together with Zr and Ta sources in 2-methoxy ethanol. The LLZTO pellets made with the prepared powder showed cubic garnet structure for all conditions when the amount of Li addition was varied from 6.2 to 7.4 mol. All the X-ray peaks of the pyrochlore phase disappeared when the Li addition was increased above 7.0 mol. When the final sintering temperature was varied, the LLZTO pellet had a pyrochlore-mixed cubic phase above $1000^{\circ}C$. However, the surface morphology became much denser when the final sintering temperature was increased. The sol-gel-driven LLZTO pellet with a sintering temperature of $1100^{\circ}C$ showed a lithium ionic conductivity of 0.21 mS/cm when Au was adopted as electrode material for the blocking capacitor. The results of this study suggest that modified sol-gel synthesis is the optimum method to obtain cubic phase of LLZTO powder for highly dense and conductive solid electrolyte ceramics.

Synthesis of Halicylindramide A Mimetics Containing Lactone Isosteres

  • Yeo, Sang-Hyuk;Seo, Hyun-Ju;Lim, Dong-Yeol
    • Bulletin of the Korean Chemical Society
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    • v.32 no.spc8
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    • pp.2916-2920
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    • 2011
  • Synthesis of halicylindramide A mimetics via solid-phase peptide synthesis is described. The N-Me-Gly-Thr residues in halicyclindramide A has been replaced by N-Me-Gly-Dpr, Lys, or N-Me-Gly-allo-Thr. Solution structures of the mimetics were compared by CD spectroscopy in an aqueous buffer and in TFE.

The Synthesis of Lithium Lanthanum Titanium Oxide for Solid Electrolyte via Ultrasonic Spray Pyrolysis (초음파 분무 열분해법을 이용한 고체전해질용 Lithium Lanthanum Titanium Oxide 제조)

  • Jaeseok, Roh;MinHo, Yang;Kun-Jae, Lee
    • Journal of Powder Materials
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    • v.29 no.6
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    • pp.485-491
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    • 2022
  • Lithium lanthanum titanium oxide (LLTO) is a promising ceramic electrolyte because of its high ionic conductivity at room temperature, low electrical conductivity, and outstanding physical properties. Several routes for the synthesis of bulk LLTO are known, in particular, solid-state synthesis and sol-gel method. However, the extremely low ionic conductivity of LLTO at grain boundaries is one of the major problems for practical applications. To diminish the grain boundary effect, the structure of LLTO is tuned to nanoscale morphology with structures of different dimensionalities (0D spheres, and 1D tubes and wires); this strategy has great potential to enhance the ion conduction by intensifying Li diffusion and minimizing the grain boundary resistance. Therefore, in this work, 0D spherical LLTO is synthesized using ultrasonic spray pyrolysis (USP). The USP method primarily yields spherical particles from the droplets generated by ultrasonic waves passed through several heating zones. LLTO is synthesized using USP, and the effects of each precursor and their mechanisms as well as synthesis parameters are analyzed and discussed to optimize the synthesis. The phase structure of the obtained materials is analyzed using X-ray diffraction, and their morphology and particle size are analyzed using field-emission scanning electron microscopy.

Reaction Characterization of Y2Ba1CU1O5 Oxides by Solid State Reaction Method and Pyrophoric Synthesis Method (고상반응법과 발화합성법에 의한 Y2Ba1CU1O5 산화물의 반응특성)

  • Park, Jeong-Shik
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

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Synthesis of Dermorphin Analogues by the Solid Phase Method and Biological Activity (고상법에 의한 Dermorphin 유사체의 합성과 생물학적 활성에 관한 연구)

  • Han, Man-So
    • Journal of the Korean Applied Science and Technology
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    • v.19 no.4
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    • pp.281-290
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    • 2002
  • Dermorphin is a hepta peptide(H-Tyr-DAla-Phe-Gly-Tyr-Pro-Ser-$NH_{2}$)with exceptionally potent and long-lasting peripheral and central activity. Dermorphin analogues, dermorphionyl(DMP)-Lys-$NH_{2}$ and DMP-Lys-Lys-$NH_{2}$ have been prepared in order to examine the effect of opiod activity. Dermorphin analogues were synthesized by the solid phase method. The crude peptide was purified by gel filter on a Sephadex LH-20, characterized with HPLC and amino acid analyzer. Analgesic potency was estimated by writhing syndrome method and Randall-Selitto method. As a result, dermorphin analogues have lower potency than that of morphine.

Novel Inhibitors of Prolyl 4-Hydroxylase; Solid-phase Synthesis of 2,2-Dimethyl-3,4-Dialkoxy-Substituted 6-Aminobenzopyran Derivatives

  • Seo, Jin-soo;Joo, Yang-Hee;Yi, Jung-Bum;Lee, Eun-Ju;Lee, Nam-Kyu;Cho, Yong-Balk;Kwak, Wie-Jong;Hwang, Jong-Yeon;Jeon, Yong-Seog;Jeon, Hyun-Suk;Yoo, Sung-eun;Yoon, Cheol-Min;Dong, Mi-Sook;Gong, Young-Dae
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.909-917
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    • 2006
  • 2,2-Dimethyl-3,4-dialkoxy-substituted 6-aminobenzopyran analogues (eg., 7 and 8) were identified as prolyl 4-hydroxylase inhibitors via a screening process using HSC-T6 and LI 90 cells that express an immortalized rat hepatic stellate cell line and as part of a test of the type I collagen contents employing the ELISA method. A subsequent lead optimization effort based on solid-phase parallel synthesis led to the identification of 2,2-dimethyl-3,4-dialkoxy-substituted 6-aminobenzopyrans as potent inhibitors of prolyl 4-hydroxylase.

