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41.
Two glasses based on lithium disilicate (LS2), with and without fluorapatite (FA), were synthesised in the Li2O-SiO2-CaO-P2O5-CaF2 system with P2O5: CaO: CaF2 ratios corresponding to fluorapatite. Glass-ceramics have then been prepared by thermal treatment. The mechanism and kinetics of crystallization as functions of grain size and rate of heating were investigated using thermal analysis methods. The smaller particles crystallize preferentially by surface crystallization, which is replaced by volume crystallization at larger particle sizes. Inclusion of FA in the LS2 favours crystallization through the surface mechanism. The onset limit for volume crystallization replacing the surface mechanism is at about 0.3 mm for pure LS2 glass and 0.9 mm for glass containing FA. The calculated activation energies of the glasses (299 ± 1 kJ mol-1 for pure LS2 glass and 288 ± 7 kJ mol−1 for glass containing FA according to Kissinger, or 313 ± 1 kJ mol-1 for pure LS2 glass and 303 ± 8 kJ mol-1 for glass containing FA according to Ozawa) indicate that the tendency of the glasses to crystallize is supported by the FA presence. Bioactivity of all samples has been proved in vitro by the formation of new layers of apatite-like phases after soaking in SBF.   相似文献   
42.
Differential scanning calorimetry was used to study the thermal characteristics and morphological structure of species produced during the ring opening polymerization of cyclic butylene terephthalate (CBT). Thermal programs consisting of a first ramp heating scan and an isothermal step, followed by cooling and a second ramp heating step, were used to study the effects of thermal history, catalyst (butyl chlorotin dihydroxide) at concentrations between 0.1 and 1.3% (w/w), and the presence of a layered silicate nanofiller (montmorillonite at 4.0%, w/w) on the structure of the resulting polymer (poly(butylene terephthalate), pCBT). Wide angle X-ray diffraction was used to monitor the degree of exfoliation of the nanocomposites.It was found that pCBT is formed in the amorphous state, and crystallizes during the heating step or during the isothermal step at temperatures lower than the equilibrium melting temperature of the polymer (). When premixed with the nanofiller, irrespective of whether this was previously intercalated with a tallow surfactant or used in its pristine form, polymerization took place at higher temperatures and most of the crystallization was found to occur during the cooling stage. In those cases where crystallization took place during either the first heating scan, or during a prolonged isothermal step below the of the polymer, the resulting crystals were found to have a higher lamellar thickness, as compared with the same polymer crystallized from the melt during the cooling step from temperatures above the polymer .  相似文献   
43.
44.
Isochronal crystallization kinetics of Cu60Zr20Ti20 bulk metallic glass has been investigated by differential scanning calorimetry. By means of the Kissinger, Ozawa, Kempen, Matusita and Gao methods, average effective activation energies for the first and second crystallization reactions in Cu60Zr20Ti20 are calculated to be about 375 ± 9 and 312 ± 11 kJ mol−1, respectively, which are smaller than the values deduced from isothermal experiments. Meanwhile, average Avrami exponents, 3.0 ± 0.1 and 3.4 ± 0.2, for two crystallization reactions in isochronal anneals, differ from the value about 2.0 in isothermal anneals. The nonidentity of the Avrami exponents and effective activation energies may be contributed to different crystallization mechanisms and the nature of non-isokinetic between isochronal and isothermal experiments. The values of frequency factor k0 for the first and second crystallization reactions of Cu60Zr20Ti20 are (1.7 ± 0.3) × 1024 and (7.0 ± 0.8) × 1018 s−1, respectively, and the large value of k0 has been discussed in terms of the atomic configuration and interaction.  相似文献   
45.
Transparent glass-nanocomposite sample [50Li2B4O7-50(SrO-Bi2O3-Nb2O5)] (mol %) was prepared by a conventional melt-quenching technique. Fluorite (Bi3NbO7) and SrBi2Nb2O9 (SBN) was produced by heat-treating the as-prepared sample at 773 K for 6 h (HT773). The nanocrystallites of fluorite and SBN phases in the Li2B4O7 glass matrix were established by differential thermal analysis (DTA) which is confirmed by X-ray powder diffraction (XRD), infrared spectroscopy and transmission electron microscopic (TEM) studies. The influence of heat-treating the as-prepared sample on the optical properties (transmission, optical band gap and Urbach energy) has been investigated. Properties such as dielectric constant and dielectric loss as a function of frequency (120 Hz -100 k Hz) and temperature (300-829 K) are reported.  相似文献   
46.
