• 제목/요약/키워드: Differential Scanning Calorimetry (DSC)

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Physicochemical Characterization of Extrudate Solid Formulation of Angelica gigas Nakai Prepared by Hot Melt Extrusion Process

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Koo, Ja Seong;Park, Cheol Ho;Kang, Wie Soo
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2018년도 춘계학술발표회
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    • pp.72-72
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    • 2018
  • The root of Angelica gigas Nakai (AGN) is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, a major challenge associated with the usage of the active compounds from AGN is their poor water solubility. Therefore, this work aimed to enhance the solubility of active compounds by a chemical (viz. surfactant) and physical (hot melt extrusion) crosslinking method (CPC). Infrared Fourier transform spectroscopy (FT-IR) revealed multiple peaks in extrudate solids representing new functional groups including carboxylic acid, alkynes and benzene derivatives. Differential scanning calorimetry (DSC) analysis of the extrudate showed lower glass transition temperature (Tg) and lower enthalpy (${\Delta}H$) (Tg: $43^{\circ}C$; ${\Delta}H$: <6 (J/g)) compared to the non-extrudate (Tg $68.5^{\circ}C$; ${\Delta}H$: 123.2) formulations. X-ray powder diffraction (XRD) analysis revealed amorphization of crystal materials in extrudate solid. In addition, nanonization, enhanced solubility and higher extraction of phenolic compounds were achieved in the extrudate solid. Among the different extrudates, acetic acid- and Span 80-mediated formulations showed superior extractions. We conclude that the CPC method successfully enhanced the production of amorphous nano dispersions from extrudate solid formulations.

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탈알루미늄화가 SAPO-11 분자체의 구조 및 산성도에 미치는 영향 (The Effect of Dealumination on the Structure and Acidity of SAPO-11 Molecular Sieve)

  • 박종열;이치헌;김수경
    • 대한화학회지
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    • 제40권3호
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    • pp.202-208
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    • 1996
  • 수열법으로 합성한 SAPO-11 분자체를 $H_4$EDTA로써 골격내의 알루미늄을 부분적으로 탈알루미늄화시킬때 24시간 탈알루미늄화까지는 골격이 안전하였으나 48시간 탈알루미늄화에 의해서는 구조가 붕괴되어 variscite($AIPO_4{\cdot}2H_2O$)와 tridymite($SiO_2$)로 변하였다. SAPO-11의 탈알루미늄화로 인하여 3607$cm^{-1}$과 3453$cm^{-1}$에서 하이드록실기에 의한 IR 흡수띠가 각각 관측되었다. 이들 하이드록실기 피크들의 세기는 탈알루미늄화의 정도에 비례하여 증가하였으며 메틸아민의 흡착에 의하여 피크가 사라지는 것으로 보아 이들은 Bronsted 산 자리임을 알 수 있었다. TPD(Temperature-Programmed Desorption) 및 DSC(Differential Scanning Calorimetry) 실험결과 탈알루미늄화된 SAPO-11에 흡착된 메틸아민과 물 분자는 탈알루미늄화가 되지않은 SAPO-11보다 높은 온도에서 그 피크들이 관측되었으며 메틸아민과 물 분자의 탈착 및 탈수 활성화 에너지는 탈알루미늄화의 정도에 비례하여 증가하였다. 이와 같은 현상은 제올라이트 분자체에 있어서와 유사하게 탈알루미늄으로 인하여 SAPO-11 분자체 내에 생성된 구조 하이드록실(srtuctural hydroxyl)기의 Bronsted 산 자리와 흡착 분자간의 보다 강한 상호작용에 기인되는 것으로 생각되었다.

