Crystallization Behavior of Amorphous Poly(l-Lactide)

Amorphous poly(l-lactide) (PLLA) was annealed in two different ways: amorphous samples were heated at a given temperature to induce crystallization (one-step annealing); and amorphous samples were first crystallized at a low temperature and subsequently annealed at a higher temperature than the crystallization temperature. Samples thus prepared were measured by DSC. The original amorphous sample exhibited an exothermic peak at about 100°C (exothermic peak I), an exothermic peak just below the melting point (exothermic peak II), and an endothermic peak when it was melted. Exothermic peak I was caused by cold crystallization. When the melting points of PLLA samples, heat-treated in various ways, were plotted as a function of annealing temperature, there was discontinuity at about 120°C. From analyses of wide-angle X-ray diffraction patterns, it was found that when amorphous PLLA was crystallized at a temperature below 120°C, crystallites of the β-form formed, and when annealed at a temperature above 120°C, crystallites of the α-form grew. Thus, exothermic peak I was attributed to cold crystallization of the β-form, and peak II was caused by the phase transition of the β-form to a more stable form.     

非晶态Cu56Zr44合金的结构及其等温退火晶化过程的研究

利用X射线衍射技术、差示扫描量热分析技术和透射电子显微镜研究了非晶态Cu₅₆Zr₄₄合金的结构及其等温退火条件下的晶化过程.实验结果表明,非晶态Cu₅₆Zr₄₄合金在室温下的短程结构类似于硬球无规密堆积分布.在703K过冷液相区内等温退火时发现,当退火时间为3min时,晶化产物主要为Cu₈Zr₃相;当退火时间为6min时,Cu₈Zr₃关键词： 非晶态 56Zr₄₄合金')" href="#">Cu₅₆Zr₄₄合金 结构 等温退火     

Structural evolution of ZrO2–mullite nanocomposites from the Si–Al–Zr–O amorphous bulk

ZrO₂–mullite nanocomposites were fabricated by in-situ-controlled crystallization of Si–Al–Zr–O amorphous bulk at 800–1250°C. The structural evolution of the Si–Al–Zr–O amorphous, annealed at different temperatures, was studied by X-ray diffraction, infrared, Laser Raman spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy. The materials consisted of an amorphous phase up to 920°C at which phase separation of Si-rich and Al, Zr-rich clusters occurred. The crystalline phases of t-ZrO₂ and mullite were observed at 950°C and 1000°C, respectively. Mullite with a tetragonal structure, formed by the reaction between Al–Si spinel and amorphous silica at low temperature, changed into an orthorhombic structure with the increase of temperature. It was the phase segregation that improved crystallization of the Si–Al–Zr–O amorphous bulk. The anisotropic growth of mullite was observed and the phase transformation from t-ZrO₂ to m-ZrO₂ occurred when the temperature was higher than 1100°C.     

57Fe Mössbauer study of amorphous Fe81B13.5Si3.5C2

The amorphous ferromagnet Fe₈₁B_13.5Si_3.5C₂ (Metglas^® 2605SC) has been investigated with Mössbauer spectroscopy. The hyperfine interaction parameters are studied between 80 and 300 K from which some characteristic properties are deduced. The behaviour of the amorphous alloy at higher temperatures has been studied by the room temperature spectra of annealed samples. After a structural relaxation process, a two step crystallization transformation is observed leading to Fe-Si alloy and Fe₂(B, C). X-ray diffraction of samples annealed at higher temperatures reveals the presence of an orthorhombic Fe-B-Si phase of which the structure changes slightly with annealing temperature.     

