• Title/Summary/Keyword: solid-phase synthesis

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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.

The Study of $K_2O-MgO-Al_2O_3-SiO_2-MgF_2$ System in Fluro-phlogopite Synthesis. (불소운모 합성에 따른 $K_2O-MgO-Al_2O_3-SiO_2-MgF_2$계의 연구)

  • 송경근;오근호;김대웅
    • Journal of the Korean Ceramic Society
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    • v.20 no.1
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    • pp.37-42
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    • 1983
  • An attempt was made to derive a possible synthetic mechanism of Fluoro-phlogopite (Mica, 4Mg.$Al_2O_3$.$6SiO_2$.$K_2O$.$2MgF_2$) The pevention of fluorine vaporization turned out to be the key in the synthesis of Mica in question.l Consequently the quinary system of Mica was seperately synthesized ; frist 4MgO.$Al_2O_3-6SiO_2$(ternary system) was sintered at 135$0^{\circ}C$ and $K_2O$ and $MgF_2$ were added and second 4MgO.$Al_2O_3-6SiO_2$.$K_2O$ (quarternary system) was heat-treated at 135$0^{\circ}C$ and $MgF_2$ was added. The ternary system resulted in Proto-enstatite Cordierite and Spinel phases while Forsterite and Leucite were shown in the quarternay system . In both methods Fluoro-phlogopite was systhesized but the solid state reactions to form Mica from the ternary system and the quarternary system were different. High temperature reactions in the formation of Mica were investigated employing XRD, DTA and SEM The study of the synthesis of Mica indirectly suggested a method of phase analysis of quinary system(MgO-$Al_2O_3-SiO_2-K_2O-MgF_2$) and quarternary system(MgO-$Al_2O_3-SiO_2-K_2O-MgF_2$) at various temperatures.

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Solid Phase Synthesis of N-(3-hydroxysulfonyl)-L-homoserine Lactone Derivatives and their Inhibitory Effects on Quorum Sensing Regulation in Vibrio harveyi (고체상 합성법에 의해 합성된 N-(3-hydroxysulfonyl)-L-homoserine Lactone 유사체들의 Vibrio harveyi 쿼럼 센싱에 대한 저해 효과)

  • Kim, Cheol-Jin;Park, Hyung-Yeon;Kim, Jae-Eun;Park, Hee-Jin;Lee, Bon-Su;Choi, Yu-Sang;Lee, Joon-Hee;Yoon, Je-Yong
    • Microbiology and Biotechnology Letters
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    • v.37 no.3
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    • pp.248-257
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    • 2009
  • The inhibitors against Vibrio harveyi quorum sensing (QS) signaling were developed by modifying the molecular structure of the major signal, N-3-hydroxybutanoyl-L-homoserine lactone (3-OH-$C_4$-HSL). A series of structural derivatives, N-(3-hydroxysulfonyl)-L-homoserine lactones (HSHLs) were synthesized by the solid-phase organic synthesis method. The in vivo QS inhibition by these compounds was measured by a bioassay system using the V. harveyi bioluminescence, and all showed significant inhibitory effects. To analyze the interaction between these compounds and LuxN, a 3-OH-$C_4$-HSL receptor protein of V. harveyi, we tentatively determined the putative signal binding domain of LuxN based on the sequence homology with other acyl-HSL binding proteins, and predicted the partial 3-D structure of the putative signal binding domain of LuxN by using ORCHESTRA program, and further estimated the binding poses and energies (docking scores) of 3-OH-$C_4$-HSL and HSHLs within the domain. In comparison of the result from this modeling study with that of in vivo bioassay, we suggest that the in silica interpretation of the interaction between ligands and their receptor proteins can be a valuable way to develop better competitive inhibitors, especially in the case that the structural information of the protein is limited.

Synthesis of Yba2Cu3O7-y Superconductor using a Low Purity BaCO3 Powder (저 순도 BaCO3 분말을 사용한 Yba2Cu3O7-y 초전도체의 합성)

  • Kim, Chan-Joong;Park, Soon-Dong;Choi, Jung-Suk;Jun, Byung-Hyuk;Moon, Jong-Baik;Lee, Sang-Heon;Sung, Tae-Hyun
    • Journal of Powder Materials
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    • v.15 no.1
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    • pp.6-12
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    • 2008
  • [ $YBa_2Cu_3O_{7-y}$ ](123) powders were synthesized by the solid state reaction method using two different purity $BaCO_3$ powders (99.75% and 99.7% purity) and $Y_2O_3$ (99.9%) and CuO (99.9%) powders. The effect of $BaCO_3$ purity on the formation of a 123 phase and the superconducting properties were investigated. The mixtures of raw powders were calcined at temperature ranges of $800^{\circ}C-880^{\circ}C$ in air and finally made into a single grain samples by a melt processing with top seeding. It was found that a 123 phase was well formed at temperature above $870^{\circ}C$, but the purity effect on the 123 formation was negligible. The single-grain 123 samples prepared from the different $BaCO_3$ powders showed the same $T_c$ value of 90.5 K and similar $J_c$ values about $10^4\;A/cm^2$ at 0 T and 77 K, and $10^3\;A/cm^2$ at 2 T and 77 K. This result indicates that the low purity, cheap price $BaCO_3$ powder can be used as a raw material for the fabrication of single-grain, high-$J_c$ superconducting levitator.

