Hydroxyapatite/poly（L-lactide） （HA/PLLA） nanocomposites were prepared by the solvent mixing method. The isothermal crystallization behavior was studied by differential scanning calorimetry （DSC） and polarized op...Hydroxyapatite/poly（L-lactide） （HA/PLLA） nanocomposites were prepared by the solvent mixing method. The isothermal crystallization behavior was studied by differential scanning calorimetry （DSC） and polarized optical microscopy （POM）. The results show that the crystallization behavior of HA/PLLA composites was strongly affected by the content of HA and crystallization temperature, and the addition of HA could promote nucleation and enhance the crystallization rate. When isothermal crystallization was carried out at 110℃, the HA/PLLA nanocomposite with 1% HA content crystallized most rapidly among all the composites and the half crystallization time was only 1.0 min. Banded spherulites were observed for the HA/PLLA composites, but no banded spherulites were seen in the crystals of PLLA under the same condition.展开更多
Isotactic polypropylene（i PP） samples obtained by pressure vibration injection molding（PVIM） and conventional injection molding（CIM） were studied by polarized-light microscopy（PLM）, respectively. It was found ...Isotactic polypropylene（i PP） samples obtained by pressure vibration injection molding（PVIM） and conventional injection molding（CIM） were studied by polarized-light microscopy（PLM）, respectively. It was found that the alternating bright and dark banded spherulites were generated in the transitional region of PVIM parts. It is the first time that the banded spherulites of isotactic polypropylene were observed in polymer processing. What＇s more, the banded spherulites were proved to be constituted of α-form crystal by hot stage polarized-light microscopy（HT-PLM） and wide angle X-ray diffraction（WAXD）. Morphology of the banded spherulites was also studied by scaning electronical microscopy（SEM）.展开更多
Spherulitic morphology of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The morphology of spherulite of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The e...Spherulitic morphology of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The morphology of spherulite of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The effect of both annealing temperature and crystallization temperature on the formation of cracks was described by polarized optical microscope (POM). Non banded spherulite (fibrils) with cracks was detected in PLLA film after annealing at 160°C (180 min.) and isothermal crystallization temperatures at 140°C and 150°C. With increasing temperature after annealing treatment the size of spherulite is increased and more cracks are formed. The maximum growth rate of spherulites was found at 130°C. The physical ageing was carried out by annealing the PLLA sample at room temperature for several annealing time (ta) from 0 h to 720 h. The enthalpy relaxation has been studied by differential scanning calorimetry (DSC) through analysis of the endothermic peak of glass transition temperature, which increased and shifted towards higher temperature as the annealing time increased.展开更多
Lamellar structures of banded spherulites of poly(e-caprolactone)/poly(vinylchloride) (PCL/PVC) blends are observed using tapping mode atomic force microscopy (AFM). Thesurface of the PCL/PVC banded spherulites presen...Lamellar structures of banded spherulites of poly(e-caprolactone)/poly(vinylchloride) (PCL/PVC) blends are observed using tapping mode atomic force microscopy (AFM). Thesurface of the PCL/PVC banded spherulites presents to be concentric periodic ups and downs. Theperiod of the bands corresponds to the extinction rings under the polarized optical microscopyobservation. The lamellae with edge-on orientation in the ridges and the flat-on lamellae in thevalleys of the banded spherulites are observed clearly. The twisting between the edge-on and flat-onlamellae is also observed.展开更多
The nonisothermal crystallization of poly(butylene dodecanedioate) was studied by differential scanning calorimetry,crystals of polyesters were observed through polarized optical microscope,and an Avrami method was us...The nonisothermal crystallization of poly(butylene dodecanedioate) was studied by differential scanning calorimetry,crystals of polyesters were observed through polarized optical microscope,and an Avrami method was used to analyze the kinetics of nonisothermal crystallization.The results showed that the crystallization temperature decreased slowly with an increase in the cooling rate.Furthermore,secondary nucleation was observed in the process of PBDD nonisothermal crystallization,and the Avrami exponential values n of PBDD indicated that the mechanism of crystallization was a tridimensional growth with heterogeneous and homogeneous nucleation.Meanwhile,the Avrami values n of P(BDD-co-BT)-20 is 1,which indicated that their mechanism of crystallization was a one-dimensional growth with heterogencous nucleation.Crystallization activation energies implied that it is easier to crystallize for copolyester.From the observed results of spherulites,it can be concluded that the size of spherulites decreases with increasing the content of terephthalic acid.展开更多