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제철 분진을 함유한 PVC 복합체 수지의 기계적 성질 (Mechanical Properties of PVC Composite Containing Iron Dust)

  • 나재운;김명열
    • Elastomers and Composites
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    • 제33권5호
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    • pp.370-376
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    • 1998
  • 고로와 전로분진(광양제철)을 함유한 PVC복합체 수지의 역학적 성질을 혼합 성분비에 따라 측정하였다. 그 결과 인장강도는 혼합될 때의 고로 분진량이 8.83wt% 일 때 증가했으나 충격강도는 큰 변화를 나타내지 않았다. 이는 PVC와 CaO, SiO, MgO, $A1_2O_3$ 및 금속입자들을 포함한 분진과의 상용성에 따른 결과로 생각된다. 열중량분석(TGA) 결과 $600^{\circ}C$ 이상에서의 잔존량(wt%)은 첨가되는 분진의 량에 비례했으며 시차주사열량계(DSC) 측정 결과 역시 고로분진의 첨가량이 8.83wt% 일때 열적 안정성은 증가했다. X-ray회절 분석 결과는 블렌드 상태와 구조를 나타냈다.

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Lifetime Prediction and Aging Behaviors of Nitrile Butadiene Rubber under Operating Environment of Transformer

  • Qian, Yi-hua;Xiao, Hong-zhao;Nie, Ming-hao;Zhao, Yao-hong;Luo, Yun-bai;Gong, Shu-ling
    • Journal of Electrical Engineering and Technology
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    • 제13권2호
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    • pp.918-927
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    • 2018
  • Based on the actual operating environment of transformer, the aging tests of nitrile butadiene rubber (NBR) were conducted systematically under four conditions: in air, in transform oil, under compression in air and under compression in transform oil to studythe effect of high temperature, transform oil and compression stress simultaneously on the thermal aging behaviors of nitrile butadiene rubber and predict the lifetime. The effects of liquid media and compression stress simultaneously on the thermal aging behaviors of nitrile butadiene rubber were studied by using characterization methods such as IR spectrosc-opy, thermogravimetric measurements, Differential Scanning Calorimetry (DSC) measurements and mechanical property measurements. The changes in physical properties during the aging process were analyzed and compared. Different aging conditions yielded materials with different properties. Aging at $70^{\circ}C$ under compression stress in oil, the change in elongation at break was lower than that aging in oil, but larger than that aging under compression in air. The compression set or elongation at break as evaluation indexes, 50% as critical value, the lifetime of NBR at $25^{\circ}C$ was predicted and compared. When aging under compression in oil, the prediction lifetime was lower than in air and under compression in air, and in oil. It was clear that when predicting the service lifetime of NBR in oil sealing application, compression and media liquid should be involved simultaneously. Under compression in oil, compression set as the evaluation index, the prediction lifetime of NBR was shorter than that of elongation at break as the evaluation index. For the life prediction of NBR, we should take into account of the performance trends of NBR under actual operating conditions to select the appropriate evaluation index.

$PEO-EDA-LiClO_4$ 블렌드계 탄성체 전해질의 제조와 특성 (Preparation and Characterization of Elastomeric Solid Electrolyte Based on $PEO-EDA-LiClO_4$ Blends)

  • 장영욱;주현석
    • Elastomers and Composites
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    • 제39권1호
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    • pp.36-41
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    • 2004
  • Poly(ethylene oxide)(PEO)와 epoxy diacrylate(EDA) 및 금속염인 LiClO_4$를 블렌드하고 자외선 가교시킴으로써 이온전도특성을 나타내는 고체 전해질을 제조하고, 제조된 전해질의 이온 전도도를 블렌드조성 염농도 및 온도 변화에 따가 측정하였다. PEO/EDA의 조성비가 70/30 wt%이고 ethylene $oxide/Li^+$의 몰비가 10인 전해질이 $25^{\circ}C$에서 $1.2{\times}10^{-5} S/cm$에 달하는 높은 이온전도도를 나타내었다. 제조된 전해질 필름은 투명하였으며 고무와 같은 탄성을 나타내었다. DSC, XRD 및 편광현미경을 이용한 모폴로지 분석으로부터 에폭시 사슬이 PEO의 결정화를 억제함으로써 완전히 무정형인 블렌드를 제조할 수 있음을 확인할 수 있었다.

