• 대한기계학회논문집A
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• 제30권8호
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• pp.976-984
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• 2006

Time-temperature superposition has been studied to determine the long-term fatigue life over millions of cycles for glassy polymers. π le superposition is supposed to make an accelerated lifetime testing (ALT) technique possible. Dog-bone shaped specimens made of carbon filled Polycarbonate (PC) were tested under fatigue, based on the stress-lifetime approach (S-N curve). Fatigue-induced localized yield-like deformation is considered as the defect leading to fatigue and its evolution behavior is characterized by a modified energy activation model in which temperature is considered as fatigue acceleration factor. This model allows the reduced time concept to account for effects of different temperature in short-term fatigue data to determine long-term fatigue life through the use of time-temperature superposition that is applicable under a low frequency and isothermal conditions. The experimental results validated that the proposed technique could be a possible method for accelerated lifetime testing (ALT) of time-dependent polymeric materials.

• Macromolecular Research
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• 제14권4호
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• pp.416-423
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• 2006

The dynamic mechanical thermal properties of poly(hexamethylene terephthalate) (PHT), poly(1,4-cyclohexylenedimethylene terephthalate) (PCT) and their P(HT-co-CT) random copolymers in the amorphous state were examined as a function of temperature and frequency. All the samples exhibited two main relaxation processes in the plot of tan ${\delta}$ versus temperature: the primary ${\alpha}$-relaxation associated with the glass transition and the secondary ${\beta}$-relaxation attributed to the local segmental motions of mostly cyclohexylene rings for PCT and to cooperative motions of methylene, carboxyl, and phenylene groups for PHT. Both ${\alpha}$- and ${\beta}$-relaxation temperatures increased with increasing CT content. The activation energy of the ${\alpha}$-relaxation increased with increasing CT content, whereas that of the ${\beta}$-relaxation decreased. The sub-glassy secondary ${\beta}$-relaxation processes of PCT and PHT were investigated in terms of the cooperativity of main-chain segmental motions.

• 오토저널
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• 제12권1호
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• pp.26-32
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• 1990

This study investigated a method for the determination of the J-integral for a tough glassy polymer such as polycarbonate plates by using the method of caustics. Comparing the values of J-integral determined by a numerical analysis and by the method of caustics, the method of caustics was found to be an effective experimental technique for the determination of the J-integral. The ratio between two J-integrals determined by the method of caustics and by finite element method converged into 1 within the limit of low load. However, it was noticed that the greater the plastic zone at the crack tip was, the lower the J-integral obtained by the reflect method of caustics. This difference may be deduced from the damage at the crack tip such as craze appeared in the polycarbonate plate. It was confirmed that the ratio of longitudinal diameter( $D_{l}$ ) to transverse diameter ( $D_{t}$) of caustics generally converged into 1 at the low load. The transition of the state of stress at the vicinity of a crack tip from plane strain to plane stress was deduced by noticing that the longitudinal diameter( $D_{l}$ ) grew faster than the transverse diameter( $D_{t}$) of caustics within the higher load range.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.182-188
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• 2014

Three new transition metal complexes based on Ozagrel $[Cu(Ozagrel)]_n$ (1), $[Zn(Ozagrel)(Cl)]_n$ (2), ${[Mn_2-(Ozagrel)(1,4-ndc)_2]{\cdot}(H_2O)}_n$ (3), (Ozagrel = 3-(4-((1H-imidazol-1-yl)methyl)phenyl)acrylic acid; 1,4-ndc = 1,4-Naphthalenedicarboxylic acid) have been hydrothermally synthesized and characterized by elemental analyse, IR, TG, PXRD, electrochemical analysis and single crystal X-ray diffraction. X-ray structure analysis reveals that 1 and 3 are 3D coordination polymers, while complex 2 is a two-dimensional network polymer, the 2D layers are further packed into 3D supramolecular architectures that are connected through hydrogen bonds. The electrochemistry of 1-3 was studied by cyclic voltammetry in methanol and water using a glassy carbon working electrode. Also, thermal decomposition process and powder X-ray diffraction of complexes were investigated.

