• Macromolecular Research
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• 제16권6호
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• pp.544-548
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• 2008

An HPLC column with a self-contained temperature control device was constructed for preparative temperature programmed interaction chromatography. Two Peltier plates were attached to a large bore column ($120{\times}22\;mm$ i.d.) and the column temperature was controlled by PID mode feed back control. At a flow rate of 1.5 mL/min, the column temperature could be increased and decreased at a rate as high as $50^{\circ}C/min$ and $10^{\circ}C/min$, respectively, which is much faster than using a column jacket and bath/circulator. The rapid heating and cooling rates allows a high repetition rate of chromatographic fractionation. The performance of the temperature controllable column was demonstrated successfully by the fractionation of homo-polymer precursors from diblock copolymers.

• Macromolecular Research
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• 제17권11호
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• pp.901-906
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• 2009

Several aromatic optically active polyamides (PA)s were synthesized from 5-(2-phthalimidiylpropanoylamino)isophthalic acid with various aromatic diamines via direct polycondensation with triphenyl phosphite and pyridine in the presence of calcium chloride and N-methyl-2-pyrrolidone under microwave irradiation and conventional heating conditions. Under the optimized conditions, the reaction mixture was irradiated for 2 min. with a 100% irradiation power (900 W). The resulting polymers were obtained in high yield and moderate inherent viscosity ranging from 0.35 to 0.60 dL/g. All synthesized polymers showed excellent solubility in amide-type solvents. Thermogravimetric analysis revealed a 10% weight loss temperature and char yield at $600^{\circ}C$ in a nitrogen atmosphere of > $350^{\circ}C$ and > 58%, respectively, which suggests that the resulting PAs have good thermal stability.

• Nuclear Engineering and Technology
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• 제55권10호
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• pp.3808-3814
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• 2023

The thermal stability of nitric acid solutions after contact with non-irradiated and irradiated tributyl phosphate (TBP) and its solution in Isopar-M has been studied. It has been established that exothermic processes occur during heating due to the interaction of soluble radiolysis products and the decomposition of the extractant with nitric acid. Such processes can occur at temperatures below 100 ℃, but unlike a thermal explosion that occurs in seconds, they are longer in time and are accompanied by weak heat evolution. Their intensity depends on the composition of the extractant, the concentration of HNO₃, and the volume ratio of the organic and aqueous phases. The presence of extractant degradation products in raffinates does not pose a risk of a rapid evolution of gaseous products during evaporation, however, the presence of reducing agents can significantly increase the intensity of the exothermic decomposition of raffinates.

• 대한화장품학회지
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• 제50권1호
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• pp.11-18
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• 2024

최근에 모발 케어 화장품 효능으로서 모발 보습 효과를 소구하려는 시도가 있지만 아직까지 모발 수분 추출을 어떤 온도에서 진행해야 하는지 평가법이 정해져 있지 않아 공인된 인체시험 평가가 없는 실정이다. 모발 수분 정량평가법을 확립하기 위해서 본 연구는 진행되었다. 모발 수분의 거동 패턴을 확인하기 위해 할로겐 수분 분석기로 온도를 다르게 하여 모발에 열을 가할 경우 수분 검출량은 가열 온도가 증가하면 계속 늘어나는 것을 확인하였다. 시차주사열량계로 모발의 흡열 반응 에너지를 평가한 결과 75 ℃ 부근에서 급격한 흡열 반응이 일어나는 특이한 현상을 관찰하였다. 인종별로 다른 모발에서도 이 현상은 관찰되었다. 모발 큐티클 장벽을 산화, 열로 손상시킨 모발에서는 급격히 상승하는 이 흡열 반응 온도가 조금 더 높은 77 ℃에서 일어났고, 이 모발을 극성오일 또는, 컨디셔닝 폴리머나 케라틴 단백질로 도포한 경우에는 73 ℃에서 관찰되었다. 이 반응이 모발 표면에서 어떤 영향을 미치는지 알아보기 위해서 원자현미경으로 마찰력을 관찰한 결과 75 ℃ 보다 높은 온도에서 가열할 때 큐티클 마찰력이 상승하고 그보다 높은 90 ℃에서는 변화가 없는 것을 관찰하였다. 마침내 75 ℃ 근처가 모발에 결합된 수분 분자의 탈착이 본격적으로 일어나는 임계온도임을 결론내렸다. 이를 통해 모발 수분을 검출해서 정량화하기 위한 조건으로 75 ℃가 가열온도로 최적합하고 이 때 검출된 수분량 10% 가량이 모발 케어 화장품 처리 전과 후를 비교할 수 있는 모발 수분 정량 기준값이 될 수 있음을 제시하였다.

