• 제목/요약/키워드: DSC measurement

검색결과 170건 처리시간 0.024초

감포지역(甘浦地域) Ca-몬모릴로나이트의 열적(熱的) 및 광물학적(鑛物學的) 특성(特性) (Thermal and Mineralogical Characterization of Ca-Montmorillonite from Gampo Area)

  • 문희수;최선경;김문영
    • 자원환경지질
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    • 제21권2호
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    • pp.175-184
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    • 1988
  • 감포지역(甘浦地域)의 용동리에서 용동리응회암(龍洞里凝灰岩)내에 배태되는 Ca-몬모릴로나이트들은 비록 동일층준(同一層準)에서 산출(産出)되나 제한적(制限的)이지만 화학조성(化學組成)의 차이(差異)가 나타난다. 이들의 열적특성은 "비정상형(型)"으로 나타나며, 탈수와 관계된 흡열반응피크의 온도(溫度)는 사면체내의 Si를 치환한 Al의 양적비에 따라 약간변화된다. 이러한 사실은 제한적인 화학조성의 변화는 열적특성에 큰 영향을 미치지 못함을 지시한다. 시차주사열량 측정결과 2가의 양이온으로 치환 된 시료의 경우 1가의 양이온으로 치환된 시료보다 흡열용량이 증가되는 경향을 보이므로 시료내의 우세한 양이온의 종류를 예상할 수 있으며, 전기음성도가 큰 이온일수록 더 많은 물분자를 취(取)함을 알수있다.

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C$_22$ -quinolinium(TCNQ) LB막의 주파수에 따른 전기적 특성 (Frequency-dependent electrical properties of $C_22$ -quinolinium(TCNQ) langmuir-blodgett films)

  • 김태완;이상국;신동명;강도열
    • E2M - 전기 전자와 첨단 소재
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    • 제8권2호
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    • pp.151-157
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    • 1995
  • Frequency-dependent electrical properties of $C_{22}$-Quinolinium(TCNQ) LB films were investigated in a frequency range of 10[Hz]-13[MHz] along a perpendicular direction. The films were heat-treated to understand an electrodynamic response in a temperature range of 20-240[.deg. C]. Frequencydependent dielectric constants show that there are two characteristic dispersions; one is a dispersion occuring near 1[MHz] coming from the orientational polarization of the molecules and the other one is an interfacial polarization effect below 1[kHz] or so when the annealing temperature is above 80 [.deg. C]. The overall frequency-dependent dielectric constant is higher near 80[.deg. C]. It may be due to a softness of the alkyl chains. Several other methods were employed to identify the internal structure change of the films. DSC(differential scanning calorimetry) data of the $C_{22}$-Quinolinium(TCNQ) molecules shows that there is an endothermic process near 110[.deg. C] and a weak exothermic process near 180[.deg. C]. While the endothermic process is related to a disordering of the alkyl chains, the exothermic process seems to be due to a chemical structure change of the TCNQ molecules. Thickness measurement by ellipsometry shows that there is a thickness drop near 100[.deg. C], and the thickness above 120[.deg. C] becomes around 20[%] of the room-temperature value.lue.

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온도변화에 따른 폴리에틸렌텔레프탈레이트 박막의 체적고유저항 특성 (Volume Resistivity Properties of Polyethylene Terephthalate Film due to Temperature Variation)

  • 윤정일;고길영;신현택;신종열;이충호;홍진웅
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2002년도 추계학술대회 논문집 Vol.15
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    • pp.224-227
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    • 2002
  • In this paper, we have investigated the physical properties and electrical conduction properties of polyethylene terephthalate film due to temperature variation, and the measurement of volume resistivity used to highmegohm meter is measured from 1 to 10 minutes when the specimen applied the voltage accroding to the step voltage appling method. From FT-IR spectrum as an analysis of physical properties, the strong absorption in wavenumbers $1019[cm^{-1}]$, $1266[cm^{-1}]$ and $1752[cm^{-1}]$ observed by the C=O and benzene ring. From the analysis of DSC, the crystalline melting points of the specimen observed in the temperature $80[^{\circ}C]$ and $263[^{\circ}C]$, respectively.