The effect of sintering dispersed and bulk,low molecular weight(M_n=50,000 Da),nano-emulsionpolytetrafluoroethylene(PTFE)particles near their melting point is described.With the nascent particles consisting of ca.75 n...The effect of sintering dispersed and bulk,low molecular weight(M_n=50,000 Da),nano-emulsionpolytetrafluoroethylene(PTFE)particles near their melting point is described.With the nascent particles consisting of ca.75 nm diameter,hexagonal,single crystals,sintering at,e.g.,350℃,results,initially,in merger of neighboring particles,followed by individual molecular motion on the substrate and the formation of folded chain,lamellar single crystals andspherulites,and on-edge ribbons.It is suggested these structures develop,with time,in the mesomorphic“melt”.Sintering ofthe bulk resin yields extended chain,band structures,as well as folded chain lamellae;end-surface to end-surface merger,possibly by end-to-end polymerization,occurs with increasing time.展开更多
Polarized optical microscopy (POM) results show that ZSM5 has great influence on both the nucleation stage and the growth stage of PEO spherulites. Part of ZSM5 particles can act as the nucleus of PEO spherulites and ...Polarized optical microscopy (POM) results show that ZSM5 has great influence on both the nucleation stage and the growth stage of PEO spherulites. Part of ZSM5 particles can act as the nucleus of PEO spherulites and thus increase the amount of PEO spherulites. On the other hand, ZSM5 can restrain the recrystallization tendency of PEO chains through Lewis acid-base interaction and hence decrease the growth speed of PEO spherulites. The increasing amount of PEO spherulites, decreasing size of PEO spherulites, and the incomplete crystalliza-tion are all beneficial for creating more continuous amorphous phases of PEO, which is very important for the transporting of Li+ ions. An adequate amount of ZSM5 can enhance the room temperature ionic conductivity of PEO-LiClO4 based polymer electrolyte for more than two mag-nitudes.展开更多
The physical vapour deposition （PVD） of gallium monotelluride （GaTe） in different crystalline habits was established in the growth ampoule, strongly depending on the temperature gradient. Proper control on the tem...The physical vapour deposition （PVD） of gallium monotelluride （GaTe） in different crystalline habits was established in the growth ampoule, strongly depending on the temperature gradient. Proper control on the temperatures of source and growth zones in an indigenously fabricated dual zone furnace could yield the crystals in the form of whiskers and spherulites. Optical and electron microscopic images were examined to predict the growth mechanism of morphologies. The structural parameters of the grown spherulites were determined by X-ray powder diffraction （XRD）. The stoichiometric composition of these crystals was confirmed using energy dispersive analysis by X-rays （EDAX）. The type and nature of electrical conductivity were identified by the conventional hot probe and two probe methods, respectively. The mechanical parameters, such as Vickers microhardness, work hardening index, and yield strength, were deduced from microindentation measurements. The results show that the vapour grown p-GaTe crystals exhibit novel physical properties, which make them suitable for device applications.展开更多
The spherulite morphology of the rolled and subsequent heat-treated isotactic polypropylene （iPP） was observed by polarized microscopy, and the crystallinity evolution of materials was also measured by the wide angl...The spherulite morphology of the rolled and subsequent heat-treated isotactic polypropylene （iPP） was observed by polarized microscopy, and the crystallinity evolution of materials was also measured by the wide angle X-ray scattering （WAXS）. Rolling led to the oblate spherulites in the deformed iPP samples. The sheared crystalline lamellae broke apart into sets of crystalline blocks during rolling. As a result, the crystallinity of the iPP samples was greatly reduced during deformation, which induced the unclear spherulites and spherulite boundaries. Subsequent heat treatment resulted in the strong reerystallization of the rolled iPP samples. But the recrystaUizatinn in this work only meant the rearrangement of the macromolecule along the unbroken crystalline lamellae and the existing small crystalline blocks in the deformed spherulites. Heat treatment did not change the shape of the spherulites formed during deformation. The recrystallization also resulted in very clear spherulites and spherulite boundaries.展开更多
