• Title/Summary/Keyword: TGA-DSC

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Synthesis of Novel (Be,Mg,Ca,Sr,Zn,Ni)3O4 High Entropy Oxide with Characterization of Structural and Functional Properties and Electrochemical Applications

  • Arshad, Javeria;Janjua, Naveed Kausar;Raza, Rizwan
    • Journal of Electrochemical Science and Technology
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    • v.12 no.1
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    • pp.112-125
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    • 2021
  • The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.

Thermal Properties of Diglycidyl Ether of Terephthalylidene-bis-(4-amino-3-methylphenol) (Diglycidyl ether of terephthalylidene-bis-(4-amino-3-methylphenol)의 열적 성질에 대한 연구)

  • Hyun, Ha-Neul;Choi, Ji-Woo;Cho, Seung-Hyun
    • Composites Research
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    • v.35 no.2
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    • pp.53-60
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    • 2022
  • This study uses Diglycidyl ether of terephthalylidene-bis-(4-amino-3-methylphenol) (DGETAM), an amine hardener 4,4'-diaminodiphenylethane (DDE) and cationic catalyst N-benzylpyrazinium hexafluoroantimonate (BPH) to make epoxy film. For analysis, 1H_NMR and FT-IR were used to verify proper synthesis, and the liquid crystallinity of DGETAM was checked using Differntial Scanning Calorimetry and Polarized Optical Microscopy. Thermal conductivity of the sample was measured using Laser Flash Apparatus. Thermal stability as well as thermal conductivity is important when used as a packaging material. Activated energy is the energy needed to generate a response, which can be used to estimate the energy required to maintain physical properties. It was obtained using the Arrhenius equation based on the data measured by isothermal decomposition using Thermogravimetric Analysis. Measurement of the thermal conductivity of epoxy films showed higher thermal conductivity when DDE was used, and it was found that thermal conductivity had an effect on thermal stability, given that it represented an activation energy similar to a film with BPH upon 5% decomposition.

Investigation on structural symmetry of CsCoCl3·2H2O crystals by magic-angle spinning 1H and static 133Cs nuclear magnetic resonance

  • Park, Sang Hyeon;Jang, Du Chang;Jeon, Hara;Gyeong, Oh Yi;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.26 no.1
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    • pp.10-16
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    • 2022
  • The phase transition temperatures of CsCoCl3·2H2O crystals are investigated via differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Three endothermic peaks at temperatures of 370 K (=TC1), 390 K (=TC2), and 416 K (=TC3) were observed for phase transitions from CsCoCl3·2H2O to CsCoCl3·1.5H2O, to CsCoCl3·H2O, and then to CsCoCl3·0.5H2O, respectively. In addition, the spin-lattice relaxation time T in the rotating frame and T1 in the laboratory frame as well as changes in chemical shifts for 1H and 133Cs near TC1 were found to be temperature dependent. Our analyses results indicated that the changes of chemical shifts, T, and T1 are associated with structural phase transitions near temperature TC1. The changes of chemical shifts, T, and T1 near TC1 were associated with structural phase transitions, owing to the changes in the symmetry of the structure formed of H2O and Cs+ ions. Consequently, the structural symmetry in CsCoCl3·2H2O crystals based on temperature is discussed by the environments of their H and Cs nuclei.

Preparation and Characterization of Poly(Arylene Ether) Having Heterocyclic Quaternary Ammonium Functional Groups for Anion Exchange Membranes (음이온교환막용 헤테로고리형 4차 암모늄 작용기를 갖는 폴리(아릴렌 이써)의 제조 및 특성 분석)

