Morphology of melt-crystallized syndiotactic polypropylene

A transmission electron microscopy (TEM) study was made to investigate the mechanism of isothermal crystallization from melt for syndiotactic polypropylene (sPP) with a syndiotactic pentad fraction of 0.92. The TEM morphologies of RuO4-stained and ultrathin-sectioned specimens revealed a clear assignment of lamellar crystals with different crystal thicknesses to their corresponding melting temperatures and types of crystal structures. It has been found that isolated, single crystal lamellae with cell III structure were grown at 140 degrees C by a plausible crystal growth mechanism with regime I. Fringed-micellar type of lamellae with cell II structure as thin as c. 4 nm were formed in the interstices of the thick chain-folded lamellae by the subsequent quenching.     

Competing Crystal Growth in Ge–Sb Phase‐Change Films

Analysis of crystal growth in thin films of phase‐change materials can provide deeper insights in the extraordinary phase transformation kinetics of these materials excellently suited for data storage applications. In the present work crystal growth in Ge_xSb_100‐x thin films with x = 6, 7, 8, 9, and 10 is studied in detail, demonstrating that the crystallization temperature increases from ～80 °C for Ge₆Sb₉₄ to ～200 °C for Ge₁₀Sb₉₀ and simultaneously the activation energy for crystal growth also significantly increases from 1.7 eV to 5.5 eV. The most interesting new finding is that in the thin films containing 8, 9, and 10 at% Ge two competing growth modes occur which can have several orders of magnitude difference in growth rate at a single external temperature: an initial mode with isotropic slow growth producing circular crystals with smooth surfaces and growth fronts and a fast growth mode producing crystals with triangular shape having rough surfaces and growth fronts indicative of dendritic‐like growth. The slow‐growth mode becomes increasingly dominant for crystallization at low temperatures when the Ge concentration is increased from 8 to 10 at% Ge. For a certain Ge concentration, the slow growth mode becomes increasingly dominant at lower temperatures and the fast growth mode at higher temperatures. Latent heat produced during crystallization is considered a principal factor explaining the observations. The fast growth mode is associated with (eutectic) decomposition generating more latent heat and instable growth fronts and the slow growth mode is associated with thermodynamically less stable homogeneously alloyed crystals generating less latent heat, but stable growth fronts.     

In situ SEM imaging at temperatures as high as 1450 degrees C

Modifications to a scanning electron microscope (SEM) and a commercially available heating stage permits in situ imaging at temperatures as high as 1450 degrees C. Here we report on the technical modifications necessary to allow such high-temperature in situ imaging. In addition, in order to underline the potential of this technique in the field of materials science, three heating-stage experiments are presented, which reveal microstructural changes occurring at high temperature. The respective in situ experiments are: (i) surface crystallization of a cordierite glass at 1050 degrees C; (ii) thermal recovery of asbestos (chrysotile) fibers at 1250 degrees C; and (iii) residual pore-structure evolution of tricalcium phosphate during sintering at 1450 degrees C.     

PVT法同质籽晶AlN晶体生长

为了获得高质量AlN晶体,通过物理气相传输(PVT)法,采用AlN籽晶进行AlN晶体生长,并通过双温区加热装置对衬底与原料之间的温差进行调节。研究结果表明,籽晶形核阶段,随着AlN籽晶与原料顶温差的减小,AlN的形核机制呈现三种模式,分别为岛生长模式、畴生长模式和螺旋位错生长模式;晶体生长阶段,通过增加AlN籽晶与原料顶温差来提高晶体生长速率,采用10℃/h的变温速率将温差从10℃增加为30℃时,AlN晶体生长模式不变,仍然保持螺旋位错生长模式,该生长模式下获得的AlN晶体结晶质量最高,(0002)面摇摆曲线半峰宽(FWHM)约为55 arcsec。     

Nd:MgO:LiNbO/sub 3/ self-frequency-doubled laser pumped by a flashlamp at room temperature

A small Xe flashlamp-pumped Nd:MgO:LiNbO/sub 3/ self-frequency-doubled laser at room temperature is described. The laser device could be operated with 400 mu J/shot output of pure green light at 26 degrees C. The threshold is smaller than 4.8 J. The optimum phase-matching could be achieved over 15 degrees C to 45 degrees C, if the crystal was aligned and no photorefractive damage was observed.<>     

Highly Crystalline Soluble Acene Crystal Arrays for Organic Transistors: Mechanism of Crystal Growth During Dip‐Coating

