水/AOT/正庚烷微乳体系中水结构的FT-IR研究

运用傅立叶变换红外光谱（ＦＴ－ＩＲ）对水／ＡＯＴ／正庚烷微乳体系中水的微结构进行了研究。结果表明，随着体系中加水量的增大，水分子Ｏ－Ｈ伸缩振动的红外光谱由３４９３ｃｍ＾－１向低频移动至３４１７ｃｍ＾－１，微乳体系中，水分子与ＡＯＴ分子的磺酸基作用的同时，与Ｎａ＾＋也有一定的作用，这两种离子对水分子Ｏ－Ｈ键的强度均有一定的影响，磺酸基的作用使水分子中Ｏ－Ｈ伸缩振动向高波数方向移动，而Ｎａ＾＋的作用与     

Small Angle X-ray Scattering Study of PS Conformation in Tetrahydrofuran Solvent with Gas Anti-solvent

Compressed gases or supercritical fluids (SCFs) are highly soluble in some liquid solvents, and thus reduces the solvent strength of the liquids1. As a result, precipitation of the dissolved solutes occurs, which is called as gas anti-solvent (GAS) process. Recently, this new technique has been used to produce fine particles of different compounds, such as polymers2. Effect of the dissolved gases on the conformation of polymer molecules is a very interesting topic. In this work, we report t…     

小角X光散射表征分散液中Nafion的微观结构

利用小角X光散射研究了全氟磺酸离子聚合物Nafion膜在不同比例的氮甲基甲酰胺和正丁醇混合溶剂中分散形成分散液的微观结构。 研究表明,主链刚性和主-侧链亲疏水性的协同作用使分散液中的Nafion呈典型的棒状胶束结构。 胶束的等效回转半径(R_g)对Nafion质量浓度表现出-0.42的标度,与聚电解质在无盐溶剂中的理论标度一致;而胶束间相关长度对Nafion质量浓度表现出-0.13的标度,与典型的中性聚合物溶液理论标度一致。 极性低的正丁醇促进Nafion主链溶剂化并利于长胶束形成,而极性高的氮甲基甲酰胺则能促进Nafion分散。 该研究将为理解Nafion分散液的性质以及湿法制备Nafion膜的微结构形成提供清晰指导。     

Conformation and Aggregation Behavior of Polyelectrolyte with Primary Amino Pendant Groups in Water or THF/Water Binary Solvent Mixture and Their Effect on the Morphology of AOT Vesicles in Aqueous Media

Cationic polyelectrolyte with primary amine pendant groups, poly (4-vinyl benzyl amine hydrochloride salt) (poly (4-VBAHS)), was characterized by static light scattering. Using light scattering measurement, the conformation transition of poly (4-VBAHS) chains in pure water, and THF/H₂O (v/v: 1/3) binary solvent mixture was discussed. Concentration-dependent multiple morphologies including interpenetrating networks, tubular micelles, branched micelles, hexagonal phases, vesicles, and needle crystals were observed by TEM. In addition, effect of poly (4-VBAHS) on the morphology, stability, and critical vesicle/micelle concentration of anionic surfactant sodium bis (2-ethylhexyl) sulfosucciante vesicles were detected using dynamic light scattering, zeta potential, surface tension, and transmission measurements.     

水／AOT／正庚烷微乳体系中磺酸根水化作用的FT—IR研究

运用傅立叶变换红外光谱（FT－IR）对水／琥珀酸（乙基已基）磺酸钠（AOT）／正庚烷微乳体系中磺酸根的水化作用进行了研究．由于微乳体系中水分子与表面活性剂分子的相互作用，S＝O对称伸缩振动的红外吸收峰向低频方向移动．体系中的加水量W0（水与AOT的摩尔比）由0.5增大至25时，磺酸根对称伸缩振动的红外吸收峰由1051．39cm－1向低频移动至1046．15cm－1．同时，由于Na 的不对称作用，AOT分子中磺酸根反对称伸缩振动分裂成两个吸收峰，分别位于正215cm-1及1245cm－1附近，两个劈裂峰的距离及各自的峰面积均随体系中加水量的变化而变化，应用二阶导数、傅立叶退卷积及曲线拟会等分辨率增强技术可更清楚地反映出这个二重峰的变化情况．固体AOT分子中碳酸根反对称伸缩振动分裂的两个峰之间频率的差值约为42cm－1，形成微乳液以后，这两个峰的差值变小，W0为20时，这两个峰频率的差值逐渐减小到29cm-1，这些变化与磺酸根的水化程度直接相关     

