• Title/Summary/Keyword: TG-DTA

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Effect of oxalic acid on the iron content of pottery stone (도석의 탈철에 관한 Oxalic acid의 영향에 관한 연구)

  • Kim Kyung-Nam;Park Hyun
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.6
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    • pp.257-261
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    • 2004
  • The pottery stones from the Taebek area consist of abundant quartz with kaolinite. In this study, the characteristics of pottery stones were examined by XRD (X-ray diffractometer), XRF (X-ray fluorescence spectrometer), TG-DTA and SEM (Scanning Electron Microscope). The chemical compositions of the raw ore showed 71.75 wt%$SiO_2$, 22.10 wt%$Al_2O_3$, 1.86 wt%CaO, 2.97 wt%$K_2O$, 0.62 wt%$Fe_2O_3$. When pottery stone of 3 mm size was leached at $80^{\circ}C$ with 10 % oxalic acid, the content of $Fe_2O_3$ was reduced from 0.62 wt% to 0.24 wt% and the whiteness was enhanced. Grinding of pottery stone was conducted by a planetary ball mill using media of zirconia, the average particle size was 2~5 $\mu\textrm{m}$.

Synthesis and Luminescence Properties of Lanthanide Complexes of a Novel Polyaminopolycarboxylate Ligand

  • Tang, Chang-Quan;Tang, Rui-Ren;Tang, Chun-Hua;Zeng, Zhi-Wen
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1283-1288
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    • 2010
  • A novel polyaminopolycarboxylate ligand with many coordination sites, N,N,$N^1,N^1,N^2,N^2$-[( 2,4,6-tri(aminomethyl)-pyridine]hexakis(acetic acid) (TPHA), was designed and synthesized and its lanthanide complexes $Na_6Tb_2$(TPHA)$Cl_6{\cdot}14H_2O$, $Na_6Eu_2$(TPHA)$Cl_6{\cdot}8H_2O$, $Na_6Gd_2$(TPHA)$Cl_6{\cdot}11H_2O$ and $Na_6Sm_2$(TPHA)$Cl_6{\cdot}9H_2O$ were successfully prepared. The ligand and the complexes were characterized by elemental analysis, IR, mass, NMR and TG-DTA. The TG-DTA studies indicated that the complexes had a high thermal stability, whose initial decomposition temperature was over $270^{\circ}C$. The luminescence properties of the complexes in solid state were investigated and the results suggested that $Tb^{3+}$ and $Eu^{3+}$ ions could be sensitized efficiently by the ligand, especially the Tb(III) complex displayed a very strong luminescence intensity (> 10000) and only displayed characteristic metal-centered luminescence. Also, the correlative comparison between the structure of ligand and luminescence properties showed how the number of the coordination atoms of ligand can be a prominent factor in the effectiveness of ligand-to-metal energy transfer.

Carbonization of Coal-Fly Ash Containing High CaO Compound (CaO 화합물이 다량 함유된 비산재의 탄산화)

  • Sim, Jun Soo;Lee, Ki Gang;Kim, Yu Taek;Kang, Seung Ku
    • Journal of the Korean Ceramic Society
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    • v.50 no.1
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    • pp.18-24
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    • 2013
  • This study was conducted to recycle fly ash containing an abundance of CaO generated from combustion in a circulating layer as a carbon storage medium. The study utilized XRD, TG-DTA and XRF analyses during the hydration of fly ash and identified calcium substances within fly ash that could be used in a carbonation process. $Ca^{2+}$ ions in the calcium substances were easily converted to hydrates. A carbonation experiment was done, which used the method of $CO_2$ gas injection to produce suspensions by mixing fly ash with distilled water. The results were analyzed using TG-DTA, XRD, and pH meter measurements. The study was able to verify that the reaction was completed at a $CO_2$ flow rate of 300cc/min approximately 30 minutes after an injection into a solution with a solid-liquid ratio of 1 : 10 of fly ash and distilled water. Moreover, the stirring time of the suspensions did not influence the reaction, and the reaction time was found to diminish as the portion of the fly ash became smaller. Thus, this study produced carbon storage fly ash having a $CO_2$ storage rate of about 71% through the utilization of the CaO content contained within fly ash.

