• Journal of Powder Materials
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• 제25권3호
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• pp.246-250
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• 2018

In this study, we investigate the deformation behavior of $Hf_{44.5}Cu_{27}Ni_{13.5}Nb_5Al_{10}$ metallic glass powder under repeated compressive strain during mechanical milling. High-density (11.0 g/cc) Hf-based metallic glass powders are prepared using a gas atomization process. The relationship between the mechanical alloying time and microstructural change under phase transformation is evaluated for crystallization of the amorphous phase. Planetary mechanical milling is performed for 0, 40, or 90 h at 100 rpm. The amorphous structure of the Hf-based metallic glass powders during mechanical milling is analyzed using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Microstructural analysis of the Hf-based metallic glass powder deformed using mechanical milling reveals a layered structure with vein patterns at the fracture surface, which is observed in the fracture of bulk metallic glasses. We also study the crystallization behavior and the phase and microstructure transformations under isothermal heat treatment of the Hf-based metallic glass.

• Korea-Australia Rheology Journal
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• 제17권1호
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• pp.21-25
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• 2005

Rheological properties and crystallization kinetics of the polypropylene (PP) block copolymer and recycled PP block copolymer were studied by advanced rheometric expansion system (ARES), differential scanning calorimetry (DSC), and optical microscopy. In the study of the dynamic rheology, it is observed that the storage modulus and loss modulus for the PP block copolymer and recycled PP block copolymer did not change with frequency. In the study of the effect of the repeated extrusion on the crystallization rate, half crystallization time of the PP samples was increased with the number of repeated extrusion in isothermal crystallization temperature ($T_c$). From the isothermal crystallization kinetics study, the crystallization rate was decreased with the increase of the number of repeated extrusion. Also, from the result of Avrami plot, the overall crystallization rate constant (K) was decreased with the increase of the number of the repeated extrusion. From the study of the optical microscopy, the size of the spherulite of the PP samples did not change significantly with the number of repeated extrusion. However, it was clearly observed that the number of the spherulite growth sites was decreased with the number of repeated extrusion. From the results of the crystallization rate, isothermal crystallization kinetics, Avrami plots, and optical microscopy, it is suggested that the crystallization rate of the PP block copolymer is decreased with the increase of the number of repeated extrusion.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.185-185
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• 2016

아크릴계 수지(resin)에 인조 흑연과 탄소나노튜브(carbon nanotube)를 1:1 비율로 혼합한 충전제(filler)와 용제(solvent) 및 기타 첨가제(additives)를 혼합하여 방열도료를 제조하여 수직방향 열전도도를 상온에서 평가하였다. 충전제의 함량을 1, 2, 5 중량 %로 변화시키며 원료들을 준비하여 교반기로 혼합한 뒤 3단 롤 밀(three roll mill)로 분산공정을 진행하여 3 종류의 도료를 제조하였다. 제조한 도료를 가로 11 mm, 세로 11 mm, 두께 0.4 mm의 Al 5052 알루미늄 기판에 스프레이 코팅 방식으로 도포한 후 $150^{\circ}C$에서 30분 동안 열경화 건조 과정을 거쳐 샘플을 제작하였다. 측정 시료의 형상은 대략적으로 Fig. 1과 같다. 열전도도는 식 $k={\alpha}{\cdot}C_p{\cdot}{\rho}$를 사용해서 계산된다. 여기서 k는 열전도도($W/m{\cdot}K$), ${\alpha}$는 열확산계수($mm^2/s$), $C_p$는 비열($J/kg{\cdot}K$), ${\rho}$는 밀도($g/cm^3$)를 나타낸다. 열확산계수는 독일 NETZSCH 사의 Laser Flash Analysis 장비(모델명 LFA 457)를 사용하여 측정하였는데, 기판 뒤쪽에서 레이저를 조사하고 도료층 전면에서 적외선 온도센서를 통해 시간에 따른 온도 상승곡선을 구한 후, 두 물체의 계면에서의 접촉 열저항(contact thermal resistance)을 감안하여 장비에 내장되어 있는 소프트웨어로 열확산계수가 계산된다. 비열은 같은 회사의 DSC(Differential Scanning Calorimetry) 200 F3 장비를 사용해 측정했으며, 밀도는 부피와 질량을 측정한 값을 이용하여 계산하였다. 도료를 도포하지 않은 bare Al plate에 대해서는 쉽게 열확산계수, 비열, 밀도를 측정하여 열전도도를 구할 수 있다. 도료가 코팅된 샘플에 대해서는 도료층을 일부 떼어내 비열을 측정하고, 밀도를 구한 후, 도료층의 열전도도가 2-layer 법으로 장비 내장 소프트웨어로 계산된다, 이때 Al 기판의 열확산계수, 비열, 밀도는 미리 측정한 bare Al plate의 값을 적용하였다. 실험 결과를 Table 1에 정리하였다. 흑연과 탄소나노튜브를 혼합한 충전제를 함유한 아크릴 복합체 박막에서 측정된 열전도도는 보통 고분자 재료의 열전도도 값의 상한 영역에 육박하는 값이며, 충전제 함량이 증가할수록 열전도도가 증가하는 경향을 보이고 있다.

