Structure and thermal stability of novel fluorophosphate glasses

A systematic investigation on glass formation in the PbF2-InF3-BaHPO4 ternary system has been carried out. These glasses have characterized by IR spectra, Raman spectra and differential thermal analysis. The results show that the structure of these glasses is mainly affected by BaHPO4 and InF3 contents. With decreasing BaHPO4 content, the glass structure gradually transforms from metaphosphate to polyphosphate. When InF3 content is low, it mainly acts as network modifier, when its content is high; it enters glass matrix and forms In(O,F)(6) groups connecting the polymerized phosphorus oxygen species. PbF2 mainly acts as network modifier in this system. Systematic variations of the glass transition temperature and the thermal stability index agree well with these results. The most stable glass with Delta T = 230 degrees C and S = 21.79 K is obtained. (c) 2004 Elsevier B.V. All rights reserved.

Physical and thermal properties of P2O5-Al2O3-BaO-La2O3 glasses

The physical and thermal properties Of P2O5-Al2O3-BaO-La2O3 glasses were investigated. The effects of glass compositions on the transition temperature, thermal expansion coefficient, density, hardness and refractive index of glasses were studied. The highest hardness of the glasses is 4143.891 MPa and the lowest thermal expansion coefficient of the glasses is 71.770 x 10(-7)/° C. A phosphate glass with high mechanical strength and good thermal characteristic is obtained.

The spectroscopic properties of Er3(+)-doped TeO2-Nb2O5 glasses with high mechanical strength performance

(100 - x)TeO2 - xNb(2)O(5) (x=5-20) mobic tellurite glasses doped with 0.5 mol.% Er2O3 were synthesized, and their thermal, mechanical, and spectroscopic properties were measured and compared to the properties of the typical 75TeO(2)-20ZnO-5Na(2)O (TZN) tellurite glass. The refractive index (n(d)), density (p), and glass transition temperature (T-g) of bulk glasses increase with the Nb2O5 content. The Vickers microhardness (H-v) of bulk glass in niobic tellurite glasses also increases with the Nb2O5 content. The values (2.5-3.2 GPa) of H, in the niobic tellurite glasses are 47-88% larger than that (1.7 GPa) in TZN glass. The effect of Nb2O5 content on absorption spectra, the Judd-Ofelt parameters Omega(t) (t = 2, 4, 6), fluorescence spectra and the lifetimes of Er3+ :I-13/2 level were also investigated, and the stimulated emission crosssection was calculated from McCumber theory. With increasing Nb2O5 content in the glass composition, the Omega(t) (t = 2, 4, 6) parameters, fluorescence full width at half maximum (FWHM) Of I-13/2 of Er3+ increase, while the I-4(13/2) lifetimes of Er3+ decreases. Compared with TZN glass, the gain bandwidth properties of Er3+-doped TeO2-Nb2O5 glass is much larger than in tellurite glass based TeO2-ZnO-Na2O system, bismush-based glass, germanate, and silicate glasses, which indicates that TeO2-Nb2O5 glasses are better choice as a practical available host material for broadband Er3+-doped amplifier. (c) 2005 Elsevier B.V. All rights reserved.

Spectral properties and stability of Er3+-doped TeO2-WO3 glass

Er3+-doped TeO2-WO3 glass was fabricated and characterized by absorption spectrum, fluorescence spectrum, Raman spectrum and stability. The Judd-Ofelt parameter ohm(t)(t = 2, 4, 6) were calculated from the absorption spectrum by the Judd-Ofelt theory. The fluorescence spectrum indicates that the fluorescence width at half-maximum (FWHM) is 66nm. The stimulated emission cross-section of Er3+ in TeO2-WO3 glass at 1532 nm was calculated to be 0.80 x 10(-20) cm(2) by McCumber theory. The phonon energy of TeO2-WO3 glass is found to be 931 cm(-1). The difference between crystallization onset temperature and glass transition temperature Delta T is 112 degrees C. These results show that Er3+-doped TeO2-WO3 glass has higher stability and good spectral properties, which were useful for broadband amplifier. (c) 2005 Elsevier B.V. All rights reserved.

