• Title/Summary/Keyword: differential thermal gravimetric analysis

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The Effect of CTAB on the Citrate Sol-gel Process for the Synthesis of Sodium Beta-Alumina Nano-Powders

  • Wang, Zaihua;Li, Xinjun;Feng, Ziping
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1310-1314
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    • 2011
  • Sodium beta-alumina (SBA) nano-powders were synthesized by the citrate sol-gel process, and the effects of the cationic surfactant n-cetyltrimethylammonium bromide surfactant (CTAB) were investigated. The structure and morphology of the nano-powders were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM) techniques, respectively. The effects of CTAB on the citrate sol-gel process and the SBA formation were investigated by thermo gravimetric/differential thermal analysis (TG/DTA) and Fourier transform infrared spectroscopy (FTIR). The conductivity of ceramic pellets of SBA was measured by electrochemical impedance spectroscopy (EIS). The results showed that the CTAB inhibited the agglomeration of SBA powders effectively and consequently decreased the crystallization temperature of SBA, about $150^{\circ}C$ lower than that of the sample without CTAB. The measured conductivity of SBA was $1.21{\times}10^{-2}S{\cdot}cm^{-1}$ at $300^{\circ}C$.

Magnetic Properties of Sn1-xFexO2 Thin Films and Powders Grown by Chemical Solution Method

  • Li, Yong-Hui;Shim, In-Bo;Kim, Chul-Sung
    • Journal of Magnetics
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    • v.14 no.4
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    • pp.161-164
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    • 2009
  • Iron-doped $Sn_{1-x}Fe_xO_2$ (x = 0.0, 0.05, 0.1, 0.2, 0.33) thin films on Si(100) substrates and powders were prepared by a chemical solution process. The x-ray diffraction (XRD) patterns of the $Sn_{1-x}Fe_xO_2$ thin films and powders showed a polycrystalline rutile tetragonal structure. Thermo gravimetric (TG) - differential thermal analysis (DTA) showed the final weight loss above $430{^{\circ}C}$ for all powder samples. According to XRD Rietveld refinement of the powders, the lattice parameters and unit cell volume decreased with increasing Fe content. The magnetic properties were characterized using a vibrating sample magnetometer (VSM) and M$\ddot{o}$ssbauer spectroscopy. The thin film samples with x = 0.1 and 0.2 showed paramagnetic properties but thin films with x = 0.33 exhibited ferromagnetic properties at room temperature. Mossbauer studies revealed the $Fe^{3+}$ valence state in the samples. The ferromagnetism in the samples can be interpreted in terms of the direct ferromagnetic coupling of ferric ions via an electron trapped in a bridging oxygen deficiency, which can be explained using the F-center exchange model.

Synthesis of New Spiro[benzo[c]fluorene-7,9'-fluorene] Dimers and Their Optical Properties

  • Seo, Jeong-A;Lee, Chil-Won;Gong, Myoung-Seon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1414-1420
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    • 2013
  • Five novel spiro[benzo[c]fluorene-7,9'-fluorene] based dyes, including 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-5-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (7), 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-9-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (8), 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-2'-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (9), 9-[spiro[benzo[c]fluorene-7,9'-fluoren]-9-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (10), and 2'-[spiro[benzo[c]-fluorene-7,9'-fluoren]-2'-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (11) were successfully prepared from the corresponding halogen and boronic acid derivatives through the Suzuki coupling reaction, respectively. Chemical structures were confirmed by $^1H$ nuclear magnetic resonance (NMR), $^{13}C$ NMR, Fourier transforminfrared spectrscopy, mass spectroscopy, and elemental analysis. The thermal properties were determined by differential scanning calorimetry and thermal gravimetric analysis. The relationships between the optical and electrochemical properties and the combined positions between these dimers were systematically investigated using UV-vis, photoluminescence (PL), and photoelectron spectroscopy. These five dimers exhibited high fluorescent quantum yields and good morphological stability with high glass transition states > $174^{\circ}C$. Dimer 7 showed a UV absorbance peak at 353 nm, emission PL peak at 424 nm, and quantum efficiency of 0.62 in a cyclohexane solution.

