• Macromolecular Research
• /
• 제14권4호
• /
• pp.408-415
• /
• 2006

Temperature-dependent, wide-angle, x-ray diffraction (WAXD) patterns and infrared (IR) spectra were measured for biodegradable poly(3-hydroxybutyrate) (PHB) and its copolymers, poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) P(HB-co-HHx) (HHx=2.5, 3.4, 10.5, and 12 mol%), in order to explore their crystal and lamellar structure and their pattern of C-H...O=C hydrogen bonding. The WAXD patterns showed that the P(HB-co-HHx) copolymers have the same orthorhombic system as PHB. It was found from the temperature-dependent WAXD measurements of PHB and P(HB-co-HHx) that the a lattice parameter is more enlarged than the b lattice parameter during heating and that only the a lattice parameter shows reversibility during both heating and cooling processes. These observations suggest that an interaction occurs along the a axis in PHB and P(HB-co-HHx). This interaction seems to be due to an intermolecular C-H...O=C hydrogen bonding between the C=O group in one helical structure and the $CH_3$ group in the other helical structure. The x-ray crystallographic data of PHB showed that the distance between the O atom of the C=O group in one helical structure and the H atom of one of the three C-H bonds of the $CH_3$ group in the other helix structure is $2.63{\AA}$, which is significantly shorter than the sum of the van der Waals separation ($2.72{\AA}$). This result and the appearance of the $CH_3$ asymmetric stretching band at $3009 cm^{-1}$ suggest that there is a C-H...O=C hydrogen bond between the C=O group and the $CH_3$ group in PHB and P(HB-co-HHx). The temperature-dependent WAXD and IR measurements revealed that the crystallinity of P(HB-co-HHx) (HHx =10.5 and 12 mol%) decreases gradually from a fairly low temperature, while that of PHB and P(HB-co-HHx) (HHx = 2.5 and 3.5 mol%) remains almost unchanged until just below their melting temperatures. It was also shown from our studies that the weakening of the C-H...O = C interaction starts from just above room temperature and proceeds gradually increasing temperature. It seems that the C-H...O=C hydrogen bonding stabilizes the chain holding in the lamellar structure and affects the thermal behaviour of PHB and its copolymers.

• 한국응용과학기술학회지
• /
• 제37권3호
• /
• pp.484-495
• /
• 2020

이 연구는 피부 각질층의 구조와 동일한 구조를 형성하는 혼합계면활성제 (MimicLipidMSM1000)로써 수크로오스다이스테아레이트, 폴리글리세릴-2다이올리에이트, 발효스쿠알란, 에르고스테롤, 10-하이드록시스테아릭애씨드로 이루어진 혼합물을 합성하였다. 이 혼합 계면활성제를 2~5wt%를 사용할 경우, 5~30층의 다중층 라멜라구조를 형성하는 인공 피부 모사체를 만들 수 있었다. 이 혼합계면활성제를 사용하여 에멀젼을 만들고, 다중층의 라멜라 상이 형성되는 것을 메커니즘 적으로 해석하였다. 이 계면활성제의 외관은 연한 갈색의 단단한 왁스이었고, HLB(hydrophilic lipophilic balance)는 12.53이었으며, 임계파라미터 값(critical parameter value)은 0.987, 산가는 0.13이었다. pH변화에 따른 안정성은 산성(3.8), 중성(7.2), 알칼리성(10.8)에서도 안정하였다. 액정의 입경은 5~25mm에서 가장 안정한 십자형 모양 (maltese cross) 라멜라액정 드롭플렛(lamellar crystalline droplet)이 형성됨을 알 수 있었다. 호모믹서의 교반속도 변화에 따른 유화입자의 크기는 2500rpm (17.9mm±2.6mm), 3500rpm (12.5mm±2.1mm), 4500rpm (6.2mm±1.8mm) 속도가 높아 질수록 작은 입자가 형성되었다. 편광현미경을 통하여 액정형성 입자를 관찰하였으며, 주사전자현미경(cryo-SEM)으로 액정의 형성 구조를 정밀하게 분석하였다. 응용분야로써, 각질층의 다중 라멜라 동일한 구조를 형성하는 피부모사체 형성 계면활성제를 사용하여 다양한 스킨케어화장료, 메이크업 케어 화장료, 두피보호용 화장료 등 다양한 처방개발에 폭 넓게 응용이 가능할 것으로 기대한다.