Fabrication and Characterization of Modified Poly(2-hydroxyethyl methacrylate)(PHEMA) Hydrogels by Thermal/Photo Polymerization

  • Lee, Minsu;Lee, Junghyun;Jang, Jihye;Nah, Changwoon;Huh, Yang-il
    • Elastomers and Composites
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    • 제54권4호
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    • pp.359-367
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    • 2019
  • Poly(2-hydroxyethyl methacrylate) (PHEMA) hydrogels modified with various co-monomers, such as N-vinyl pyrrolidone (NVP), glycidyl methacrylate (GMA), and glycerol monomethacrylate (GMMA), were prepared to investigate the effect of adding a co-monomer on the water contents, surface wettability, and tensile modulus. These polymers were synthesized by thermal- and photo-polymerization in the presence of azobisisobutyronitrile (AIBN) and diphenyl(2,4,6-trimethylbenzoyl)-phosphineoxide (TPO) as the initiators. The characteristics of the hydrogels were analyzed via FTIR and UV/Vis spectroscopies, contact angle measurements, and tensile modulus measurements with UTM. Regarding the properties of water in the hydrogels, the ratio between free to bound water was investigated using differential scanning calorimetry (DSC). The effects of adding the co-monomers on the water content, surface wettability, and tensile modulus for soft contact lenses were also investigated. In the case of p(HEMA-co-NVP) hydrogels, the increase in the equilibrium water content (EWC) was primarily due to the increase in the bound water content. For p(HEMA-co-GMMA) hydrogels, an increase in free water content was the main reason for the increased EWC. In contrast, in the case of p(HEMA-co-GMA) hydrogels, a decrease in bound water content was observed to be the main factor that reduced the EWC. Photo-polymerized PHEMA hydrogels showed enhanced surface wettability and tensile modulus as compared to those produced via thermal polymerization.

플라즈마 중합법에 의한 스티렌 박막의 분자 구조 및 분자량 제어에 관한 연구 (A Study on the molecular structure and molecular weight control of styrene films by plasma polymerization)

  • 김종택;최충양;박종관;박응춘;이덕출
    • 한국진공학회지
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    • 제6권3호
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    • pp.213-219
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    • 1997
  • 본 연구에서는 내전극 정전결합 유동가스형 반응장치를 이용하여 플라즈마 중합 스 티렌 박막을 제작하고 적외선분광스펙트럼, 열분해가tm크로마토그래피, 시차주사열량계 및 겔투과성 크로마토그래피의 분석을 통하여 중합조건이 분자구조 및 분자량 분포에 미치는 영향을 조사하였다. 위의 결과로부터 개시 모노머의 화학적 특성과는 다른 고도로 가교된 박막이 생성되었으며, 방전압력, 방전전력 및 가스의 유량 등의 중합조건 조절에 의해 분자 구조, 가교도, 분자량 분포 등의 제어가 가능함이 판명되었다. 따라서 내전극 정전결합 유동 가스형 반응장치에 의해 수행된 플라즈마중합법은 중합조건의 조절에 의해 센서의 감지막, 광도전성 소자 및 포토 레지스트 등에 응용가능한 기능성 유기박막의 제작에 좋은 특성을 나타내는 것을 알 수 있었다.

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XLPE 절연층과 반도전층 재료의 비열 및 열전도 측정 (Specific Heat and Thermal Conductivity Measurement of XLPE Insulator and Semiconducting Materials)

