大豆脲酶诱导碳酸钙沉淀的多因素影响分析

本文探究了多个影响因素对大豆脲酶诱导碳酸钙沉淀(SICP)的影响,以优选出主要影响因素并提供其最佳范围.首先分析了脲酶浓度和温度对脲酶活性的影响;之后通过正交实验设计,进行25种工况的SICP水溶液实验,研究不同因素组合下Ca2+利用率的变化规律;最后借助扫描电子显微镜观测不同工况下生成碳酸钙的形态.结果表明:低温有利...     

Profile-sapphire and its structural perfection

The paper is concerned with the growing of sapphire of various profiles and with the investigation of its structural perfection. It is shown that the kind of the crystallographic forms and the dislocation structure essentially depends on the degree of overheating of the melt. Near the surface of profiled crystals wide dislocation-free zones (upto 200 μm) may be obtained. A dependence of the length of the mosaic block boundary on the rate of growing can be observed. A high ratio of the area of the radiating surface to the crystal volume gives the possibility of a rapid growing of profile crystals.     

Negative Poisson’s ratio of two-dimensional hard cyclic tetramers

A two-dimensional system of hard, cyclic tetramers has been investigated by constant pressure Monte Carlo (MC) simulations with variable shape of the periodic box. The molecules (tetramers) are composed of four identical hard disks (atoms) with centers forming a square with sides equal to the diameter of the disks. The elastic constants and the Poisson’s ratio are determined by the analysis of strain fluctuations and the reference state of the system. The singular behavior of the elastic constants is in agreement with free volume theory. It has been found that the hard cyclic tetramer system is auxetic – that is, the Poisson’s ratio of the tetramer system is negative.     

Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.     

SAPO-34/CZA复合晶体相结构性质及催化CO2加氢反应研究

采用共沉淀包覆法制备了SAPO-34/CZA双功能复合催化剂,研究了复合相比例对催化剂晶体结构性质和CO2加氢制低碳烯烃催化性能的影响.采用XRD、FT-IR、SEM、BET、NH3-TPD和CO2-TPD等手段对不同催化剂的晶相组成、骨架结构、微观形貌、孔结构及表面酸碱性进行了分析表征.研究结果表明,复合相比例对SAPO-34/CZA双功能复合催化剂的结构性质和催化性能影响较大.质量比为1∶1时,制得复合催化剂具有明显微孔和介孔特征(微孔比表面积53.15 m2·g-1、介孔比表面积59.84 m2·g-1、总比表面积为113.00 m2·g-1、总孔容0.41 cm3·g-1、平均孔径14.57 nm),具有特殊包覆结构及存在复合相界面,构造了特殊反应路径,微介孔层级结构强化耦合反应,表现出较高催化性能.在还原温度285 ℃、反应温度325 ℃、压力3.0 MPa、V(H2)/V(CO2)=3.0、空速(SV)3500 mL·g-1·h-1的条件下,CO2转化率为64.80;,低碳烯烃选择性为49.68;.与物理共混催化剂SAPO-34/CZA-M相比,CO2转化率和低碳烯烃选择性分别提高了31.98;和2.43;.     

Investigation of the photovoltaic performance of the polycrystalline silicon p–n junction by a photothermal measurement

For establishing a new methodology for evaluating an effect of the grain boundaries, both the piezoelectric photo-thermal (PPT) and the surface photo-voltage (SPV) measurements of polycrystalline Si p–n junction samples with different volume fractions of grain boundaries were carried out. We could define the signal intensity ratio of SPV/PPT as the key indicator of photovoltaic performance. This is because the PPT signal implies the phonon emitting carrier loss, whereas the SPV denotes the photo-excited carrier accumulation at the surface and the junction interface. It was found that the SPV/PPT ratio and solar cell efficiency decreased with increasing volume fraction of the grain boundaries. Present experimental results demonstrated that one can directly estimate the photovoltaic performance of in-process polycrystalline Si p–n junction wafer by adopting the combination of the PPT and the SPV methodologies without electrodes. Since the PPT detects the non-radiative recombination process, present methodology and the laser-beam-induced current and the photoluminescence imaging methods are complementary. By complementary use of these methods, it becomes possible to investigate the characteristic of grain boundary.     