The preparation of uniform large‐area highly crystalline organic semiconductor thin films that show outstanding carrier mobilities remains a challenge in the field of organic electronics, including organic field‐effect transistors. Quantitative control over the drying speed during dip‐coating permits optimization of the organic semiconductor film formation, although the kinetics of crystallization at the air–solution–substrate contact line are still not well understood. Here, we report the facile one‐step growth of self‐aligning, highly crystalline soluble acene crystal arrays that exhibit excellent field‐effect mobilities (up to 1.5 cm V^?1 s^?1) via an optimized dip‐coating process. We discover that optimized acene crystals grew at a particular substrate lifting‐rate in the presence of low boiling point solvents, such as dichloromethane (b.p. of 40.0 °C) or chloroform (b.p. of 60.4 °C). Variable‐temperature dip‐coating experiments using various solvents and lift rates are performed to elucidate the crystallization behavior. This bottom‐up study of soluble acene crystal growth during dip‐coating provides conditions under which one may obtain uniform organic semiconductor crystal arrays with high crystallinity and mobilities over large substrate areas, regardless of the substrate geometry (wafer substrates or cylinder‐shaped substrates).     

Growth and Characterization of Pure and Cd-Doped Zinc Tris-Thiourea Sulfate (ZTS) Single Crystals

Single crystals of pure and Cd-doped zinc tris-thiourea sulfate (ZTS) were grown for frequency conversion applications by a low temperature solution growth method, allowing slow evaporation of the water solvent at a constant temperature. The solubility of ZTS was found to increase with the concentration of Cd in the aqueous solution. The optical transparency was found to increase in the Cd-doped crystals as compared to that in the undoped crystals. The doping of Cd was confirmed quantitatively by the atomic absorption spectroscopy and qualitatively by Fourier transform infrared spectroscopy. From the powder x-ray diffraction study, it was found that the lattice constants (a, b and c) decrease with the concentration of Cd in ZTS, but the change in the crystal symmetry and space group has not been reported. A?change in growth habit of Cd-doped crystals has been observed. Thermo-gravimetric and differential thermal analysis was employed to learn the thermal stability of the grown crystals, and 2 mol% Cd-doped ZTS crystal was found to thermally stable up to 230 °C. The second harmonic generation (SHG) efficiency measurement reveals improvement in the SHG efficiency, as 4 mol% Cd-doped ZTS crystal has 1.36 times more SHG efficiency as compared to the pure ZTS crystal.     

Development of inclusion-free CdZnTe substrates from crystals grown by the vertical-gradient freeze method

With the aim of fabrication of (111) and (211) CdZnTe inclusion-free substrates for molecular-beam epitaxy (MBE) and liquid-phase epitaxy (LPE) growth of mercury cadmium telluride (MCT), we focused on fundamental research of the process of crystallization and cooling to room temperature. Based on the study of inclusion formation in dependence of Cd overpressure above the melt, an optimized process of crystal solidification was established. A key result of this study is the position of the Cd pressure, where inclusion-free crystals were fabricated without post-growth annealing. The crystals with a diameter of 100 mm and a height 40–50 mm were fabricated by the vertical-gradient freeze method (VGFM). The resulting ingots exhibit very good crystallographic quality, with a single-crystalline part filling 60–80% of the crystal volume. Substrates with orientation (111) and (211) and dimensions up to 4 × 4 cm were fabricated.     

LD端面泵浦圆柱形Nd：YAG晶体热效应研究

建立了圆柱形激光晶体的热传导模型。通过求解泊松方程,得到了在不同Nd离子掺杂浓度和不同泵浦光半径情况下激光晶体内的温度和温度场分布。研究结果表明,当其他条件不变时,随着Nd离子掺杂浓度的增加,Nd:YAG晶体端面中心温度会升高,而晶体中心轴温度却会快速衰减。对于相同晶体,在泵浦功率一定时,随着泵浦光斑半径的减小,Nd:YAG晶体端面中心温度会升高。如果采用低掺杂浓度的晶体作为增益介质,同时合理增加泵浦光斑半径,则可以有效抑制晶体的热效应。这一结论为提高激光器的稳定性、研究晶体的热效应提供了理论依据。     

Structural and electrical analysis of poly-Ge films fabricated by e-beam evaporation for optoelectronic applications

We have investigated the relationship between structural and electrical properties of Ge thin films deposited on single crystal silicon (100) substrates by electron beam evaporation at room temperature. Post-thermal annealing was applied to obtain poly-crystalline Ge thin films. The structural effects of the annealing temperature and annealing time on the crystallization of Ge films were analyzed using Raman and X-ray diffraction measurements. Raman and X-ray diffraction spectra revealed a structural evolution from amorphous to crystalline phase with increasing annealing temperature and annealing time. It was found that high quality poly-crystalline Ge films were obtained with crystallization ratio of 90% at an annealing temperarure of 500 °C following the crystallization threshold of 450 °C. Effects of structural ordering on the electrical properties were investigated through current-voltage characteristics of fabricated heterostructure devices (Ge/p-Si). Smooth cathode-anode interchange in the diode behavior has been clearly observed following the structural ordering as a function of annealing temperature in a systematic way. These outcomes could be exploited for engineering of low-cost Ge based novel electronic and opto-electronic devices.     