  • 이경용;양종석;최용성;박대희
    • 대한전기학회논문지:전기물성ㆍ응용부문C
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    • 제55권1호
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    • pp.6-10
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    • 2006
  • To improve mean-life and reliability of power cable, we have investigated specific heat (Cp) and thermal conductivity of XLPE insulator and semiconducting materials in 154(kV) underground power transmission cable. Specimens were respectively made of sheet form with EVA, EEA and EBA added $30[wt\%],$ carbon black, and the other was made of sheet form by cutting XLPE insulator in 154(kV) power cable. Specific heat (Cp) and thermal conductivity were measured by DSC (Differential Scanning Calorimetry) and Nano Flash Diffusivity. Specific-heat measurement temperature ranges of XLPE insulator were from $20[^{\circ}C]\;to\;90[^{\circ}C],$ and the heating rate was $1[^{\circ}C/mon].$ And the measurement temperatures of thermal conductivity were $25[^{\circ}C],\;55[^{\circ}C]\;and\;90[^{\circ}C].$ In case of semiconducting materials, the measurement temperature ranges of specific heat were from $20[^{\circ}C]\;to\;60[^{\circ}C],$ and the heating rate was $1[^{\circ}C/mon].$ And the measurement temperatures of thermal conductivity were $25[^{\circ}C],\;55[^{\circ}C].$ In addition we measured matrix of semiconducting materials to show formation and growth of carbon black in base resins through the SEM. From these experimental results, both specific heat and thermal conductivity were increased by heating rate because volume of materials was expanded according to rise in temperature.

Post space preparation timing of root canals sealed with AH Plus sealer

  • Kim, Hae-Ri;Kim, Young Kyung;Kwon, Tae-Yub
    • Restorative Dentistry and Endodontics
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    • 제42권1호
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    • pp.27-33
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    • 2017
  • Objectives: To determine the optimal timing for post space preparation of root canals sealed with epoxy resin-based AH Plus sealer in terms of its polymerization and influence on apical leakage. Materials and Methods: The epoxy polymerization of AH Plus (Dentsply DeTrey) as a function of time after mixing (8, 24, and 72 hours, and 1 week) was evaluated using Fourier transform infrared (FTIR) spectroscopy and microhardness measurements. The change in the glass transition temperature ($T_g$) of the material with time was also investigated using differential scanning calorimetry (DSC). Fifty extracted human single-rooted premolars were filled with gutta-percha and AH Plus, and randomly separated into five groups (n = 10) based on post space preparation timing (immediately after root canal obturation and 8, 24, and 72 hours, and 1 week after root canal obturation). The extent of apical leakage (mm) of the five groups was compared using a dye leakage test. Each dataset was statistically analyzed by one-way analysis of variance and Tukey's post hoc test (${\alpha}=0.05$). Results: Continuous epoxy polymerization of the material with time was observed. Although the $T_g$ values of the material gradually increased with time, the specimens presented no clear $T_g$ value at 1 week after mixing. When the post space was prepared 1 week after root canal obturation, the leakage was significantly higher than in the other groups (p < 0.05), among which there was no significant difference in leakage. Conclusions: Poor apical seal was detected when post space preparation was delayed until 1 week after root canal obturation.

Thermal properties and mechanical properties of dielectric materials for thermal imprint lithography

  • Kwak, Jeon-Bok;Cho, Jae-Choon;Ra, Seung-Hyun
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2006년도 하계학술대회 논문집 Vol.7
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    • pp.242-242
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    • 2006
  • Increasingly complex tasks are performed by computers or cellular phone, requiring more and more memory capacity as well as faster and faster processing speeds. This leads to a constant need to develop more highly integrated circuit systems. Therefore, there have been numerous studies by many engineers investigating circuit patterning. In particular, PCB including module/package substrates such as FCB (Flip Chip Board) has been developed toward being low profile, low power and multi-functionalized due to the demands on miniaturization, increasing functional density of the boards and higher performances of the electric devices. Imprint lithography have received significant attention due to an alternative technology for photolithography on such devices. The imprint technique. is one of promising candidates, especially due to the fact that the expected resolution limits are far beyond the requirements of the PCB industry in the near future. For applying imprint lithography to FCB, it is very important to control thermal properties and mechanical properties of dielectric materials. These properties are very dependent on epoxy resin, curing agent, accelerator, filler and curing degree(%) of dielectric materials. In this work, the epoxy composites filled with silica fillers and cured with various accelerators having various curing degree(%) were prepared. The characterization of the thermal and mechanical properties wasperformed by thermal mechanical analysis (TMA), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), rheometer, an universal test machine (UTM).

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