Isobaric and isochoric properties of decahydroisoquinoline,an extremely fragile glass-former

Pressure–volume–temperature (PVT) measurements were obtained on decahydroisoquinoline (DHIQ). From the resulting equation of state in combination with previously reported dielectric relaxation data, an analysis of the volume contribution to the dynamics was carried out for this very fragile glass-former (isobaric fragility, m_P = 163). We find that the ratio of the isochoric and isobaric fragilities equals 0.71 ± 0.02, reflecting a strong temperature effect, consistent with the large fragility. The relaxation times superpose when plotted versus temperature times the specific volume raised to the 3.55 power. This is a larger value of the exponent than expected based on the fragility of DHIQ. The implication is that for molecular glass-formers, the classical Lennard-Jones 6–12 repulsive potential may represent the limit for fragile liquids.     

基质组分配比对Cs2LiYCl6∶Ce晶体生长及闪烁性能的影响

Cs₂LiYCl₆∶Ce(CLYC∶Ce)是一种具有良好能量分辨率、高光输出,以及优秀的中子/伽马分辨能力的新型闪烁晶体,但因其组分复杂,晶体生长很困难。本文使用坩埚下降法分别生长了LiCl占57%、60%和63%(摩尔分数)及CsCl与YCl₃比例为1.9∶1和2.1∶1共5种不同组分配比的CLYC晶体,发现LiCl占比为60%的组分得到的CLYC相体积占比最大,而改变CsCl与YCl₃的比例对晶体生长没有明显的积极作用。5 mm×5 mm×5 mm和φ25 mm×10 mm样品在¹³⁷Cs激发下的能量分辨率分别为4.8%和5.6%。CLYC晶体在662 keV伽马射线激发下的闪烁衰减时间为17 ns、436 ns和3 603 ns。     

Dissolution retardation of solid silica during glass-batch melting

During glass-batch melting, solid silica (quartz) usually dissolves last. The measured rate of dissolution, while the temperature was increasing at a constant rate, was compared with the hypothetical diffusion-controlled volume flux from regularly distributed particles through concentration layers of a uniform thickness. The actual rate was up to two orders of magnitude lower than that of the “ideal” case, revealing a progressive inhibition of silica dissolution. As a measure of this retarded dissolution, we introduced a retardation factor defined as a ratio of the actual and “ideal” dissolution rates measured as the volume flux at the melt-particle interface. The severe inhibition of silica dissolution has been attributed to the irregular spatial distribution of silica particles that is associated with the formation of nearly saturated melt on a portion of their surfaces. Irregular shapes and unequal sizes of particles also contribute to their extended lifetime.     

循环流化床粉煤灰可控制备高纯F型八面沸石研究

利用粉煤灰制备沸石分子筛是其高值化利用的重要方向之一.以循环流化床粉煤灰为原料,采用酸浸预处理-氢氧化钠碱熔活化-水热晶化法制备F型八面沸石,并用于吸附亚甲基蓝.考察酸浸温度、碱熔温度及碱灰质量比对粉煤灰结构的影响及碱熔温度、碱灰质量比、液固比及晶化时间对沸石的结构和形貌的影响.通过XRD和SEM对粉煤灰沸石的晶体结构和形貌进行表征.结果表明,利用循环流化床粉煤灰制备高纯F型八面沸石适宜条件为碱熔温度550℃,碱灰质量比1.5:1,液固比12 mL/g,晶体导向剂用量10;,晶化温度100℃,晶化时间20 h.其比表面积高达357 m2/g,且对亚甲基蓝的饱和吸附量高达178 mg/g.     

等离子体增强CVD法沉积的微晶硅薄膜的微结构研究

本文系统研究了PECVD法沉积μc-Si薄膜中衬低温度、氢气稀释率和射频功率等参数对μc-Si薄膜结构特性的影响.表明:随着衬低温度的增加、氢气稀释率的增大、射频功率的提高,薄膜的晶化率增大.沉积薄膜的晶化率最大可达80;,表面粗糙度大约为30nm.通过对反应过程中的能量变化进行了分析,得到反应为放热反应,且非晶结构对沉积参数比较敏感.     

