Effect of pH on the Crystallization of Homogeneously Precipitated Nanosized PZT Powder

Nanosized lead zirconate titanate (PZT) powder with Zr:Ti ratio in the morphotropic phase boundary region was synthesized by homogeneous precipitation of metal ions. The powder precipitated at 90°C and at pH 6.7 resulted single-phase perovskite lead zirconate titanate powder when calcined at 550°C and above for 4 hours in air. The solution pH and the precipitation temperature strongly affect the composition of the calcined powder. The results obtained by structural characterization of homogeneously precipitated powder were compared with that obtained from the conventional precipitation method using ammonia in terms of crystallization, homogeneity, and microstructure. The homogeneously precipitated powder showed smaller particle size, minimum agglomeration and uniform shape on calcination and annealing. Powdered samples that precipitated by homogeneous precipitation crystallized directly to perovskite PZT, without any intermediate pyrochlore phase formation. In contrast, the NH₃ precipitated powder converted to perovskite PZT via metastable pyrochlore and it showed phase segregation upon annealing at higher temperatures. The reaction kinetics has been studied by X-ray diffraction, differential thermal analysis, and differential scanning calorimetry.     

Psychological separation, attachment security, vocational self-concept crystallization, and career indecision: A structural equation analysis.

Structural equation modeling was used to test theoretically based models in which psychological separation and attachment security variables were related to career indecision and those relations were mediated through vocational self-concept crystallization. In contrast to previous studies, which have found either weak or no support for a relation between separation or attachment security variables and career indecision, results based on a sample of 350 college students indicated that some components of separation and attachment security did relate to career indecision in a theoretically supportable direction. Results also revealed that regardless of whether global or component career indecision measures were used, separation and attachment security effects on indecision were at least partially mediated through vocational self-concept crystallization. The strongest mediated relations were observed for the effects of attachment anxiety and maternal separation. (PsycINFO Database Record (c) 2010 APA, all rights reserved)     

Criteria and methodology for the evaluation of conservation interventions on treated porous stone susceptible to salt decay

Susceptibility of stone to salt decay is directly related to its microstructural and mechanical characteristics. In the present work, a porous stone from a quarry in Cyprus was examined. Samples of this stone were consolidated and protected with certain conservation materials. The modification of microstructural characteristics of the stone was evaluated by mercury intrusion porosimetry, while its mechanical characteristics were measured by compressive and bending strength tests. From these data, the susceptibility of Cyprus stone to salt (NaCl) decay was estimated. The values of crystallization pressure of NaCl were calculated and compared to the experimentally measured compressive and tensile strength of the stone, in order to examine the probability of stone disruption due to salt crystallization. The development of the phenomenon after coarse pores’ filling with crystals, i.e. crystallization of salts in capillaries or mechanical failure of the stone, was determined by thermodynamic analysis. Additionally, artificial weathering tests of marine salt spray were performed for the evaluation of stone’s durability after the conservation. The treated stone proved to be resistant to salt decay, as it presented ameliorated microstructural and mechanical characteristics, concerning decay due to soluble salt crystallization. The most possible thermodynamic scenario was small pores repletion with crystals, avoiding mechanical failure of the stone.     

含两种不同共聚组分改性聚酯的结晶速率

添加己二酸、间苯二甲酸,聚乙二醇对PET进行改性,合成样品。用DSC法研究合成共聚物的等温结晶动力学。结果表明,在所选择的温度范围内,共聚物很好的符合Avrami方程。随温度的升高,共聚物的结晶速度常数K和Avrami指数n逐渐减小,结晶速度G逐渐降低。含2种柔性组分的共聚酯随着一种柔性组分含量的增加,结晶速率G上升;含一种刚性一种柔性组分的共聚酯随刚性组分含量的增加,结晶速率G下降。     

Crystallization of Polymer-Derived Silicon Carbonitride at 1873 K under Nitrogen Overpressure

The chemical stability of an amorphous silicon carbonitride ceramic, having the composition 0.57SiC·0.43Si₃N₄·0.49C is studied as a function of nitrogen overpressure at 1873 K. The ceramic suffers a weight loss at p _N2 < 3.5 bar (1 bar = 100 kPa), does not show a weight change from 3.5 to 11 bar, and gains weight above 11 bar. The structure of the ceramic changes with pressure: it is crystalline from 1 to 6 bar, amorphous at ∼10 bar, and is crystalline above ∼10 bar. The weight-loss transition, at 3.5 bar, is in excellent agreement with the prediction from thermodynamic analysis when the activities of carbon, SiC, and Si₃N₄ are set equal to those of the crystalline forms; this implies that the material crystallizes before decomposition. The amorphous to crystalline transition that occurs at ∼10 bar, and which is accompanied by weight gain, is likely to have taken place by a different mechanism. A nucleation and growth reaction with the atmospheric nitrogen is proposed as the likely mechanism. The supersaturation required to nucleate α-Si₃N₄ crystals is calculated to be 30 kJ/mol.     

Melting and crystallization behaviour of elastoplastic semicrystalline copolymers: poly(ether ester)

The melting and crystallization behaviour of an elastoplastic semi-crystalline poly(etherester) has been studied by differential scanning calorimetry. The shape of the melting endotherm is strongly dependent on heating rate and annealing time and results from the sum of simultaneous melting and crystallization phenomena. Samples prepared by different techniques, i.e. by solvent evaporation or by melt extrusion, behave very differently owing to specific crystal morphologies. By applying the Hoffman-Weeks plot, the equilibrium melting temperature has been extrapolated. The Avrami treatment allows the calculation of the index n and of the rate constant K from the isothermal kinetic data.     

熔融温度对PP中成核剂的异相成核作用的影响

用DSC研究了熔融温度对不同类型成核剂成核PP的异相成核作用的稳定性的影响。观察到随熔融温度提高，纯PP的成核作用稳定，降温结晶温度基本不变。而有机磷酸盐类成核剂成核PP的结果温度比纯PP的高，而且异相成核作用受熔融温度的影响也很小。但山梨醇类成核剂成核PP的异相成核作用随熔融温度提高，结晶温度逐步降低明显，表明其异相成核作用对热不稳定。     

Structure and properties of injection‐molded polypropylenes with different molecular weight distribution and tacticity characteristics

Two series of polypropylenes with different molecular weight distribution and tacticity characteristics were injection molded into flexural test specimens by varying cylinder temperature and the effects of the molecular weight distribution and tacticity on the structure and properties of the moldings were studied. Measured propertied were flexural modulus, flexural strength, heat distortion temperature, Izod impact strength, and mold shrinkage and structures studied were crystallinity, the thickness of skin layer, a*‐axis‐oriented component fraction and crystalline orientation functions. The relations between the structures and properties were also studied. It was found that the molecular weight distribution and tacticity characteristics affect the properties mainly through the molecular orientation and crystallinity, respectively. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2142–2156, 2002     

Rates of Crystallization of Dried Lactose-sucrose Mixtures

The isothermal crystallization kinetics of glassy lactose/sucrose mixtures were studied at several storage temperatures (close to T_g and T_m). The kinetic parameters implicit in the Avrami equation were determined. Activation energies for transport (E_D) and surface nucleation (W*) were also found and correlated to the molar composition of the lactose/sucrose mixtures. A monotonic increase in the half crystallization time (t_1/z), Avrami index (n), % crystallization per day, activation energy for transport (E_D) and surface nucleation energy (W*) and a decrease in the crystallization velocity constants (K) were related to the increase in the lactose content of lactose/sucrose mixtures.