A METHOD OF PREPARING SPHERICAL NANO-CRYSTAL CELLULOSE WITH MIXED CRYSTALLINE FORMS OF CELLULOSE Ⅰ AND Ⅱ

A new kind of nano-crysta cellulose (NCC) prepared from natural cotton fiber has been obtained by the method ofacid hydrolysis. Compared to most other nanophase materials that derive from inorganic materials, our products are preparedfrom natural cotton fibers. The products are of spherical shape with mixed crystal forms of cellulose I and II. The preparationconditions determine the properties of the products. Prior treatment is a critical procedure. The properties of the products arealso strongly affected by such conditions as the kinds of acids used, the ratio of the acid mixture, the acid concentration, theultrasonic agitation time and hydrolysis temperature. The number average molecular weight of NCC is determined by gelpermeation chromatography (GPC). The particle size and shape were determined by transmission electron microscopy(TEM). X-ray diffraction was used to detect the crystallinity and average crystallite size of the panicle.

Approach to lattice-related/content-specific spectral ranges of near-infrared diffuse reflectance spectroscopy of cefazolin sodium and the construction of a quantitative model for the determination of cefazolin sodium content in different crystal forms

Cefazolin sodium can form both α- and β-form crystals. It also can form dehydrated crystalline and amorphous products through different production processes. Because different polymorphic medicines usually have different physical and chemical properties, it is critical to emphasize the crystallization control of polymorphic medicines. Near-infrared （NIR） analysis, which incorporates a combination of NIR spectroscopic techniques and multivariate chemometric methods, is considered a powerful tool for the determination of the crystallinity of polymorphic drugs. The selection of optimal spectral ranges that correlate with the lattice specificity and content specificity is crucial to obtaining a specific NIR model. In the present work, near-infrared （NIR） spectra of cefazolin sodium with different crystal forms created through different processes were studied. The results suggest that wavelengths within the range of 9102.7-8597.5 cm-1 is related to the specificity of the cefazolin sodium crystal lattice and that the range of 6001.6-5496.4 cm i is associated with the quantitative content of cefazolin sodium. The two ab- sorptions are caused by the second overtone of the C-H stretching band （3nC-H） and the first overtone of C-H stretching band （2uC-H）, respectively. Using these results, we established a suitable method of constructing a universal quantitative model by using mixed samples in different crystal forms as a calibration set, selecting a content-specific range （6001.6-5496.4 cm-l）, and adding lattice-related spectral ranges where appropriate. This may provide a framework for the construction of prediction models for polymorphic medicines.

Crystal Form Transition during Heating of Solvent-induced Crystalline Syndiotactic Polystyrene

The phase transition of two kinds of solvent-induced crystalline syndiotactic polystyrene (sPS). gamma-sPS and delta(c)-sPS, has been studied via WAXD and DSC. gamma-sPS transform to a-sPS at 195-225 degrees C before melt during heating, whereas delta(e)-sPS transform to first gamma-sPS and then a-sPS at 100-200 degrees C and 200-215 degrees C, respectively. The transition of delta(e)-gamma and gamma-a occurs for below melting point of sPS indicates they are all solid-solid transition.

ANNEALING INDUCED VARIATION OF CRYSTALLINE STRUCTURE AND MECHANICAL PROPERTIES OF SYNDIOTACTIC POLYPROPYLENE FIBERS

Syndiotactic polypropylene （sPP） as-spun fiber （sPP1） and drawn fiber （sPP2） were prepared by melt-spinning and melt-spinning/hot-drawing, respectively. The structure transition of the two fibers induced by annealing at different temperatures and the corresponding mechanical properties were subsequently investigated by the combination of Fourier transform infrared spectroscopy （FTIR）, wide-angle X-ray diffraction （WAXD） and tensile testing. The results indicate that the chain conformation and crystal forms of the two sPP fibers are not obviously changed at low annealing temperature （40℃）. With increasing the annealing temperature, the trans-planar conformation and mesophase in sPP1 and sPP2 fibers can be completely transformed to helical conformation and crystal form I under tension. Upon removing the tension, a small amount of mesophase and trans-planar conformation will be regained. The mechanical properties of the annealed fibers are manifestly dependent on their initial structure and the annealing temperature.

MELTING BEHAVIOR OF LOW ETHYLENE CONTENT POLYPROPYLENE COPOLYMERS WITH AND WITHOUT NUCLEATING AGENTS

The melting behavior of polypropylene (PP) and low ethylene content polypropylenecopolymer with and without nucleating agent samples crystallized under both isothermal and non-isothermal conditions were studied by Differential Scanning Calorimeter (DSC) and X-raydiffraction. Multiple melting behavior were observed depending on the existence of nucleatingagent and crystallization conditions. The observed phenomena have been discussed by the effect ofnucleating agent on perfection of crystal and the melting and recrystallization of imperfect crystalto a more perfect crystal during the heating process of samples.

