• 한국환경농학회지
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• 제11권3호
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• pp.225-234
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• 1992

Thermal decomposition was conducted to investigate the influence of the various factors on stability of a new insecticide, [O, O-Diethyl O-(1-phenyl-3-trifluoromethyl-5-pyrazoyl) thiophosphoric acid ester : KH-502], in view of those informations applicable for industrial exploitation. In the thermal decomposition experiment, KH-502 was, after mixing with Fe, Cu and adjustment of moisture and pH conditions, subjected to three temperatures, 25, 50, and $100^{\circ}C$. Results for stability, and degradation pattern of KH-502 from the above experiment can be summarized as follows: 1. Main products of the thermal decomposition when this was conducted in the closed system were identified as following five compounds:O, O, O-Triethylthiophosphoric acid(TEPA), 1-Phenyl-3-trifluoromethyl-5-ethoxypyrazole(PTMEP), 1-Phenyl-2-ethyl-3-trifluoromethyl-5-hydroxypyrazole(PETMHP), O, O-Diethyl O-(1-phenyl-3-trifluoromethyl-5-pyrazoyl)phosphoric acid ester(KH-502 oxo form), O, S-Diethyl O-(1-phenyl-3-trifluoromethyl-5-pyrazoyl)phospho rothiolate(S-ethyl KH-502). However, compounds such as oxo form and S-ethyl KH-502 were not identified when the thermal decomposition was proceeded in the open system. 2. KH-502 was stable at 25 and 50$^{\circ}C$, but it was decomposed at 100$^{\circ}C$ following the first-order kinetics at the early stages of decomposition. 3. Rate constants for the thermal decomposition of KH-502 at 100$^{\circ}C$ were in the orders of Cu powder addition 0.344>Cu plate addition 0.21>moisture addition 0.05>closed system=open system=iron addition=pH 5.5 adjustment 0.04>pH 8.5 adjustment 0.027 day$^{-1}$, representing KH-502 was decomposed fast at Cu powder treatment and slow at pH 8.5 adjustment. 4. Half-life for the thermal decomposition of KH-502 at 100$^{\circ}C$ was in the orders of Cu powder addition 2.02

• 분석과학
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• 제18권5호
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• pp.386-390
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• 2005

The zinc(II) complex, $Zn(NCS)_2(C_3H_4N_2S)_2$, I, has been synthesized and characterized by single crystal X-ray diffraction, thermal analysis and infrared spectroscopy. The complex I crystallizes in the triclinic system, $P\bar{1}$ space group with a = 7.587(1), b = 8.815(1), $c=12.432(2){\AA}$, ${\alpha}=75.584(8)$, ${\beta}=83.533(9)$, ${\gamma}=68.686(8)^{\circ}$, $V=750.0(2){\AA}^3$, Z = 2, $R_1=0.036$ and ${\omega}R_2=0.101$. The central Zn(II) atom has a tetrahedral coordination geometry, with the heterocyclic nitrogen atoms of 2-aminothiazole ligands and the nitrogen atoms of isothiocyanate ligands. The crystal structure is stabilized by one-dimensional networks of the intermolecular $N-H{\cdots}S$ hydrogen bonds between the amino group of 2-aminothiazole ligands and the sulfur atom of isothiocyanate ligands. Based on the results of thermal analysis, the thermal decomposition reaction of complex I was analyzed to have three distinctive stages such as the loss of 2-aminothiazole, the decomposition of isothiocyanate and the formation of metal oxide.