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기계적 합금화법에 의한 Fe2O3-Zn계 연자성 복합분말의 제조 및 특성평가 (Synthesis and Characterization of Soft Magnetic Composite Powders in Fe2O3-Zn System by Mechanical Alloying)

  • 이충효
    • 한국재료학회지
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    • 제30권2호
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    • pp.74-80
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    • 2020
  • Synthesis of composite powders for the Fe2O3-Zn system by mechanical alloying (MA) has been investigated at room temperature. Optimal milling and heat treatment conditions to obtain soft magnetic composite with fine microstructure were investigated by X-ray diffraction, differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM) measurement. It is found that α-Fe/ZnO composite powders in which ZnO is dispersed in α-Fe matrix can be obtained by MA of Fe2O3 with Zn for 4 hours. The change in magnetization and coercivity also reflects the details of the solid-state reduction process of hematite by pure metal of Zn during MA. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine at 900 ~ 1,000 ℃ under 60 MPa. Shrinkage change after SPS of sample MA'ed for 5 hrs was significant above 300 ℃ and gradually increased with increasing temperature up to 800 ℃. X-ray diffraction results show that the average grain size of α-Fe in the α-Fe/ZnO composite sintered at 900 ℃ is in the range of 110 nm.

열처리에 따른 제2상 석출이 Al-4.5%Cu 합금의 열 물성에 미치는 영향 (Influences of Precipitation of Secondary Phase by Heat Treatment on Thermal Properties of Al-4.5%Cu Alloy)

  • 최세원
    • 한국재료학회지
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    • 제30권8호
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    • pp.435-440
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    • 2020
  • The relationship between the precipitation of secondary phase and the thermal properties of Al-4.5%Cu alloy (in wt.%) after various heat treatments has been studied. Solid solution treatment of alloy was performed at 808 K for 6 hours, followed by warm water quenching; then, the samples were aged in air at 473 K for different times. The thermal diffusivity of the Al-4.5%Cu alloy changed with the heat treatment conditions of the alloy at temperatures below 523 K. The as-quenched specimen had the lowest thermal diffusivity, and as the artificial aging time increased, the thermal diffusivity of the specimen increased in the temperature range between 298 and 523 K. For the specimen aged for five hours, the thermal conductivity was 12% higher than that of the as-quenched specimens at 298 K. It is confirmed that the thermal diffusivity and thermal conductivity of the Al-4.5%Cu alloy significantly depend on their thermal history at temperatures below 523 K. The precipitation and dissolution of the Al2Cu phase were confirmed via DSC for the alloys, and the formation of coefficient of thermal expansion peaks in TMA was caused by precipitation. The precipitation of supersaturated solid solution of Al-4.5%Cu alloys had an additional linear expansion of ≈ 0.05 % at 643 K during thermal expansion measurement.

Sonochemical Synthesis, Thermal Studies and X-ray Structure of Precursor [Zr(acac)3(H2O)2]Cl for Deposition of Thin Film of ZrO2 by Ultrasonic Aerosol Assisted Chemical Vapour Deposition

  • Hussain, Muzammil;Mazhar, Muhammad;Rauf, Muhammad Khawar;Ebihara, Masahiro;Hussain, Tajammal
    • Bulletin of the Korean Chemical Society
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    • 제30권1호
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    • pp.92-96
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    • 2009
  • A new precursor [$Zr(acac)_{3}(H_{2}O)_{2}$] was synthesized by Sonochemical technique and used to deposit thin $ZrO_{2}$ film on quartz and ceramic substrate via ultrasonic aerosol assisted chemical vapour deposition (UAACVD) at 300 ${^{\circ}C}$ in oxygen environment followed by annealing of the sample for 2-3 minutes at 500 ${^{\circ}C}$ in nitrogen ambient. The molecular structure of the precursor determined by single crystal X-ray analysis revealed that the molecules are linked through intermolecular hydrogen bonds forming pseudo six and eight membered rings. DSC and TGA/FTIR techniques were used to determine thermal behavior and decomposition temperature of the precursor and nature of evolved gas products. The optical measurement of annealed $ZrO_{2}$ film with tetragonal phase shows optical energy band gap of 5.01 eV. The particle size, morphology, surface structure and composition of deposited films were investigated by XRD, SEM and EDX.

