• 제목/요약/키워드: solid-phase synthesis

검색결과 313건 처리시간 0.021초

Synthesis of $La_{1-x}Sr_xCoO_3$ (x≤0.2) at Low Temperature from PVA-polymeric Gel Precursors

  • 권호진;박동곤;국승태;박휴범;김건
    • Bulletin of the Korean Chemical Society
    • /
    • 제18권12호
    • /
    • pp.1249-1256
    • /
    • 1997
  • Single phase La1-xSrxCoO3 (x≤0.2) was synthesized as a uniform sized 100 nm particulates with relatively high surface area of 20-30 m2/g, at low temperature (≥600 ℃), from a polymeric gel precursors prepared by using poly(vinyl alcohol) as homogenizer. No minor phase developed during the crystallization when polymer/metal mole ratio was higher than 3. As the polymer/metal mole ratio was raised in the gel, the amount of carbonaceous residues in the amorphous solid precursor prepared by heating the gel at 300 ℃ increased. Most of the residues were eliminated by exothermic thermal decomposition around 400 ℃. The amount of residual carbon (less than 1%) left in the crystalline La1-xSrxCoO3 decreased as more polymer was used, eliminating detrimental effect which might be posed by using large amount of organic homogenizer. The crystal structure of La1-xSrxCoO3 synthesized at temperature lower than 800 ℃ was observed to be shifted from rhombohedral to more symmetric cubic. The structure shifted back to rhombohedral as the cubic sample was annealed at 1000 ℃.

수산화암모늄나이트레이트(HAN)의 습식합성 및 이중 유기용매를 이용한 고체상 추출 (Wet Synthesis of Hydroxylammonium Nitrate (HAN) and Solid Phase Extraction Using Dual Organic Solvents)

  • 김소희;권윤자;전종기;조영민
    • 공업화학
    • /
    • 제31권3호
    • /
    • pp.317-322
    • /
    • 2020
  • 수산화암모늄나이트레이트(HAN; NH3OHNO3)는 낮은 용융점과 증기압의 특성을 가지고 있고, 상대적으로 높은 산소균형을 이루고 있는 이온성 화합물이다. 본 연구에서는 높은 함량의 액상추진제를 제조하기 위한 산화제로 활용하기 위하여 이중용매를 적용하여 고체입자상으로 얻었다. 감압 하에서 액상의 HAN으로부터 수분을 증발시킨 후, 반용매로서 아세톤과 에탄올을 적용하여 추출한 입자상의 HAN에는 13.8 wt%의 수분이 포함되어 있었다. 아세톤을 단독으로 적용하였을 때, 합성수율은 질량기준으로 최대 88%이었고, TGA로 측정된 최대 함량은 86.2%, 분해온도는 160~205℃ 범위로 나타났다.

고상법에 의한 Sr3Al2O6 형광체의 분말합성 및 발광특성 (Synthesis of Sr3Al2O6 Phosphors by Solid State Reaction and Its Luminescent Properties)

  • 김수진;원형일;원창환
    • 한국세라믹학회지
    • /
    • 제48권3호
    • /
    • pp.241-245
    • /
    • 2011
  • A red strontium aluminate phosphor ($Sr_3Al_2O_6:Eu^{3+},Eu^{2+}$) is synthesized using a solid state reaction method in air and reducing atmosphere. The investigation of firing temperature indicates that a single phase of $Sr_3Al_2O_6$ is formed when the firing temperature is higher than $1300^{\circ}C$. The effect of firing temperature and doping concentration on luminescent properties are investigated. $Sr_3Al_2O_6$ phosphor exhibits the typical red luminescent properties of $Eu^{3+}$ and $Eu^{2+}$.

Synthesis and Fragmentation of Furoxanaldehydes in the Gas Phase for Nanopatterned Alkyne Formation on a Solid Surface

  • Kim, Gi-Young;Kim, Ju-Cheon;Lee, Seung-Hee;Kim, Hyung-Jin;Hwang, Kwang-Jin
    • Bulletin of the Korean Chemical Society
    • /
    • 제30권2호
    • /
    • pp.459-463
    • /
    • 2009
  • Furoxanaldehydes possessing phenyl or alkenyl groups at the 3- or 4-position of the furoxan ring were designed for alkyne formation on a solid surface. Furoxans 2 and 3 were prepared from the corresponding alkenes 2a and 3a by the reaction with NaN$O_2$ in acetic acid. Furoxan 4, in which the furoxan ring is conjugated with a double bond, was prepared from bis(bromomethyl)benzene 4a in 5 steps using the Wittig reaction of aldehyde 1 as the key step. The electron beam-mediated fragmentation of furoxanaldehydes 1-4 in a mass spectrometer was exploited by focusing on alkyne formation on the solid surface. The fragmentation of furoxan 3 possessing diaryl groups afforded diarylacetylene at high efficiency, suggesting that the aryl group conjugated with the furoxan ring could facilitate alkyne formation with the evolution of NO.