Crystallization Kinetics of Nucleated Polypropylene with Organic Phosphates

The crystallization kinetics of isotactic polypropylene (iPP) and nucleated iPP with two organic phosphates, sodium salt (NA7) and triglyceride ester (NA8) of 2,2'-methylene-bis(4,6-di-tert-butylphenyl) phosphoric acid, were investigated by means of a differential scanning calorimeter under isothermal and nonisothermal conditions. During isothermal crystallization, a modified Avrami equation was used to describe the crystallization kinetics. Moreover, kinetics parameters, such as the Avrami exponent, n, the crystallization rate constant, k, and the half-time of crystallization, τ_1/2, are compared. The results showed that a dramatic decrease of the half-time of crystallization, as well as a significant increase of the overall crystallization rate, were observed in the presence of the organic phosphates. During nonisothermal crystallization, the primary crystallization was analyzed using the Ozawa model, leading to similar Avrami exponents for iPP and iPP/NA7, which means simultaneous nucleation with three-dimensional spherulitic growth. However, for iPP/NA8, the Avrami exponent in nonisothermal crystallization is evidently different from that in isothermal crystallization, which would indicate a different mechanism of crystal growth. Adding the nucleating agent to iPP makes the overall crystallization activation energy increase.     

Crystallization of α and γ Phases in Isotactic Polypropylene with Low Ethylene Content: Isothermal Crystallization and Secondary Crystallization

Crystallization and melting behaviors of isotactic polypropylene (iPP) with low ethylene content during an isothermal process and on heating just after it are investigated by means of in situ x-ray diffraction. At every isothermal temperature investigated here, the formations of α and γ phases are confirmed. The ratio of γ to α increases with an increase in isothermal temperature. On heating just after the isothermal process, the γ starts melting at a lower temperature than the α. This may be due to the small crystallite size of the γ crystallization during the isothermal process. On cooling after the completion of the isothermal crystallization, the secondary crystallization accelerates, and the γ phase crystallizes predominantly. The fractionation is considered to occur in the primary crystallization during the isothermal process. The low-molecular-weight portion of the materials, which remained in amorphous regions of the spherulite during the isothermal process, crystallizes into the γ phase in the secondary crystallization. Furthermore, the fractionation behavior seems to be enhanced at higher temperatures.     

A metastable hard magnetic phase in the crystallization process of the Fe75Si11B10Nb3Sn1 alloy

A very interesting characteristic of FeSiB based amorphous alloys is its soft magnetic behavior. Most of these alloys remains soft along the crystallization process up to the nucleation of the iron borides. Examples of this are the widely studied Finemet and the FeSiBSn. In this work the crystallization of Fe₇₆Si₁₁B₁₀Nb₃ and Fe₇₅Si₁₁B₁₀Nb₃Sn₁ is studied by means of X-ray diffraction, Mössbauer spectroscopy and coercive magnetic field measurements after one hour isothermal annealing at different temperatures. In the crystallization process of the latter alloy a hard magnetic phase appeared when the samples were annealed above 773 K. The soft magnetic behavior was recovered after annealing at 873 K. The hyperfine parameters as well as the X-ray diffraction patterns are reported.     

Detailed study of ultra-soft magnetic properties of Fe74Cu0.8Nb2.7Si15.5B7

The magnetic properties of nanocrystalline Fe₇₄Cu_0.8Nb_2.7Si_15.5B₇ alloy, which were rapidly solidified and then annealed at various temperatures between 475 and 650°C for different holding time, have been studied. Grain size, silicon content and the lattice parameter of α-Fe(Si) nanograins at the annealing temperatures were determined. Curie temperature of the amorphous phase was determined from the temperature dependence of permeability. For higher annealing temperatures and times, some Si diffused out of the α-Fe(Si) phase and formed an ordered DO₃ phase of Fe₃Si. This changed the overall magnetostriction and average anisotropy of the matrix, which deteriorated the magnetic softness of the material at higher annealing temperatures. Ultra-soft magnetic properties were achieved by averaging the random anisotropy via exchange interaction. Hysteresis loops for samples in as-cast and annealed conditions have also been studied.     

