Investigation of Temperature Dependency of Morphological Properties of Thermoplastic Polyurethane using WAXS and SAXS Monitoring

Polyether and polyether/ester based TPU （thermoplastic polyurethanes） were investigated with wide-angle XRD （X-ray diffraction） and SAXS （small angle X-ray scattering）. Furthermore, SAXS measurements were performed in the temperature range of 30 ℃ to 130 ℃. Polyether based polymers exhibit only one broad diffraction signal in a region of 2 θ 15° to 25°. In case of polyurethanes with ether/ester modification, the broad diffraction signal arises with small sharp diffraction signals. SAXS measurements of polymers reveal the size and shape of the crystalline zones of the polymer. Between 30 ℃ and 130 ℃ the size of the crystalline zone changes significantly. The size decreases in most of investigated TPU. In the case of Desmopan 9365D an increase of the particle size was observed.

Synthesis and characterization of pure mesoporous zirconia thin film with two-dimensional hexagonal framework

Pure mesoporous ZrO2 thin film with two-dimensional hexagonal framework mesostructure has been successfully prepared by using a nonionic triblock copolymer as the structure-directing agent and ZrCl4 as the zireonia source through evaporation-induced self-assembly approach. The resulting materials were characterized by X-ray diffraction, scanning electron microscope, and nitrogen adsorption ,neasurenlents. The obtained mesoporous ZrO2 thin film has a nanocrystalline inorganic framework （tetragonal zirconia） and narrowly distributed mcsopore size （6. 7 nm in diameter].

WAXD and FTIR Studies of Electron Beam Irradiated Biodegradable Polymers

Poly（L-lactic acid） （PLLA） and poly（e-caprolactone） （PCL） have been receiving much attention lately due to their biodegradability in human body as well as in the soil, also due to their biocompatibility, environmentally friendly characteristics and non-toxicity. Morphology of biodegradable polymers affects the rate of their biodegradation. A polymer that has high degree of crystallinity will degrade at a slower rate due to the inherent increased stability. PCL homopolymer crosslinking degree increases with increasing doses of high energy radiation. On the other hand, the irradiation ofPLLA homopolymer promotes mainly chain-scissions at doses below 250 kGy. In the present work, twin screw extruded films of PLLA and PCL biodegradable homopolymers and 50：50 （w：w） blend were electron beam irradiated using electron beam accelerator Dynamitron （E = 1.5 MeV） from Radiation Dynamics, Inc. at doses in the range of 50 kGy to 103 kGy in order to evaluate the effect of electron beam radiation. Wide-angle X-ray diffraction （WAXD） patterns of non irradiated and irradiated samples were obtained using a diffractometer Rigaku Denki Co. Ltd., Multiflex model; and Fourier transform infrared spectroscopy （FTIR） spectra was obtained using a NICOLET 4700, attenuated total reflectance （ATR） technique. By WAXD patterns of as extruded non irradiated and irradiated PLLA it was verified broad diffusion peaks corresponding to amorphous polymer. There was a slight increase of the mean crystallite size of PCL homopolymer with increasing radiation dose. PCL crystalline index （CI） decreased with radiation dose above 500 kGy. But then, PLLA CI increased with radiation dose above 750 kGy. From another point of view, PLLA presence on the 50：50 blend did not interfere on the observed mean crystallite size increase up to 250 kGy. From 500 kGy to 103 kGy the crystallite size of PCL was a little bigger in the blend than the homopolymer. In contrast, FTIR results have shown that this technique was not sensitive enough to observe the degradation promoted by ionizing radiation of the studied homopolymers and blends, and neither on the miscibility of the blends.