Electrochemical Characteristics of Carbon Coated SnO2-SiO2 Anode Materials (탄소 피복된 SnO2-SiO2 음극활물질의 전기화학적 특성)

  • Jeong, Gu-Hyun;Na, Byung-Ki
    • Clean Technology
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    • v.19 no.1
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    • pp.44-50
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    • 2013
  • Tin-based materials for lithium ion battery have been proposed as new anode candidates owing to their higher specific capacity and relatively high lithium insertion potential. Tin-based materials have been extensively studied as possible replacements for carbon anodes in lithium ion batteries. However, the large volume expansion results in severe particle cracking with loss of electrical contact, giving irreversible capacity losses which prevent the widespread use of tin-based materials in lithium batteries. So remaining studies of tin-based materials are alleviating volume expansion and improving cycle performance. In this work, $SnO_2-SiO_2$ composites were manufactured with sol-gel method to overcome their volume expansion. Carbon was coated with 10 vol% propylene gas. The characteristics of active material and the effect of heat treatment were investigated with TG/DTA, XRD, SEM and FT-IR. Electrochemical characteristics of these composites were measured with CR2032 type coin cells. Carbon coated $SnO_2-SiO_2$at $300^{\circ}C$ heat treatment showed the best electrochemical performance.

Effects of Drying Agents on the Drying and Calcination in Synthesis of Mullite by Sol-Gel Process (졸-겔법에 의한 mullite합성시 건조 첨가제가 건조 및 소성에 미치는 영향)

  • Hahm, Yeong-Min;Hong, Young-Ho;Choi, Seung-Il
    • Applied Chemistry for Engineering
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    • v.4 no.3
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    • pp.497-504
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    • 1993
  • The effect of DCCA (Drying Control Chemical Additives) on the drying of gel was investigated in order to determine an optimum drying condition of mullite precursor through sol-gel process. Aluminium sec-butoxide was synthesized from aluminium foil and then mullite powders were synthesized from Tetra-ethyl-ortho-silicate (TEOS) and the aluminium sec-butoxide. N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane, and Oxalic acid were used as DCCA. Mullite powders that were calcined at 200, 900, 1100, and $1250^{\circ}C$ for 2hr were analysed by XRD, TG-DTA, FT-IR, and SEM in order to investigate structural change and characteristics of calcined powders. The results of this work showed that the drying time of gel was reduced to about half in the presence of 0.1mol DMF compared with the absence of DCCA and also calcined powders were obtained without remarkable structural change despite of the addition of DCCA.

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Preparations of PZT Ceramic by Solution Combustion Synthesis (용액연소합성방법에 의한 PZT세라믹의 제조)

  • 이상진;윤존도;권혁보;전병세
    • Journal of the Korean Ceramic Society
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    • v.39 no.1
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    • pp.74-78
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    • 2002
  • In this study, the solution combustion method was employed to synthesize perovskite PZT ceramics. Multicomponent oxides can be prepared by the solution combustion synthesis using redox exothermic reaction of precursor solutions. The results of DTA/TG showed exothermic peaks in 214$^{\circ}C$ and 350$^{\circ}C$. Those were caused by the differences of the thermal decomposition behavior of oxidizer and fuel. The combustion reaction was completed at 370$^{\circ}C$ during heating procedure, but the product was not transformed into perovskite. The thermal decomposition behavior of both oxidizer and fuel were considered during solution combustion process at 600$^{\circ}C$, which showed tetragonal single phase PZT ceramics with 50 nm crystalline size. The lattice constant a was 3.997 ${\pm}$ 0.001 ${\AA}$ and the lattice constant c was 4.147${\pm}$0.001 ${\AA}$.

LiLa1-xNdx(MoO4)2 Single Crystal Growth by the Czochralski Method (쵸크랄스키법에 의한 LiLa1-xNdx(MoO4)2 단결정 육성 연구)

  • Bae In-Kook;Chae Soo-Chun;Jang Young-Nam;Kim Sang-Bae
    • Journal of the Korean Ceramic Society
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    • v.41 no.9
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    • pp.677-683
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    • 2004
  • Nd:LLM (Nd:LiLa(MoO$_4$)$_2$) single crystals for the laser host material were grown by the Czochralski method. The Nd:LLM grown single crystals cracked easily, and the reasons of cracks are generally related with phase transition, incongruent melting, chemical heterogeneity of composition, geometric thermal structures of imbalance and growth direction. We confirmed that phase transition is not observed by TG-DTA thermal analysis, and the XRD analysis revealed congruent melting in our products. It was confirmed that the volatilization of Li$_2$O composition is the important reason of chemical heterogeneity. The geometric thermal profile of the resistance furnace of our own design was controlled with a crucible height. Also, Nd:LLM crystal affected growth direction, and was the best quality in case of (101) growth direction. The distribution and effective distribution coefficient of Nd$^{3+}$ ion were accomplished by PIXE analysis.s.

