• Title/Summary/Keyword: Calcination effects

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Characterization of the Catalytic Heteropoly Compounds using Solid-state NMR

  • Kim, Y;Lee, W
    • Journal of the Korean Magnetic Resonance Society
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    • v.1 no.1
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    • pp.45-58
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    • 1997
  • Heteropoly compounds, H3PMo12O40, CsxH3-xPMo12O40, and vanadium containing heteropoly compound were characterized by Solid-state broad line 1H MAS NMR, 31P MAS NMR, and High Speed MAS 51V NMR spectroscopy of quadrupolar nuclei. The effects of calcination, dehydration, and the number of protons on the structure of heteropoly compounds were studied. The results of this study demonstrate that these Solid-state NMR techniques are very useful tools to study heteropoly compounds.

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Characteristics of Crystallinity and Morphology of Barium Titanate Particles Prepared by Spray Pyrolysis (분무열분해 공정에 의해 합성된 바륨 티타네이트 분말의 결정화 및 형태 특성)

  • Lee, Kyo Kwang;Jung, Kyeong Youl;Kim, Jung Hyun;Koo, Hye Young;Ju, Seo Hee;Kang, Yun Chan
    • Korean Chemical Engineering Research
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    • v.43 no.4
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    • pp.517-524
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    • 2005
  • Barium titanate ($BaTiO_3$) particles were prepared by spray pyrolysis from spray solution containing organic additives. The effects of the type and amount of organic precursors on the crystal structure and morphology of the $BaTiO_3$ particles were investigated. It was found that the morphology of $BaTiO_3$ particles before and after calcination depended on the type of organic additives such as citric acid, ethylene glycol and polyethylene glycol. Among these organic additives, citric acid was the most effective to prepare $BaTiO_3$ particles with nano-structured morphology consisting with uniform size nanometer particles after calcination. It was also found that the phase transformability of the metastable cubic phase to the tetragonal one during calcination could be improved by increasing the content of citric acid in the spray solution. As a result, $BaTiO_3$ particles prepared from spray solution containing high concentration of citric acid had good tetragonality, uniform and fine size, and high BET surface area after calcination. $BaTiO_3$ particles prepared by spray pyrolysis had nanometer size and uniform morphology after simple ball milling process.

PTCR Effects in Molten Salt System Synthesized Semiconductive $BaTiO_3$ (용융염 합성법에 의한 반도성 $BaTiO_3$의 PTCR 효과)

  • 윤기현;오기영
    • Journal of the Korean Ceramic Society
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    • v.22 no.3
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    • pp.13-18
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    • 1985
  • Semiconductive $Ba_{0.9}Sr_{0.1}TiO_3$ was prepared by both the Calcining of mixed Oxides (C. M. O) and the Molten Salt Synthesis(M.S.S) methods to investigate the PTCR effects. In the Molten Salt Synthesis method the temperature of calcination for Synthesis of $BaTiO_3$ could be lowered from 110$0^{\circ}C$ to 80$0^{\circ}C$. The M.S.S Specimens had smaller grain size and more homogeneous size distribution at the same sintering temperature as compared with the C. M. O specimens. The M. S. S. specimens showed greater PTCR effects and current variations in the time vs. current charac-teristics than those of C. M. O Specimens.

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Synthesize multi-walled carbon nanotubes via catalytic chemical vapour deposition method on Fe-Ni bimetallic catalyst supported on kaolin

  • Aliyu, A;Abdulkareem, AS;Kovo, AS;Abubakre, OK;Tijani, JO;Kariim, I
    • Carbon letters
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    • v.21
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    • pp.33-50
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    • 2017
  • In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide ($NiFe_2O_4$). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The $N_2$ adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

Synthesis of ${\alpha}$-Alumina Nanoparticles Through Partial Hydrolysis of Aluminum Chloride Vapor (염화알미늄 증기의 부분가수분해를 통한 알파 알루미나 나노입자 제조)