Spectroscopic properties and thermal stability of Er3+-doped tungsten-tellurite glass for waveguide amplifier application

Tungsten-tellurite glass with molar composition of 60TeO(2)-30WO(3)-10Na(2)O has been investigated for developing planar broadband waveguide amplifier application. Spectroscopic properties and thermal stability of Er3+-doped tungsten-tellurite glass have been discussed. The results show that the introduction Of WO3 increases significantly the glass transition temperature and the maximum phonon energy. Er3+-doped tungsten-tellurite glass exhibits high glass transition temperature (377 degrees C), large emission cross-section (0.91 x 10(-20) cm(2)) at 1532 nm and broad full width at half maximum (FWHM), which make it preferable for broadband Er3+-doped waveguide amplifier application. (c) 2005 Elsevier B.V. All rights reserved.

Effect of lithium-sodium mixed-alkali on phase transformation kinetics in Er3+/Yb3+ co-doped aluminophosphate glasses

Er3+ doped aluminophosphate glasses with various Na2O/Li2O ratios were prepared at 1250 degrees C using a silica crucible to study mixed alkali effect (MAE). The effect of relative alkali content on glass transition temperature, crystallization temperature and thermal stability were investigated using differential scanning calorimetry (DSC). In addition, apparent activation energies for crystallization, E, were determined employing the Kissinger equation. The effect of Al2O3 content on the magnitude of MAE was also discussed. No mixed-alkali effect is observed on crystallization temperature. (c) 2006 Elsevier B.V. All rights reserved.

利用DSC和EPR技术研究杜仲种子的贮藏条件

种子贮藏稳定性对于种质资源的长期保存具有重要意义，目前关于种子贮藏的最新理论为玻璃态理论，该理论认为种子的玻璃化有利于种子的长期贮藏。当种子处于玻璃态时，玻璃化物质的高度粘滞性降低了种子细胞内分子流动性，阻止了细胞质中分子的扩散，从而减少老化过程中细胞结构的损伤和化学组分的变化，延缓种子老化劣变反应速率，延长贮藏寿命。评价玻璃态的一个重要指标是玻璃化转变温度，当种子贮藏于玻璃化温度或以下10℃～30℃范围内时，种子具有最佳的贮藏稳定性。因此，检测种子的玻璃化转变温度对于种子的长期有效贮藏具有重要指导意义。 本研究将差示量热扫描技术（DSC）与电子顺磁共振波谱仪技术（EPR）应用于杜仲种子玻璃化转变温度方面的研究。在DSC方法中，选用4.4%～31.6%含水量范围的杜仲种胚分别进行了DSC图谱扫描。EPR方法选用3-羧基-2,2,5,5-四甲基吡咯烷-1-氧（3-carboxy-2,2,5,5-tetramethylpyrrolidine-1-oxyl，CP）和2,2,6,6-四甲基哌啶（4-hydroxy-2,2,6,6-tetramethyl-1-piperidinyloxy，TEMPO）作为探针标记杜仲种胚， 利用EPR技术测定不同含水量杜仲种胚的分子运动，通过对EPR图谱参数的分析计算，最终确定不同含水量杜仲种胚的玻璃化转变温度。 DSC实验结果显示，含水量为22.3%、28.0%、31.6%的杜仲种胚在0℃ 左右出现了一个水的熔融峰。该熔融峰的面积代表了自由水含量的多少，随着种胚含水量的降低该熔融峰面积减小。4.4%～31.6%含水量范围的杜仲种胚在-28℃左右还出现了一个熔融峰，推测此峰为杜仲种胚中某类物质熔融所形成的熔融峰。然而在此曲线上我们未观察到标志玻璃化转变的“台阶”出现。 CP-EPR实验的结果表明，利用EPR测定得到含水量为4.4%～11.6%的杜仲种胚在-110℃～20℃温度范围内，同一含水量的杜仲种胚随着温度的升高，分子运动速率加快;在同一温度条件下，高含水量的种胚比低含水量种胚的分子运动速率快。通过CP-EPR波谱两外缘峰最大距离（2Azz）的测定和数据统计分析，得到含水量为4.4%、5.7%、8.6%、10.3%、11.6%杜仲种胚的玻璃化转变温度分别约为44℃、25℃、4℃、-31℃、-43℃。可以把测定的杜仲种胚的这几个含水量的玻璃化转变温度与杜仲种子贮藏相结合，用于指导杜仲种子的贮藏。 TEMPO-EPR实验测定分析得到含水量为2.1%、3.4%、4.8%、8.3%、11.2% 的杜仲种胚的玻璃化转变温度分别为-21℃、-18℃、-24℃、-20℃、-27℃，玻璃化转变温度随含水量升高其变化的规律不明显，这与CP-EPR实验测得的结果有着较明显的差别。通过分析，认为对于脂质含量较高的杜仲种胚，随着含水量的降低，作为标记化合物的TEMPO随着脱水进入脂相，从而不能真实反映出不同含水量种胚的分子运动情况。与TEMPO标记相比，CP标记可能能够更真实地反映不同含水量杜仲种胚细胞质分子运动的情况，根据其分子运动情况得到的玻璃化转变温度更准确。