Morphology of single inhalable particle in the air polluted city of Shijiazhuang,China

In the typical air polluted city of Shijiazhuang, single inhalable particle samples in non-heating period, heating period, dust storm days, and snowy days were collected and detected by SEM/EDS （scanning electron microscopy and energy dispersive X-ray spectrometry）. The particle morphology was characterized by the 6 shape clusters, which are： irregular square, agglomerate, sphere, floccule, column or stick, and unknown, by quantitative order. The irregular square particles are common in all kinds of samples; sphere particles are more, and column or stick are less in winter samples; in the wet deposit samples, agglomerate and floccule particles are not found. The surface of most particles is coarse with fractal edge, which can provide suitable chemical reaction bed in the polluted atmospheric environment. New formed calcium crystal is found to demonstrate the existence of neutralized reaction, explaining the reason for the high SO2 emission and low acid rain frequency in Shijiazhuang. The three sorts of surface patterns of spheres are smooth, semi-smooth, and coarse, corresponding to the element of Si-dominant, Si-Al-dominant, and Fe-dominant, The soot particle is present as floccule with average size around 10 μm, considerably larger than the former reported results, but wrapped or captured with other fine particles to make its appearance unique and enhance its toxicity potentially. The new formed calcium crystal, the 3 sorts of sphere surface patterns, and the unique soot appearance represent the single inhalable particle＇s morphology characteristics in Shijiazhuang City.

Solid-to-molecular-orientational-hexatic melting induced by local environment determined defect proliferations

Two-dimensional(2D)melting is a fundamental research topic in condensed matter physics,which can also provide guidance on fabricating new functional materials.Nevertheless,our understanding of 2D melting is still far from being complete due to existence of possible complicate transition mechanisms and absence of effective analysis methods.Here,using Monte Carlo simulations,we investigate 2D melting of 60°rhombs which melt from two different surface-fullycoverable crystals,a complex hexagonal crystal(cHX)whose primitive cell contains three rhombs,and a simple rhombic crystal(RB)whose primitive cell contains one rhomb.The melting of both crystals shows a sequence of solid,hexatic in molecular orientation(Hmo),and isotropic phases which obey the Berezinskii-Kosterlitz-Thouless-Halperin-Nelson-Young(BKTHNY)theory.However,local polymorphic configuration(LPC)based analysis reveals different melting mechanisms:the cHX-Hmotransition is driven by the proliferation of point-like defects during which defect-associated LPCs are generated sequentially,whereas the RB-Hmotransition is driven by line defects where defect-associated LPCs are generated simultaneously.These differences result in the observed different solid-Hmotransition points which areφA=0.812 for the cHX-HmoandφA=0.828 for the RB-Hmo.Our work will shed light on the initial-crystal-dependence of 2D melting behavior.

THE PREPARATION AND STUDY ON THE NANO-TiO2/SILK FIBROIN COMPOSITE FILMS BY THE SOL-GEL METHOD

Based on the sol-gel technique using butyl titanate as oxide precursor, the regenerated SF （silk fibroin）/nano-TiO2 composite films were synthesized. Different amounts of butyl titanate to SF were used to verify this effect on the characteristics of the formed materials. Samples were characterized by thermogravimetric analysis, X-ray diffractometry, UV, AFM and FT-IR spectroscopy. The experimental results reveal that, compared to the pure silk fibroin films, the mechanical strength of these regenerated SF/nano-TiO2 composite films were increased and the dissolubility in water of SF/nano-TiO2 composite films in aqueous solution were decreased. The diameter of nano-TiO2 particle films was about 80nm through UV and AFM. The nano-TiO2 particles were well dispersed in the regenerated silk fibroin. It was found that the crystal structures of the composite films were transited from typical Silk I to typical Silk H by the XRD and FTIR. Furthermore, the crystallinity of the composite films was obviously improved. Through the TGA, it was demonstrated that the heat transition temperature of composite films was also enhanced.

Recycling of waste residue in aluminum production process

The preparation of crystal form of Al（OH）3 from the deposited residues of anodizing lines in the process of producing aluminum was studied. Alkali is used to dissolve the residue, and then blow CO2 is bellowed in, finally a kind of useful crystal Al（OH）3 is accessed by hydrolysis. The yield of the crystal Al（OH）3 was affected by temperature, pH and flow rate of CO2. The experimental results showed that under constant stirring, the optimized conditions was to control the temperature of 75-85℃, pH 7.5-9.0, CO/flow rate 60-80 mL/min. Using this method, the purpose of recovering valuable resources of Al, cleaning up the environment, and recycling of the by-product of Na2CO3 was achieved. It was of good economic and social benefits.