The surface morphology of free-surface PCL ringed spherulites was investigated by using atomic force microscopy. The spherulites were obtained by crystallization of PCL/PVC blends of different compositions. It was fou...The surface morphology of free-surface PCL ringed spherulites was investigated by using atomic force microscopy. The spherulites were obtained by crystallization of PCL/PVC blends of different compositions. It was found that the ringed spherulite exhibited regularly fluctuating rings on its surface. Compared with the bright-dark ring pattern of the spherulite under a polarizing microscope, it was proved that the optical characteristics of the ringed spherulite under polarizing microscope coincided with its surface characteristics. The bright rings in polarizing micrographs of the spherulite coincided with the convex rings on its surface, while the dark rings coincided with the concave rings.展开更多
基金supported by the National Natural Science Foundation of China(Key Project No.50733003 and Project No.20604030)the International Cooperation fund of Science and Technology(Key project 20071314) from the Ministry of Science and Technology of Chinathe fund from Chinese Academy of Sciences(KGCX-YW-208)
文摘Hydroxyapatite/poly（L-lactide） （HA/PLLA） nanocomposites were prepared by the solvent mixing method. The isothermal crystallization behavior was studied by differential scanning calorimetry （DSC） and polarized optical microscopy （POM）. The results show that the crystallization behavior of HA/PLLA composites was strongly affected by the content of HA and crystallization temperature, and the addition of HA could promote nucleation and enhance the crystallization rate. When isothermal crystallization was carried out at 110℃, the HA/PLLA nanocomposite with 1% HA content crystallized most rapidly among all the composites and the half crystallization time was only 1.0 min. Banded spherulites were observed for the HA/PLLA composites, but no banded spherulites were seen in the crystals of PLLA under the same condition.
文摘Isotactic polypropylene（i PP） samples obtained by pressure vibration injection molding（PVIM） and conventional injection molding（CIM） were studied by polarized-light microscopy（PLM）, respectively. It was found that the alternating bright and dark banded spherulites were generated in the transitional region of PVIM parts. It is the first time that the banded spherulites of isotactic polypropylene were observed in polymer processing. What＇s more, the banded spherulites were proved to be constituted of α-form crystal by hot stage polarized-light microscopy（HT-PLM） and wide angle X-ray diffraction（WAXD）. Morphology of the banded spherulites was also studied by scaning electronical microscopy（SEM）.
文摘Spherulitic morphology of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The morphology of spherulite of pure poly lactic acid (PLLA) PLLA have investigated after thermal annealing. The effect of both annealing temperature and crystallization temperature on the formation of cracks was described by polarized optical microscope (POM). Non banded spherulite (fibrils) with cracks was detected in PLLA film after annealing at 160°C (180 min.) and isothermal crystallization temperatures at 140°C and 150°C. With increasing temperature after annealing treatment the size of spherulite is increased and more cracks are formed. The maximum growth rate of spherulites was found at 130°C. The physical ageing was carried out by annealing the PLLA sample at room temperature for several annealing time (ta) from 0 h to 720 h. The enthalpy relaxation has been studied by differential scanning calorimetry (DSC) through analysis of the endothermic peak of glass transition temperature, which increased and shifted towards higher temperature as the annealing time increased.
基金supported by the National Natural Science Foundation of China(Grant Nos.20174049 and 20131160730)
文摘Lamellar structures of banded spherulites of poly(e-caprolactone)/poly(vinylchloride) (PCL/PVC) blends are observed using tapping mode atomic force microscopy (AFM). Thesurface of the PCL/PVC banded spherulites presents to be concentric periodic ups and downs. Theperiod of the bands corresponds to the extinction rings under the polarized optical microscopyobservation. The lamellae with edge-on orientation in the ridges and the flat-on lamellae in thevalleys of the banded spherulites are observed clearly. The twisting between the edge-on and flat-onlamellae is also observed.
文摘The nonisothermal crystallization of poly(butylene dodecanedioate) was studied by differential scanning calorimetry,crystals of polyesters were observed through polarized optical microscope,and an Avrami method was used to analyze the kinetics of nonisothermal crystallization.The results showed that the crystallization temperature decreased slowly with an increase in the cooling rate.Furthermore,secondary nucleation was observed in the process of PBDD nonisothermal crystallization,and the Avrami exponential values n of PBDD indicated that the mechanism of crystallization was a tridimensional growth with heterogeneous and homogeneous nucleation.Meanwhile,the Avrami values n of P(BDD-co-BT)-20 is 1,which indicated that their mechanism of crystallization was a one-dimensional growth with heterogencous nucleation.Crystallization activation energies implied that it is easier to crystallize for copolyester.From the observed results of spherulites,it can be concluded that the size of spherulites decreases with increasing the content of terephthalic acid.