Nonlinear optical properties and thermal stability of the poled polymer NTAB/PEK-c

Films of high glass' transition temperature polymer polyetherketone doped with chromophore 2,2'[4-[(5-nitro-2-thiazolyl)azophenyl]-amino]-bisethanol NTAB) were prepared, poled by the corona-onset poling setup which includes a grid voltage making the surface-charge distribution uniform at elevated temperature. The thickness of the films was measured by the Model 2010 Prism Coupler system. Second harmonic generation d(33) was measured by the second harmonic generation method, and the d33 is 38.12 pm/V at 1064 nm under the absorption correction. The nonlinear optical activity maintains is 80% of its initial value. (C) 2002 Elsevier Science B.V. All rights reserved.

Dielectric relaxation of poled polymer DCNP/PMMA

We have prepared the polymer thin films of a 3-(1,1-dicyanothenyl)-1-phenyl-4,5-dihydro-1H-pyrazole (DChTP)/poly (methyl methacrylate) (PMMA) guest-host system by spin coating. In order to investigate their temporal and temperature stability, we have measured their dielectric relaxation spectra including the frequency dependence of the real and imaginary parts of dielectric constants. The investigated frequency ranged from 50 Hz to 10 MHz. The measured temperature range above the glass transition temperature T-g (95 degrees C) of the DCNP/PMMA system was from 95 degrees C to 1250C. By using the Adam-Gibbs model, the temperature dependence of the characteristic time tau above T-g was fitted, and the values of the characteristic times tau below T-g were estimated. The lifetimes of the polymer were evaluated by the Kohlrausch-Williams Watts (KWW) empirical decay model. (C) 2000 Elsevier Science B.V. All rights reserved.

Crystallographic and magnetic properties of R3Fe29-xVxN4 (R = Y, Ce, Nd, Sm, Gd, Tb, and Dy)

A systematic investigation of crystallographic and magnetic properties of nitride R3Fe29-xVxN4 (R = Y, Ce, Nd, Sm, Gd, Tb, and Dy) has been performed. Nitrogenation leads to a relative volume expansion of about 6%. The lattice constants and unit cell volume decrease with increasing rare-earth atomic number from Nd to Dy, reflecting the lanthanide contraction. On average, the Curie temperature increases due to the nitrogenation to about 200 K compared with its parent compound. Generally speaking, nitrogenation also results in a remarkable improvement of the saturation magnetization and anisotropy fields at 4.2 K and room temperature for R3Fe29-xVxN4 compared with their parent compounds. The transition temperature indicates the spin reorientations of R3Fe29-xVxN4 for R = Nd and Sm are at around 375 and 370 K which are higher than that of R3Fe29-xVx, for R = Nd and Sm 145 and 140 K, respectively. The magnetohistory effects of R3Fe29-xVxN4 (R = Ce, Nd, and Sm) are observed in low fields of 0.04 T. After nitrogenation the easy magnetization direction of Sm3Fe26.7V2.3 is changed from an easy-cone structure to the b-axis. As a preliminary result, a maximum remanence B-r of 0.94 T, an intrinsic coercivity mu(0)H(C) of 0.75 T, and a maximum energy product (B H)(max) of 108.5 kJ m(-3) for the nitride magnet Sm3Fe26.7V2.3N4 are achieved by ball-milling at 293 K.