• 한국응용과학기술학회지
• /
• 제33권3호
• /
• pp.540-548
• /
• 2016

sodium bis-(2-ethylhexyl)sulfosuccinate-water 라멜라 액정의 비뉴톤 유동곡선을 cone-plate 레오메타를 사용하여 여러 농도와 온도 조건에서 얻었다. 이러한 비뉴톤 유동곡선을 비뉴톤 유동식에 적용하여 유동파라메타를 구하였다. 특별히 주목할 점은 액정시료의 전단속도에 대한 전단응력은 증가와 감소에서 틱소트로피와 다일레턴시 현상을 보여 hysteresis loop를 나타내고 있다는 점이다. sodium bis-(2-ethylhexyl)sulfosuccinate-water 라멜라 액정은 작은 전단속도에서는 약한 젤 현상을 보이지만 응력이 한계 응력 이상에서는 비 선형 점탄성 성질을 나타낸다. 전단속도 감소에서 분산계는 전단속도가 증가할 때 측정된 값 보다는 큰 구조변화와 전단응력을 유지하고 있다.

• 대한화장품학회지
• /
• 제24권3호
• /
• pp.6-16
• /
• 1998

Ceramides are currently emerging as the major skin care ingredients due to !heir barrier properties in the stratum corneum of the human skin. Thus, major cosmetic companies have developed synthetic ceramide analogs for their own use. In this study, several ceramide mimic compounds , new skin barrier lipids, were designed and synthesized, and their physical and biological properties were investigated to evaluate their skin care capability. Several structures were designed from the variation of hydrophobic alkyl chain and hydrophilic moiety by the use of molecular modeling software. The selected targets were synthesized, and their properties and activities were studied as the pure form, in the emulsion, or in the lamellar mixture containing cholesterol and fatty acid. Some compounds, such as 1,3-bis(N-(2-hydroxyethyl)-palmitoylamino)-2-hydroxypropane, enhanced the restoration of skin barrier damaged by SDS(sodium dodecyl sulfate), and by acetone treatment. The rate of restoration was comparable to that of natural ceramides. The synthesized compounds alleviated SDS induced skin irritation and facilitated lamellar phase liquid crystal formation. The treatment of 1,3-Dis(N-(2-hydroxyethyl)-palmitoylam ino)-2-hyd roxypropane on the acetone damaged skin revealed that the compound promoted the recovery of intercellular lipid lamellar structure of stratum corneum layer. The replacement of palmitoyl groups of the compound with shorter alkyl chain gave lower emulsion viscosity and liquid crystal density, suggesting easier formulation and poorer barrier activity. Most of the synthesized compounds were non-irritable in various toxicological tests proving that they can be safely introduced to the skin care formulations.