A Study of Physicochemical Characteristics and Adsorption properties of Cs and Sr of Natural Zeolite from Kuryongpo in Korea (한국 구룡포산 천연 제올라이트의 이화학적 특성 및 Cs과 Sr 흡착 특성 연구)

  • Bayarsaikhan Battsetseg;Hu Sik Kim;Hyeon Uk Choo;Jong Sam Park;Woo Taik Lim
    • Korean Journal of Mineralogy and Petrology
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    • v.36 no.2
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    • pp.117-124
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    • 2023
  • X-ray diffraction analysis, X-ray fluorescence analysis, thermal differential and thermos gravimetric analysis, cation exchange capacity analysis, and Cesium (Cs), Strontium (Sr) adsorption experiments were performed to investigate the physical and chemical properties of natural zeolite from Guryongpo in Korea. As a result of X-ray diffraction analysis, minerals such as mordenite, heulandite, clinoptilolite, and illite are contained, and as a result of X-ray fluorescence analysis, elements such as SiO2, Al2O3, CaO, K2O, MgO, Fe2O3 and Na2O are contained, and the cation exchange capacity was 148.6 meq/100 g. As a result of thermal differential and thermos gravimetric analysis, it was confirmed that the thermal stability was excellent up to 600 ℃. As a result of the adsorption equilibrium experiment over time, the equilibrium was reached within 30 min. for Cesium (Cs) and within 8 hr. for Strontium (Sr), and the adsorption rates of Cesium (Cs) and Strontium (Sr) were 80% and 18%, respectively. As a result of the single-component isothermal adsorption experiment, in conformed to the Langmuir model, and the maximum Cesium (Cs) adsorption amount was 131.5 mg/g, which was high, while the Strontium (Sr) maximum adsorption amount was 29.5 mg/g, which was low. In the case of the natural zeolite used in this study, the content of minerals including 8-rings such as clinoptilolite, heulandite, and mordenite is high, showing high selectivity for Cesium (Cs).

Slow Cook-Off Test and Evaluation for HTPE Insensitive Propellants (HTPE 둔감추진제 완속가열 시험평가)

  • Yoo, Ji-Chang;Kim, Chang-Kee;Kim, Jun-Hyung;Lee, Do-Hyung;Min, Byung-Sun
    • Journal of the Korean Society of Propulsion Engineers
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    • v.14 no.6
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    • pp.31-37
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    • 2010
  • This study was carried out to investigate the thermal decomposition and execute EIDS slow cook-off test for the propellant ingredients and 2 kinds of HTPE propellants. The thermal analysis of the propellant ingredients used in this study showed that the thermal stability of these materials decreases in the following order : AP > HTPE > AN > BuNENA. In addition, propellant HTPE 002 containing AN showed that an endothermic process at around $125^{\circ}C$ corresponding to the solid phase change(II$\rightarrow$I) of AN was followed by the exothermic process of BuNENA/AN mixture up to $200^{\circ}C$. In EIDS slow cook-off tests, HTPE 001 and HTPE 002 reacted at around $250^{\circ}C$ and $152^{\circ}C$ respectively, and both of them showed sudden temperature increase curves at $115^{\circ}C$. The critical temperatures, $T_c$, of thermal explosion for the propellants HTPE 001 and HTPE 002, were obtained from both the non-isothermal curves at various heating rates and Semenov's thermal explosion theory. Kissinger's method that was used to calculate $T_c$ was also employed to obtain the activation energies for thermal decompositions.

Solution Processable Symmetric 4-Alkylethynylbenzene End-Capped Anthracene Derivatives

  • Jang, Sang-Hun;Kim, Hyun-Jin;Hwang, Min-Ji;Jeong, Eun-Bin;Yun, Hui-Jun;Lee, Dong-Hoon;Kim, Yun-Hi;Park, Chan-Eon;Yoon, Yong-Jin;Kwon, Soon-Ki;Lee, Sang-Gyeong
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.541-548
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    • 2012
  • New candidates composed of anthracene and 4-alkylethynylbenzene end-capped oligomers for OTFTs were synthesized under Sonogashira coupling reaction conditions. All oligomers were characterized by FT-IR, mass, UV-visible, and PL emission spectrum analyses, cyclic voltammetry (CV), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), $^1H$-NMR, and $^{13}C$-NMR. Investigation of their physical properties showed that the oligomers had high oxidation potential and thermal stability. Thin films of DHPEAnt and DDPEAnt were characterized by spin coating them onto Si/$SiO_2$ to fabricate top-contact OTFTs. The devices prepared using DHPEAnt and DDPEAnt showed hole field-effect mobilities of $4.0{\times}10^{-3}cm^2$/Vs and $2.0{\times}10^{-3}cm^2$/Vs, respectively, for solution-processed OTFTs.

A Thermal Study of the Harmful Chemical Species of Charcoal and Their Transformation during Combustion (숯의 유해물질과 이들의 연소 중 상변화에 대한 열분석 연구)