  • Park, Hoey Kyung;Yoo, Youn Sug;Park, Kyun Young;Jung, Kyeong Youl
    • Korean Chemical Engineering Research
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    • v.49 no.5
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    • pp.664-668
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    • 2011
  • Spherical alumina precursors represented by $AlO_xCl_y(OH)_z$, 30~200 nm in particle diameter, were prepared by partial hydrolysis of $AlCl_3$ vapor in a 500 ml reactor. Investigated on the particle morphology and size were the effects of the reaction time, the stirring speed and the reaction temperature. The particle morphology and size was insensitive to the reaction time in the range 20 to 300 s. The variation of the stirring speed from 0 to 300 and 800 rpm showed that the particle size was the largest at 0 rpm. As the temperature was varied from 180 to 190, 200, $140^{\circ}C$, the particle size showed a maximum at $190^{\circ}C$. By calcination of the as-produced particles at $1,200^{\circ}C$ for 6h with a heating rate of $10^{\circ}C$/min, ${\alpha}$-alumina particles 45 nm in surface area equivalent diameter were obtained. The particle shape after calcination turned wormlike due to sintering between neighboring particles. A rapid calcination at $1400^{\circ}C$ for 0.5 h with a higher heating rate of $50^{\circ}C$/min reduced the sintering considerably. An addition of $SiCl_4$ or TMCTS(2,4,6,8-tetramethylcyclosiloxane) to the $AlCl_3$ reduced the sintering effectively in the calcination step; however, peaks of ${\gamma}$ or mullite phase appeared. An addition of $AlF_3$ to the particles obtained from the hydrolysis resulted in a hexagonal disc shaped alumina particles.

Catalytic Deep Oxidation of Volatile Organic Compounds Toluene and Toluene+Xylene over γPt/γ-Al2O3 Catalysts at Lower Temperatures (알루미나에 담지한 백금 촉매상에서 휘발성 유기화합물 톨루엔 및 톨루엔+자일렌의 저온산화)

  • Kim Sang-Hwan;Kang Tae-Sung;Yang Hee-Sung;Nhu Y Vu Trinh;Park Hyung-Sang
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.6
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    • pp.799-807
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    • 2006
  • The catalytic activity of $Pt/{\gamma}-Al_2O_3$ catalysts for the oxidation of toluene and toluene+xylene mixture was investigated in the microreactor of fixed-bed type. The calcination temperatures and loadings of $Pt/{\gamma}-Al_2O_3$ catalysts played the important role in the activity of catalysts for the oxidation of toluene. The increasing calcination temperatures and loadings of $Pt/{\gamma}-Al_2O_3$ catalysts increased the crystallite size of the platinum to result in the higher oxidation activity of catalysts. The catalytic activity for the toluene oxidation over $Pt/{\gamma}-Al_2O_3$ catalysts turned out to be increasing in the order of $500^{\circ}C\;<\;800^{\circ}C<600^{\circ}C\;<\;700^{\circ}C$ for calcination temperatures and 0.1 wt% < 0.3 wt% < 1.0 wt% for platinum loadings, respectively. The 1.0 wt% $Pt/{\gamma}-Al_2O_3$ catalysts calcined at $700^{\circ}C$ for 3 hrs in the air showed the highest activity for the oxidation of the toluene. The decrease of oxidation activity of $Pt/{\gamma}-Al_2O_3$ catalysts calcined at $800^{\circ}C$ might result from the decrease of active sites by sintering of platinum metals as well as ${\gamma}-Al_2O_3$ supports. The 1.0wt% $Pt/{\gamma}-Al_2O_3$ catalyst showed the activity from the lower temperature at $120^{\circ}C$, reached the light-off temperature ($T_{50%}$) at $180^{\circ}C$, and leveled off its activity at $340^{\circ}C$ with the conversion of 100% 'Mutual promotion' effects were observed for the binary mixture of toluene and xylene. The activity of the easy-to-oxidize toluene was slightly increased with the existence of the xylene. It might suggest the different mechanism for the oxidation of toluene and xylene on the $Pt/{\gamma}-Al_2O_3$ catalysts on different sites, and its reaction of gaseous oxygen.