Synthesis of Single-Crystalline InSb Nanowires Using CVD Method and Study of Growth Mechanism in Open and Close System (CVD 방법을 이용한 단결정 InSb 나노와이어의 성장과 Open/Close 시스템에서의 반응 메커니즘 연구)

  • Kang, Eun Ji;Park, Yi-Seul;Lee, Jin Seok
    • Journal of the Korean Vacuum Society
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    • v.22 no.6
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    • pp.306-312
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    • 2013
  • Single-crystalline InSb nanowire was synthesized on $SiO_2$ wafer via vapor-liquid-solid (VLS) mechanism using chemical vapor deposition method. According to the source container system (open or close) which contain InSb powder and $SiO_2$ wafer, the single-crystalline InSb nanowires have different growth mechanisms. Structural characterization of the InSb nanowires was examined by scanning electron microscope (SEM). Composition of the nanowires was investigated using x-ray diffraction (XRD) and energy dispersive x-ray spectroscopy (EDS). This study demonstrates that length and diameter of the InSb nanowires are long and thick using open-boat system by VLS and additional vapor-solid (VS) mechanisms, because open-boat system can carry a large amount of vapor-phase InSb precursor than close-boat system.

A novel approach for rice straw agricultural waste utilization: Synthesis of solid aluminosilicate matrices for cesium immobilization

  • Panasenko, A.E.;Shichalin, O.O.;Yarusova, S.B.;Ivanets, A.I.;Belov, A.A.;Dran'kov, A.N.;Azon, S.A.;Fedorets, A.N.;Buravlev, I. Yu;Mayorov, V. Yu;Shlyk, D. Kh;Buravleva, A.A.;Merkulov, E.B.;Zarubina, N.V.;Papynov, E.K.
    • Nuclear Engineering and Technology
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    • v.54 no.9
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    • pp.3250-3259
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    • 2022
  • A new approach to the use of rice straw as a difficult-to-recycle agricultural waste was proposed. Potassium aluminosilicate was obtained by spark plasma sintering as an effective material for subsequent immobilization of 137Cs into a solid-state matrix. The sorption properties of potassium aluminosilicate to 137Cs from aqueous solutions were studied. The effect of the synthesis temperature on the phase composition, microstructure, and rate of cesium leaching from samples obtained at 800-1000 ℃ and a pressure of 25 MPa was investigated. It was shown that the positive dynamics of compaction was characteristic of glass ceramics throughout the sintering. Glass ceramics RS-(K,Cs)AlSi3O8 obtained by the SPS method at 1000 ℃ for 5 min was characterized by a high density of ~2.62 g/cm3, Vickers hardness ~ 2.1 GPa, compressive strength ~231.3 MPa and the rate of cesium ions leaching of ~1.37 × 10-7 g cm-2·day-1. The proposed approach makes it possible to safe dispose of rice straw and reduce emissions into the atmosphere of microdisperse amorphous silica, which is formed during its combustion and causes respiratory diseases, including cancer. In addition, the obtained is perspective to solve the problem of recycling long-lived 137Cs radionuclides formed during the operation of nuclear power plants into solid-state matrices.

Effect of the pH of Pyrophoric Synthetic Solution on the Formation Kinetics of Y1Ba2Cu3O7-x Superconducting Phase (발화합성용액의 pH가 Y1Ba2Cu3O7-x 초전도상 생성 속도에 미치는 영향)

  • Park, J.S.;Kim, Y.S.;Yang, S.W.;Kim, C.Y.;Shin, H.S.
    • Applied Chemistry for Engineering
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    • v.9 no.2
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    • pp.165-171
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    • 1998
  • The $Y_1Ba_2Cu_3O_{7-x}$(123) superconductor powders were prepared by pyrophoric synthesis method(PSM) using $Y_2O_3$(99.9%), $BaCO_3$(99.9%), and CuO(99.9%) powders. The phase formation and reaction kinetics of 123 superconductor manufactured with powders prepared in various pHs of pyrophoric synthetic solution have been studied through the experiments at various heat treatment temperatures and times. Inductively coupled plasma(ICP) spectroscopy and scanning electron microscopy(SEM) measurements were performed to examine the composition and morphology of the sample. X-ray diffraction(XRD) analysis was done to determine phase formation and conversion ratio of Y-Ba-Cu-O systems. The 123 powder prepared at pH 7(${\pm}0.3$) yields the best result in terms of purity, homogeneity, and reactivity. The activation energies(${\Delta}E_a$) of 123 phase formation were found to be 191 kJ/mol and 230kJ/mol in solid state reaction method and pyrophoric synthesis method, respectively.