Synthesis of a Novel Phosphorus-containing Flame Retardant for Epoxy Resins

  • Xu, Hong-Jun;Jin, Fan-Long;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • 제30권11호
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    • pp.2643-2646
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    • 2009
  • In this study, a novel phosphorus-containing flame retardant copolymer of spirocyclic pentaerythritol di(phosphate monochloride) and bisphenol S (SPD-BS) was successfully synthesized and used as a flame retardant in diglycidyl ether of bisphenol A (DGEBA) epoxy resins. The chemical structure of the SPD-BS was characterized using FT-IR and $^1H$ NMR spectra. The thermal properties were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The effects of SPD-BS and nano-$CaCO_3$ on the flame-retardant properties of DGEBA/SPD-BS systems were evaluated by measurement of the burning rate. As a result, the thermal stabilities of the DGEBA/SPD-BS systems were decreased with increasing SPD-BS content. The flame-retardant properties and char yields of the systems were significantly increased when SPD-BS content increased. The synergism of nano-$CaCO_3$ incorporation on flame retardancy was found for the DGEBA/SPD-BS systems.

비고용 V-Cu계 MA합금의 중성자 및 X선 회절에 의한 상분석 (Phase Analysis of Immiscible V-Cu MA Powders by Neutron and X-ray Diffraction)

  • 이충효;조재문;이상진;김지순
    • 한국재료학회지
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    • 제14권5호
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    • pp.348-352
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    • 2004
  • The mechanical alloying (MA) effect in immiscible V-Cu system with positive heat of mixing was studied by not only the neutron and X-ray diffraction but also the analysis of DSC spectra. The total energy, ΔHt accumulated during MA for the mixture of $V_{50}$ $Cu_{50}$ / powders increased with milling time and approached the saturation value of 14 kJ/mol after 120 h of milling. It can be seen that the free energy difference between the amorphous phase and the pure V and Cu powders with an atomic ratio 5:5 is estimated to be 11 kJ/mol by Miedema et al. This is thermodynamically taken as one of the evidences for the amorphization. The structural changes of V-Cu MA powders were characterized by the X-ray diffraction and neutron diffraction. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. The neutron diffraction data definitely indicate that the amorphization proceeds gradually but incompletely even after 120 h of MA and bcc-Cu Bragg peaks appears after 60 h of MA.

A Study on the Deintercalation Reaction of Li-Graphite Intercalation Compounds

  • 오원천;김범수
    • Bulletin of the Korean Chemical Society
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    • 제21권1호
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    • pp.101-104
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    • 2000
  • Li-graphite intercalation compounds (GICs), synthesized at elevated temperature and pressure, were allowed to decompose spontaneously in the atmosphere. The decomposition processes were analyzed by of X-ray diffraction, DSC analysis, FT-IR measurements, UV/VIS spectrophotometry. The deintercalation reaction of the Li-GICs ceased after 6 weeks and only the residual compounds could be observed. A strong exothermic reaction was observed at 300 $^{\circ}C$ in thermal decomposition, and relatively stable decomposition curves were formed. A few endothermic curves have been observed at 1000 $^{\circ}C.$ After 6 weeks deintercalation reaction time of GICs, many exothermic and endothermic reactions were accompanied at the same time. In addition the reactions of the functional groups such as aromatic rings, nitrogen, $-CH_3$, $-CH_2$ etc. of GDIC obtained by the above reaction were confirmed by FT-IR spectrum. UV/VIS spectrophotometric measurement clearly shows the formation of a minimum energy value ($R_{min}$) for the compounds between Li-GICs as a starting material and Li-GDICs obtained until after 3 weeks of the deintercalation reaction, while they were no clear energy curves from 4 weeks of reaction time, because of the formation of the graphite structure, of high stages and of the Li compounds surrounding the graphite in the deintercalation reaction.

고분자전해질막의 노후화에 따른 기계적 특성 변화에 관한 연구 (A Study on the Change of Mechanical Property According to the Aging of Polymer Electrolyte Membrane)

  • 김승환;어준우;서영진;황철민;정영관
    • 한국수소및신에너지학회논문집
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    • 제33권2호
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    • pp.176-182
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    • 2022
  • Since the various characteristics of the polymer electrolyte membrane are not clearly identified, it is difficult to predict and design applications for various conditions. In this study, as a previous study on the aging of the polymer electrolyte membrane, a study was conducted on the change of mechanical properties according to the aging of the polymer electrolyte membrane. Through the tensile test of Nafion 117, the mechanical properties change due to aging was confirmed. As a result of the tensile test, it was confirmed that the aged Nafion 117 had reduced tensile strength. Through DSC measurement, aged Nafion confirmed that the glass transition temperature and enthalpy change were low, which is thought to be the effect of molecular motion and transition due to the lapse of time. The effect is thought to cause a difference in the amount of change in enthalpy, resulting in a difference in mechanical properties during tension.