초음파 분무에 의한 (Y,Gd)$BO_3:Eu^{3+}$ 형광체의 제조와 이의 발광 특성 (The Synthesis of (Y,Gd)$BO_3:Eu^{3+}$Phosphor by Ultrasonic Spray and Their Photoluminance Properties)

  • 김대수;김성우;이임렬
    • 한국전기전자재료학회:학술대회논문집
    • /
    • 한국전기전자재료학회 1999년도 추계학술대회 논문집
    • /
    • pp.107-110
    • /
    • 1999
  • The ultrasonic spray method was employed to make (Y,Gd)BO$_3$:Eu Phosphor, and its optical properties under 147nm VUV and 254 nm UV excitations were characterized and then compared with that produced by the solid-state reaction. The mixed solution of acetate hydrates of Y, Gd, Eu and boric acid diluted in water or methanol was used as the precursor fur the spray. It was found that (Y,Gd)BO$_3$:Eu phosphor made by this ultrasonic spray had a spherical shape and fine particle size of 1${\mu}{\textrm}{m}$. The crystalline structure for the as-sprayed phosphor was amorphous, but it converted into the same polycrystalline phase of solid state reaction after post heat treatment at 110$0^{\circ}C$ for 2hr. The emitting intensity under VUV and UV excitations for the spray-formed (Y,Gd)BO$_3$:Eu phosphor, however, was inferior to the later one. The excitation spectra were also studied and compared under VUV and UV excitations to explain the change of emitting intensity with Gd substitution in (Y$_{1-x}$ Gd$_{x}$)BO$_3$:Eu Phosphors made by spray and solid state reaction.on.

  • PDF

탄소 촉매에 의하여 성장된 별-모양 ZnO 나노 구조물의 합성과 광학적 특성 (Synthesis and optical properties of star-like ZnO nanostructures grown on with carbon catalyst)

  • 정일현;채명식;이의암
    • 반도체디스플레이기술학회지
    • /
    • 제9권2호
    • /
    • pp.1-6
    • /
    • 2010
  • Star-like ZnO nanostructures were grown on SI(100) substrates with carbon(C) catalyst by employing vapor-solid(VS) mechanism. The morphologies and structure of ZnO nanostructures were investigated by Field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and Raman spectrum, Photoluminescence spectrum. The results demonstrated that the as-synthesized products consisted of star-like ZnO nanostructure with hexagonal wurtzite phase. Nanostructures grown at 1100 were mainly star-like in structure with diameters of 500 nm. The legs of the star-like nanostructures were preferentially grown up along the [0001] direction. A vapor.solid (VS) growth mechanism was proposed to explain the formation of the star-like structures. Photoluminescence spectrum exhibited a narrow emission band peak around 380 nm and a broad one around 491 nm. Raman spectrum of the ZnO nanostructures showed oxygen defects in ZnO nanostructures due to the existence of Ar gas during the growth process, leading to the dominant green band peak in the PL spectrum.

$Pb(Zn_{0.6}Mg_{0.4})_{1/3}Nb_{2/3}O_3$[PZMN] 합성시 전구체 혼합방법에 따른 반응 경로변화 (Variations of Reaction Sequence with Precusor Mixing Methods in the Formation of $Pb(Zn_{0.6}Mg_{0.4})_{1/3}Nb_{2/3}O_3$[PZMN])

  • 김봉철;김정주;김남경;조상희
    • 한국세라믹학회지
    • /
    • 제35권5호
    • /
    • pp.458-464
    • /
    • 1998
  • Variations of reaction sequence of $Pb(Zn_{0.6}Mg_{0.4})_{1/3}Nb_{2/3}O_3$[PZMN] with precusor mixing methods were ex-amined using X-ray diffraction and dielectric characteristics. In the present study three different types of precursor mixing methods (oxide mixing PbO+$ZnNb_2O_6+MgNb_2O_6$[Zn+MN] and PbO+(Zn,Mg)$Nb_2O_6$[ZMN] precursor mixing) were adopted. When the oxide mixing method was used for the PZMN synthesis a Zn-rich perovskite phase and pyrochlore phase were formed. Compared with PbO+ZN+MN precursor mixing method the PbO-ZMN precursor led to a lowering of the formation temperature for perovskite sin-gle phase. These variation of composition and formation temperature of the perovskite phase were dis-cussed in terms of the difference in the solid-reaction requence between these three different types of pre-cursor mixing.