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A Study on the Synthesis of Gd-doped $CeO_2$ and Sr-doped $LaMnO_3$ Powders and Phase Stability in Their Interface (Gd-doped $CeO_2$ 와 Sr-doped $LaMnO_3$ 분말의 합성 및 그 계면에서의 상 안정성 연구)

  • 정승훈;김남진;이덕열
    • Journal of the Korean Ceramic Society
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    • v.34 no.6
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    • pp.652-658
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    • 1997
  • The phase stability in the interface of Sr-doped LaMnO3(LSM)/Gd-doped CeO2(CGO) was examined in this study in order to check the feasibility of using LSM as the cathode material in a low-temperature SOFC(solid oxide fuel cell) using CGO as the electrolyte. For the purpose, CGO powders of Ce0.82Gd0.18O0.91 and two LSM powders having different compositions, La0.9Sr0.1MnO3(LSM10) and La0.5Sr0.5MnO3(LSM50), were synthesized using Pechini method. Then, specimens having the LSM/CGO interface were prepared, heat-treated at 130$0^{\circ}C$ for up to 3 days, and analyzed by XRD and STEM/EDX. Face-centered cubic CGO powders of less than 10 nm size were obtained by calcination of polymeric precursor formed in the process at 45$0^{\circ}C$. Higher calcination temperature of $700^{\circ}C$ was necessary for monoclinic LSM10 and cubic LSM50 powders. LSM powders were coarser than CGO and observed to be in the range of 50~100 nm. No trace of LSM-CGO interaction product was found in the XRD pattern. Also it was known from the concentration profile in the vicinity of the interface that interdiffusion was occurred over only a small penetration depth of ~100 nm order.

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Effect of BaF2 as a Flux in Solid State Synthesis of Y3Al5O12:Ce3+ (고상법을 이용한 Y3Al5O12:Ce3+의 제조에서 BaF2가 미치는 영향)

  • Won, Hyung-Seok;Hayk, Nersisyan;Won, Chang-Whan;Won, Hyung-Il
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.604-610
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    • 2011
  • The effect of $BaF_2$ flux in $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) formation was investigated. Phase transformation of $Y_3Al_5O_{12}$(YAG) was characterized by using XRD, SEM, and TEM-EDS, and it was revealed that the sequential formation of the $Y_4Al_2O_9$(YAM), $YAlO_3$(YAP) and $Y_3Al_5O_{12}$(YAG) in the temperature range of 1000-1500$^{\circ}C$. Single phase of YAG was revealed from 1300$^{\circ}C$. In order to find out the effect of $BaF_2$ flux, three modeling experiments between starting materials (1.5$Al_2O_3$-2.5$Y_2O_3$, $Y_2O_3$-$BaF_2$, and $Al_2O_3$-$BaF_2$) were done. These modeling experiments showed that the nucleation process occurs via the dissolution-precipitation mechanism, whereas the grain growth process is controlled via the liquid-phase diffusion route. YAG:Ce phosphor particles prepared using a proposed technique exhibit a spherical shape, high crystallinity, and an emission intensity. According to the experimental results conducted in this investigation, 5% of $BaF_2$ was the best concentration for physical, chemical and optical properties of $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) that is approximately 10-15% greater than that of commercial phosphor powder.

Synthesis of Cocoa Butter Alternative from Coconut Oil Fraction and Palm Oil Fractions by Lipase-Catalyzed Interesterification (Coconut Oil 분별유와 Palm 분별유로부터 효소적 Interesterification에 의한 코코아 버터 대체유지 합성)

  • Bae, Sang-Kyun;Lee, Kyung-Su;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.10
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    • pp.1487-1494
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    • 2010
  • Structured lipid (SL) for cocoa butter alternative was synthesized by interesterification of coconut oil fraction and palm stearin (6:4 and 8:2, by weight) in a shaking water bath at $60^{\circ}C$ and 180 rpm. It was performed for various reaction times (1, 2, 3, and 6 hr). The reaction was catalyzed by sn-1,3 specific Lipozyme TLIM (immobilized lipase from Thermomyces lanuginosus). SL-solid part was obtained from acetone fractionation at $0^{\circ}C$. SL-solid part was blended with other palm oils and fractions for desirable property of cocoa butter alternative (SL-solid part : palm middle fraction : palm stearin solid : palm oil, 70.4:18.4:2.9:8.3, by weight). In reversed-phase HPLC analysis, triacylglycerol species of cocoa butter alternative had partition number of 40 (10.77%), 42 (13.06%), 44~46 (17.38%) and 48 (51.88%). Major fatty acids of cocoa butter alternative were lauric acid (16.5%), myristic acid (12.28%), palmitic acid (46.03%), and linoleic acid (14.75%). Solid fat content (SFC) and polymorphic form (${\beta}'$ form) of cocoa butter alternative prepared were similar to those of commercial cocoa butter replacer (CBR).