Isothermal Crystallization of Isotactic Polypropylene Nucleated with a Novel Aromatic Heterocyclic Phosphate Nucleating Agent

The incorporation of a nucleating agent into isotactic polypropylene (iPP) is one of the most important and widely used methods to improve performance in the polypropylene industry. Aromatic heterocyclic phosphate salt is a kind of highly effective nucleating agent for iPP and one of the typical products is a compound nucleating agent based on 2, 2-methylene-bis (4, 6-di-tert-butylphenyl) phosphate hydroxyl aluminum (commercial product name: ADK NA-21). In this paper the isothermal crystallization kinetics of iPP nucleated with the α-nucleating agent NA-21, investigated using differential scanning calorimetry (DSC), is described with the crystallization data being analyzed by using the classic Avrami method. During isothermal crystallization the addition of nucleating agent NA-21 dramatically shortened the crystallization half time (t_1/2) of iPP under the same conditions and the crystallization activation energy, ΔE, decreased from 422 kJ/mol for virgin iPP to 369 kJ/mol with the addition of NA-21. Thus, the addition of NA-21 significantly increased the crystallization rate of iPP.     

Crystallization behavior and microstructure of Fe75Co6Zr9B10 alloy

Fe₇₅Co₆Zr₉B₁₀ amorphous alloy prepared by melt-spinning was annealed at various temperatures. The crystallization behavior and microstructure were investigated by differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The three exothermal peaks in the DTA curve of Fe₇₅Co₆Zr₉B₁₀ amorphous alloy correspond to the formations of α-Fe and α-Mn type phases, the growth of BCC-Fe volume fraction at the expense of α-Mn and residual amorphous phase and the precipitations of Fe₃Zr, etc. intermetallic compounds, respectively. The second exothermic peak is not influenced by heating rate, but it shifts to a higher temperature region with increasing preannealing temperature of Fe₇₅Co₆Zr₉B₁₀ alloy. The α-Mn type phase is metastable and its lattice parameter determined by TEM is 0.8830 nm. AFM images show the development of surface morphology of alloy after annealing. The particle size increases with increasing annealing temperature.     

Pulsed laser deposition and annealing of Dy-Fe-B thin films on melt-spun Nd-Fe-B ribbons for improved magnetic performance

Pulsed laser deposition of 250-nm thick, amorphous Dy₂Fe₁₄B layers on 40-μm thick Nd₂Fe₁₄B melt-spun ribbons was conducted to improve coercivity and energy product. The coated ribbons were subsequently annealed by two methods: (1) furnace annealing in an inert-gas controlled quartz furnace using tantalum foil at 1173 K for 2 h; (2) laser annealing using a continuous wave CO₂ laser with power varying from 10 to 20 W for 0.2 s (estimated temperatures using a thermal model were 993-1528 K). X-ray diffraction was used to identify the microstructural phases and grain size. Magnetic hysteresis tests were conducted at 300 K using a SQUID magnetometer with a maximum field of 5.0 T. Results showed a 10% increase in coercivity and 30% increase in energy product in coated over uncoated samples that were furnace-annealed. However, the coated and laser-annealed samples exhibited soft magnetic behavior with almost zero coercivity. The incomplete crystallization of amorphous phase and precipitation of α-Fe during laser annealing are found to be responsible for the observation of poor magnetic performance.     

Kinetics of the apparent isothermal and non-isothermal crystallization of the α-Fe phase within the amorphous Fe81B13Si4C2 alloy

Kinetics of the apparent isothermal and the non-isothermal crystallization of α-Fe phase within the amorphous Fe₈₁B₁₃Si₄C₂ alloy were investigated by an X-ray diffraction (XRD) and by a differential scanning calorimetry (DSC). It was established that the apparent isothermal crystallization of α-Fe phase within amorphous Fe₈₁B₁₃Si₄C₂ alloy could be described by the Johnson-Mehl-Avrami (JMA) kinetic model (with parameter n_iso=4.0). The apparent isothermal crystallization process includes a constant rate of nucleation and three-dimensional growth of nuclei. The results of X-ray diffraction (XRD) data of the isothermally crystallized samples confirmed the above established kinetic model. From the kinetic analysis of the non-isothermal crystallization of the α-Fe phase within this amorphous alloy, it was concluded that the autocatalytic two-parameter Šesták-Berggren (SB) reaction model (with kinetic exponents M=0.72 and N=1.02) describes well the studied process under the given conditions. The non-isothermal crystallization process involves the constant nucleation rate of stable nuclei with additional secondary two-dimensional (surface) nucleation and overlapping of the growing nuclei on account of the non-isothermal activation.     