• 대한화장품학회지
• /
• 제29권2호
• /
• pp.181-191
• /
• 2003

This study described about method that form liquid crystal gel (LCG) by main ingredient with hydrogenated lechin (HL) in OW emulsion system. Result of stability test is as following with most suitable LCG's composition. Composition of LCG is as following. To form liquid crystal, an emulsifier used $4.0\;wt\%$ of cetostearyl alcohol (CA) by $4.0\;wt\%$ of HL as a booster, Moisturizers contained $2\;wt\%$ of glycerin and $3.0\;wt\%$ of 1.3-butylene glycol (1,3-BG). Suitable emollients used $3.0\;wt\%$ of cyclomethicone, $3.0\;wt\%$ of isononyl isononanoate (ININ), $3.0\;wt\%$ of cerpric/carprylic triglycerides (CCTG), $3.0\;wt\%$ of macademia nut oil (MNO) in liquid crystal gel formation. On optimum conditions of LCG formation, the pHs were formed all well under acidity or alkalinity conditions. Considering safety of skin, PH was the most suitable $\pm61.0$ ranges. The stable hardness of LCG formation appeared best in $32\;dyne/cm^2.$ Particle of LCG is forming size of $1{\~}20\;{\mu}m$ um range, and confirmed that the most excellent LCG is formed in $1{\~}6\;{\mu}m$ range. According to result that observe shape of LCG with optical or polarization microscope, LCG could was formed, and confirmed that is forming multi-layer lamellar type structure around the LCG. Moisturizing effect measured clinical test about 20 volunteers. As a result, moisturizing effect of LCG compares to placebo cream was increased $30.6\%$. This could predicted that polyol group is appeared the actual state because is adsorbed much to round liquid crystal droplets to multi-lamellar layer's hydrophilic group. It could predicted that polyol group is vast quantity present phase that appear mixed because is adsorbed to round liquid crystal to multi-lamellar layer's hydrophilic group. This LCG formation theory may contribute greatly in cosmetics and pharmacy industry development.

• 공업화학
• /
• 제21권6호
• /
• pp.603-609
• /
• 2010

수첨 인지질의 하나인 distearoylphosphatidylcholin (DSPC)을 주로 하면서 피부보습에 도움을 주는 용매인 glycerin (GLY)에 의해 팽윤되어 형성된 라멜라 액정상 구조에 피부장벽을 구성하는 지질 중 하나로서 ceramide 3 (CER3)이 함께 배향될 때 나타나는 함량 의존적 거동을 DSC, XRDs, PM 및 Cryo-SEM에 의해 고찰하였다. CER3은 매우 결정성이 높지만, DSPC와의 구조적인 유사성을 가지고 있어 DSPC 20.0 wt% 함량대비 7.0 wt%까지는 탈리 없이 배향되지만, 그 이상을 배향시킬 경우 CER3이 액정 내에서 탈리되어 자체로 GLY에 팽윤되어 또 다른 액정상을 형성하는 것을 XRD의 특성피크 발현과 DSC의 공융점 거동을 통해 확인할 수 있었다. 또한 CER3이 액정 내에 배향되면서 DSPC만으로 이루어진 액정에서 보이는 SPP패턴뿐만 아니라, 피부 각질층에서 주로 나타나는 LPP패턴도 SAXD분석을 통해 확인되어, CER3을 적용시 인간피부와 보다 흡사한 액정구조를 형성함을 확인하였다. Cryo-SEM을 이용하여 DSPC만으로 이루어진 액정과 여기에 CER3이 도입된 액정을 비교한 결과, CER3은 액정의 구조를 보다 두텁고, 견고하게 함을 알 수 있었다.

• 한국전기전자재료학회:학술대회논문집
• /
• 한국전기전자재료학회 2010년도 춘계학술회의 초록집
• /
• pp.11-11
• /
• 2010

In order to design for nano structured materials with enhanced thermoelectric properties, the alloys in the pseudo-binary $Bi_2Te_3$-PbTe system were investigated for their micro structure and thermal properties. For this synthesis the liquid alloys were cooled by water quenching method. The micro structure images were taken by using electron probe micro analyzer (EPMA). Dendritic and lamellar structures were clearly observed with the variation in the composition ratio between $Bi_2Te_3$ and PbTe. It was confirmed that a metastable compounds is $PbBi_2Te_4$ in the The $Bi_2Te_3$-PbTe system. The change in the composition increasing $Bi_2Te_3$ ratio causes to change structure from dendritic to lamellar. Seebeck coefficient of alloys 5 which the mixture rate of $Bi_2Te_3$ is 83% was measured as the highest value. In contrast, the others decreased by increasing $Bi_2Te_3$. n-type characteristics was observed at all condition except alloy 6 which $Bi_2Te_3$ ration is 91%. The power factors of all samples were calculated with Seebeck coefficient and resistivity. Also the thermal conductivity was measured by using laser flash analyzer (LFA). In this work, the microstructures and thermal properties have been measured as a function of ratio of $Bi_2Te_3$ in the $Bi_2Te_3$-PbTe system.