Oscillatory “reactions” involving the oxygen and carbon background impurities in silicon undergoing heat treatment

The effect of the heat treatment (for 1 h at 750–1100°C) of silicon on the transport of the oxygen and carbon impurities between the impurity-defect clusters, which are present in dislocation-free n-Si crystals, and the crystal matrix was studied. The observed nonmonotonic variations of oxygen and carbon concentrations in the above clusters are interpreted as resulting from oscillatory “reactions” that proceed during accommodation of these clusters when the crystal temperature varies (increases). The temperature limits of such oscillatory “reactions” are estimated.     

Liquid phase epitaxy for the production of YBa2Cu3O7-δ coated conductor

The liquid phase epitaxy (LPE), which is performed under ambient pressure with simple growth apparatus, allows us to fabricate high-Jc YBa₂Cu₃O_7-δ (YBCO) crystalline thick films at high growth rate. We propose that the LPE growth of YBCO films on single crystalline oxide fibers is another way to produce YBCO-coated conductors for power application. In the conventional case of using BaO–CuO melt as a solvent, by which the YBCO crystals grow at about 1000°C, YBCO coating on yttria-stabilized zirconia (YSZ) or SrTiO₃ (STO) single crystalline fibers has not been successfully achieved because of their reaction with the solvent. Recently we have discovered that BaF₂ added as a solution decreases the crystallization temperature of YBCO down to 900°C and suppress the reactivity with no degradation of superconductivity of the YBCO crystal. The YBCO-coated fibers are successfully prepared using this solution. The behavior of critical current under magnetic fields shows that these YBCO-coated fibers have the potential to be used under a high magnetic field at the temperature of liquid nitrogen.     

The effects of hydrogen on aluminum-induced crystallization of sputtered hydrogenated amorphous silicon

The effects of hydrogen on aluminum-induced crystallization (AIC) of sputtered hydrogenated amorphous silicon (a-Si:H) were investigated by controlling the hydrogen content of a-SiH films. Nonhydrogenated (a-Si) and hydrogenated (a-Si:H) samples were deposited by sputtering and plasma-enhanced chemical vapor deposition (PECVD). All aluminum films were deposited by sputtering. Hydrogen was introduced into the sputter-deposited a-Si films during the deposition. After deposition, the samples were annealed at temperatures from 200°C to 400°C for different periods of time. X-ray diffraction (XRD) patterns were used to confirm the presence and degree of crystallization in the a-Si:H films. For nonhydrogenated films, crystallization initiates at a temperature of 350°C. The crystallization of sputter-deposited a-Si:H initiates at 225°C when 14% hydrogen is present in the film. As the hydrogen content is decreased, the crystallization temperature increases. On the other hand, the crystallization initiation temperature for PECVD a-Si:H containing 11at.%H is 200°C. Further study revealed that the crystallization initiation temperature is a function, not only of the total atomic percent hydrogen in the film, but also a function of the way in which the hydrogen is bonded in the film. Models are developed for crystallization initiation temperature dependence on hydrogen concentration in a-Si:H thin films.     

Optimization of fluorine passivation of stainless steel surfaces

The optimum conditions for the fluorine passivation of 316L stainless steel are described. The direct fluoridation products formed at temperatures of 320°C or lower are composed solely of FeF₂ , while those which were formed at the temperatures of 330°C or higher have a compound-phase composition of FeF₂ and FeF ₃. At a critical temperature (400°C for 316L stainless steel) of the thermal modification process, FeF₃ is converted to FeF₂ and disappears completely as the temperature rises. Meanwhile, CrF₃ is formed at a certain temperature (440°C for 316L stainless steel). The two-phase composition gets further crystallized as the thermal modification temperature rises. As the crystal growth induces the cracks on the fluoridated film, it is very difficult to form a satisfactory passivation film from the two-phase composition by thermal modification. It is confirmed that excellent passivation film has been obtained from the single-phase composition by the optimum fluoridation following the optimum thermal modification     

ZnS微球的制备及吸光性能研究

采用溶剂热法,以醋酸锌和硫脲为原料,去离子水和无水乙醇的混合溶液为反应介质制备了ZnS微球。利用XRD、SEM、UV-Vis吸收光谱探讨了反应温度和时间对产物晶型、颗粒形貌以及吸光性能的影响。结果表明:ZnS微球的晶型和形貌对反应温度比较敏感,反应时间对晶体的结晶度和吸光率影响较大。采用溶剂热法的最佳合成温度为150℃左右,反应时间为12 h;该条件下生成的ZnS微球物相较为纯净、结晶完全,且分散性良好,带隙约为3.3 eV。     

