• Title/Summary/Keyword: 하소 반응

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Synthesis of potassium titanate by wet process (습식법에 의한 티탄산칼륨 섬유의 합성)

  • 강대갑;송종택
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.5 no.3
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    • pp.278-283
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    • 1995
  • The potassium titanate fibres were synthesized with wet process by the addition of KOH solution to the TiOz gel produced by the reaction between element titanium particles and $H_2O_2$ solution at $50^{\circ}C$. And then they were characterized by XRD, SEM and FT - IR. It was found that potassium titanate fibres were mainly affected by KOH/TiOz mole ratio, synthesis time and aging time in this wet process employed. For $KOH/TiO_2 = 1/1$, synthesizing time 24 hrs, aging time 24 hrs and calcination temperature of TEX>$900^{\circ}C$ for 1 hr, their products were mainly found to be potassium tetratitanate which had thin and long fibres in the range of 10 ~ 20 mm. As the synthesizing time increased and the amount of KOH decreased, potassium tetratitanate was converted into potassium hexatitanate. Also, the length of their fibres became short.

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A Study on Calcination and Reduction of AUC (Ammonium Uranyl Carbonate) -Characteristics and Phase Change of Powder- (AUC(Ammonium Uranyl Carbonate)의 하소 및 환원 반응 -분말의 특성 및 상변화-)

  • 김응호;최청송;박진호;장인순
    • Journal of the Korean Ceramic Society
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    • v.30 no.4
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    • pp.279-288
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    • 1993
  • A study on calcination and reduction of AUC(ammonium uranyl carbonate, (NH4)4UO2(CO3)3) has been carried out by using TG-DTA in N2, air and H2 atmospheres, respectively. Phases of various intermediate obtained during thermal analysis of AUC in different atmospheres were confirmed by XRD. Powder characteristics of each intermediate were investigated by measuring particle size and specific surface area, and also observed by SEM. As a results, regardless of applied atmosphere AUC was calcined into amorphous UO3, which was converted to $\alpha$-U3O8 Via $\alpha$-UO3 in both H2 and N2 atmosphere, but directly into $\alpha$-UO3 in air atmosphere. Further reduction of U3O8 was only detectable in hydrogen atmosphere. During calcination and reduction, average particle size was reduced to less than 30% of original value without morphology change. Specific surface area was dramatically increased with release of NH3, CO2 and H2O from AUC powder and reached maximum value around 25$0^{\circ}C$, and then gradually decreased with the increase of temperature due to sintering effect of uranium oxides such as UO3 and U3O8. It was also found that the change of average crystallite size and pore size were closely related to the changes of specific surface area of uranium oxides.

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A Synthesis of Spherical Shape $TiO_2-SiO_2$ Complex via Solvothermal Process and Thermal Properties at Non-Isothermal (용매열합성을 이용한 구형 $TiO_2-SiO_2$ 복합체 제조 및 열적특성)

  • Cho Tae-Hwan;Park Seong-Jin
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.2 s.35
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    • pp.141-147
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    • 2005
  • Nanomaterial $TiO_2-SiO_2$ was synthesized by hydrolysis and condensation process using 2-propanol(2-PrOH) and was characterized by FT-IR, DSC, XRD and FE-SEM. FT-IR spectra were measured to investigate Ti-0-Si absorption peak. DSC thermal analysis results appllied to Ozawa equation were used to calculate to activation energy of crystallization. It was found that the changes of X-ray diffraction patterns and FWHM obtained XRD measurement depended on calcination temperature. In FE-SEM analysis, particle size changed by quantity changes of Ti-alkokide.

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Morphology of Barium Titanyl Oxalate Produced by Homogeneous Precipitation from Acidic Solution of Dimethyl Oxalate (Dimethyl Oxalate에 의한 균일 침전법으로 생성된 Barium Titanyl Oxalate의 형태학적 연구)

  • Min, Chonkyu;Lee, Chul
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.203-208
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    • 1997
  • Barium titanyl oxalate(BTO) was precipatated by utilizing the thermal decomposition of dimethyl oxalate in acidic aqueous solution having $BaCl_2$ and $TiCl_4$. Particle morphology of BTO was influeneced by the various experimental factors. i.e.. the faster rate to nucleation with higher temperature and the higher ratio of [DMO]/[$Ba^{2+}+Ti^{4+}$] was found to correspond to the faster rate of transformation of particle size distribution from unimodal to broad unimodal through bimodal. The BT powder obtained by calcination at $900^{\circ}C$ in air consists of larger particles than BT generated by general coprecipitation method and shows tetragonal symmetry. The stirring during reaction was also found to have much effect upon characteristics of BTO and BT.