CuZr as well as CoZr are well known metallic glass-formers in a wide compositional range. Since the binary Cu-Co system exhibits a metastable liquid-liquid miscibility gap, i.e. Cu and Co tend to separate from each other, the ternary Cu-Co-Zr system is a promising candidate to form phase separated glass-glass composites. In this work (Cu60Co40)1 − xZrx metallic glasses with relatively low Zr contents of x = 37 and x = 32 were prepared by melt spinning and investigated by in-situ small-angle and wide-angle X-ray scattering (SAXS/WAXS) and differential scanning calorimetry (DSC). Certain heat treated samples were additionally investigated by high-resolution transmission electron microscopy (HRTEM). Even for x = 32 there are no indications for any kind of phase separation in the as-quenched state within experimental resolution, i.e. the critical temperature Tc for a liquid-liquid phase separation has already decreased from 1556 K for binary Cu60Co40 to a temperature below the glass transition temperature Tg = 762(5)K found for (Cu60Co40)68Zr32. Combined in-situ SAXS/WAXS and HRTEM investigations reveal that thermal annealing also does not induce an amorphous-amorphous phase separation. Instead the formation of nano crystallites of a so far unknown Cu-rich/Zr-poor phase with relatively low activation energy for crystallization Ea = 116(7) kJ/mol at temperatures far below the crystallization temperature deduced from DSC measurements is observed.  相似文献   
47.
D. Roy  H. Raghuvanshi 《Journal of Non》2011,357(7):1701-1704
The crystallization behavior and thermal stability of amorphous phases of Al65Cu20Ti15 alloy obtained by mechanical alloying were investigated by using in-situ X-ray diffraction and differential scanning calorimetry (DSC) under non isothermal and isothermal conditions. The result of a Kissinger analysis shows that the activation energy for crystallization is 1131 kJ/mol. The higher stability against crystallization of Al65Cu20Ti15 amorphous alloy is attributed to the stronger interaction of atoms in the Al-Cu-Ti system and formed of complicated compound like Al5CuTi2 and Al4Cu9 as primary phases. The isothermal crystallization was modeled by using the Johnson-Mehl-Avrami (JMA) equation. The Avarami exponents suggest that the isothermal crystallization is governed by a three-dimensional diffusion-controlled growth.  相似文献   
48.
We report a novel approach for fabrication of cubic ZrWMoO8 applying a melt quenching method. The stoichiometric mixture of ZrO2, WO3 and MoO3 in a 1:1:1 M ratio was melted and quenched at room temperature by pouring the melts between two metal plates. The quenched sample was characterized by X-ray diffraction (XRD), differential thermal analysis (DTA) and scanning electron microscopy (SEM) analysis. As quenched material is polyphase contains above 70% ZrWMoO8. The obtained composite is thermal stable up to 930 °C. The ZrWMoO8 was indexed as cubic with a lattice parameter a = 9.1263 (3) Å calculated by the “PowderCell” program. By SEM observation it was established that the microstructure of bulk composite material is built up of one-direction orientated agglomerates with cuboid crystal morphology.  相似文献   
49.
Glasses, whose basic composition was based on the CaO-MgO-SiO2 system and doped with B2O3, P2O5, Na2O, and CaF2, were prepared by melting at 1400 °C for 1 h. Raman and infrared (IR) spectroscopy revealed that the main structural units in the glass network were predominantly Q1 and Q2 silicate species. The presence of phosphate and borate units in the structure of the glasses was also evident in these spectra. X-ray analysis showed that the investigated glasses devitrified at 750 °C and higher temperatures. The crystalline phases of diopside and wollastonite dominated, but weak peaks, assigned to akermanite and fluorapatite, were also registered in the diffractograms. The presence of B2O3, Na2O, and CaF2 had a negligible influence on the assemblage of the crystallized phases, but it caused a reduction of crystallization temperature, comparing to similar glasses of the CaO-MgO-SiO2 system.  相似文献   
50.
A.X. Lu  Z.B. Ke  Z.H. Xiao  X.F. Zhang  X.Y. Li 《Journal of Non》2007,353(28):2692-2697
Utilizing P2O5 as nucleation agent, a Li2O-ZnO-Al2O3-SiO2 glass was prepared by conventional melt quenching technique and subsequently converted to glass-ceramics with different crystal phases. During the processing, two-step heat-treatments including nucleation and crystallization were adopted. The effects of heat-treatment on the crystal type, the microstructure and the thermal expansion behavior of the glass-ceramics were studied by means of differential scanning calorimetry, X-ray powder diffraction analysis, scanning electron microscopy and thermal expansion coefficient tests. It was shown that the crystallization of occurred after the glass was treated at 580 °C. As the temperature increased from 580 °C to 630 °C, cristobalite and were identified as main and second crystal phases, respectively, in the glass-ceramic. An increase in the temperature to 700 °C, the β-quartz solid solution in the glass-ceramic accompanied by a decrease in cristobalite content. The transformation from to γ0-Li2ZnSiO4 took place from 700 °C to 750 °C. The resulting crystallization phases in the glass-ceramics obtained at the temperature higher than 750 °C were β-quartz solid solution and γ0-Li2ZnSiO4. The glass-ceramics containing or β-quartz solid solution crystal phase possessed a microstructure formed by the development of dendritic crystals. The thermal expansion coefficient of the glass-ceramics varied from 36.7 to 123.8 × 10−7 °C−1 in the temperature range of 20-400 °C, this precise value is dependent on the type and the proportion of the crystalline phases presented.  相似文献   
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