• 열처리공학회지
• /
• 제33권4호
• /
• pp.173-179
• /
• 2020

The purpose of this study was to investigate comparatively the microstructural characteristics and hardness of discontinuous precipitates (DPs) in Mg-9%Al alloy, which were formed by continuous cooling (CC) from 678 K to RT and isothermal aging (IA) at 413 K, respectively. In as-cast state, the Mg-9%Al alloy consisted of partially divorced eutectic β(Mg₁₇Al₁₂) particles with a small amount of DPs showing (α+β) lamellar morphology adjacent to the β particles. The DPs formed by CC had interlamellar spacings in a broad range of 0.85~2.12 ㎛ (1.51 ㎛ in average) owing to the various formation temperatures in response to continuous cooling process. Meanwhile, the DPs formed by IA had relatively narrower interlamellar spacings of 0.14~0.29 ㎛ (0.21 ㎛ in average), which is associated with the low and constant formation temperature. Thinner and higher volume fraction of β phase layers were noticeable in the DPs formed by IA. Higher hardness values were obtained in the DPs formed by IA than the DPs formed by CC, which may well be ascribed to the finer lamellar structure and higher β phase content of the DPs formed by IA.

• 한국분말재료학회지
• /
• 제4권4호
• /
• pp.243-251
• /
• 1997

Engine valve-shaped TiAl-Mn intermetallics containing 43.5 to 47.5at%Al (Mn/Al=0.036) are successively fabricated by reactive sintering the elemental powder mixtures near-net shaped by extrusion and die forging. A duplex structure consisted of lamellar grains and equiaxed $\gamma$ grains is developed for all compositions, and the areal fraction of the lamellar grains(or equiaxed $\gamma$ grains) decreases (or increases) with increasing Al content. As Al content increased, the elongation increases with accompanying decrease in yield strength and ultimate tensile strength at both room temperature and 80$0^{\circ}C$. This indicates that the suitable composition is Ti-45at%Al-1.6at%Mn in considering the balance of ambient and elevated tensile properties. The reactive-sintered Ti-45Al-1.6Mn alloy shows superior oxidation resistance not only to the plasma arc melted one but also to the heat resistance steel STR35(representative exhaust valve head material for automotive engine). The reactive-sintered Ti-45Al-1.6Mn alloy coated with an oxidizing scale exhibits a better wear resistance than induction hardened martensitic steel STR11(representative exhaust valve tip material for automotive engine).

• 한국세라믹학회지
• /
• 제33권1호
• /
• pp.56-64
• /
• 1996

A large amount of papers about the cubic-to-tetragonal phase transition the ferroelectric domain structures of the BaTiO3 were already reported but there exist still some needs to observe the domain behaviors directly. In this study the domain structures of the tinned plates prepared from ta single crystal grown by the TSSG technique were observed using a polarizing microscope TE and X-ray topography. The spatial relation be-tween the orientation states of domains was investigated and the effects of external stresses and electric fields on the behaviors of ferroelectric and ferroelastic domains were studied. All the 90$^{\circ}$walls cut off in the crystal are the wedge shaped lamellar domains and all the straight boundaries in the observed domain patte군 can be interpreted as the head-to-tail 90$^{\circ}$walls. The irregular overlapped boundaries commonly observed by using a polarizing microscope and X-ray topography are complex combinations of well-known 90$^{\circ}$walls and are domain walls were predominant and were stabilized after surface polishing. In the paraelectric phase region the domain walls vanished but the residual surface strain patterns could be seen at the same positions of the stabilized 90$^{\circ}$a-a walls in the tetragonal phase region, These stabilized walls resulted from the surface strain had a memory effect in domain formation during the repeated phase transitions and could notr be affected by an external electtric field.