负载磁性纳米粒子球形聚电解质刷的小角X光光散射表征

通过光乳液聚合法在聚苯乙烯球上接枝聚丙烯酸链形成球形聚电解质刷(SPB),以SPB为纳米反应器,通过共沉淀法原位制备了四氧化三铁磁纳米粒子(MNP),并多次负载增加体系中的磁含量。通过小角X光光散射表征手段,研究了SPB中负载MNP的含量和分布规律。结果表明:在刷子层中,随着负载次数增加,MNP的含量增加,其浓度分布变得越来越不均匀,并且浓度分布由铁离子、亚铁离子的浓度分布和空间阻力共同决定。     

琥珀酸二异辛酯磺酸钠微乳体系中纳米银的制备及其连续相的影响

在琥珀酸二异辛酯磺酸钠(AOT)为表面活性剂、环己烷为连续相形成的微乳体系中, 利用水合肼还原AgNO₃制备了分散性良好的纳米银. 利用紫外-可见(UV-Vis)光谱和透射电镜(TEM)对所得产物进行了表征, TEM显微图像表明形成粒子为球形结构, 平均粒径为5.10 nm, 标准偏差为2.84 nm. 分别利用正己烷、正庚烷、正辛烷、环己烷和十二烷等作连续介质, 研究了微乳液中连续相对纳米银形成的影响. 随着正烷烃碳链长度的增加, 微乳液中胶束之间的交换速率增大, 形成粒子的平均粒径逐渐减小. 十二烷形成的微乳体系制备的纳米银溶胶具有最宽的共振吸收峰, 所得的纳米银粒子平均粒径最小. 环己烷形成的微乳液中反胶束具有特殊的界面强度, 导致纳米银晶核的形成速率过低, 纳米银晶粒的生长不完全.     

左旋18—甲基炔诺酮—硅橡胶缓释体系小角激光散射法研究

以小角激光前向散射和背散射法研究了左旋１８－甲基炔诺酮－甲基乙烯基硅橡胶缓释体系的光散射时效行为，用紫外分光光度法测定释放过程，讨论药物释放过程中高分子链段运动和聚合物结构对药物释放的影响．     

Characterization of Nano-Scale Parallel Lamellar Defects in RDX and HMX Single Crystals by Two-Dimension Small Angle X-ray Scattering

Nano-scale crystal defects extremely affect the security and reliability of explosive charges of weapons. In this work, the nano-scale crystal defects of 1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) single crystals were characterized by two-dimension SAXS. Deducing from the changes of SAXS pattern with sample stage rotating, we firstly found the parallel lamellar nano-scale defects in both RDX and HMX single crystals. Further analysis shows that the average diameter and thickness of nano-scale lamellar defects for RDX single crystal are 66.4 nm and 19.3 nm, respectively. The results of X-ray diffraction (XRD) indicate that the lamellar nano-scale defects distribute along the (001) in RDX and the (011) in HMX, which are verified to be the crystal planes with the lowest binding energy by the theoretical calculation.     

胶体分散体系与有序分子组合体的小角X射线散射研究

小角X射线散射(SAXS)是当前化学、物理、生物等学科前沿交叉领域--软凝聚态物质的一个强有力研究工具.本文评述了SAXS方法自身的优势及其在胶体分散体系与有序分子组合体研究中的广泛应用,重点论述了对粒子尺寸或孔径大小分布、胶体体系分散状态、长程有序结构以及混合体系之间相互作用的测量与表征等.     

The Study of Cavitation in HDPE Using Time Resolved Synchrotron X-ray Scattering During Tensile Deformation

Real time synchrotron Small-Angle and Wide-Angle X-ray Scattering was performed during the tensile deformation of a high-density polyethylene copolymer. The changes of the structure in the crystalline and in the amorphous domains were followed during the three characteristic stages of the load-displacement curves: The elastic stage and the plastic range composed of the stage of the lowering load in the force-displacement-curve (yielding) and the strain hardening. Competitive phenomena like crystallite fragmentation and cavitation were found to occur simultaneously in the phase of lowering the load but at different length scale. We prove that the void formation occurs mainly during yielding. During strain hardening there was no further increase of the void volume fraction, only changes in void size.     

原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响

采用原位小角X射线散射和扫描电子显微镜研究了热拉过程中,拉伸比和拉伸温度对熔融拉伸法制备的聚丙烯微孔膜晶体和孔洞结构的影响.研究结果表明,冷拉、热定型过程中片晶簇被分离开,其内部结构在热拉过程中不发生分离等变形;随着热拉拉伸比的增加,片晶簇间架桥长度不断增大;与冷拉、热定型样品相比,热拉后的微孔膜架桥沿垂直于拉伸方向具有较好的周期性.不同的拉伸温度结果表明,架桥长度随拉伸温度升高而增加;温度过高时架桥会发生熔融.     

