Constantino C J L, Job A E, Simões R D, Giacometti J A, Zucolotto V, Oliveira O N, Gozzi G, Chinaglia D L
Faculdade de Ciências e Tecnologia--UNESP, 19060-900--Presidente Prudente, SP, Brazil.
Appl Spectrosc. 2005 Mar;59(3):275-9. doi: 10.1366/0003702053585336.
The phase transition from the non-polar alpha-phase to the polar beta-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous because it is a nondestructive technique. Films of alpha-PVDF were subjected to stretching under controlled rates at 80 degrees C, while the transition to beta-PVDF was monitored by the decrease in the Raman band at 794 cm(-1) characteristic of the alpha-phase, along with the concomitant increase in the 839 cm(-1) band characteristic of the beta-phase. The alpha-->beta transition in our PVDF samples could be achieved even for the sample stretched to twice (2x-stretched) the initial length and it did not depend on the stretching rate in the range between 2.0 and 7.0 mm/min. These conclusions were corroborated by differential scanning calorimetry (DSC) and X-ray diffraction experiments for PVDF samples processed under the same conditions as in the Raman scattering measurements. Poling with negative corona discharge was found to affect the alpha-PVDF morphology, improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, i.e., X-ray diffraction and infrared spectroscopy.
利用显微拉曼光谱对聚偏二氟乙烯(PVDF)从非极性α相到极性β相的相变进行了研究,该技术具有优势,因为它是一种无损技术。α-PVDF薄膜在80℃下以可控速率进行拉伸,同时通过α相特征峰794 cm(-1)处拉曼峰的降低以及β相特征峰839 cm(-1)处拉曼峰的相应增加来监测向β-PVDF的转变。即使对于拉伸至初始长度两倍(2倍拉伸)的样品,我们的PVDF样品中的α→β转变也能实现,并且在2.0至7.0 mm/min的拉伸速率范围内不依赖于拉伸速率。这些结论通过差示扫描量热法(DSC)和X射线衍射实验得到了证实,这些实验针对与拉曼散射测量相同条件下处理的PVDF样品进行。发现负电晕放电极化会影响α-PVDF的形态,增强与该晶相相关的拉曼峰。对于拉伸至更高比例的薄膜,这种影响最小化。值得注意的是,其他实验技术,即X射线衍射和红外光谱,未观察到电晕诱导效应。