• Bulletin of the Korean Chemical Society
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• 제31권10호
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• pp.2867-2872
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• 2010

Two new energetic organic alkali metal salts, 1,1-diamino-2,2-dinitroethylene rubidium salt [Rb(FOX-7)${\cdot}H_2O$] and 1,1-diamino-2,2-dinitroethylene cesium salt [Cs(FOX-7)${\cdot}H_2O$], were synthesized by reacting of 1,1-diamino-2,2-dinitroethylene (FOX-7) and rubidium chloride or cesium chloride in alkali methanol aqueous solution, respectively. The thermal behaviors of Rb(FOX-7)${\cdot}H_2O$ and Cs(FOX-7)${\cdot}H_2O$ were studied with DSC and TG methods. The critical temperatures of thermal explosion of the two compounds are 216.22 and $223.73^{\circ}C$, respectively. Specific heat capacities of the two compounds were determined with a micro-DSC method, and the molar heat capacities are 217.46 and $199.47\;J\;mol^{-1}\;K^{-1}$ at 298.15 K, respectively. The adiabatic times-to-explosion were also calculated to be a certain value of 5.81 - 6.36 s for Rb(FOX-7)${\cdot}H_2O$, and 9.92 - 10.54 s for Cs(FOX-7)${\cdot}H_2O$. After FOX-7 becoming alkali metal salts, thermal decomposition temperatures of the compounds heighten with the rise of element period, but thermal decomposition processes become intense.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1572-1576
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• 2006

A dimeric precursor, $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ for the CVD of copper metal films, (dmaeH = N,N-dimethylaminoethanol) was synthesized by the reaction of copper(II) acetate monohydrate ($Cu(OCOCH_3)_2{\cdot}H_2O$) and dmaeH in toluene. The product was characterized by m.p. determination, elemental analysis and X-ray crystallography. Molecular structure of $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ shows that a dimeric unit $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ is linked to another through hydrogen bond and it undergoes facile decomposition at 300 C to deposit granular copper metal film under nitrogen atmosphere. The decomposition temperature, thermal behaviour, kinetic parameters, evolved gas pattern of the complex, morphology, and the composition of the film were also investigated.

• Nuclear Engineering and Technology
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• 제34권4호
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• pp.323-330
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• 2002

Various types of compounds were tested with the aspects of decomposition and formation of residue in a $CO_2$ or 7H$_2$+93$N_2$ atmosphere. The evaporation temperature range of each compound was determined from thermogravimetric curve. Decomposition of dicarbon amide, stearic acid, acrowax and zinc stearate was studied by thermogravimetry in $CO_2$ or in 7H$_2$+93$N_2$ atmosphere. All compounds were decomposed in $CO_2$ atmosphere at lower than 40$0^{\circ}C$, but the residue, ZnO remained for zinc stearate. ZnO did not decompose in $CO_2$ atmosphere up to 130$0^{\circ}C$, but reduced into Zn metal and disappeared in the temperature range of $600^{\circ}C$ to 120$0^{\circ}C$ in 7H$_2$+93$N_2$ atmosphere. The effect of residue, which trapped in closed pores of sintered pellet, on the thermal stability was studied using the resintering test at 1$700^{\circ}C$ in 7H$_2$+93$N_2$ atmosphere. In the case of oxidative sintered pellet with admixing zinc stearate, the cavity formation accompanied with a density drop after resintering is due to the pressure of the Zn gases trapped in the isolated pores.

• 한국재료학회지
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• 제11권11호
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• pp.953-959
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• 2001

Homogeneous spherical W-Co salt powders were made by spray drying of aqueous solution of ammonium $metatungstate(NH_4)_6(H_2W_{12}O_{40}){\cdot}4H_2O,\; AMT)$ and cobalt nitrate $hexahydrate(Co(NO_3)_2{\cdot}6H_2O)$. The thermal decomposition process of spray dried W-Co salt powders was studied by TG, XRD, SEM, TEM and FT-IR. Spray dried W-Co salt powders were calcined for 1 hour in the temperature from$ 350^{\circ}C$ to $800^{\circ}C$ in atmosphere of air. At the temperatures over $600^{\circ}C$, spherical $CoWO_4/WO_3$ composite oxide powders were obtained. The primary particle size of W/Co composite oxide powders increased with increasing thermal decomposition temperature due to the particle growth. The observed crystallite size by TEM was in the range of 60nm and that of $CoWO_4$ calculated by Scherrer's formula at $800^{\circ}C$ was smaller than 55nm. The crystallite site was identified by XRD and TEM.