• 한국세라믹학회지
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• 제40권8호
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• pp.751-757
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• 2003

10 wt% A1$_2$O$_3$-Y$_2$O$_3$-CaO를 첨가한 SiC-30 wt% TiC 분말을 스파크 플라즈마 소결(SPS) 방법을 사용하여 급속 치밀화 하였다. SPS 공정은 매우 빠른 승온 속도와 짧은 시간에 완전 치밀한 시편을 얻을 수 있다. 본 실험에서, 승온 속도와 압력은 $100^{\circ}C$/min과 40MPa이고, 소결 온도 범위는$1600^{\circ}C$~$1800^{\circ}C$이었으며, 10min 동한 유지하였다. $Al_2$O$_3$, $Y_2$O$_3$ 및 CaO를 첨가한 SiC-30 wt% TiC 복합체는 $1700^{\circ}C$ 이상 온도에서 스파크 플라즈마 소결 방법으로 완전 치밀화가 이루어졌다. 모든 SPS 공정 온도에서 탄화큐소으 상전이나 YAG 결정상의 형성 없이 3C-SiC와 TiC 만이 XRD에서 나타났다. 급속 소결한 SiC-30 wt% TiC 복합체의 미세구조는 비교적 작은 등축상 SiC 결정립과 비교적 큰 TiC 결정립으로 구성되었다. $1750^{\circ}C$에서 제조한 시편의 이축강도능 635.2MPa이고, 파괴인성은 6.12 MPaㆍ$m^{1/2}$이었다.

• 한국결정성장학회지
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• 제13권4호
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• pp.176-181
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• 2003

0.5wt% $B_4$C를 첨가한 SiC분말로부터 스파크 플라즈마 소결(SPS)로 급속 치밀화 하였다. 이 공정의 독특한 특징은 매우 빠른 승온 속도와 짧은 시간에 완전 치밀한 시편을 얻을 수 있는 가능성이다. 승온 속도와 가압력은 $100^{\circ}C$/min 과 40MPa으로 유지시켰는데, 소결 온도와 유지 시간은 각각 1800, 1850, 1900과 $1950^{\circ}C$ 그리고 10, 20과 30min으로 하였다. $1950^{\circ}C$에서 SPS 소결한 시편은 거의 이론밀도에 이르렀다. $1850^{\circ}C$에서 3C로부터 6H로 상전이 되는 것이 XRD에서 나타났다. 급속 소결한 SiC 세라믹스는 2$\mu\textrm{m}$ 이하 크기의 초미세 등축 입자와 폭 0.5∼2$\mu\textrm{m}$, 길이 3∼10$\mu\textrm{m}$의 길게 자란 입자의 이중 미세구조로 구성되었다. 이축강도는 소결 유지 시간이 증가할수록 증가하였다. $1950^{\circ}C$에서 30min 유지하면 392.7 MPa의 강도에 도달하였는데. 기공이 줄어들면 강도가 상승하는 일반적인 경향과 일치한다. 한편, 소결 유지시간이 증가할수록 파괴 인성은 증가하고 있지만. 2.17∼2.34MPa$.$$m^{1/2}$의 낮은 값을 유지하고 있는데, 파단면이 거의 입내 파괴 모드에 기인하는 것으로 생각된다.

• 한국식품과학회지
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• 제29권1호
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• pp.9-14
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• 1997

자색고구마의 동결, 해동 및 blanching방법에 따른 색소의 변화를 조사하였다. $-5^{\circ}C$보다 $-20^{\circ}C$ 그리고 $-40^{\circ}C$에서 동결한 자색고구마는 $4^{\circ}C$로 해동시에 해동시간이 길어질수록 색소함량이 급격하게 감소하는 경향을 보였다. $20^{\circ}C$에서의 해동은 $4^{\circ}C$해동에 비해 뚜렷이 색소함량이 감소하였고, $60^{\circ}C$에서 해동시에는 색소의 함량에 대한 동결온도의 영향이 작았으며, microwave가열을 이용하여 3분간 급속해동하고 추출한 색소의 함량은 각 동결온도에 따라 큰 차이가 없었다. Microwave blanching으로 해동한 것은 동결온도에 대해 영향이 미미하였다. 동결전에 blanching처리한 경우는 해동시에 공기의 접촉 유무가 색소의 추출량에 큰 차이가 없었으며 자색고구마 색소감소를 억제하기 위해서는 $3{\sim}4$분 동안의 microwave blanching이 $100^{\circ}C$에서는 $10{\sim}15$분 정도의 가열이 적당하였다.