Thermally Stable Guest-Host Polyetherketone Poled Polymer for Electro-Optical Applications

The high glass transition temperature polymer polyetherketone doped with disperse red 13 (DR13/PEK-c) has been prepared by the spin-coating method. Through in situ second-harmonic generation, the corona poling temperature was optimized by measuring the temperature dependence of the in situ second-harmonic generation signal intensity under the poling electric field. The linear electro-optic coefficients of the poled polymer films have been determined at 632.8 nm by using a simple interferometric technique. The polymer system was measured after 13 000 h, and found that it remained at 80% of its initial value.

EFFECT OF STRUCTURAL RELAXATION ON THE DEFORMATION BEHAVIOR OF A Zr64.13Cu15.75Ni10.12Al10 BULK METALLIC GLASS UNDER NANOINDENTATION

Structural relaxation by isothermal annealing below the glass transition temperature is conducted on a Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass. The effect of structural relaxation on thermal and mechanical properties was investigated by differential scanning calorimetry and instrumented nanoindentation. The recovery of the enthalpy in the DSC curves indicates that thermally unstable defects were annihilated through structural relaxation. During nanoindentation, the structural relaxation did not have a significant influence on the serrated plastic flow behavior. However, Structural relaxation shows an obvious effect in increasing both the hardness and elastic modulus, which is attributed to the annihilation of thermally unstable defects that resulted from the relaxation.

EFFECT OF STRUCTURAL RELAXATION ON THE DEFORMATION BEHAVIOR OF A Zr64.13Cu15.75Ni10.12Al10 BULK METALLIC GLASS UNDER NANOINDENTATION

Structural relaxation by isothermal annealing below the glass transition temperature is conducted on a Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass. The effect of structural relaxation on thermal and mechanical properties was investigated by differential scanning calorimetry and instrumented nanoindentation. The recovery of the enthalpy in the DSC curves indicates that thermally unstable defects were annihilated through structural relaxation. During nanoindentation, the structural relaxation did not have a significant influence on the serrated plastic flow behavior. However, Structural relaxation shows an obvious effect in increasing both the hardness and elastic modulus, which is attributed to the annihilation of thermally unstable defects that resulted from the relaxation.

The synthesis and characterization of novel liquid crystalline, meso-tetra[4-(3,4,5-trialkoxybenzoate)phenyl]porphyrins

Five, novel, meso-tetra[4-(3,4,5-trialkoxybenzoate)phenyl]porphyrins and their metal complexes were synthesized and their molecular structures were confirmed by H-1 NMR, FTIR spectroscopy and elemental analysis. Mesomorphic studies using DSC, polarizing optical microscope and X-ray diffraction revealed that all compounds exhibited thermotropic columnar mesophases over a wide mesophase temperature range and low liquid crystalline-crystal line transition temperature. (c) 2007 Elsevier Ltd. All rights reserved

Preparation and Characterization of Interpenetration Polymer Network Films Based on Poly(vinyl alcohol) and Poly(acrylic acid) for Drug Delivery

A series of full interpenetrating polymer network (full-IPN) films of poly(acrylic acid) (PAA)/poly (vinyl alcohol) (PVA) were prepared by radical solution polymerization and sequential IPN technology. Attenuated total reflectance-Fourier transform infrared spectroscopy, swelling properties, mechanical properties, morphology, and glass transition temperature of the films were investigated. FTIR spectra analysis showed that new interaction hydrogen bonds between PVA and PAA were formed. Swelling property of the films in distilled water and different pH buffer solution was studied. Swelling ratio increased with increasing PAA content of IPN films in all media, and swelling ratio decreased with increasing PVA crosslink degree. Tensile strength and elongation at break related not only to the constitution of IPNs but also to the swelling ratio of IPNs.