• 전기화학회지
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• 제10권3호
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• pp.190-195
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• 2007

본 연구는 뇨 속에 있는 에피네피린을 선택적으로 정량하기 위한 새로운 전기화학적 센서를 제작하고 그 특성을 연구한 것이다. 전극의 제작은 유리질 탄소전극에 촉매능이 있는 니켈(II)거대고리 착물을 전착시킨 후, 그 위에 생체적합성이 좋으며 음의 하전을 띤 polyuretane benzyl L-glutamate(PUBLG)로 막을 입힌 이중 폴리머 전극이다. 이 전극은 뇨 속에 있는 많은 방해물질에 대하여 좋은 선택성을 보였으며, 우수한 장기 안정성을 보였다. 최적 실험조건하에서 이 전극을 이용한 에피네피린의 정량범위는 $8.0\;{\times}\;10^{-7}\;M$에서 $2.0\;{\times}\;10^{-4}\;M$이고, 검출한계는 $1.0\;{\times}\;10^{-7}\;M$이다. 완충용액으로 5 배 희석한 뇨 시료에서 에피네피린의 회수율은 6 회 측정에서 $101.5({\pm}3.2)%$ 이었다.

• 대한화학회지
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• 제45권5호
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• pp.429-435
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• 2001

단량체인 N,N'-bis(2-pyrrol-1-yl-propyl)-4,4'-bipyridine(bpb)을 유리탄소전극 상에 전기화학적으로 중합한 고분자 피막전극을 erichrome black T(EBT) 와 glutathione(GSSG)의 1:1 용액으로 수식하여 GC/poly-bpb, EBT, GSSG형의 전극을 제작하고 이로써 Zn(II)을 포집한 전극을 제작하였다. 수식된 피막 내에서 이온의 확산계수는 아연이온이 포집되기 전후에 각각 2.43${\times}10^{-15}$과 9.14${\times}10^{-15}cm^2s^{-1}$으로 피막내의 전기화학적 활성자리에서 이탈이 거의 일어나지 않는 안정한 전극이다. 중합된 bpb의 양이 2.83${\times}10^4gmol^{-1}$에 대하여 1.17${\times}10^4gmol^{-1}$의 아연이온이 포집되었다. 이들 중에 산화-환원 과정에서 회합/해리에 관여하는 이온은 포집된 180개의 이온들 중에서 81.7%였다. 이는 EBT 만으로 수식된 전극에서 보다 3배정도 큰 값이다.

• Bulletin of the Korean Chemical Society
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• 제27권1호
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• pp.65-70
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• 2006

An amperometric glucose biosensor has been developed based on the use of the nanoporous composite film of sol-gel-derived zirconia and perfluorosulfonated ionomer, Nafion, for the encapsulation of glucose oxidase (GOx) on a platinized glassy carbon electrode. Zirconium isopropoxide (ZrOPr) was used as a sol-gel precursor for the preparation of zirconia/Nafion composite film and the performance of the resulting glucose biosensor was tuned by controlling the water content in the acid-catalyzed hydrolysis of sol-gel stock solution. The presence of Nafion polymer in the sol-gel-derived zirconia in the biosensor resulted in faster response time and higher sensitivity compared to those obtained at the pure zirconia- and pure Nafion-based biosensors. Because of the nanoporous nature of the composite film, the glucose biosensor based on the zirconia/Nafion composite film can reach 95% of steady-state current less than 5 s. In addition, the biosensor responds to glucose linearly in the range of 0.03-15.08 mM with a sensitivity of 3.40 $\mu$A/mM and the detection limit of 0.037 mM (S/N = 3). Moreover, the biosensor exhibited good sensor-to-sensor reproducibility (~5%) and long-term stability (90% of its original activity retained after 4 weeks) when stored in 50 mM phosphate buffer at pH 7 at 4 ${^{\circ}C}$.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2009년도 제38회 동계학술대회 초록집
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• pp.98-98
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• 2010

