92 resultados para Crystallization process

em Chinese Academy of Sciences Institutional Repositories Grid Portal


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Glass transition and crystallization process of bulk Nd60Al10Fe20Co10 metallic glass were investigated by means of dynamic mechanical thermal analysis (DMTA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electronic microscopy (SEM). It is shown that the glass transition and onset crystallization temperature determined by DMTA at a heating rate of 0.167 K/s are 480 and 588 K respectively. The crystallization process of the metallic glass is concluded as follows: amorphous alpha-->alpha' + metastable FeNdAl novel phase -->alpha' + primary delta phase-->primary delta phase + eutectic delta phase Nd3Al phase + Nd3Co phase. The appearance of hard magnetism in this alloy is ascribed to the presence of amorphous phase with highly relaxed structure. The hard magnetism disappeared after the eutectic crystallization of amorphous phase.

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The in situ crystallization kinetics of syndiotactic poly(propylene) (sPP) has been investigated by synchrotron small-angle X-ray scattering (SAXS). The structure evolutions during the isothermal crystallization of sPP with different shear rates have been observed. The results show that shear accelerates the process of crystallization kinetics. Even under low shear rate, the lamellae can be distinctly oriented. In contrast, the lamellar parameters such as the long period, lamellar thickness, and the scattering invariant 0 can change obviously only under high shear rate.

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The final structure of molten syndiotactic polypropylene (sPP) sheared under different conditions was investigated by synchrotron small-angle x-ray scattering (SAXS) and wide-angle x-ray diffraction (WAXD) techniques to elucidate the shear effects on sPP crystalline structure. The results obtained from the WAXD show that there is no variation on crystalline form but a little difference on the orientation of the 200 reflection. The SAXS data indicate that the lamellar thickness and long period have not been affected by shear but the lamellar orientation is dependent on shear. The experimental data of sPP crystallization from sheared melt may indicate a mesophase structure that is crucial to the shear effects on the final polymer multiscale crystalline structures.

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A notable amount of PP beta-crystal (30%, by X-ray diffraction pattern) has been found in the PP samples as polymerized at normal static isothermal crystallization conditions without using any extra nucleating agents. Existence of catalyst residues in the sample is decisive, which slows down the crystallization rate facilitating the formation of beta-form spherulites. Comparatively, high molecular weight PP favors the formation of beta-form spherulites, deducting from no beta-crystal detected in the degraded samples. Finally, high isotacticity is also required for obtaining qualitative beta-form spherulites, demonstrated by increased beta-crystal content after removal of weak crystalline fraction of the sample.

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Melting recrystallization processes of melt-sheared films of polypropylene (S28C) fractions have been investigated in situ by polarized optical microscope equipped with CCD camera and hot-stage. Actually, the morphological developments in the melting recrystallization are partially reappearance of oriented crystallization processes during melt-shearing the fractions, which is due to a memory effect of oriented structure of polymer. For low molecular weight fraction, only incomplete spherulites with some orientation along shear direction are observed in the melting recrystallization processes of the sheared films. For middle molecular weight fractions, extended chain fiber crystals(or bands) are formed first at higher temperatures, and the bands can act as self-nuclei (i. e., row nuclei), resulting in epitaxial growth of chain-folded lamellae(or fibril), i. e., the formation of cylindrites, with further decrease of the crystallization temperature. For high molecular weight fraction, however, it is not possible to shear the melt film because of its high melt viscosity. When the low molecular weight fraction in which no fiber crystals or cylindrites are observed, are mixed with small amount(about 1%-2%) of the high molecular weight fraction, quite large number of cylindrites are formed during the melting recrystallization process of its sheared film, which implies that the component of high molecular weight plays an important role in the formation of cylindrites during the shear process of polypropylene.

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The crystallization process and morphology of poly(aryl ether ether ketone ketone) containing meta-phenyl links (PEEKmK) have been investigated by transmission electron microscopy and electron diffraction. The results indicate that the thin films of PEEKmK isothermally crystallized from both the glassy state and the melt at the temperature range of 180 similar to 250 degrees C consist of two kinds of morphological forms, i. e. large (order of mu m), flat-on single crystals and narrow, lath-like, edge-on lamellae, The latter consists of the spherulites. Meanwhile, the growing process of the two kinds of morphological forms has been discussed.

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The structural evolution and property changes in Nd60Al10Fe20Co10 bulk metallic glass (BMG) upon crystallization are investigated by the ultrasonic method, x-ray diffraction, density measurement, and differential scanning calorimetry. The elastic constants and Debye temperature of the BMG are obtained as a function of annealing temperature. Anomalous changes in ultrasonic velocities, elastic constants, and density are observed between 600–750 K, corresponding to the formation of metastable phases as an intermediate product in the crystallization process. The changes in acoustic velocities, elastic constants, density, and Debye temperature of the BMG relative to its fully crystallized state are much smaller, compared with those of other known BMGs, the differences being attributed to the microstructural feature of the BMG.

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Mg65 Cu25 Gdlo bulk metallic glass and its carbon nanotube reinforced composite were prepared. Differential scanning calorimeter (DSC) was used to investigate the kinetics of glass transition and crystallization processes. The influence of CNTs addition to the glass matrix on the glass transition and crystallization kinetics was studied. It is shown that the kinetic effect on glass transition and crystallization are preserved for both the monothetic glass and its glass composite. Adding CNTs in to the glass matrix reduces the influence of the heating rate on the crystallization process. In addition, the CNTs increase the energetic barrier for the glass transition. This results in the decrease of GFA . The mechanism of the GFA decrease was also discussed.