  • LEE, SANG HYEOK;YOO, DONG JIN
    • Journal of Hydrogen and New Energy
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    • v.33 no.4
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    • pp.372-382
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    • 2022
  • In this study, anion exchange membranes were prepared by synthesizing the main chain into a poly(arylene ether) (PAE) structure, and the structures capable of improving the physical and chemical stability of the membrane by introducing a heterocyclic quaternary ammonium functional groups were studied. The chemical structure and thermal properties of the prepared polymer were confirmed by 1H-NMR, FT-IR, TGA, and DSC, and surface analysis was performed through AFM measurement. Additionally, dimensional stability and chemical properties was studied by measuring water uptake and swelling ratio, IEC and ionic conductivity. At 90℃, the quaternized poly(arylene ether) (QPAE)/1-methylpiperidine (MP) membrane exhibited the highest ionic conductivity of 27.2 mS cm-1, while the QPAE/1-methylimidazole (MI) membrane and QPAE/1-methylmorpholine (MM) membrane exhibited values of 14.5 mS cm-1 and 11.5 mS cm-1, respectively. In addition, the prepared anion exchange membrane exhibited high chemical stability in alkaline solution.

Effects of Catalyst Dispersion for Reaction Energy Control on Eco-AZ91 MgH2 (Eco-AZ91 MgH2의 반응열 제어에 미치는 촉매 분산 효과)

  • SOOSUN LEE;SONG SEOK;TAE-WHAN HONG
    • Journal of Hydrogen and New Energy
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    • v.34 no.6
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    • pp.631-640
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    • 2023
  • This study selected Eco-AZ91 MgH2, which shows high enthalpy as a material for this purpose, as the basic material, and analyzed the change in characteristics by synthesizing TiNi as a catalyst to control the thermodynamic behavior of MgH2. In addition, the catalyst dispersion technology using graphene oxide (GO) was studied to improve the high-temperature aggregation phenomenon of Ni catalyst and to secure a source technology that can properly disperse the catalyst. XRD, SEM, and BET analysis were conducted to analyze the metallurgical properties of the material, and TGA and DSC analysis were conducted to analyze the dehydrogenation temperature and calorific value, and the correlation between MgH2, TiNi catalyst, and GO reforming catalyst was analyzed. As a result, the MgH2-5 wt% TiNi at GO composite could lower the dehydrogenation temperature to 478-492 K due to the reduction of the catalyst aggregation phenomenon and the increase in the reaction specific surface area, and an experimental result for the catalyst dispersion technology by GO could be ensured.

Variations in electrode characteristics through simplification of phosphorus-doped NiCo2O4 electrode manufacturing process (인이 도핑된 NiCo2O4 전극 제조 공정의 간소화를 통한 전극 특성의 변화)

  • Seokhee-Lee;Hyunjin Cha;Jeonghwan Park;Young Guk Son;Donghyun Hwang
    • Journal of the Korean institute of surface engineering
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    • v.56 no.5
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    • pp.299-308
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    • 2023
  • In this study, phosphorus (P)-doped nickel cobaltite (P-NiCo2O4) and nickel-cobalt layered double hydroxide (P-NiCo-LDH) were synthesized on nickel (Ni) foam as a conductive support using hydrothermal synthesis. The thermal properties, crystal structure, microscopic surface morphology, chemical distribution, electronic state of the constituent elements on the sample surface, and electrical properties of the synthesized P-NiCo2O4 and P-NiCo-LDH samples were analyzed using thermogravimetric analysis-differential scanning calorimetry (TGA-DSC), X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). The P-NiCo2O4 electrode exhibited a specific capacitance of 1,129 Fg-1 at a current density of 1 Ag-1, while the P-NiCo-LDH electrode displayed a specific capacitance of 1,012 Fg-1 at a current density of 1 Ag-1. When assessing capacity changes for 3,000 cycles, the P-NiCo2O4 electrode exhibited a capacity retention rate of 54%, whereas the P-NiCo-LDH electrode showed a capacity retention rate of 57%.