Preparation and Characterization of La0.8Ca0.2MnO3 (La0.8Ca0.2MnO3의 합성 및 특성연구)

  • 정미원;이지윤;김현정
    • Journal of the Korean Ceramic Society
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    • v.40 no.5
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    • pp.434-440
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    • 2003
  • The powders of L $a_{0.8}$C $a_{0.2}$Mn $O_3$ Colossal Magnetoresistance (CMR) materials were synthesized by sol-gel process. Lanthanum(H), Calcium(II) and Manganese(III) 2,4-Pentanedionate were dissolved in a mixed binary solution consisted of propionic acid and methanol with PEG (15 wt%) aqueous solution. The progress of reactions was monitored by FT-IR spectroscopy. The Lao scao.2Mn03 gel powders were annealed at various temperatures. The structural changes were investigated by FT-IR, CP/MAS $^{ 13}$C solid state NMR spectroscopy and XRD. The thermochemical property, particle characterization, microstructure of sintered sample, and cation composition of gel powder were studied by TG/DTA, FE-SEM and ICP-AES. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

Low temperature synthesis of ZnO nanopowders by the polymerized complex method (착체중합법을 이용한 ZnO 나노분말의 저온합성)

  • 권용재;김경훈;임창성;심광보
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.12 no.5
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    • pp.229-233
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    • 2002
  • Nano-sized ZnO particles were successfully synthesized at low temperatures by a polymerized complex method via an organochemical route. The polymeric precursors could be prepared using Zn nitrate hexahydrate and a mixed solution of citric acid and ethylene glycol as a chelating agent and a reaction medium. The polymeric precursors were calcined at temperatures from 300 to $700^{\circ}C$ for 3 h, and evaluated for degree of crystallization process, thermal decomposition, surface morphology and crystallite size. The thermal decomposition and crystallization process were analyzed by TG-DTA, FI-IR and XRD. The morphology and crystallite size of the calcined particles were evaluated by scanning electron microscopy (SEM), transmittance electron microscopy (TEM) and Scherrer's equation. Crystallization of the ZnO particles was detected at $300^{\circ}C$ and entirely completed above $400^{\circ}C$. Particles calcined between 400 and $700^{\circ}C$ showed a uniform size distribution with a round shape. The average particle sizes calcined at $400^{\circ}C$ for 3 hour were 30~40nm showing an ordinary tendency to increase with the temperatures.

The Effects of Cr-Substitution in Ferrite Catalysts and the Catalytic Dehydrogenation of Ethylbenzene (페라이트 촉매의 Cr 치환효과와 에틸벤젠의 탈수소반응)

  • Lim, Ki-Chul;Kim, Eul-San;Lee, Ho-In
    • Applied Chemistry for Engineering
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    • v.2 no.3
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    • pp.279-288
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    • 1991
  • Mg- and Zn-ferrites having spinel structure, a kind of complex oxides showing the advantageous properties of constituent single metal oxides, were selected to find a relationship between their catalytic activities in the dehydrogenation of ethylbenzene to styrene and the catalytic properties. For the structural and physical analyses of ferrites, XRD, BET, TG/DTA, ESCA, TEM, and TPD methods were employed. The effects of Cr-substitution were intensively studied by the experimental methods mentioned above. Chromium which showed a preferential tendency to diffuse to the surface acted as a structural promoter by increasing surface area and stability of catalyst structure. In the dehydrogenation of ethylbenzene, catalytic activity, and the effects of Cr-substitution were investigated. Oxygen mobility was decreased with the amount of Cr-substitution in $MgCr_xFe_{2-x}O_4$, which resulted in the increase of selectivity to styrene and the suppression of total oxidation.

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