• 한국세라믹학회지
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• 제49권2호
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• pp.167-172
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• 2012

Fine diamond powders are synthesized with a 420 ${\phi}$ cubic press and stack-cell composed of Kovar ($Fe_{54}Ni_{29}Co_{17}$) (or Kovar+7 ${\mu}m$-thick Zn electroplated) alloy and graphite disks. The high pressure high temperature (HPHT) process condition was executed at $1500^{\circ}C$ for 280 seconds by varying the nominal pressure of 5.7~10.6 GPa. The density of formation, size, shape, and phase of diamonds are determined by optical microscopy, field emission scanning electron microscopy, thermal gravimetric analysis-differential thermal ammnlysis (TGA-DTA), X-ray diffraction (XRD), and micro-Raman spectroscopy. Through the microscopy analyses, we found that 1.5 ${\mu}m$ super-fine tetrahedral diamonds were synthesized for Zn coated Kovar cell with whole range of pressure while ~3 ${\mu}m$ super-fine diamond for conventional Kovar cell with < 10.6 GPa. Based on $750^{\circ}C$ exothermic reaction of diamonds in TGA-DTA, and characteristic peaks of the diamonds in XRD and micro-Raman analysis, we could confirm that the diamonds were successfully formed with the whole pressure range in this research. Finally, we propose a new process for super-fine diamonds by lowering the pressure condition and employing Zn electroplated Kovar disks.

• 공업화학
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• 제4권1호
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• pp.75-81
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• 1993

$Ni^{2+}-Faujasite$의 열화학적 안정성을 시차열분석(DTA), 열중량분석(TGA), X선 회절분석(XRD) 및 양자화학적 계산을 통해 고찰하였다. $Ni^{2+}-Faujasite$의 탈수현상은 373-773 K의 온도 구간에서 나타났다. 골격내 T자리를 표현하는 분자모델을 설정하여 전체 에너지와 Wiberg 결합차수를 CNDO/2 분자궤도법을 통해 계산하였다. 계산된 결과는 제올라이트의 결정성 감소가 골격내 Al-O결합의 약화에 직접적으로 연관되어 있음을 나타내었다.

• 약학회지
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• 제19권4호
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• pp.219-226
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• 1975

Physical and chemical properties on the aging inhibition mechanism of hydrous aluminum oxide were studied by means of dehydration velocity, activation energy, DTA, TGA, IR spectra, X-ray diffraction and TMA. During aging, changes may occur in the hydrous aluminum oxide structure which results in a loss of acid reactivity and in crystal formation to the hydrated hydrous alumina. The results obtained from the X-ray diffraction pattern and DTA, TGA thermogram studies showed that the aging product stabilized with either sorbitol or mannitol was hydrous aluminum oxide ($Al_{2}O_{3}{\cdot}xH_{2}O$) but the aging product not stabilized with either sorbitol or mannitol product not stabilized was hydrated hydrous aluminum oxide $Al_{2}O_{3}{\cdot}xH_{2}O{\cdot}yH_{2}O$. The activation energy of dehydration of the hydrous almina was about 17 Kcal. mol$^{1}$ deg$^{-1}$ which was observed a little less than that of 22 kcal.mol.$^{-1}$ deg.$^{-1}$ of or mannitol, the inhibition mechanism in the aging process from oxide is assumed to prevent the formation of the hydrated hydrous aluminum oxide and the aging process is thought of as analogous to the polymorphic transformations which occur as a system converts to its most stable state.