Voronoi polyhedra analysis of MD simulated silicate glasses

The relationship between the volume and the surface of Voronoi polyhedra (VP) appeared to be an effective tool for the characterization of the structure of MD simulated silicate glasses. This feature was demonstrated on the series of binary potassium-silicate glasses with the alkali content ranging from 5 to 20 mol%. Moreover, the temperature dependence of the slope of the above dependence, when expressed for various types of central atoms (Si, O and K in our case) was studied. Each type of central atom is characterised by its own iron line linearly relating the volume of VP to its properly powered surface, so that new geometrical constrains to the VP was found.     

Packing as a probe of structure in alkaline earth glass systems

Packing is an intrinsic property of glass, defined as the ratio of ionic volume to molar volume, and is a useful parameter for analyzing structural changes with composition. Alkali based glasses show two trends in packing, one dominated by the oxygen covalent network for the small ions, Li and Na, and one ionically dominated by the metal cations for the large, K, Rb and Cs cases [S. Giri, C. Gaebler, J. Helmus, M. Affatigato, S.A. Feller, J. Non-Cryst. Solids 347 (2004) 87]. We have found that alkaline earth glasses do not display these behaviors, and in this paper we determined the packing fractions of these glasses and compared them with the alkali case. Further, we considered the structural implications of the packing trends.     

VHF-PECVD制备微晶硅薄膜的微结构研究

用甚高频等离子体化学气相沉积(VHF-PECVD)法在玻璃衬底上低温制备了不同沉积时间微晶硅薄膜.用拉曼散射光谱仪、X射线衍射(XRD)、原子力显微镜(AFM)等表征手段对薄膜的微观结构进行了研究.研究结果表明:随着沉积时间的延长,薄膜呈岛状生长,薄膜晶粒度在微晶核形成后迅速升高并逐渐饱和;其微观结构经历了"非晶相→非晶/微晶混合相→微晶相"的演变过程.本实验制备的微薄膜仍以(111)为优化取向.     

The structural transformation and properties of spin-on poly(silsesquioxane) films by thermal curing

In this study, the structural transformation and properties of five commercially available poly(silsesquioxanes) by thermal curing were investigated, including poly(hydrogen silsesquioxanes) (HSQ and T12), and poly(methylsilsesquioxanes) (MSQ, T7 and T9). These materials with a different cage/network ratio and side groups (Si-H and Si-CH₃). The FTIR spectra show that the poly(silsesquioxane) films have different contents of the Si-O-Si cage and network structures, which significantly affects the refractive index and dielectric constant. The shifting of the Si-O-Si network band in the FTIR spectra can be correlated with their molecular structures. The refractive indices and dielectric constants of the studied poly(silsesquioxane) films increase with increasing the Si-O-Si network content. The retention of the Si-H or Si-CH₃ side group suggests the existence of the cage structures in the poly(silsesquioxane) films. The Si-O-Si cage structure results in a larger free volume than the Si-O-Si network structure in the poly(silsesquioxane) films and thus reduces the refractive index and dielectric constant. It is supported by the porosity result. The order of the refractive index in the studied poly(silsesquioxanes) films is T12>HSQ for the Si-H side group and T7>T9>MSQ with the Si-CH₃ side group, which can be correlated with the Si-O-Si network content. The poly(silsesquioxane) film with the Si-CH₃ side group has a lower refractive index than the Si-H side group at the same Si-O-Si network content, which is probably due to the steric hindrance effect of the CH₃ group.     