• Korean Journal of Materials Research
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• 제22권9호
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• pp.454-458
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• 2012

Various adhesive materials are used in flip chip packaging for electrical interconnection and structural reinforcement. In cases of COF(chip on film) packages, low temperature bonding adhesive is currently needed for the utilization of low thermal resistance substrate films, such as PEN(polyethylene naphthalate) and PET(polyethylene terephthalate). In this study, the effects of anhydride and dihydrazide hardeners on the low-temperature snap cure behavior of epoxy based non-conductive pastes(NCPs) were investigated to reduce flip chip bonding temperature. Dynamic DSC(differential scanning calorimetry) and isothermal DEA(dielectric analysis) results showed that the curing rate of MHHPA(hexahydro-4-methylphthalic anhydride) at $160^{\circ}C$ was faster than that of ADH(adipic dihydrazide) when considering the onset and peak curing temperatures. In a die shear test performed after flip chip bonding, however, ADH-containing formulations indicated faster trends in reaching saturated bond strength values due to the post curing effect. More enhanced HAST(highly accelerated stress test) reliability could be achieved in an assembly having a higher initial bond strength and, thus, MHHPA is considered to be a more effective hardener than ADH for low temperature snap cure NCPs.

• Korean Journal of Materials Research
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• 제21권5호
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• pp.283-287
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• 2011

As the performance of microelectronic devices is improved, the use of copper as a heat dissipation member is increasing due to its good thermal conductivity. The high thermal conductivity of copper, however, leads to difficulties in the joining process. Satisfactory bonding with copper is known to be difficult, especially if high shear and peel strengths are desired. The primary reason is that a copper oxide layer develops rapidly and is weakly attached to the base metal under typical conditions. Thus, when a clean copper substrate is bonded, the initial strength of the joint is high, but upon environmental exposure, an oxide layer may develop, which will reduce the durability of the joint. In this study, an epoxy adhesive formulation was investigated to improve the strength and reliability of a copper to copper joint. Epoxy hardeners such as anhydride, dihydrazide, and dicyandiamide and catalysts such as triphenylphosphine and imidazole were added to an epoxy resin mixture of DGEBA and DGEBF. Differential scanning calorimetry (DSC) analyses revealed that the curing temperatures were dependent on the type of hardener rather than on the catalyst, and higher heat of curing resulted in a higher Tg. The reliability of the copper joint against a high temperature and high humidity environment was found to be the lowest in the case of dihydrazide addition. This is attributed to its high water permeability, which led to the formation of a weak boundary layer of copper oxide. It was also found that dicyandiamide provided the highest initial joint strength and reliability while anhydride yielded intermediate performance between dicyandiamide and dihydrazide.