  • PDF

EFFECT OF SOYBEAN EXTRUSION ON NITROGEN METABOLISM, NUTRIENT FLOW AND MICROBIAL PROTEIN SYNTHESIS IN THE RUMEN OF LAMBS

  • Ko, J.Y.;Ha, J.K.;Lee, N.H.;Yoon, C.S.
    • Asian-Australasian Journal of Animal Sciences
    • /
    • 제5권3호
    • /
    • pp.571-582
    • /
    • 1992
  • Soybeans were dry extruded at three different temperatures (125, 135 and $145^{\circ}C$) for 30 s. Four lambs fitted with cannulae in the rumen and abomasums were used in a balanced $4{\times}4$ Latin square design. Lambs were fed at 2 h intervals for 12 times a day with automatic feeder to maintain steady state conditions in digestive tract. A dual-phase marker system was used to estivate ruminal flow rate of both liquid and solid digesta. Objectives of this study were to determine the effect of extrusion temperature of raw soybean on the ruminal liquid and solid dilution rate, nitrogen digestion and flow at the abomasum and availability of amino acid in lambs. There were no significant effects of extrusion on liquid and solid dilution rate, and liquid volume. Ruminal liquid flow rate was not influenced by extrusion and ranged from 389 to 435 ml/hr. Extrusion had no influence on ruminal OM digestion and flow rate to the abomasums. Dietary N flow to the abomasums increased (p < 0.05) as extruding temperature increased. Extruding temperature had a significant effect (p < 0.05) on flow of N escaping ruminal degradation and ranged from 34.91 to 57.38%. Microbial N synthesized/kg OMTDR ranged from 27 to 37 g and highest with $145^{\circ}C$ ESB diet. Extrusion decreased the amount of degradable amino acid in the rumen and increased the supply of amino acid to the lower gut, especially with 135 and $145^{\circ}C$ ESB diets.

SHS 마이크로파에 의한 TiZrB$_2$ 복합재료의 합성 및 특성연구 (A Study on Synthesis and Characterization of TiZrB$_2$ Composite by SHS Microwave)

  • 이형복;윤영진;오유근;안주삼
    • 한국세라믹학회지
    • /
    • 제36권1호
    • /
    • pp.7-14
    • /
    • 1999
  • SHS 마이크로파를 이용하여 티타늄, 지르코니움과 보론분말을 혼합하여 TiZrB2 고용체를 합성된 분말의 분말특성과 소결체의 소결특성을 연구하였다. 합성 중 온도 profile 결과 연소온도와 연소속도는 Zr의 몰비가 증가함에 따라 증가 하였으며, Ti0.2Zr0.8B2조서에서 연소온도와 연소속도는 285$0^{\circ}C$, 14.6m/sec로 최고값을 얻었다. 190$0^{\circ}C$에서 30 MPa의 압력으로 60분간 고온가압소결한 TiZrB2고용체는 TiB2와 ZrB2로 상분리가 최고값을 얻었다. 190$0^{\circ}C$에서 30MPa의 압력으로 60분간 고압가압소결한 TiZrB2 고용체는 TiB2와 ZrB2로 상분리가 일어나 복합체가 형성되었으며, Ti0.8Zr0.2B2에서 가장 좋은 물성값을 나타내었는데 상대밀도, 꺽임강도, 파괴인성 및 경도는 각각 99%, 680MPa, 7.3MPam1/2, 2750Kg/$ extrm{mm}^2$이었다.

  • PDF

MOCVD를 이용한 금속 촉매 종류에 따른 β-Ga2O3 나노 와이어의 제작과 특성 (Catalytic synthesis and properties of β-Ga2O3 nanowires by metal organic chemical vapor deposition)

  • 이승현;이서영;정용호;이효종;안형수;양민
    • 한국결정성장학회지
    • /
    • 제27권1호
    • /
    • pp.1-8
    • /
    • 2017
  • Metal organic chemical vapor deposition(MOCVD) 방법을 이용하여 금속 촉매에 따른 ${\beta}-Ga_2O_3$ 나노 와이어의 제작과 특성에 대해 연구하였다. 본 연구의 성장 조건에서 ${\beta}-Ga_2O_3$ 나노 와이어의 성장이 가능한 금속 촉매는 Au, Cu 그리고 Ni이 있었으며 각 금속 촉매로 성장한 나노 와이어는 성장률과 형상에 많은 차이가 있었다. Ni 촉매 성장의 경우에는 Vapor-Solid(VS) 과정이 ${\beta}-Ga_2O_3$ 나노 와이어 성장의 주된 메커니즘이고 Au, Cu 촉매 성장의 경우에는 Vapor-Liquid-Solid(VLS) 과정이 주된 성장 메커니즘 임을 확인할 수 있었다. 또한, 촉매의 종류에 따라서 ${\beta}-Ga_2O_3$ 나노 와이어의 광학적 특성도 다르게 나타나는 것을 확인할 수 있었다. 반면, 동일한 성장 조건에서 Ti, Ag 그리고 Sn 금속은 나노 와이어 성장을 위한 촉매로 작용하지 못하였다. 본 연구에서는 금속 촉매에 따른 나노 와이어의 성장 가능 여부와 성장한 나노 와이어의 특성 변화가 금속 촉매의 녹는 점, 금속- Ga의 공융 점과 관련이 있음을 상태도와 연관 지어 밝혀내었다.