Bulk single crystal growth of silicon-germanium

Si-Ge single crystals up to 68 mm diameter and up to 17 at.% germanium were grown using a modified Czochralski technique. Pre-grown large diameter single crystal silicon seeds with various crystallographic orientations were used as templates for solidification to reduce cap crystallization time and to ensure single crystallinity at desired crystal diameters. A discussion is presented of the influences of seed preparation, crystal growing parameters and post-growth processing on the Si-Ge bulk single crystals produced using this new technique. The modified Czochralski technique described in this paper is ultimately intended for the manufacture of 100–200 mm diameter Si-Ge substrates.     

钡镓锗透明微晶玻璃的制备及性能

文中通过微晶化工艺制备出钡镓锗透明微晶玻璃,并研究了其透红外性能和力学性能。结果表明,810~910℃热处理0.5 h 时,钡镓锗微晶玻璃析出单一ZrO2 晶体。处理温度为830℃时,钡镓锗微晶玻璃中开始析出少量ZrO2 晶粒,尺寸约几个纳米;处理温度升到870℃时,平均晶粒尺寸为250 nm;晶化温度高于870℃时,晶粒数量显著增多,晶粒粗大,而且发生团聚现象。晶化温度为810~850℃时,可以获得透红外性能和力学性能兼顾的钡镓锗透明微晶玻璃;处理温度为870℃时,钡镓锗微晶玻璃的力学性能出现极值,但透红外性能降低;若继续升高处理温度,钡镓锗微晶玻璃的透红外性能和力学性能均下降。     

Catalytic and Electron Conducting Carbon Nanotube–Reinforced Lysozyme Crystals

Novel reinforced cross‐linked lysozyme crystals containing homogeneous dispersions of single‐walled carbon nanotubes bundles (SWCNTs) are produced and characterized. The incorporation of SWCNTs inside lysozyme crystals gives rise to reinforced composite materials with tunable mechanical strength and electronic conductivity, while preserving the crystal quality and morphology. These reinforced crystals show increased catalytic activity at higher temperatures, being active even above the denaturation temperature. The electron transport through the crystals is linked to the content and distribution of SWCNT bundles inside the crystals. The electron conduction through the crystals is isotropic and very efficient, presenting high conductivity values up to 600 nS at very low (0.05 wt%) SWCNT concentration. To obtain these crystals, a new protocol based on the in situ crystallization of lysozyme in composite SWCNT–peptide hydrogels is developed. These peptide hydrogels are able to homogeneously disperse bundles of hydrophobic SWCNTs allowing first, the crystallization of the enzyme lysozyme and second, transferring the new properties of the inorganic component to the crystals. Taken together, these composite crystals represent an example of the versatility of proteins as biological substrates in the generation of novel functional materials, opening the door to use them in catalysis and bioelectronics at macroscale.     

Nd:YVO4晶体的弹性常数

利用高精度高频超声技术 ,在室温常压下 ,脉冲回波重合法测定了四方晶系 YVO4 和分别掺质 1at- % ,2 at- % Nd3 的 Nd:YVO4 晶体的声速 ,根据声波沿晶体不同对称方向传播的纵波和横波速度 ,得到六个独立的二阶弹性常数 C11,C4 4,C66,C3 3 ,C12 和 C13 ,由此计算了热力学参数德拜温度 ,并比较 Nd3 掺入量对它们的影响。还报道了弹性常数 C66的异常变化 ,在一对 (0 10 )面上 ,沿[0 10 ]极化方向施加对顶挤压时 ,相应的横波脉冲回波强度急剧减弱 ,传播时间也发生明显变化     

process and mechanism of growth of YBa2Cu3O6+x single crystal by the pulling method

Continuous growth of YBa₂Cu₃O_6+x(Y123) single crystals was achieved by the modified pulling method1 using BaO+CuO(3:5) solvent and Y₂BaCuO₅(Y211) solute. Y211 solid was placed at the bottom of the crucible. Temperature was set ten degrees higher at the bottom than on the surface of the solution. The crystal rotation speed was 120 rpm at first; but as the crystal radius increased, it was reduced to prevent increasing the interface temperature. The maximum crystal growth rate was about 0.2 mm/h. The crystal growth direction was controlled by the seed crystal direction.2 Two-dimensional numerical simulation was performed using a finite-difference method by a supercomputer to investigate the solution flow and temperature distribution.