• Macromolecular Research
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• 제12권2호
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• pp.195-205
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• 2004

We have synthesized new aromatic polyesters (DiPEG-HQ and DiPEG-BP) by condensation polymerization of a terephthalic acid derivative bearing a pendant oligo(oxyethylene) (DP = 7, MW = 350), which has a methoxy terminal group, and two different aromatic diols, hydroquinone and 4,4'-biphenoI. The synthesized polymers were characterized by differential scanning calorimetry (DSC), polarizing microscopy, and X-ray diffractometry for their liquid crystallinity (LC), thermal transitions, and structural morphologies in mesophases. The morphology of the LC phases depends strongly on the length of the rigid backbone repeating unit. The DiPEG-BP polymer having a longer repeating unit exhibits both layered and nematic structures before isotropization, whereas the DiPEG-HQ polymer having a shorter repeating unit shows only the layered structure in the mesophase. We found that the layer spacing for DiPEG-HQ is larger than that for DiPEG-BP. Both polymers easily form complexes with LiCF$_3$SO$_3$; we studied this complex formation by FT-IR spectroscopy. The layer spacing of the polymer-electrolyte composites increases upon increasing the amount of the lithium salt. The polymer/salt electrolyte mixtures we investigated at molar ratios of EO:salt in the range of 5-20 exhibit electrical conductivity values at 40$^{\circ}C$ of 2.4${\times}$10$\^$5/ and 1.1${\times}$10$\^$－5/ S/cm for DiPEG-HQ/LiCF$_3$SO$_3$ and DiPEG-BP/LiCF$_3$SO$_3$, respectively. At 80 $^{\circ}C$, these values are higher: 4.6${\times}$10$\^$－3/ and 1.1${\times}$10$\^$－4/ S/cm, respectively. The activation energy of conductivity depends strongly on the salt concentration.

• Textile Coloration and Finishing
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• 제8권2호
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• pp.1-7
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• 1996

Thermotropic liquid-crystalline polyurethanes were synthesized by the polyaddition reaction of such para-substiuted diisocyanate monomer as 1,4-phenylene diisocyanate(1,4-PDI) and 2,5-tolylene diisocyanate(2,5-TDI), with 4,4'-bis($\omega$-hydroxyalkoxy)biphenyls(BPm: $HOC_{m}OC_{6}H_{4}C_{6}H_{4}OC_{m}H_{2m}OH$; m is the carbon number of the hydroxyalkoxy group). These polyurethanes have mesogenic biphenyl units in the main chain. Properties of polymers were studied by differential scanning calorimetry, wide-angle X-ray scattering, thermogravimetic analysis, polarizing microscopy, and infraed spectroscopy. DSC thermograms for these polymers exhibited two endothermic peaks corresponding to phase transitions of melting and isotropization. Mesomorphic behavior of the polyurethanes were also observed under the polarizing microscope. For example, polyurethane 2,5-YDI/BP5 with [$\theta$]=0.44 prepared from 2,5-TDI and BP5 exhibited a liquid crystalline phase from 194 to 205$^{\circ}C$. Infrared spectrum study indicated that the hydrogen bonding between urethane linkages affected the mesomorphism. The thermostabilities of polyurethanes 2,5-TDI/BP5 and 1,4-PDI/BP5 were measured at a heating rate of 1$0^{\circ}C$/min in air. The temperatures of 5% weight loss for 2,5-TDI/BP5 and 1,4-PDI/BP5 were 297 and 334$^{\circ}C$, respectively.

• Food Science and Biotechnology
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• 제18권4호
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• pp.855-860
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• 2009