Synthesis and characterization of α-mangostin imprinted polymers and its application for solid phase extraction

  • Zakia, Neena;Zulfikar, Muhammad A.;Amran, Muhammad B.
    • Advances in materials Research
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    • v.9 no.4
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    • pp.251-263
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    • 2020
  • α-mangostin imprinted polymers have been synthesized by a non-covalent imprinting approach with α-mangostin as a template molecule. The α-mangostin molecularly imprinted polymers (MIPs) prepared by radical polymerization using methacrylic acid, ethlylene glycol dimethacrylate, benzoyl peroxide, and acetonitrile, as a monomer, crosslinker, initiator, and porogen, respectively. The template was removed by using methanol:acetic acid 90:10 (v/v). The physical characteristics of the polymers were investigated by Fourier Transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The rebinding studies were carried out by batch methods. The results exhibited that the MIPs was able to adsorb the α-mangostin at pH 2 and the contact time of 180 min. The kinetic adsorption data of α-mangostin performed the pseudo-second order model and followed the Langmuir isotherm model with the adsorption capacity of 16.19 mg·g-1. MIPs applied as a sorbent material in solid-phase extraction, namely molecularly imprinted solid-phase extraction (MISPE) and it shows the ability for enrichment and clean-up of α-mangostin from the complex matrix in medicinal herbal product and crude extract of mangosteen (Garcinia mangostana L.) pericarp. Both samples, respectively, which were spiked with α-mangostin gives recovery more than 90% after through by MISPE in all concentration ranges.

Synthesis and Phase Transformation Behavior of YAG Powders by a Mechanochemical Solid Reaction (기계화학적 고상반응에 의한 YAG 분말의 합성 및 상 형성 거동에 관한 연구)

  • Jung Hyun-Gi;Hwang Gil-Ho;Lim Kwang-Young;Lee Young-Hun;Kang Sung-Goon
    • Journal of Powder Materials
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    • v.13 no.4 s.57
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    • pp.243-249
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    • 2006
  • Yttrium aluminum garnet (YAG) powders were synthesized via mechanochemical solid reaction using $Y_2O_3$ with three types of aluminum compounds. $Y_2O_3$ reacted mechanochemically with all A1 compounds and formed YAM (yttrium aluminum monoclinic), YAG and YAP (yttrium aluminum perovskite) phases depending on the starting materials. The ground samples containing ${\gamma}-A1_2O_3$ showed the best reactivity, whereas the ground sample containing A100H, which had the largest surface area, exhibited pure YAG after calcination at $1200^{\circ}C$. The sample containing Al had the least reactivity, producing YAP along with YAG at $1200^{\circ}C$. The types and grinding characteristics of the starting materials and grinding time are believed to be important factors in the mechanochemical synthesis of YAG.

Nano-particles of Mechanochemical Synthesis

  • Urakaev, Farit Kh.
    • Journal of the Speleological Society of Korea
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    • no.71
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    • pp.5-11
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    • 2006
  • A theoretical investigation of the solid phase mechanochemical synthesis of nano sized target product on the basis of dilution of the initial powdered reagent mixture by another product of an exchange reaction is presented. On the basis of the proposed 3 mode particle size distribution in mechanically activated mixture, optimal molar ratios of the components in mixture are calculated, providing the occurrence of impact friction contacts of reagent particles and excluding aggregation of the nanosized particles of the target reaction product. Derivation of kinetic equations for mechanochemical synthesis of nanoscale particles by the final product dilution method in the systems of exchange reactions is submitted. On the basis of obtained equations the necessary times of mechanical activation for complete course of mechanochemical reactions are designed. Kinetics of solid phase mechanosynthesis of nano TlCl by dilution of initial (2NaCl+$Tl_2SO_4$) mixture with the exchange reaction product (diluent,$zNa_2SO_4$, z=z*=11.25) was studied experimentally. Some peculiar features of the reaction mechanism were found. Parameters of the kinetic curve of nano TlCl obtained experimentally were compared with those for the model reaction KBr+TlCl+zKCl=(z+1) KCl+TlBr (z=z1*=13.5), and for the first time the value of mass transfer coefficient in a mechanochemical reactor with mobile milling balls was evaluated. Dynamics of the size change was followed for nanoparticle reaction product as a function of mechanical activation time.

Synthesis of Cyclic Antifreeze Glycopeptide and Glycopeptoids and Their Ice Recrystallization Inhibition Activity

  • Ahn, Mija;Murugan, Ravichandran N.;Shin, Song Yub;Kim, Eunjung;Lee, Jun Hyuck;Kim, Hak Jun;Bang, Jeong Kyu
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3565-3570
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    • 2012
  • Until now, few groups reported the antifreeze activity of cyclic glycopeptides; however, the tedious synthetic procedure is not amenable to study the intensive structure activity relationship. A series of N-linked cyclic glycopeptoids and glycopeptide have been prepared to evaluate antifreeze activity as a function of peptide backbone cyclization and methyl stereochemical effect on the rigid Thr position. This study has combined the cyclization protocol with solid phase peptide synthesis and obtained significant quantities of homogeneous cyclic glycopeptide and glycopeptoids. Analysis of antifreeze activity revealed that our cyclic peptide demonstrated RI activity while cyclic glycopeptoids showed no RI activity. These results suggest that the subtle changes in conformation and Thr orientation dramatically influence RI activity of N-linked glycopeptoids.