  • Yoon, Hye-On;Kim, Ki-Hyun
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.2
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    • pp.101-110
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    • 2011
  • Charcoal burning in the process of manufacture and ordinary use often release many constituent chemical species. As a result of open burning, the chemical composition as well as the physical properties of original material changes through the modification of surface properties of charcoal. Surface modification could be more responsible toward the outside elements for surface adsorption, it becomes easy to adsorb more toxic elements through surface adsorption. In this study, four kinds of commercially available charcoal were studied against the chemical and thermal stability along with the heavy metals and organic hazardous substances. Thermo gravimetric analysis (TGA) and differential scanning calorimetry, from room temperature to $400^{\circ}C$, were performed to study the weight loss and the changes in the behavior of those substances. According to TGA analysis, about 10% of weight loss was happened before $200^{\circ}C$. It was found that related weight loss of this temperature region may responsible to the gas phase organic matter. Natural charcoal, K1 and C1 show 15% of loss during the reaction heated to $400^{\circ}C$, while the artificial charcoal K2, C2 show the weight loss of about 20% was found. This is consistent with the main organic matter and VOC analysis results shown. Chemical composition based on the x-ray diffraction analysis was carried out. X-ray diffraction analysis reveals the existence of chemical additive in the forms of $Ba(NO_3)_2$, $BaCO_3$, and $NaNO_3$.

Variation in optical, dielectric and sintering behavior of nanocrystalline NdBa2NbO6

  • Mathai, Kumpamthanath Chacko;Vidya, Sukumariamma;Solomon, Sam;Thomas, Jijimon Kumpukattu
    • Advances in materials Research
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    • v.2 no.2
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    • pp.77-91
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    • 2013
  • High quality nanoparticles of neodymium barium niobium ($NdBa_2NbO_6$) perovskites have been synthesized using an auto ignition combustion technique for the first time. The nanoparticles thus obtained have been characterized by powder X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy and transmission electron microscopy. UV-Visible absorption and photoluminescence spectra of the samples are also recorded. The structural analysis shows that the nano powder is phase pure with the average particle size of 35 nm. The band gap determined for $NdBa_2NbO_6$ is 3.9 eV which corresponds to UV-radiation for optical inter band transition with a wavelength of 370nm. The nanopowder could be sintered to 96% of the theoretical density at $1325^{\circ}C$ for 2h. The ultrafine cuboidal nature of nanopowders with fewer degree of agglomeration improved the sinterability for compactness at relatively lower temperature and time. During the sintering process the wide band gap semiconducting behavior diminishes and the material turns to a high permittivity dielectric. The microstructure of the sintered surface was examined using scanning electron microscopy. The striking value of dielectric constant ${\varepsilon}_r=43$, loss factor tan ${\delta}=1.97{\times}10^{-4}$ and the observed band gap value make it suitable for many dielectric devices.

Comparative Analysis of the Characteristics of Natural Zeolites from Mongolia, Korea, and the United State (몽골, 한국, 미국 천연 제올라이트의 특성 비교 분석)

  • Battsetseg, Bayarsaikhan;Kim, Hu Sik;Kim, Young Hun;Kim, Jeong Jin;Lim, Woo Taik
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.2
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    • pp.141-151
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    • 2022
  • The 16 natural zeolites collected from Mongolia (6 types), the United States (1 type), and Korea (9 types) were characterized by XRD, XRF, TGA, DTA, and CEC analysis. All 16 samples are composite minerals. Two or more mineral phases co-exist and consist primarily of minerals such as clinoptilolite, heulandite, mordenite, and chabazite. In certain samples, minerals like illite and quartz were present as impurities. The XRF analysis showed that the 16 natural zeolites contain SiO2, Al2O3, K2O, CaO, Na2O, MgO, and Fe2O3 oxides. The cation exchange capacity of the U-1 sample was 223.3 meg/100 g, which is higher than the rest of the samples. M-6 sample in Mongolian natural zeolite and K-1 sample in Korean natural zeolite showed the highest cation exchange capacity at 166.6 meg/100 g. As a result of thermal differential and thermos gravimetric analysis, all 16 samples showed excellent thermal stability up to 600℃.

Second Order Nonlinear Optical Polyimides Containing Organic Chromophores with an Oxadiazole Segment (옥사디아졸 결합의 유기 발색단이 도입된 이차비선형 광학 이미드 고분자)

  • Do, Jung Yun;Kim, Bong Gun;Kwon, Ji-Yun
    • Applied Chemistry for Engineering
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    • v.18 no.1
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    • pp.77-83
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    • 2007
  • It is essential that second order nonlinear optical materials have low optical propagation losses in the wavelengths of second harmonic generation for practical applications in waveguides. Three dipolar chromophores substituted with nitro, cyano, and alkyl sulfone as an electron withdrawing group were prepared. The UV-Vis absorption spectra of the cyano and alkylsulfone chromophores showed a blue-shift compared to the nitro chromophore. The introduction of oxadiazole segment in the chromophore structure led to similar spectral shift. The blue-shift can produce low optical loses at second harmonics. The chromophores were successfully attached to a polyimide, yielding side chain polymers. The nonlinear optical property of the prepared optical polymers was determined by measuring electro-optic coefficient at 1.55 mm. The polymers exhibited high glass transition temperature of over $185^{\circ}C$ and thermal stability to $300^{\circ}C$ through differential scanning calorimeter analysis and thermal gravimetric analysis.