Physicochemical properties of starches isolated from 3 new potato cultivars developed by Potato Valley Ltd. were investigated and compared to those of starch isolated from 'Superior' being distributed prominently in Korea. Significant differences were observed in physicochemical properties such as granule size, amylose content, phosphorus content, water binding capacity, swelling power, solubility, and in vitro digestibility of starches from different potato cultivars. Thermal properties were evaluated using differential scanning calorimetry (DSC), and onset gelatinization temperatire ($T_o$), peak temperature ($T_p$), and enthalpies of gelatinization (${\triangle}H$) of different potato cultivars ranged as $58.0{\pm}0.3-61.7{\pm}0.4^{\circ}C,\;63.7{\pm}0.2-$ $66.5{\pm}0.0^{\circ}C$, and $15.6{\pm}0.5-17.0{\pm}0.3$ J/g, respectively. Pasting properties were evaluated using a rapid visco analyzer (RVA), and pasting temperature, peak viscosity, and final viscosity of different potato cultivars ranged as $65.0{\pm}0.1-68.9{\pm}0.1^{\circ}C$, $8,163.7{\pm}196.3-9,035.7{\pm}6.4$ cp, and $4,397.7{\pm}166.7-7,025.0{\pm}271.3$ cp, respectively. Especially, 'Gogu valley' starch showed the highest values in the amylose and phosphorus content among tested potato cultivars and higher water binding capacity, swelling power, and solubility than those of other tested starches. And it also showed high pasting temperature, peak viscosity, trough viscosity, and final viscosity as compared to other tested starches.

• Journal of Pharmaceutical Investigation
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• 제32권2호
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• pp.73-80
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• 2002

Cefuroxime axetil is a cephalosporin antibiotic having a high activity against a wide spectrum of Grampositive and Gram-negative microorganisms. It is a cephalosporin antibiotic which exist as 2 diastereoisomers: diastereoisomer A and B. It shows polymorphism of three forms: a crystalline form having a melting point of about $180^{\circ}C$, a substantially amorphous form having a high melting point of about $135^{\circ}C$ and a substantially amorphous form having a low melting point of about 70^{\circ}C$. The crystalline form of cefuroxime axetil is slightly soluble in water because diastereoisomer A has lower solubility than B in water. Substantially amorphous form of which there are no difference in solubility between diastereoisomer A and B has better solubility than crystalline form, but it forms a thicker gel than crystalline form upon contact with an aqueous medium. Based on this reason, cefuroxime axetil is not readily absorbable in the gastrointestinal tract, rendering its bioavailability on oral administration very low. The object of this study was to develop an improved non-crystalline cefuroxime axetil composition having a high physicochemical stability and bioavailability. A non-crystalline cefuroxime axetil solid dispersant showing no peak on a Differential Scanning Calorimetry (DSC) scan is prepared by dissolving cefuroxime axetil and a surfactant in an organic solvent; suspending a water-insoluble inorganic carrier in the resulting solution; and spray drying the resulting suspension to remove the organic solvent, said solid dispersant having an enhanced dissolution and stability of cefuroxime axetil and being useful for the preparation of a pharmaceutical composition for oral administration. Tablet was formulated with this cefuroxime axetil solid dispersant, disintegrants and other ingredients. It disintegrated and dissolved easily and dynamically in dissolution medium, so showed a good dissolution profile.

• Journal of Pharmaceutical Investigation
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• 제40권1호
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• pp.9-14
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• 2010

Lacidipine used for the treatment of hypertension has low water solubility and is classified as BCS Class II category. Gelucire-based solid dispersions (SD) containing lacidipine were prepared by solvent evaporation method to enhance drug dissolution. The powdered forms of SD showed irregularly spherical shape. Thermal behaviors of SD from differential scanning calorimetry indicated that distinct endothermic peak of lacidipine ($184^{\circ}C$) was shifted to lower region ($150.1^{\circ}C$). Drug was present in a crystalline form. NMR spectra also showed some molecular interaction between drug and Gelucire. There was no significant difference in DSC and NMR behaviors between Gelucire 44/14 and Gelucire 50/13. The initial dissolution rate of SD-loaded tablet linearly increased both in water and in water containing 1% tween 20, and much higher than the commercial tablet, $Vaxar^{(R)}$. When the amount of SD was increased, the release rate was greater. The Gelucire 50/13 showed higher dissolution than the Gelucire 44/14. The produced solid dispersion with various kinds of excipients and making tablets, it was found that solid dispersions can increase the solubility in artificial gastric juice and finally increases dissolution rate.