Effects of the Preparation Process on the Synthesis and the Luminescence of Ba2SiO4:Eu2+ Phosphor Powders (합성공정이 Ba2SiO4:Eu2+ 형광체 분말의 합성과 발광특성에 미치는 영향)

  • Park, Jung Hye;Kim, Young Jin
    • Journal of the Korean Electrochemical Society
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    • v.16 no.3
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    • pp.184-189
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    • 2013
  • $Ba_2SiO_4:Eu^{2+}$ ($B_2S:Eu^{2+}$) powders were prepared by firing the dry gel obtained by the sol-gel and the hybrid process (sol-gel and combustion), respectively, and their structure and luminescence were investigated. Tetraethyl orthosilicate (TEOS) was used as a Si source. The phase transition was observed with the TEOS content. With 1.2M TEOS, the powders prepared by the sol-gel process without prior calcination were composed of the $B_2S:Eu^{2+}$ single phase, whereas those by the sol-gel and the hybrid process with prior calcination consisted of the dominant $B_2S:Eu^{2+}$ and minor $BaSiO_3:Eu^{2+}$ ($BS:Eu^{2+}$) phases and their emission intensities were approximately two times higher than those without prior calcination. The hybrid process could reduce the process time innovatively compared to the sol-gel process, even though the former was a little inferior to the latter in the emission intensity of $B_2S:Eu^{2+}$. With 1.1M TEOS, the $B_2S:Eu^{2+}$ single phase was obtained by the hybrid process, and its green emission was observed at 505 nm originated from the $4f^65d^1{\rightarrow}4f^7$ transition of $Eu^{2+}$ ions.

NiO/La2O3-ZrO2/WO3 Catalyst Prepared by Doping ZrO2 with La2O3 and Modifying with WO3 for Acid Catalysis

  • Sohn, Jong-Rack;Choi, Hee-Dong;Shin, Dong-Chul
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.821-829
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    • 2006
  • A series of catalysts, $NiO/La_2O_3-ZrO_2/WO_3$, for acid catalysis was prepared by the precipitation and impregnation methods. For the $NiO/La_2O_3-ZrO_2/WO_3$ samples, no diffraction lines of nickel oxide were observed, indicating good dispersion of nickel oxide on the catalyst surface. The catalyst was amorphous to X-ray diffraction up to 300 ${^{\circ}C}$ of calcination temperature, but the tetragonal phase of $ZrO_2$ and monoclinic phase of $WO_3$ by the calcination temperatures from 400 ${^{\circ}C}$ to 700 ${^{\circ}C}$ were observed. The role of $La_2O_3$ in the catalyst was to form a thermally stable solid solution with zirconia and consequently to give high surface area and acidity. The high acid strength and high acidity were responsible for the W=O bond nature of complex formed by the modification of $ZrO_2$ with $WO_3$. For 2-propanol dehydration the catalyst calcined at 400 ${^{\circ}C}$ exhibited the highest catalytic activity, while for cumene dealkylation the catalyst calcined at 600 ${^{\circ}C}$ showed the highest catalytic activity. 25-$NiO/5-La_2O_3-ZrO_2/15-WO_3$ exhibited maximum catalytic activities for two reactions due to the effects of $WO_3$ modifying and $La_2O_3$ doping.

Extrusion of Pellet-type Adsorbents Employed with Alum Sludge and H2S Removal Performance (알럼 슬러지를 이용한 입상흡착제 압출 및 황화수소 제거 성능)

  • Park, Nayoung;Bae, Junghyun;Lee, Choul Ho;Jeon, Jong-Ki
    • Clean Technology
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    • v.19 no.2
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    • pp.121-127
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    • 2013
  • The objective of this study is optimization of extrusion process for preparation of pellet-type adsorbents employed with alum sludge. Effects of water content and methyl cellulose as a binder on the possibility of extrusion and physical properties of pellet-type adsorbents were investigated. The physical characteristics of the pellet-type adsorbents were studied using nitrogen adsorption and compression strength. With a ratio of water to sludge, 63/100, the adsorbent was well extruded with a cylindrical form and the compressive strength was the highest. With increasing methyl cellulose content, the compressive strength of pellet-type adsorbent could be improved, but the specific surface area decreased. The breakthrough time of the hydrogen sulfide could be increased significantly through calcination and the breakthrough capacity reached to 1,700 mg/g, which seems to be due to increase of surface area during calcination.