晶面角自动测量中的数据处理

介绍了一种对X射线衍射峰信号进行自动判别峰位的数据处理方法。此方法用于定向仪的自动测控系统,在对人造石英单晶切片的晶面角进行测量时,得到比较令人满意的结果。

Preparation and Structure of Poly(ethylene-co-vinylacetate)/Montmorillonite Nanocomposites

Poly(ethylene-co-vinylacetate)/sodium montmorillonite(EVA/MMT)and Poly(ethylene-co-vinylacetate)/organophilic montmorillonite(EVA/o-MMT)nanocomposite were prepared by solid-state mixing.The morphology and structure of the composites were explored by scanning electron microscopy(SEM),wide-angle X-ray diffraction(WAXD),differential scanning calorimetry(DSC),and dynamic mechanical analysis(DMA).The results showed that the intercalated nanocomposite was successfully synthesized for EVA/o-MMT system,while in the EVA/MMT nanocomposite,MMT were poorly dispersed in the order of μm.An unexpected rubbery plateau modulus of EVA/o-MMT nanocomposite above melting point of EVA was explored by DMA.The possible origins of this high-temperature modulus were analyzed.

The Preparation and Characterization of Vermiculite Hydrosol

The dispersibility of vermiculite is the key factor that affects the application of vermiculite.In this paper,the milled natural vermiculite was pillared by organic quaternary ammonium salts.Then the pillared vermiculite was ground and homogenized under the existence of dispersive agent to form a stable vermiculite hydrosol system.Small angle X-ray diffraction(SA-XRD),fourier transform infrared spectroscopy(FTIR),and thermogravimetric analyses(TGA)were used to characterize the structure and thermal property of the vermiculite.The results indicate that the exfoliated vermiculite is successfully obtained.The analyses of laser particle size analyzer,transmission electron microscope(TEM),and Tyndall phenomenon analyzer demonstrate that the vermiculite hydrosol prepared is a stable hydrosol system.

Mechanical and thermal properties of mesogen-jacketed liquid crystalline polymer/epoxy resin composites

The effects of mesogen-jacketed liquid crystalline polymer poly(dipropyl vinylterephthalate)(PDPVT) on the mechanical and thermal properties of diglycidyl ether of bisphenol-A(DGEBA) epoxy resin were investigated by impact test, tensile test and thermogravimetric analysis(TGA). The mechanism underlying the enhancement of mechanical properties of epoxy resin was studied using 1D wide-angle X-ray diffraction(WAXD) and scanning electron microscope(SEM). It was found that the mechanical properties of 1 wt%–5 wt% PDPVT/DGEBA composites were significantly improved compared to neat epoxy resin. Especially, the epoxy resin with 3 wt% PDPVT had the greatest increase in mechanical properties, with the impact strength, tensile strength and elongation while breaking increased by 87%, 59% and 174%, respectively. The increased mechanical strength was due to the fact that PDPVT maintained liquid crystalline phase in cured PDPVT/DGEBA composites, which would blunt the crack tip and prevent crack propagation. Moreover, PDPVT had slight effect on the thermal stability properties of epoxy resin.

Physio-and chemo-dual crosslinking toward thermoand photo-response of azobenzene-containing liquid crystalline polyester

Combining the stability of chemical crosslinking and the processability of physical crosslinking is a well-established strategy to design new materials with desirable stimuli–responsive properties. Herein, a series of azobenzenebased thermotropic liquid crystalline polyesters were synthesized by introducing mesogenic dial named 4,4＇-bis（6-hydroxyhexyloxy）azobenzene（BHHAB）, 2-phenylsuccinic acid（PSA）, and different contents of 1,2,3-propanetricarboxylic acid（PTA） as the chemical crosslinker. All these polyesters showed good thermal stability and smectic liquid crystalline phase. Wide-angel X-ray diffraction（WAXD） and the fluorescence emission spectra confirmed the existence of π–πstacking interactions as the physical crosslinking in the polymer chains, particularly at the lower content of PTA. However, when the PTA content increased, the chemical crosslinking changed the chain conformation, and thus the intensity of physical crosslinking slackened gradually. Combining the physical and chemical crosslinking, these polyesters showed the thermoplastic processability, thermal shape memory, heat-assisted healing and photoresponsive behaviors. Taking advantages of these features, these multiple stimuli–responsive polymers can bring more chances for smart materials such as soft actuator.