• 대한화학회지
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• 제55권4호
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• pp.612-619
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• 2011

1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB)의 란탄(III) 착물을 합성하여 원소분석, 몰전기전도도 측정, IR, UV-Vis. 및 NMR 스펙트럼으로 특성을 조사하였다. 스펙트럼 데이터로부터 PB가 pyrazolidinedione 고리의 두 카르보닐 산소를 통해 이배위 및 일이온화 리간드로 배위됨을 규명하였다. 몰전기전도도 데이터로부터 이들 착물이 비전해질임을 규명하였다. 이들 착물의 열적 행동을 공기 중에서 TG 및 DTG로 연구한 결과, 탈수화, 열적 안전성 및 열분해에 관한 정보를 얻을 수 있었다. 최종 생성물은 해당 금속의 산화물로 밝혀졌다. 탈수화 및 분해 단계에 대한 열역학 및 반응속도 파라메터를 구하였다. 분해 단계에 대한 음의 엔트로피 값은 반응물보다 활성화 착물이 더 질서있는 구조를 갖는다는 것을 의미하며, 이때 반응은 정상보다 느렸다. 이러한 연구를 바탕으로 착물의 분자식이 $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La 및 Ce) 그리고 $[Ln(PB)_3 (H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd 및 Sm)임을 규명하였다.

• Elastomers and Composites
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• 제31권2호
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• pp.122-129
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• 1996

The Thermal decomposition of the ${\alpha}-Cellulose$ and NaCl was studied using a thermal analysis technique in the steam of nitrogen gas with 30ml/min at various heating ranges from 4 to $20^{\circ}C/min$. The Derivative and Integral method used to be obtained values of activation energy of decomposition reaction. 1. The values of activation energy evaluated by Derivative and Intergral method were consistent with each other very well. 2. The maximum value of heat of decomposition evalated by DSC method was ${\alpha}-Cellulose/NaCl= 90/10$. 3. The thermogravimetric trace curve agreed with the theoretical equation.

• 대한금속재료학회지
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• 제48권12호
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• pp.1123-1129
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• 2010

In order to apply the Sievert's type automatic apparatus to thermal analysis of hydrogen absorbing materials, the dehydrogenation of the Mg-H system was investigated. As the initial wt% of hydrogen was increased to 4.4, the peak temperature of evolution rate shifted to higher temperature. However, with the initial wt% of hydrogen higher than 4.4, peak temperature of evolution rate did not change. The peak temperatures of evolution rate obtained by automatic apparatus were almost the same as those measured by a manual apparatus. As the heating rate was increased, the peak temperatures increased; the peak temperatures for heating rates 1, 2 and 3 K/min were 664, 687 and 702 K, respectively. The activation energy for the decomposition of Mg hydride was 101 kJ/mol. The Sievert's type automatic apparatus can be successively applied to the thermal analysis of metal hydride.

• 한국추진공학회지
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• 제14권5호
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• pp.32-44
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• 2010

고체 추진기관 노즐의 2차원 열반응 및 삭마 해석 코드를 활용하여 노즐 부품의 숯 및 삭마현상을 연구하였다. Arrhenius 식을 이용한 내부 열분해 모델 상수는 TGA(열중량분석기) 실험으로 얻었다. 탄소와 $H_2O$, $CO_2$의 산화반응에 의한 화학적 삭마는 Zvyagin이 제안한 삭마모델 과 반응속도 상수를 이용하여 해석을 수행하였다. 삭마에 의한 경계조건 및 격자 이동은 상용해석 프로그램인 MSC-Marc-ATAS에서 적용되는 Rezoning-remeshing 기법을 사용하였다. 해석된 숯 및 삭마 두께는 연소시험 결과 값과 최대 20% 오차를 보였다. 향후 열방호 시스템의 성능을 모사하기 위하여 내부 온도 및 열유속을 실시간 측정하면 3차원 FEM 통합 열구조 해석에 적용될 것으로 기대된다.