Formation of β-iPP in Isotactic Polypropylene/Acrylonitrile–Butadiene–Styrene Blends: Effect of Resin Type,Phase Composition,and Thermal Condition

The formation of β-iPP (β-modification of isotactic polypropylene) in the iPP/ABS (acrylonitrile–butadiene–styrene), iPP/styrene–butadiene (K resin), and iPP/styrene–acrylonitrile (SAN) blends were studied using differential scanning calorimery (DSC), wide angle X-ray diffraction (WAXD), and scanning electron microscopy (SEM). It was found that α-iPP (α-modification of isotactic polypropylene) and β-iPP can simultaneously form in the iPP/ABS blend, whereas only α-iPP exists in the iPP/K resin and iPP/SAN blend samples. The effects of phase composition and thermal conditions on the β-iPP formation in the iPP/ABS blends were also investigated. The results showed that when the ABS content was low, the ABS dispersed phase distributed in the iPP continuous phase, facilitating the growth of β-iPP, and the maximum amount of β-iPP occurred when the composition of iPP/ABS blend approached 80:20 by weight. Furthermore, it was found that the iPP/ABS blend showed an upper critical temperature T _c * at 130°C for the formation of β-iPP. When the crystallization temperature was higher than the T _c *, the β-iPP did not form. Interestingly, the iPP/ABS blend did not demonstrate the lower critical temperature T _c ** previously reported for pure iPP and its blends. Even if the crystallization temperature decreased to 90°C, there was still β-iPP generation, indicating that ABS has a strong ability to induce the β-iPP. However, the annealing experiments results revealed that annealing in the melt state could eliminate the susceptibility to β-crystallization of iPP.     

Annealing effects on the structure and electrical characteristics of amorphous Er2O3 films

Amorphous Er 2 O 3 films are deposited on Si (001) substrates by using reactive evaporation.This paper reports the evolution of the structure,morphology and electrical characteristics with annealing temperatures in an oxygen ambience.X-ray diffraction and high resolution transimission electron microscopy measurement show that the films remain amorphous even after annealing at 700 C.The capacitance in the accumulation region of Er 2 O 3 films annealed at 450 C is higher than that of as-deposited films and films annealed at other temperatures.An Er 2 O 3 /ErO x /SiO x /Si structure model is proposed to explain the results.The annealed films also exhibit a low leakage current density (around 1.38 × 10 4 A/cm 2 at a bias of 1 V) due to the evolution of morphology and composition of the films after they are annealed.     

The influence of Cu and Nb on the crystallization products of annealed FeCuNbSiB

Depending on different Nb and Cu concentration, we studied the formation of nano- and microcrystalline phases in differently annealed samples of FeCuNbSiB. First, the kinetics of crystallization was explored by measuring the temperature-dependent electrical resistivity and magnetization. After this, we collected Mössbauer spectra and did an X-ray diffraction analysis of annealed samples at chosen temperatures to discover the different crystalline phases. It was found how the onset of crystallization had been shifted towards other temperatures. The analysis of Mössbauer spectra shows that building up the well-known DO₃ structure of Fe₃Si is disturbed in the alloy without Cu. At higher Nb content, we resolve two different crystallization steps in the formation of Fe₃Si and a new crystalline phase, probably being a structure like Fe₂₃B₆.     

Annealing effects on the optical and structural properties of Al2O3/SiO2 films as UV antireflection coatings on 4H-SiC substrates

Al₂O₃/SiO₂ films have been prepared by electron-beam evaporation as ultraviolet (UV) antireflection coatings on 4H-SiC substrates and annealed at different temperatures. The films were characterized by reflection spectra, ellipsometer system, atomic force microscopy (AFM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. As the annealing temperature increased, the minimum reflectance of the films moved to the shorter wavelength for the variation of refractive indices and the reduction of film thicknesses. The surface grains appeared to get larger in size and the root mean square (RMS) roughness of the annealed films increased with the annealing temperature but was less than that of the as-deposited. The Al₂O₃/SiO₂ films maintained amorphous in microstructure with the increase of the temperature. Meanwhile, the transition and diffusion in film component were found in XPS measurement. These results provided the important references for Al₂O₃/SiO₂ films annealed at reasonable temperatures and prepared as fine antireflection coatings on 4H-SiC-based UV optoelectronic devices.     