Shape-stabilized phase change materials with high phase change enthalpy based on synthetic comb-like poly(acrylonitrile-co-ethylene glycol)for thermal management

Shape-stabilized poly（acrylonitrile-co-ethylene glycol） （PANEG） copolymer with comb-like structure was prepared via simple free-radical solution polymerization, where acrylic acid poly（ethylene glycol） methyl ether ester （MPEGA） and acrylonitrile （AN） were employed as monomers. Fourier transform infrared spectroscopy （FTIR）, 1H and 13C nuclear magnetic resonance spectroscopy （1H and 13C NMR）, wide-angle X-ray diffraction （WXAD） were used to characterize the chemical structure of resultant PANEG. In addition, the influences of MPEGA contents on energy storage performance, thermal reliability and thermal stability of PANEG materials were evaluated based on differential scanning calorimetry （DSC）, polarizing optical microscopy （POM）, thermal infrared imager and thermogravimetry analyzer （TG）. The comb-like PANEG demonstrated a favorable temperature regulation performance and thermal reliability. With the increase of MPEGA contents, the enthalpy of PANEG increased, and when the content of MPEGA was 80 wt%, the phase change enthalpy of synthesized PANEG-80 reached to 106.70 J/g with a stable heat storage performance after 100 thermal cycling. Thermal infrared images and cooling curves revealed that synthetic PANEG could sustain a temperature in ranges of 22-31 ℃ for continuous 25 min, presenting excellent temperature regulation performance. Also, comb-like PANEG could be uniformly dissolved in dimethyl sulfoxide （DMSO）, indicating that PANEG phase change fibers with potential applications in fields of intelligent thermoregulating textile and heat energy management could be obtained via one-step wet spinning.

The thermodynamic properties of flow-induced precursor of polyethylene

Flow-induced preordering or precursor(FIP) has been studied in a series of lightly cross-linked high-density polyethylene with a combination of extensional rheology and in situ synchrotron radiation small-angle X-ray scattering(SAXS) and wide-angle X-ray diffraction(WAXD) measurements. Based on the incipient strains of SAXS and WAXD signals during extension in a large temperature range, strain-temperature diagrams for flow-induced preordering and nucleation were constructed and revealed that flow-induced crystallization(FIC) undergoes two stages: melt-precursor transition(MPT) and precursor-nuclei transition(PNT). At different temperatures, FIP with different inner structures and morphologies can be induced by strain; these embryos have shape and structure that are related to those of the corresponding critical nuclei. With the strain-temperature diagrams, the thermodynamic properties of FIP are deduced, which shows that compared with the relative nuclei the FIP always has a lower bulk free energy(?H) and a much lower surface free energy(?e). In extreme cases(high temperature), the ?e of FIP can be negligible. The quantitative estimation of the thermodynamic parameters suggests the existence of variant FIPs, which plays a vital role for the subsequent progress of PNT and the whole process of FIC.

Multi-responsive red solid emitter: Detection of trace water and sense of relative humidity

A multi-responsive D-A type compound(CYQ)based on pyrone and triphenylamine was designed and successfully synthesized. The target compound exhibited distinct aggregation-enhanced emission(AEE) effect.Solvatochromic experiment and density functional theory(DFT) indicated CYQ possessed excellent intramolecular charge transfer(ICT) ability. Besides, its mechanofluorochromic property(MFC) was found with a 37 nm redshift. Powder wide-angle X-ray diffraction(PXRD) and differential scanning calorimetry(DSC) measurements were performed to demonstrate the transformation from the crystalline to amorphous states upon grinding. Surprisingly,CYQ displayed a hypersensitive response to trace water in organic solvents with an excellent detection limit as low as 0.0096% in tetrahydrofuran(THF). Furthermore, it was found that the fluorescent intensity of CYQ declined progressively upon humidity rise, and its color change can be witnessed by naked eyes. Therefore, the relative humidity(RH) sensing strategy guarantees the AIEgen to become a colorimetric sensor under various conditions.