添加CaSO4·2H2O为晶种制备磷石膏半水硫酸钙晶须

以固体废弃物磷石膏为原料,在传统常压醇水热法的基础上添加CaSO₄·2H₂O为晶种制备半水硫酸钙晶须。采用单因素试验法探究了晶种含量、丙三醇含量和磷石膏质量分数对晶须结构和形貌的影响,确定晶须的最佳制备工艺条件。采用SEM和XRD对样品进行表征分析,实验结果表明:添加CaSO₄·2H₂O晶种制备晶须的长径比(49.29)比只添加丙三醇的样品的长径比(30.99)提高了近60%;当丙三醇与水的体积比(V)为1、晶种含量为1%、磷石膏质量分数为5%时制备的晶须的平均直径为0.65 μm,长径比达到了62.15,晶须的尺寸均匀。这说明添加1%CaSO₄·2H₂O晶种、V为1的丙三醇和质量分数为5%的磷石膏在常压下能制备出高长径比和尺寸均匀的半水硫酸钙晶须。     

Kovacs effect in PMMA observed by low-frequency Raman scattering (boson peak)

The physical aging of the poly(methyl methacrylate) glass (PMMA) is described by its effects on the refractive index, that reflects the change of mean specific volume, and, on the other hand, on the low-frequency Raman scattering, i.e., on the boson peak. The boson peak depends mainly on the cohesion fluctuations. The memory or so-called Kovacs effect is observed by the appearance of a minimum of refractive index (i.e. a maximum of volume) as a function of the aging time at a higher temperature subsequent to an aging at lower temperature. The minimum of refractive index corresponds to a maximum of the boson peak intensity. However, the cohesion is not directly related to the volume, so that the evolution of the refractive index does not mimic exactly that of the boson peak intensity. Information on the change of cohesion by aging is obtained by enthalpy measurement. The obtained experimental results are discussed in the frame of the heterogeneous cohesion or elasticity at the nanometric scale. This clarifies the phenomenon of physical aging and the consequent Kovacs effect.     

Cystamine-incorporated gelatin microsphere and its redox-responsive release property

Reduction-responsive cystamine-incorporated gelatin microspheres were prepared by an emulsification method. On SEM micrograph, the microsphere, prepared at pH 9.0 and at the carboxyl/amino group molar ratio of 1:1, was sphere-like and its diameter was a few to 100 µm. The gelatin to cystamine ratio of the microsphere was about 1:0.2 (w/w), determined by energy dispersive X-ray spectroscopy. Two endothermic peaks were observed around 92°C and 126°C, which were thought to be the melting point of gelatin-rich phase and that of cystamine-rich phase, respectively. The microsphere released its payload (FITC-dextran) in dithiothreitol (a reducing agent) concentration-dependent manner.     

Electrical characterization of ion conducting biopolymeric gel complexes

Gum Arabica is a naturally occurring conducting biomaterial biopolymer, its various aspects of electrical and structural characteristics have been investigated in our earlier works. In the present work the ionic gel formation of Gum Arabica and its electro-chemical application were experimentally investigated. Hot concentrated aqueous solution of Gum Arabica with phosphoric acid, minimum 16% of solute, was found to form ionic hydrogel on slow cooling. It consists of polyelectrolyte molecules cross-linked by phosphate ions by chemical bonds into an integrated spatial network in water solvent. The increase in surface to volume ratio shows a gel collapse to provide transparent solid material. Gel formation of Gum Arabica was also studied with chromium and molybdenum oxide as cross-linking agent. The various studies carried out on the mentioned materials to investigate its structural and electrical characteristics are XRD, DSC, SEM and impedance spectroscopy. The said gel was found to provide a good electro-chemical cell with suitable redox pair.     

Evolution of hierarchical‐structured CaCO3 in binary mixed solvent

Calcium carbonate with hierarchical structure was synthesized in water/organic compound binary soluvent by a chemical solution process within CaCl₂/NaCO₃ reaction system. Acetone, isopropanol, glycol, tetrahydrofuran were selected as the organic compound. Evolution of the hierarchical structure of CaCO₃ was investigated. The as‐prepared products were characterized by X‐ray diffraction (XRD) and scanning electron microscopy (SEM). CaCO₃ aggregations with spicate hierarchical structure were obtained with a high volume fraction of the organic solvent. Aspect ratio of the hierarchical structure increases to the highest when the volume fraction was 50%. Solvent with low dielectric constant was conducive to the oriented aggregation of the CaCO₃ grains.