Study on Explosion Characteristics and Thermal Stability of Activated Carbon (활성탄의 폭발특성과 열안정성에 관한 연구)

  • Yi-Rac Choi;Dong-Hyun Seo;Ou-Sup Han;Hyo-Geun Cha
    • Journal of the Korean Institute of Gas
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    • v.27 no.3
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    • pp.134-140
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    • 2023
  • Activated carbon is a carbonaceous material mainly used as a gaseous or liquid adsorbent. As fire-related accidents occur consistently due to the accumulation of heat of adsorption and oxidation of volatile organic compounds, the explosive characteristics and thermal stability of powdered and granular activated carbon made from coal and coconut shells were evaluated. As a result of the particle size analysis, the powdered activated carbon was in the particle size range (0.4~3) ㎛, and thermal properties such as exothermic onset temperature and decomposition behavior were analyzed using a differential scanning calorimetry and a thermogravimetric analysis. As a result of the evaluation of the explosion hazards for dust, both coal-based and coconut-based powdered activated carbon are classified as St1 class with weak explosion, but this is a relative and does not mean that the explosion hazards is absolutely low. Therefore, it is necessary to establish countermeasures for reducing the damage.

A Study on the Bonding Strength, Reactivity and Thermal Properties of Epoxy Resin Mixed with ESBO (에폭시수지-ESBO 혼용 비율에 따른 목재접착제의 접착력, 반응성 및 열분석에 관한 연구)

  • Choi, Jin Lim;Park, Heon
    • Journal of the Korean Wood Science and Technology
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    • v.35 no.3
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    • pp.36-44
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    • 2007
  • The purpose of this study was to investigate thermal stability, reactivity, and bonding strength of existing epoxy resin mixed with the epoxidized soybean oil (ESBO) in order to use soybean oil economically. In the dry shear test, the marked strengths showed $30.5kgf/cm^2$ at the ratio of ESBO to epoxy resin 9 : 1 and $6.2kgf/cm^2$ at the ratio 8 : 2. The bonding strengths of the others, except mixing ratios 2 : 8 and 1 : 9, exceeded the requirement of Korean plywood standard of $7.0kgf/cm^2$. In the wet shear test, the result was $5.8kgf/cm^2$ at the ratio 9 : 1. There were no thickness swelling and moisture absorption in the water resistance of the film. The value of activation energy, Tg (${\Delta}E$), by DSC analysis showed between $110^{\circ}C$ and $120^{\circ}C$ through all ratios. Epoxy in the epoxy resin fully reacted with the hardener (TETA), but it is difficult to decide that epoxys in the ESBO were reacted directly with the hardener from FT-IR analysis. As the mixing ratio of ESBO increased, the thermal stabilities dropped from TGA analysis. From the comprehensive view on the results of above experiments, it could be confirmed through experiments that the ESBO in the mixed adhesive of epoxy resin/ESBO played a role as an extending agent level of epoxy adhesive, and we were able to know that in order to utilize ESBO as an adhesive, a study should be performed on the condition of hardening, inducible of the hardening reaction.

THERMAL ANALYSIS OF THE DUAL CURED RESIN CEMENTS ACCORDING TO CURING CONDITION (중합조건에 따른 dual cured resin cement의 열분석적 연구)