退火处理Fe43Co43Hf7B6Cu1非晶合金的正电子湮没研究

对熔体急冷法制备的Fe₄₃Co₄₃Hf₇B₆Cu₁非晶合金进行了200,300,400和500 ℃保温30 min的退火处理,用正电子湮没寿命谱、X射线衍射、穆斯堡尔谱等方法研究了退火后试样的结构及结构缺陷变化.结果表明,在非晶合金的制备态,正电子主要在非晶基体相空位尺寸的自由体积中湮没,湮没寿命τ₁为158.4 ps,强度I₁关键词： 43Co₄₃Hf₇B₆Cu₁非晶')" href="#">Fe₄₃Co₄₃Hf₇B₆Cu₁非晶 退火处理 正电子湮没寿命 结构与结构缺陷     

非晶Fe73.5Cu1Nb3Si13.5B9合金激光纳米化的超精细结构研究

在CO₂激光功率为50—300W、扫描速度为20mm/s、激光散光斑为20mm照射条件下 ，诱导非 晶Fe_735Cu₁Nb₃Si_135B9带中发生结构重组，产生定量纳米α-F e(Si)晶相形成双相组织结构材料. 利用穆斯堡尔谱研究了非晶Fe_735C u₁Nb₃Si_135B₉合金激光纳米化的 超精细结构. 实验结果表明，激光诱导非晶 Fe_735Cu₁Nb₃Si_135B ₉纳米化后，其超精细磁场的分布随 着激光功率变 化由单峰向双峰变化，在高功率辐照时， 出现了双峰分布，并且峰位向高场移动. 高激光 功率辐照非晶Fe_735Cu₁Nb₃Si_{135B9合金纳米晶化相有四种超精细结 构，即2个超精细磁场较小的初晶相和2个超精细磁场较大的纳米晶化相. 其中超精细磁场较 大(17—25MA/m)的α-Fe(Si)相为DO3结构. 关键词： 激光 纳米晶α-Fe（Si) 735}Cu₁Nb< sub>3Si_135B₉')" href="#">非晶Fe_735Cu₁Nb< sub>3Si_135B₉ 超精细结构 超精细磁场     

Crystallization of Fe-B amorphous alloy powders produced by chemical reduction

The crystallization behaviour of the Fe?B amorphous alloy powders prepared by the chemical reduction method has been investigated by Mössbauer spectroscopy. In comparison to amorphous ribbons prepared by melt-spinning, a different crystallization behaviour has been observed. After annealing the amorphous samples entirely crystallized into three crystalline phases: α-Fe, Fe₃B, and Fe₂B. In the case of Fe₈₀B₂₀ amorphous alloy ribbons produced by melt-spinning technique eutectic crystallization is commonly observed and results in the crystalline phases: α-Fe and Fe₃B. This kind of crystallization was not observed in the chemically prepared samples. The metastable tetragonal Fe₃B phase transformed completely into α-Fe and Fe₂B after annealing at 973 K for one hour.     

退火气压对Bi3.25La0.75Ti3O12铁电薄膜的微观结构和铁电性能的影响

采用sol-gel法在Pt/TiO₂/SiO₂/p-Si(100)衬底上制备了Bi_3.25La_0.75Ti₃O₁₂(BLT)铁电薄膜,研究了在750 ℃时不同退火气压(p_{O2:10^-4—3 atm)对薄膜微观结构和电学性能的影响.XRD和拉曼光谱结果表明在10^-4和3 atm氧气压下退火 关键词： 3.25}La_0.75Ti₃O₁₂')" href="#">Bi_3.25La_0.75Ti₃O₁₂ 铁电性能 sol-gel法 正交化度