Robitzer Mike, David Laurent, Rochas Cyrille, Di Renzo Francesco, Quignard Françoise
Institut Charles Gerhardt Montpellier, UMR 5253 CNRS-ENSCM-UM2-UM1, Matériaux Avancés pour la Catalyse et la Santé, ENSCM, 8 rue Ecole Normale, 34296 Montpellier Cedex 5, France.
Langmuir. 2008 Nov 4;24(21):12547-52. doi: 10.1021/la802103t. Epub 2008 Oct 10.
Ca-alginate materials were studied by small-angle X-ray scattering (SAXS) at different steps of conversion from gel to aerogel in order to determine the relation between the polymer organization at the nanoscale in the gels and the final dry aerogel. In all cases, i.e. before and after the different exchanges of solvents and after the formation of the aerogel, the SAXS patterns exhibit an asymptotic behavior at low q values (in the experimental q range 7x10(-3) up to 2.10(-2) A(-1)) close to I(q) approximately q(-1), indicative of randomly oriented rod-like scattering objects. The evolution of the diameter of such rod-like objects was thus deduced from the maxima observed on Kratky plots, i.e. I(q) q2 vs q. The results are in perfect agreement qualitatively (rod-like anisometry type of the scattering objects) and quantitatively (diameter of the rods) with direct SEM observations of the morphology of aerogels and with the results of N2 adsorption on the aerogel. This is evidence that in the chosen experimental processing conditions, the morphology of the aerogel depends on the morphology of pre-existing objects within the gel, i.e. that the structure of the aerogel provides a correct image of the structure of the parent gel.
为了确定凝胶中纳米级聚合物结构与最终干燥气凝胶之间的关系,采用小角X射线散射(SAXS)对不同转化步骤(从凝胶到气凝胶)的钙藻酸盐材料进行了研究。在所有情况下,即在不同溶剂交换前后和气凝胶形成后,SAXS图案在低q值(在实验q范围7×10⁻³至2.10⁻² Å⁻¹)处呈现渐近行为,接近I(q)≈q⁻¹,这表明存在随机取向的棒状散射物体。因此,根据在Kratky图上观察到的最大值,即I(q) q²对q,推导出此类棒状物体直径的演变。结果在定性(散射物体的棒状各向异性类型)和定量(棒的直径)方面与气凝胶形态的直接扫描电子显微镜观察结果以及气凝胶上N₂吸附的结果完全一致。这证明在所选的实验加工条件下,气凝胶的形态取决于凝胶中预先存在的物体的形态,即气凝胶的结构提供了母体凝胶结构的正确图像。