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This paper reports that an optical diagnostic system consisting of Mach-Zehnder interferometer with a phase shift device and image processor has been used for study of the kinetics of protein crystal growing process. The crystallization process of protein crystal by vapour diffusion is investigated. The interference fringes are observed in real time. The present experiment demonstrates that the diffusion and the sedimentation influence the crystallization of protein crystal which grows in solution, and the concentration capillary convection associated with surface tension occurs at the vicinity of free surface of the protein mother liquor, and directly affects on the outcome of protein crystallization. So far the detailed analysis and the important role of the fluid phenomena in protein crystallization have been discussed a little in both space- and ground-based crystal growth experiments. It is also found that these fluid phenomena affect the outcome of protein crystallization, regular growth, and crystal quality. This may explain the fact that many results of space-based investigation do not show overall improvement.

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Real-time phase shift Mach-Zehnder interference technique, imaging technique, and computer image processing technique were combined to perform a real-time diagnosis of NaClO3 crystal, which described both the dissolution process and the crystallization process of the NaClO3 crystal in real-time condition. The dissolution fringes and the growth fringes in the process were obtained. Moreover, a distribution of concentration field in this process was obtained by inversion calculation. Finally, the buoyancy convection phenomenon caused by gravity in the crystal growth process was analyzed. The results showed that this convection phenomenon directly influences the growth rate of each crystal face in the crystal.

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Crystal formation process of charged colloidal particles is investigated using Brownian dynamics (BD) simulations. The particles are assumed to interact with the pair-additive repulsive Yukawa potential. The time evolution of crystallization process and the crystal structure during the simulation are characterized by means of the radial distribution functions (RDF) and mean square displacement (MSD). The simulations show that when the interaction is featured with long-range, particles can spontaneously assemble into body-centered-cubic (BCC) arrays at relatively low particle number density. When the interaction is short-ranged, with increasing the number density particles become trapped into a stagnant disordered configuration before the crystallization could be actualized. The simulations further show that as long as the trapped configurations are bypassed, the face-centered-cubic (FCC) structures can be achieved and are actually more stable than BCC structures. (C) 2010 Elsevier Inc. All rights reserved.

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In this study of the synthesis of SAPO-34 molecular sieves, XRD, SEM, XRF, IR and NMR techniques were applied to monitor the crystalloid, structure and composition changes of the samples in the whole crystallization process in order to get evidence for the crystallization as well as Si incorporation mechanism of SATO-34. XRD results revealed that the crystallization contained two stages. In the first 2.5 h (the earlier stage), high up to similar to80% of relative crystallinity could be achieved and the crystal size of SAPO-34 was almost the same as that of any longer time, indicating a fast crystallization feature of the synthesis. In this stage, IR revealed that the formation of SAPO-34 framework structure was accompanied by the diminution of hydroxyls, suggesting that crystal nuclei of SAPO-34 may arise from the structure rearrangement of the initial gel and the condensation of the hydroxyls. NMR results reveal that the template and the ageing period are crucial for the later crystallization of SAPO-34. Preliminary structure units similar to the framework of SAPO-34 have already formed before the crystallization began (0 h and low temperature). Evidence from IR, NMR, and XRF shows that the formation of the SAPO-34 may be a type of gel conversion mechanism, the solution support and the appropriate solution circumstance are two important parameters of the crystallization of SAPO-34. Meanwhile, NMR measurements demonstrated that about 80% of total Si atoms directly take part in the formation of the crystal nuclei as well as in the growth of the crystal grains in the earlier stage (<2.5 h). Evidence tends to support that Si incorporation is by direct participation mechanism rather than by the Si substitution mechanism for P in this stage (<2.5 h). In the later stage (>2.5 h), the relative content of Si increased slightly with a little decrease of Al and P. The increase of Si(4Al) and the appearance of the Si(3Al), Si(2Al), Si(1Al) and Si(OAl) in this stage suggest that substitution of the Si atoms for the phosphorus and for the phosphorus and aluminum pair takes place in the crystallization. The relationship among structure, acidity and crystallization process is established, which suggests a possibility to improve the acidity and catalytic properties by choosing a optimum crystallization time, thus controlling the number and distribution of Si in the framework of SAPO-34. (C) 2002 Elsevier Science Inc. All rights reserved.

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Recently a debate about the initial crystallization process which has not been the hotspot for a long time since the theory proposed by Hoffman- Lauritzen (LH) dominated the field arose again. For a long time the Hoffman-Lauritzen model was always confronted by criticism,and some of the points were taken up and led to modifications, but the foundation remained unchanged which deemed that before the nucleation and crystallization the system was uniform. In this article the classical nucleation and growth theory of polymer crystallization was reviewed, and the confusion of the explanations to the polymer crystallization phenomenon was pointed out. LH theory assumes that the growth of lamellae is by the direct attachment of chain sequences from the melt onto smooth lateral sides.

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The isothermal crystallization behavior of poly(L-lactic acid)/organo-montmorillonite nanocomposites (PLLA/OMMT) with different content of OMMT, using a kind of twice-functionalized organoclay (TFC), prepared by melt intercalation process has been investigated by optical depolarizer. In isothermal crystallization from melt, the induction periods (t(i)) and half times for overall PLLA crystallization (100 degrees C <= T-c <= 120 degrees C) were affected by the temperature and the content of TFC in nanocomposites. The kinetic of isothermal crystallization of PLLA/TFC nanocomposites was studied by Avrami theory. Also, polarized optical photomicrographs supplied a direct way to know the role of TFC in PLLA isothermal crystallization process. Wide angle X-ray diffraction (WAXD) patterns showed the nanostructure of PLLA/TFC material, and the PLLA crystalline integrality was changed as the presence of TFC. Adding TFC led to the decrease of equilibrium melting point of nanocomposites, indicating that the layered structure of clay restricted the full formation of crystalline structure of polymer.