文摘The effect of sintering dispersed and bulk,low molecular weight(M_n=50,000 Da),nano-emulsionpolytetrafluoroethylene(PTFE)particles near their melting point is described.With the nascent particles consisting of ca.75 nm diameter,hexagonal,single crystals,sintering at,e.g.,350℃,results,initially,in merger of neighboring particles,followed by individual molecular motion on the substrate and the formation of folded chain,lamellar single crystals andspherulites,and on-edge ribbons.It is suggested these structures develop,with time,in the mesomorphic“melt”.Sintering ofthe bulk resin yields extended chain,band structures,as well as folded chain lamellae;end-surface to end-surface merger,possibly by end-to-end polymerization,occurs with increasing time.
基金supported by the State Key Basic Research Program of China(2002CB211803).
文摘Polarized optical microscopy (POM) results show that ZSM5 has great influence on both the nucleation stage and the growth stage of PEO spherulites. Part of ZSM5 particles can act as the nucleus of PEO spherulites and thus increase the amount of PEO spherulites. On the other hand, ZSM5 can restrain the recrystallization tendency of PEO chains through Lewis acid-base interaction and hence decrease the growth speed of PEO spherulites. The increasing amount of PEO spherulites, decreasing size of PEO spherulites, and the incomplete crystalliza-tion are all beneficial for creating more continuous amorphous phases of PEO, which is very important for the transporting of Li+ ions. An adequate amount of ZSM5 can enhance the room temperature ionic conductivity of PEO-LiClO4 based polymer electrolyte for more than two mag-nitudes.
基金financially supported by the Major Research Project of University Grants Commission,New Delhi(No.33-38/2008-10(SR))
文摘The physical vapour deposition （PVD） of gallium monotelluride （GaTe） in different crystalline habits was established in the growth ampoule, strongly depending on the temperature gradient. Proper control on the temperatures of source and growth zones in an indigenously fabricated dual zone furnace could yield the crystals in the form of whiskers and spherulites. Optical and electron microscopic images were examined to predict the growth mechanism of morphologies. The structural parameters of the grown spherulites were determined by X-ray powder diffraction （XRD）. The stoichiometric composition of these crystals was confirmed using energy dispersive analysis by X-rays （EDAX）. The type and nature of electrical conductivity were identified by the conventional hot probe and two probe methods, respectively. The mechanical parameters, such as Vickers microhardness, work hardening index, and yield strength, were deduced from microindentation measurements. The results show that the vapour grown p-GaTe crystals exhibit novel physical properties, which make them suitable for device applications.
文摘The spherulite morphology of the rolled and subsequent heat-treated isotactic polypropylene （iPP） was observed by polarized microscopy, and the crystallinity evolution of materials was also measured by the wide angle X-ray scattering （WAXS）. Rolling led to the oblate spherulites in the deformed iPP samples. The sheared crystalline lamellae broke apart into sets of crystalline blocks during rolling. As a result, the crystallinity of the iPP samples was greatly reduced during deformation, which induced the unclear spherulites and spherulite boundaries. Subsequent heat treatment resulted in the strong reerystallization of the rolled iPP samples. But the recrystaUizatinn in this work only meant the rearrangement of the macromolecule along the unbroken crystalline lamellae and the existing small crystalline blocks in the deformed spherulites. Heat treatment did not change the shape of the spherulites formed during deformation. The recrystallization also resulted in very clear spherulites and spherulite boundaries.
基金This work was supported by The National Natural Science Foundation of China and also The State Science and Technology Commission of China under The National Key Project for Fundamental Research "Macromolecular Condensed State".
文摘The surface morphology of free-surface PCL ringed spherulites was investigated by using atomic force microscopy. The spherulites were obtained by crystallization of PCL/PVC blends of different compositions. It was found that the ringed spherulite exhibited regularly fluctuating rings on its surface. Compared with the bright-dark ring pattern of the spherulite under a polarizing microscope, it was proved that the optical characteristics of the ringed spherulite under polarizing microscope coincided with its surface characteristics. The bright rings in polarizing micrographs of the spherulite coincided with the convex rings on its surface, while the dark rings coincided with the concave rings.
