Single crystal morphology and structural data of a series of polyesters derived from 1,8-octanediol

The morphology of solution grown single crystals of a series of polyesters derived from 1,8-octanediol and either an even or an odd dicarboxylic acid has been investigated. Different crystallization conditions (solvent and temperature) were tested for these polyesters whose dicarboxylate unit varied from pimelate to sebacate. Crystals showed a lozenge morphology with a degree of truncation which for a given solvent changed with the crystallization temperature. Curvature of growth faces, striations on the lamellar surface and a bilayered morphology were features that were observed in some cases. Polyethylene decoration highlighted a crystal sectorization and suggested a molecular folding parallel to the crystal growth faces.The studied polyesters always showed a single crystalline structure, according to electron and X-ray diffraction data. A practically all trans molecular conformation could always be deduced. Unit cell geometry changed from orthorhombic to monoclinic and the molecular content was variable in the studied series (two or four molecular segments).Lamellae gave rise to well-defined electron diffraction patterns that allowed the setting angle of molecular segments to be determined. A good agreement between simulated and experimental hk0 diffraction patterns was always found. Packing along the chain axis direction was completely defined for the sebacate derivative.     

原子力显微镜原位观察球晶界面上片晶的生长

当结晶聚合物由熔融冷却或从浓溶液中析出结晶时 ,在不存在应力和流动的情况下 ,一般形成球晶 .球晶在一定的生长时期内呈现球形外观 ,在偏光显微镜下通常呈现Maltese黑十字消光图样 .球晶作为一种常见的结晶形态 ,由片晶堆积而成[1,2 ] .Keith和Padden认为形成球晶的体系包含杂质和聚合物链 ,由于杂质在片晶生长界面的富集导致片晶产生小角度分叉 ,这样片晶能填满球状的空间[1,2 ] .近年来的研究表明球晶是由一个片晶开始生长 ,片晶在生长过程中不断的诱导成核使片晶分叉 ,首先形成片晶捆束 ,然后片晶向各个方向发散生长 ,最终形成球晶[3…     

Sample preparation by focused ion beam micromachining for transmission electron microscopy imaging in front-view

This article deals with the development of an original sample preparation method for transmission electron microscopy (TEM) using focused ion beam (FIB) micromachining. The described method rests on the use of a removable protective shield to prevent the damaging of the sample surface during the FIB lamellae micromachining. It enables the production of thin TEM specimens that are suitable for plan view TEM imaging and analysis of the sample surface, without the deposition of a capping layer. This method is applied to an indented silicon carbide sample for which TEM analyses are presented to illustrate the potentiality of this sample preparation method.     

预热处理对超高分子量聚乙烯层积状片晶凝胶膜结构的影响

由准稀溶液速冷制备的超高分子量聚乙烯（ＵＨＭＷＰＥ）凝胶膜，具有片晶（Ｌａｍｅｌｌａ）取向平行于膜面的层积状结构，在１２９—１３４℃的温度范围内拉伸，可获得超高拉伸比（λ＞２００）．通过ＩＲ及Ｘ－ｒａｙ衍射等方法研究发现，拉伸前用不同温度退火处理后，凝胶膜的片晶微结构产生明显变化，在对应于超高拉伸温度范围内，其结晶度增加，微晶的ｃ和ｂ轴方向尺寸变大，而ａ轴方向的尺寸减小，从理论上对这一变化过程作了考察，并讨论了超高拉伸取向性与这些结构变化的关系以及可超拉伸取向性的最佳温度范围．     

辐照异相成核结晶PA1010体系的ESR研究——结晶表面积对俘陷自由基的影响

本文通过ＷＡＸＤ，ＤＳＣ方法讨论成核剂（Ｎｄ２Ｏ３）对ＰＡ１０１０的聚集态结构的影响。用ＥＳＲ研究辐照不同聚集态结构ＰＡ１０１０体系的俘陷自由基行为。结果表明：俘陷自由基—ＣＨ２ＣＯＮＨＣＨＣＨ２—主要存在于结晶表面，结晶的表面积越大，俘陷自由基—ＣＨ２ＣＯＮＨＣＨＣＨ２—的含量越高，在一定条件下，如升温，常温放置一段时间，转化为俘陷自由基—ＣＨ２Ｃ＝Ｏ的量也越大；俘陷自由基－ＣＨ２Ｃ＝Ｏ主要存在于非晶区。     

Morphology and structure of poly(p-dioxanone)

The morphology of solution grown single crystals of poly(p-dioxanone) was investigated. Different crystallization conditions (solvent, precipitant agent and temperature) were tested. Dendritic growth, screw dislocations and striations were observed. Crystals usually exhibited a lozenge morphology, whose apex angle changed with the crystallization conditions. In all cases, however, a single crystal electron diffraction pattern was recorded. Spherulitic morphologies were obtained by evaporation of formic acid solutions. Lamellae gave rise to well resolved electron diffraction patterns that allowed determination of the main packing characteristics. Patterns of tilted specimens helped establish an orthorhombic unit cell, whose parameters indicate a deviation from the all trans molecular conformation. Quantum mechanical calculations were performed on small model compounds to study the conformational preferences. Simulated diffraction patterns were consistent with a unit cell containing four repeat units and a P2₁2₁2₁ space group. Molecular packing suggests the existence of different kinds of folds for an assumed adjacent reentry. Polyethylene decoration hardly highlighted a crystal sectorization. Also enzymatic degradation of lamellar crystals was evaluated by using a Pseudomonas cepacia lipase.