  • Lee, In-Bog;Chung, Kwan-Hee;Um, Chung-Moon
    • Restorative Dentistry and Endodontics
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    • v.24 no.2
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    • pp.265-285
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    • 1999
  • The purposes of this investigation were to observe the reaction kinetics of five commercial dual cured resin cements (Bistite, Dual, Scotchbond, Duolink and Duo) when cured under varying thicknesses of porcelain inlays by chemical or light activation and to evaluate the effect of the porcelain disc on the rate of polymerization of dual cured resin cement during light exposure by using thermal analysis. Thermogravimetric analysis(TGA) was used to evaluate the weight change as a function of temperature during a thermal program from $25{\sim}800^{\circ}C$ at rate of $10^{\circ}C$/min and to measure inorganic filler weight %. Differential scanning calorimetry(DSC) was used to evaluate the heat of cure(${\Delta}H$), maximum rate of heat output and peak heat flow time in dual cured resin cement systems when the polymerization reaction occured by chemical cure only or by light exposure through 0mm, 1mm, 2mm and 4mm thickness of porcelain discs. In 4mm thickness of porcelain disc, the exposure time was varied from 40s to 60s to investigate the effect of the exposure time on polymerization reaction. To investigate the effect on the setting of dual cured resin cements of absorption of polymerizing light by porcelain materials used as inlays and onlays, the change of the intensity of the light attenuated by 1mm, 2mm and 4mm thickness of porcelain discs was measured using curing radiometer. The results were as follows 1. The heat of cure of resin cements was 34~60J/gm and significant differences were observed between brands (P<0.001). Inverse relationship was present between the heat of reaction and filler weight % the heat of cure decreased with increasing filler content (R=-0.967). The heat of reaction by light cure was greater than by chemical cure in Bistite, Scotchbond and Duolink(P<0.05), but there was no statistically significant difference in Dual and Duo(P>0.05). 2. The polymerization rate of chemical cure and light cure of five commercially available dual cured resin cements was found to vary greatly with brand. Setting time based on peak heat flow time was shortest in Duo during chemical cure, and shortest in Dual during light cure. Cure speed by light exposure was 5~20 times faster than by chemical cure in dual cured resin cements. The dual cured resin cements differed markedly in the ratio of light and chemical activated catalysts. 3. The peak heat flow time increased by 1.51, 1.87, and 3.24 times as light cure was done through 1mm, 2mm and 4mm thick porcelain discs. Exposure times recommended by the manufacturers were insufficient to compensate for the attenuation of light by the 4mm thick porcelain disc. 4. A strong inverse relationship was observed between peak heat flow and peak time in chemical cure(R=0.951), and a strong positive correlations hip was observed between peak heat flow and the heat of cure in light cure(R=0.928). There was no correlationship present between filler weight % or heat of cure and peak time. 5. The thermal decomposition of resin cements occured primarily between $300^{\circ}C$ and $480^{\circ}C$ with maximum decomposition rates at $335^{\circ}C$ and $440^{\circ}C$.

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Hydrogen and Ethanol Gas Sensing Properties of Mesoporous P-Type CuO

  • Choi, Yun-Hyuk;Han, Hyun-Soo;Shin, Sun;Shin, Seong-Sik;Hong, Kug-Sun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.222-222
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    • 2012
  • Metal oxide gas sensors based on semiconductor type have attracted a great deal of attention due to their low cost, flexible production and simple usability. However, most works have been focused on n-type oxides, while the characteristics of p-type oxide gas sensors have been barely studied. An investigation on p-type oxides is very important in that the use of them makes possible the novel sensors such as p-n diode and tandem devices. Monoclinic cupric oxide (CuO) is p-type semiconductor with narrow band gap (~1.2 eV). This is composed of abundant, nontoxic elements on earth, and thus low-cost, environment-friendly devices can be realized. However, gas sensing properties of neat CuO were rarely explored and the mechanism still remains unclear. In this work, the neat CuO layers with highly ordered mesoporous structures were prepared by a template-free, one-pot solution-based method using novel ink solutions, formulated with copper formate tetrahydrate, hexylamine and ethyl cellulose. The shear viscosity of the formulated solutions was 5.79 Pa s at a shear rate of 1 s-1. The solutions were coated on SiO2/Si substrates by spin-coating (ink) and calcined for 1 h at the temperature of $200{\sim}600^{\circ}C$ in air. The surface and cross-sectional morphologies of the formed CuO layers were observed by a focused ion beam scanning electron microscopy (FIB-SEM) and porosity was determined by image analysis using simple computer-programming. XRD analysis showed phase evolutions of the layers, depending on the calcination temperature, and thermal decompositions of the neat precursor and the formulated ink were investigated by TGA and DSC. As a result, the formation of the porous structures was attributed to the vaporization of ethyl cellulose contained in the solutions. Mesoporous CuO, formed with the ink solution, consisted of grains and pores with nano-meter size. All of them were strongly dependent on calcination temperature. Sensing properties toward H2 and C2H5OH gases were examined as a function of operating temperature. High and fast responses toward H2 and C2H5OH gases were discussed in terms of crystallinity, nonstoichiometry and morphological factors such as porosity, grain size and surface-to-volume ratio. To our knowledge, the responses toward H2 and C2H5OH gases of these CuO gas sensors are comparable to previously reported values.

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