小角X射线散射在高分子研究中的应用

本文综述了小角X射线散射理论,并介绍了小角散射在高分子溶液、结晶聚合物、嵌段共聚物和离聚物等研究中的应用.     

丁二酸二异辛酯磺酸钠对微乳液毛细管电泳分离蛋白质的影响

本研究探讨了在生理条件下,同时分离酸性和碱性蛋白质的毛细管电泳方法。在120mmol/L十二烷基硫酸钠(SDS) 5mmol/L丁二酸二异辛酯磺酸钠(AOT) 110mmol/L正辛烷 500mmol/L正丁醇 3mmol/LNa2B4O7 3mmol/LNaH2PO4(pH6.7)的微乳体系中,分离电压20kV,25min内完成核糖核酸A、细胞色素C、牛血清蛋白、α-淀粉酶和β-乳球蛋白5种不同酸、碱性蛋白质基线分离;分离效率为7.8×105～4.4×105/m;迁移时间的RSD为1.5%(n=11)。并讨论了蛋白质在AOT组成的复配微乳体系中的分离机制。     

The relationship of conductivity to the morphology and crystallinity of polyaniline controlled by water content via reverse microemulsion

Conducting polyaniline (PANI) with the controllable morphology and crystallinity were successfully synthesized with different water content () in the reverse microemulsion stabilized with sodium bis(2-ethylhexyl)-sulfosuccinate (AOT). In the microemulsion, the systems containing the different amounts of water will show the different phase behaviors and structures. The influence of water content on morphology and crystallinity of conducting PANI was characterized by a number of techniques such as Fourier transform infrared spectra, UV–Visible, scanning electron microscopy, transmission electron microscopy, and X-ray powder diffraction and conductivity. In particular, we focus on the understanding of the relationship between the morphology and the crystallinity and the conductivity of PANI powder. With the increasing of the water content (W ₀ = 13.9, 27.8, 55.5, and 111.1) in the microemulsion system, the morphology and the crystallinity obviously changed and the values of relative conductivity are 0.05, 0.11, 2.7, and 1.8 S/cm, respectively.     

Small‐Angle Neutron Scattering from Elastomeric Networks in which the Junctions Alternate Regularly in their Functionality

We compute scattering form factors for SANS from labeled paths in Gaussian phantom networks in which junctions alternate regularly in their functionality (the number of chains emanating from a junction). Our calculations are based on the James‐Guth model of rubber‐like elasticity, which assumes that fluctuations are strain independent, while mean vectors transform affinely with the applied strain. Kratky plots for scattering from isotropic and uniaxially stretched bifunctional networks are computed and compared with corresponding plots for the simpler unifunctional networks. The results show the effects of the length of the labeled path, extent of deformation, direction of scattering with respect to the principal axis of the deformation and the functionalities of the network junctions.

     

傅立叶变换红外光谱对琥珀酸-2-乙基己基磺酸钠非极性溶液中 反胶束结构的研究

利用衰减全反射傅立叶变换红外光谱(ATR-FTIR), 对琥珀酸-2-乙基己基磺酸钠(AOT)的反胶束结构进行了研究. 通过对红外光谱进行二维相关分析, 可以分辨出AOT分子在CCl4溶液中具有旁式和反式两种结构, 随着温度的升高, 旁式结构向反式结构转变, 反胶束体系能量降低, 38 ℃时, 反式结构所占比例达到最大值, 此时反胶束具有最大尺寸, 并处于最稳定的能量状态. 随着温度的进一步升高, 反式结构开始向旁式结构转变, 反胶束尺寸变小, 直至最后反胶束被破坏.     

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

Application of low-cost carbon black from lignin highly depends on the materials properties, which might by determined by raw material and processing conditions. Four different technical lignins were subjected to thermostabilization followed by stepwise heat treatment up to a temperature of 2000 °C in order to obtain micro-sized carbon particles. The development of the pore structure, graphitization and inner surfaces were investigated by X-ray scattering complemented by scanning electron microscopy and FTIR spectroscopy. Lignosulfonate-based carbons exhibit a complex pore structure with nanopores and mesopores that evolve by heat treatment. Organosolv, kraft and soda lignin-based samples exhibit distinct pores growing steadily with heat treatment temperature. All carbons exhibit increasing pore size of about 0.5–2 nm and increasing inner surface, with a strong increase between 1200 °C and 1600 °C. The chemistry and bonding nature shifts from basic organic material towards pure graphite. The crystallite size was found to increase with the increasing degree of graphitization. Heat treatment of just 1600 °C might be sufficient for many applications, allowing to reduce production energy while maintaining materials properties.