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다양한 활성제 이온이 도핑된 La2WO6 형광체의 제조와 발광 특성

  • Ryu, Hyeon-Tae;Hong, Sun-Gi;Im, Myeong-Hwan;Lee, Eun-Gyeong;Sin, Yu-Hui;Jo, Sin-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.191.1-191.1
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    • 2015
  • 최근에 백색 발광다이오드를 개발하기 위한 고효율의 형광체 개발에 많은 연구가 집중되고 있다. 본 연구에서는 $La_2WO_6$ 모체 결정에 다양한 활성제 이온인 $Eu^{3+}$, $Dy^{3+}$, $Sm^{3+}$, $Tb^{3+}$를 각각 도핑하여 다양한 발광 파장을 갖는 고효율의 형광체를 제조하였다. 합성한 형광체 분말은 초기물질 $La_2O_3$, $WO_3$, 희토류 원소 ($Eu_2O_3$, $Dy_2O_3$, $Sm_2O_3$, $Tb_4O_7$)를 각각 화학양론적으로 준비하여 고상반응법으로 제조하였으며, 이때 하소 공정은 $400^{\circ}C$에서 3시간, 소결 공정은 $1050^{\circ}C$에서 5시간 유지하여 합성하였다. $La_2WO_6:Eu^{3+}$ 형광체 분말의 경우에 320, 395, 465 nm에서 강한 흡광 파장이 발생하였으며, 파장 320 nm로 여기 시켰을 때 최대 발광 세기는 618 nm에서 관측되었다. $Sm^{3+}$을 도핑한 형광체의 흡광 스펙트럼은 310, 375, 406, 475 nm에서 발생하였으며, 310 nm로 여기 시켰을 때 602 nm의 강한 주황색 발광 신호가 나타났다. $Dy^{3+}$가 도핑된 $La_2WO_6$ 형광체는 575 nm에 강한 발광 피크를 갖는 황색을 나타내었으며, 흡광 파장은 313 nm 이었다. $Tb^{3+}$를 도핑한 형광체의 주 흡광 스펙트럼은 316 nm에서 발생하였고, 발광 스펙트럼은 545 nm에 피크를 갖는 녹색 발광 신호가 나타났다. 활성제이온의 종류에 따른 형광체의 흡광과 발광, 결정 구조의 특성을 체계적으로 제시하고자 한다.

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Application of Response Surface Method for Modeling of Room Temperature Resistivity of $(Ba_{0.8-x}Sr_{0.2})Y_xTiO_3$ ($(Ba_{0.8-x}Sr_{0.2})Y_xTiO_3$의 상온비저항을 모델링하기 위한 반응표면분석법의 적용)

  • Moon, Hyung Chul;Noh, Tae Yong;Kim, Seung Won;Lee, Chul
    • Journal of the Korean Chemical Society
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    • v.42 no.6
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    • pp.652-656
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    • 1998
  • $(Ba_{0.8-x}Sr_{0.2})Y_xTiO_3\;(BSYT)$ powders were prepared by the calcination of metal-oxalate precipitates, which were obtained by wet chemical method using Ba, Sr, Y and Ti-nitrates and oxalic acid. Yttrium content, sintering temperature and cooling rate were taken as experimental factors. Response surface method was applied to modelling of the room temperature resistivity of BSYT. The results indicated that the Yttrium content had larger effect on the room temperature resistivity and minimum room temperature resistivity was at Yttrium content of 0.24 mol%. The validity of a modelling equation was confirmed by comparing the measured room temperature resistivity with the calculated one.

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A study on the gas reaction mechanism in catalyst/$SnO_2$ gas sensor (촉매/$SnO_2$ 가스 센서의 반응 구조에 관한 연구)

  • 이재홍;김창교;김진걸;조남인;김덕준
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.2
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    • pp.276-283
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    • 1997
  • A dry impregnation method was used for preparing pellet type Pt/$SnO_2$ gas sensor. The crystal structure, direction of the crystal, crystal size and microstructure between the catalyst and the support ($SnO_2$) were characterized with electron diffraction analysis, transmission electron microscopy, scanning electron microscopy. The characterization indicates that when Pt/$SnO_2$ sample is calcined at $400^{\circ}C$, the Cl content associated with the Pt phase diminishes and the part of Pt is moved into $SnO_2$ support. This results in the enhancement of gas sensitivity. After the reactor with a Pt/$SnO_2$ sample was run with a flow rate of 30 sccm (a mixture of 0.5% $H_2$ in $_N2$) for a while, the resistance of $SnO_2$ was saturated, but the $SnO_2$ kept absorbing $H_2$ gas. This indicates that the surface state was saturated. For the 14 ppm $H_2$ gas, the sensitivity of Pt/$SnO_2$ devices was about 81% at an operating temperature of $300^{\circ}C$.