• Archives of Pharmacal Research
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• 제2권1호
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• pp.49-64
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• 1979

In an atempt to elucidate further physicochemical properties of furosemide-PVP coprecipitates, extensive investigations such as TLC, UV,IR, NMR, X-ray diffraction, TGA and DTA studies were carried out for the furosemide test systems. X-ray diffraction studies revealed that the pure furosemide and the furosemide contained within a physical mixture were crystalline in nature. However, there was no crystallinity evident in the 1:5 furosemide-PVP 40,000 coprecipitate system, even after standing for two years. The various ratio furosemide-PVP 40,000 coprecipitate systems revealed that the coprecipitate containing a greater amount of PVP 40,000 than that of furosemide showed a crystalline state of furosemide and that the minimum amounts of PVP to make amorphous form of furosemide was 1:1 ratio of furosemide to PVP. From the furosemide-PVP coprecipitate systems with PVP of different molecular weights of 10,000, 40,000 and 360,000, all the 1:1 ratio coprecipitates did not exhibit any crystallinity of furosemide, whereas all the 2:1 ratio coprecipitates showed a presence of crystalline furosemide. All the coprecipitated preparations with PEG 4,000 and with PEG 6,000 showed the diffraction peaks indicating the presence of crystalline furosemide. The comparison of infrared spectra of the physical mixture and the coprecipitate showed an interaction such as association between the functional groups of furosemide and PVP in the molecular level, whereas the studies by TLC, UV and NMR showed its dissociation in methanol solution. The weight losses in TGA curves showed all the same patterns. However, a little different transition form in DTA thermograms was shown between the physical mixture and the coprecipitate, indicating the different thermal property.

• 한국화재소방학회논문지
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• 제26권6호
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• pp.99-108
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• 2012

본 연구에서는 최근 빈번히 발생하고 있는 폐타이어의 가공 및 저장상황에서의 산화열에 의한 자연발화현상을 규명하기 위해 폐타이어 분쇄물에 대한 화재 재연실험과 가공 및 저장장소에서 수거한 화재 잔존물에 대한 면밀한 성분 분석 및 발화개시온도, 무게감량, 반응열 등을 분석하였다. 이를 위해 열축적이 용이한 폐타이어 분쇄물 2.5~15 mm 범위의 파쇄된 분쇄물을 대상으로 재연실험 및 DSC 및 TGA, DTA, DTG, GC/MS를 통한 열분석을 시행하여 자연발화의 가능성에 대한 과학적인 개연성을 부여하고자 하였다. 연구결과를 살펴보면 재연실험을 통하여 관찰한 결과 48시간 저장시에 온도의 급상승($178^{\circ}C$) 및 탄화현상, 연기발생이 관찰되었다. 또한 DTA, DTG 분석한 결과 $166.15^{\circ}C$에서 최초 중량감소가 일어나는 것으로 분석되었다. 아울러 DSC 및 TGA를 이용한 폐타이어 분쇄물 1(Unburnt)의 실험결과 $180^{\circ}C$ 부근에서 열분해를 시작하는 것으로 나타나 폐타이어의 발화 개시온도는 $160{\sim}180^{\circ}C$라고 말할 수 있다. 그리고 $305^{\circ}C$에서 최초 원료 무게의 10 % 중량감소가 있었고, 원료 무게의 50 % 중량감소는 $416^{\circ}C$로 분석되었다. 또한 GC/MS와 DSC를 이용한 산화성 및 자기반응성시험에 있어서는 1,3 cyclopentnadiene 등 산화성성분이 다량 검출되었지만 표준물질과 폐타이어 분쇄물과의 열분석실험결과 기준치 이하로 분석되어 자기반응성은 없는 것으로 분석되었다. 따라서 폐타이어의 산화열에 의한 자연발화현상을 방지하기 위해서는 분쇄시 열축적이 적거나 없는 냉동파쇄방식 등의 가공공정으로 전환유도를 고려해야하며 현재 파쇄 분쇄물을 대형 마대(500 kg)로 저장하는 방식에서, 마대를 소형화하여 분쇄물을 분산 저장하는 등의 방법으로 열축적을 방지해야한다.