Ion beam irradiation has been extensively used for surface modification of polymers, glassy metals and amorphous and crystalline materials at micron and submicron scales. The surface structures created by exposure to an ion beam range from dots, steps and one-dimensional straight wrinkles to highly complex hierarchical undulations and ripples. In general, the morphology of these nanoscale features can be selected by controlling the ion beam parameters (e.g. fluence and acceleration voltage), making ion beam irradiation a promising method for the surface engineering of materials. In the work, we presented that ion beam irradiation results in creation of a peculiar nanoscale dimple-like structure on the surface of polyimide - a common polymer in electronics, large scale structures, automobile industry, and biomedical applications. The role of broad Ar ion beam on the morphology of the structural features was investigated and insights into the mechanisms of formation of these nanoscale features were provided. Moreover, a systematic experimental study was performed to quantify the role of ion beam treatment time, and thus the morphology, on the coefficient of friction of polyimide surfaces covered by nanostructure using a tribo-experiment. Nano-indentation experiment were performed on the ion beam treated surfaces which shows that the hardness as well as the elastic modulus of the polyimide surface increased with increase of Ar ion beam treatment time. The increased of hardness of polyimide have been explained in terms of surface structure as well as morphology changes induced by Ar ion beam treatment.

• 한국정밀공학회지
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• 제3권1호
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• pp.40-49
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• 1986

Crack, craze and void are common defects which may be found in the bulk of polymeric materials such as either themoplastics or thermosets. The healing phenomena, autohesion, of these defects are known to be a intrinsic material property of various polymeric materials. However, only a few experimental and theoretical investigations on crack, void and craze healing phenomena for various polymeric materials have been reported up to date [1, 2, 3]. This may be partly due to the complications of healing processes and lacking of appropriate theoretical developments. Recently, some investigators have been urged to study the healing phenomena of various polymenic materials since the significance of the use of polymer based alloys or composites has been raised in terms of specific strength and energy saving. In the earlier published reports [1, 2, 3, 4], the crack and void healing velocity, healing toughness and some other healing mechanical and physical properties were measured experimentally and compared with predicted values by utilizing a simple model such as the reptation model under some resonable assumptions. It seems, however, that the general acceptance of the proposed modeling analyses is yet open question. The crack healing processes seem to be complicate and highly dependent on the state of virgin material in terms of mechanical and physical properties. Furthermore, it is also strongly dependent on the histories of crack, craze and void development including fracture suface morphology, the shape of void and the degree of disentanglement of fibril in the craze. The rate of crack healing may be a function of environmental factors such as healing temperature, time and pressure which gives different contact configurations between two separated surfaces. It seems to be reasonable to assume that the crack healing processes may be divided in several distinguished steps like stress relaxation with molecular chain arrangement, surface contact (wetting), inter- diffusion process and com;oete healing (to obtain the original strength). In this context, it is likely that we no longer have to accept the limitation of cumulative damage theories and fatigue life if it is probable to remove the defects such as crack, craze and void and to restore the original strength of polymers or polymer based compowites by suitable choice of healing histories and methods. In this paper, we wish to present a very simple and intuitive theoretical model for the prediction of healed fracture toughness of cracked or defective polymeric components. The central idea of this investigation, thus, may be the modeling of behavior of chain molecules under healing conditions including the effects of chain scission on the healing processes. The validity of this proposed model will be studied by making comparisons between theoretically predicted values and experimentally determined results in near future and will be reported elsewhere.

• Bulletin of the Korean Chemical Society
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• 제31권4호
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• pp.976-980
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• 2010

A series of arylacetylene resins with siloxane units were synthesized by the condensation reactions of m-diethynylbenzene magnesium reagents with various $\alpha,\omega$-bis(chloro)dimethylsiloxanes. These resins are liquids and are miscible with common organic solvents at room temperature. The structures of the resins were characterized by FT-IR, $^1H$ NMR, $^{13}C$ NMR, $^{29}Si$ NMR, and gel permeation chromatography (GPC). The thermal behaviors of the resins were examined with differential scanning calorimetry (DSC). These resins have good processability. They can be thermally cross-linked through the ethynyl groups to produce cured resins. The thermal and thermooxidative stabilities of the cured resins were studied by thermogravimetric analysis (TGA). The cured resins possess high thermal and thermooxidative stability. Their decomposition occurs at above $500^{\circ}C$ in both $N_2$ and air. With increasing the length of siloxane units in the resins, the thermal stability of the cured resins decreases in $N_2$. When the cured resins were sintered above $1450^{\circ}C$ under argon, hard and glassy SiOC ceramics were obtained. These SiOC ceramics have the decomposition temperatures at 5% weight loss above $800^{\circ}C$ in air.