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Synthesis and Luminescence Properties of $GdNbO_4$ : $Eu^{3+}$ Phosphors

  • Gwon, Bang-Gil;Jo, Sin-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.324-325
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    • 2011
  • 최근에 고효율의 적색 형광체를 합성하여 형광 램프, 음극선관, X-선 검출기, 전계 발광 디스플레이에 응용하기 위하여 다양한 모체 결정과 활성체를 도핑하는 연구가 활발히 진행되고 있다. 본 연구에서는 $GdNbO_4$ 모체 결정에 $Eu^{3+}$ 이온 활성체를 주입하여 합성함으로써 새로운 적색 형광체의 발광 세기와 입자의 형상을 최적화 시키고자 한다. 형광체 분말 시료의 제조는 Eu의 함량을 0, 0.05, 0.10, 0.15, 0.20 mol로 변화시키면서 고상 반응법을 이용하여 합성하였다. 초기 물질 Gd2O3 (99.99%), $Nb_2O_5$ (99.99%), $Eu_2O_3$ (99.9%)를 화학 적량으로 측량하고 에탄올과 ZrO2 볼과 함께 플라스틱 병에 넣어 400 rpm의 속도로 24시간 볼밀 작업을 수행한 후에, 혼합된 분말의 볼을 걸러내고 60$^{\circ}C$에서 20시간 동안 건조하였다. 건조된 시료를 막자 사발에 넣고 잘게 갈아서 체로 걸러낸 다음에 세라믹 도가니에 넣고 전기로에서 분당 5$^{\circ}C$씩 승온하여 500$^{\circ}C$에서 10시간 동안 1차 하소한 후에, 계속 온도를 승온시켜 1,200$^{\circ}C$에서 3시간 동안 소결하여 합성하였다. XRD 회절 패턴의 경우에, $Eu^{3+}$의 함량에 관계없이 모든 세라믹은 JCPDS (22-1104)에 제시된 회절상과 일치하는 사방정계의 결정 구조를 가짐을 확인할 수 있었다. 주 피크는 28.4$^{\circ}$에서 최대값을 갖는 (121)면에서 발생하는 회절 신호이었다(Fig. 1). 적색 형광체 분말의 광학 및 표면 특성은 PL, PLE와 SEM으로 조사되었으며, 세라믹 분말의 형광 특성과 결정 구조, 표면 형상에 대한 자세한 논의가 제시될 것이다.

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Sintering of Alumina in the Presence of Oxynitride Additives (Oxynitride의 첨가에 의한 알루미나의 소결)

  • Bae, Won-Tae;Kim, Hae-Du
    • 연구논문집
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    • s.30
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    • pp.111-119
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    • 2000
  • Sintering of alumina powder was studied in the presence of Y-Si oxide and oxynitride additives. The main crystalline phase of the sintering aids pre-reacted at $1400^{\circ}C$ was $\alpha$ - $Y_2$$SiO_2$>$O_7$. Y-N apatite was co-existed in the Si-40N sintering aid because of its high content of N. During the sintering process, liquid phases were formed by the reaction between additives and alumina, and these liquid phases promote the densification of alumina. SEM micrographs showed that uniform grain growth occurred in the system with oxide additive(Si-0N). In the case of oxynitride additive system(Si-20N and Si-40N), bimodal microstructure was observed due to the exaggerated grain growth, As the nitrogen content in the additive system increased the exaggerated grain growth occurred extensively. Bloating, which seemed to be originated by the liberation of $N_2$ gas, occurred un the Si-40N oxynitride additive system.

A Study on the Formation of Hydrous Ferric Oxide from Ferrous Sulfate (黃酸第一鐵로부터 含水酸化鐵生成에 關한 硏究)

  • Sung Joo Kyung;Suhl Soo Duk;Whang Yong Kil
    • Journal of the Korean Chemical Society
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    • v.19 no.2
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    • pp.142-146
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    • 1975
  • The formation of iron oxide hydroxide in a ferrous sulfate was studied in different contents of iron in the solution at a temperature range of 90 to $100^{\circ}C$ under 1${\sim}$3 atmospheres. The Mohr's salt thus formed was hydrolyzed under 1 to 3 atmospheres, in 14 to 72 g/l of iron content in the solution pH 3 or 6 for two hours at 90 to $100^{\circ}C$. The results obtained was as follows; 1) In Mohr's salt solution, as the iron content was increased, with decreasing the concentration of hydrogen ion, the yield of iron oxide hydroxide was gradually increased. 2) When iron content in Mohr's salt solution was 42.81 g/l, 91.5% of iron was recovered in the form of $\alpha$-goethite similar to yellow grade of natural goethite. 3) When $\alpha$-goethite obtained was calcined of $500^{\circ}C$, it was turned into ${\alpha}$-ferric oxide with a redish brown colour.

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