• 한국세라믹학회지
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• 제39권2호
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• pp.113-119
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• 2002

The effect of ultrasonic radiation is reported for silica-poly(ethylene glycol) system prepared without the solvent using sol-gel processing by varying various parameters such as ultrasonic irradiation time, PEG content and HCl/TEOS molar ratio. The property of sonogel is compared with classic gel which has been prepared with ethanol as a solvent by traditional sol-gel processing. SEM, BET, DTA-TGA, density and Vickers hardness measurements are carried out for analyzing the samples. The gelation time is found strongly dependent on radiation time, PEG content and pH value, and has been discussed on the basis of existing theories. The $SiO_2-10$ & 20 wt% PEG sonogel exhibited superior optical, physical and gel properties as compared to the classic gel, hence, found suitable for device applications. The ultrasonic radiation increased the density and surface area, and also reduced the pore size which is well supported by the shift in the peak of DTA curve. The DTA thermogram was found similar to that of pure silica gel.

• Fibers and Polymers
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• 제4권4호
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• pp.195-198
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• 2003

Epoxidized polybutadiene (EPB) was prepared by polybutadiene (PB) with m-chloroperbenzoic acid (MCPBA) in homogeneous solution. EPB was blended with poly(3-hydroxybutyrate) (PHB) up to 30 wt% by solution-precipitation procedure. The thermal decomposition of PHB/EPB blends was studied by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and differential thermal analysis (DTA). The thermograms of PHB/EPB blends contained a two-step degradation process, while that of pure PHB sample exhibited only one-step degradation process. This degradation behavior of PHB/EPB blends, which have a higher thermal stability as measured by maximum decomposition temperature and residual weight, is probably due to crosslinking reactions of the epoxide groups in the EPB component with the carboxyl chain ends of PHB fragments during the degradation process, and the occurrence of such reactions can be assigned to the exothermic peaks in their DTA thermograms.

• Bulletin of the Korean Chemical Society
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• 제32권2호
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• pp.498-502
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• 2011

The divergent synthesis of novel phosphorus-containing dendrimer with 4,4'-sulphonyldiphenol at the core has been accomplished involving simple condensation reactions using $P(O)Cl_3$, $P(S)Cl_3$, 3-amino-phenol, 3-hydroxy-benzaldehyde, and 2-butyn 1, 4-diol. The final compound was a Schiff's base macromolecule possessing 4 imine bonds, 8 acetylenic bonds and 8 OH groups at the periphery. The structures of intermediate compounds were confirmed by IR, NMR ($^1H$, $^{13}C$ and $^{31}P$), LC-Mass and C, H, N analysis. The structure of the final dendrimer (5) was confirmed by IR, NMR ($^1H$, $^{13}C$ and $^{31}P$), MALDI-TOF-MS, and C, H, N analysis. The surface morphological characteristics of the final dendrimer were understood by Scanning Electronic Microscopic study (SEM). The thermal stability of the final dendrimer was studied by TGA/DTA analysis.

• 한국세라믹학회지
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• 제29권4호
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• pp.328-334
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• 1992

TiO2 sols were prepared by hydrolysis and polymerization of titanium tetra-isopropoxide (TTIP) in the presence of diethanolamine (DEA). The optimal mole ratio of water to TTIP is 2 and the concentration of the TiO2 sol 0.7 M. Golden TiN films without cracks were obtained by dipping Si(110) wafers into the TiO2 sol and followed by nitridation in NH3 at 1100$^{\circ}C$ for 5 h. The TiN films were studied by an optical microscope, DTA, TGA and X-ray analysis.

• 한국세라믹학회지
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• 제11권3호
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• pp.14-18
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• 1974

Magnesite single crystals up to 250 microns were synthesized from an equi-molar solution of MgCl2 and Na2CO3 in the micro-autoclave at 180-20$0^{\circ}C$. The lattice constant of synthetic magnesite was obtained a=4.6369(7), c=15.0230(10)A.U. by a least squares analysis based on the UNICS Program (Sakurai 1967) was applied to 28 reflections. Results of X-ray powder diffraction and of DTA, TGA, IRA, and EPMA studies indicate that synthesized magnesite has properties to those of natural magnesite.