• 한국세라믹학회지
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• 제42권8호
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• pp.567-574
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• 2005

Densification of SiC powder with additives of total amount of2, 4, 8 $wt\%$ Al-B-C was carried out by Spark Plasma Sintering (SPS). The unique features of the process are the possibilities of a very fast heating rate and a short holding time to obtain fully dense materials. The heating rate and applied pressure were kept at $100^{\circ}C/min$ and 40 MPa, while the sintering temperature and holding time varied from 1700 - $1800^{\circ}C$ for 10 - 40 min, respectively. The SPS-sintered specimens with different amount of Al-B-C at $1800^{\circ}C$ reached near-theoretical density. The $3C{\rightarrow}6H,\;15R{\rightarrow}4H$ phase transformation of SiC was enhanced by increasing the additive amount. The microstructure of SiC sintered up to $1750^{\circ}C$ consisted of fine equiaxed grains. In contrast, the growth of large elongated grains in small matrix grains was shown in sintered bodies at $1800^{\circ}C$, and the plate-like grains interlocking microstructure had been developed by increasing the holding time at $1800^{\circ}C$. The grain growth rate decreases with increasing amount of Al-B-C in SiC starting powder, however, the both of volume fraction and aspect ratio of large grains in sintered body increased.

• 대한기계학회논문집A
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• 제24권10호
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• pp.2552-2559
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• 2000

Most of ferrous b.c.c weld materials have martensitic transformation during rapid cooling after welding. It is well known that volume expansion due to the phase transformation could influence on the relaxation of welding residual stress. To apply this effect practically, it is necessary to establish a numerical model which is able to estimate the effect of phase transformation on residual stress relaxation quantitatively. For this purpose, the analysis is carried out in two regions, i.e., heating and cooling, because the variation of material properties following a phase transformation in cooling is different in comparison with the case in heating, even at the same temperature. The variation of material properties following phase transformation is considered by the adjustment of specific heat and thermal expansion coefficient, and the distribution of residual stress in analysis is compared with that of experiment by previous study. In this study, simplified numerical procedures considering phase transformation, which based on a commercial finite element package was established through comparing with the experimental data of residual stress distribution by other researcher. To consider the phase transformation effect on residual stress relaxation, the transition of mechanical and thermal property such as thermal expansion coefficient and specific heat capacity was found by try and error method in this analysis. In addition to, since the transformation temperature changes by the kind and control of alloying elements, the steel with many kinds of transformation temperature were selected and the effect of transformation on stress releasement was investigated by the numerical procedures considering phase transformation.

• Journal of Welding and Joining
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• 제32권3호
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• pp.95-101
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• 2014

Joining of grey cast iron by fusion welding has much difficulties for its extremely low ductility and low toughness because of the flake form of the graphite. And the brittle microstructure, i.e. ledeburite may be formed during fusion welding by its rapid cooling rates. By these kinds of welding problem, preheat and post heat treatment temperature must be increased to avoid weld crack or welding problems. In order to avoid these fusion welding problem, friction welding of cast iron was carried out for improving joint soundness, establishing friction welding variables. There is no factor for evaluating friction weldability in continuous drive type friction welding. In this point of view, this study proposed the parameters for calculating friction weld heat input. The results obtained are as follows ; 1. There was a close relationship between tensile strength and flash appearance of friction welded joint. 2. Tensile strength was decreased and flash was severely oxidized as increasing frictional heating time. 3. As increased forging pressure $P_2$, flash had a large crack and tensile strength was decreased. 4. As powdered graphite by rotational frictional force induced flat surface and hindered plastic flow of metal, tensile strength of welded joint was decreased. 5. Heat input for continuous drive type friction welding could be calculated by the factors of $P_1$, $P_2$ and upset distance(${\delta}$).