Preparation, Crystal Structure and Properties of a New Crystal Form of Diammonium 5,5＇-bistetrazole-1,1＇-diolate

A new crystal form of diammonium 5,5＇-bistetrazole-1,1＇-diolate （1） was prepared by two novel methods and fully characterized by using IR, NMR spectroscopy, elementary analysis, single crystal X-ray crystallography and thermal gravity/differential thermal analysis （TG/DTA）. Crystalline 1 was found as monoclinic and space group of P21/c （14）. The TG/DTA analysis showed that the decomposition temperature of 1 was 287.8℃ with a mass loss of 91.2% in the range of 220-300℃ at a heating rate of 5℃/min. The sensitivities test towards impact, friction of 1 indicated that 1 has much lower sensitivities than those of RDX/HMX and is comparable to those of TNT, which suggested that 1 could be used as a good candidate of new insensitive energetic compound.

A new equilibrium form of zircon crystal

The surface tensions of the {100}, {110}, {101} and {211} faces are calculated by using Machenzie's method. A new equilibrium form of zircon crystal is then derived on the basis of Wulf's Law. This theoretic form consists of {100} prismatic faces and {211} pyramidal faces, which is different from that of the prediction by the periodic bond chain theory. The discovery of the equilibrium form of zircon crystal provides a clue for understanding of the morphology of zircon crystals formed in deep magma chamber, indicating that zircon morphology is an indicator of crystallization conditions.

EFFECT OF VACUUM ON THE CRYSTAL FORM AND MORPHOLOGY OF THE EVAPORATED FILM OF COPPER PHTHALOCYANINE

In a previous paper, we have reported the relationship between the crystallite orientation of the evaporated film of copper phthalacyanine （PcCu） （α-form） and the incident angle of molecular beam at 10-5 torr. In this paper, we shall show some research results about vacuum effects on the crystal forms and the morphology of the evaporat-

Direct TEM Observation of Phase Separation and Crystallization in Cu_(45)Zr_(45)Ag_(10)Metallic Glass

The structural evolution of Cu_（45）Zr_（45）Ag_（10） metallic glass was investigated by in situ transmission electron microscopy heating experiments. The relationship between phase separation and crystallization was elucidated. Nucleation and growth-controlled nanoscale phase separation at early stage were seen to impede nanocrystallization, while a coarser phase separation via aggregation of Ag-rich nanospheres was found to promote the precipitation of Cu-rich nanocrystals.Coupling of composition and dynamics heterogeneities was supposed to play a key role during phase separation preceding crystallization.

Equilibrium Crystallization Temperature of Syndiotactic Polystyrene γ Form

The crystallization behavior of syndiotactic polystyrene（s PS） γ form undergoing annealing at various temperatures was investigated using the thermodynamic phase diagram based on Strobl＇s crystallization theory. On the basis of the differential scanning calorimetric results, it was observed that γ form melt-recrystallization occurred at a higher temperature with the increasing lamellar thickness, which resulted from the pre-annealing at the elevating temperature after acetone induced crystallization. Further temperature dependent small-angle X-ray scattering（SAXS） measurement revealed the evolution of the γ form lamellae upon heating until phase transition, involving three different regimes： lamellae stable region（25-90 °C）, melt-recrystallization region（90-185 °C） and pre-phase transition region（185-195 °C）. As a result, recrystallization line, equilibrium recrystallization line and melting line were developed for the s PS γ form crystallization process. Since the melt of γ form involved a γ-to-α/β form phase transition, the melting line was also denoted as the phase transition line in this special case. Therefore, the equilibrium crystallization temperature and melting（phase transition） temperatures were determined at around 390 and 220 °C on the basis of the thermodynamic phase diagram of the s PS γ form.

Developments of New Sheet Metal Forming Technology and Theory in China

Developments of new sheet metal forming technology and theory in China are reviewed in detail in this paper.Advances of crystal plasticity on the deformation mechanism of Mg alloy are firstly described, especially its applications on the prediction of sheet forming process. Then, a new macroscopic constitutive model is introduced, which possesses an enhanced description capacity of tension/compression anisotropy and anisotropic hardening. In order to take into account the twinning process of hexagonal close-packed material, a modified hierarchical multi-scale model is also established with adequate accuracy in a shorter computational time. The advanced forming limit of sheet metal, mainly about aluminum alloy, is also investigated. Besides the above theory developments, some new sheet metal forming technologies are reviewed simultaneously. The warm forming technology of Mg alloy is discussed. New processes to form sheet parts and to bend tubes are proposed by using hard granules. On the other hand, a new kind of ultra-high-strength steel based on typical22 Mn B5 by introducing more residual austenite and Cu-rich phase to increase the elongation and strength and its novel forming method that integrates hot stamping and quenching participation are proposed. Progresses in sheet hydroforming,press forging and electromagnetic forming of sheet metal parts are also summarized.