Thermally induced structural transitions of nylon 4 9 as a new example of even-odd polyamides

Crystalline morphology and structure of nylon 4 9 have been studied by means of optical and transmission electron microscopies, and X-ray diffraction. Rhombic crystals were characteristic of crystallization from glycerin dilute solutions, although the final morphology was dependent on the crystalliz...

Descripción completa

Detalles Bibliográficos
Autores: Olmo, Cristian, Casas, Maria Teresa, Martínez, Juan Carlos, Franco García, María Lourdes|||0000-0001-5968-285X, Puiggalí, Jordi|||0000-0002-0640-4474
Tipo de recurso: artículo
Fecha de publicación:2018
País:España
Institución:Universitat Autònoma de Barcelona
Repositorio:Dipòsit Digital de Documents de la UAB
Idioma:inglés
OAI Identifier:oai:ddd.uab.cat:202506
Acceso en línea:https://ddd.uab.cat/record/202506
https://dx.doi.org/urn:doi:10.3390/polym10020198
Access Level:acceso abierto
Palabra clave:Crystalline structure
Hydrogen bonds
Lamellar morphology
Polyamides
Spherulites
Synchrotron radiation
Thermal transitions
Descripción
Sumario:Crystalline morphology and structure of nylon 4 9 have been studied by means of optical and transmission electron microscopies, and X-ray diffraction. Rhombic crystals were characteristic of crystallization from glycerin dilute solutions, although the final morphology was dependent on the crystallization temperature. In any case, a single electron diffraction pattern was always obtained, being characteristic a 2 mm symmetry and reflections at spacings that were indicative of a projected rectangular unit cell with hydrogen bonds established along two planar directions (i.e., the diagonals of the unit cell), as it was determined from related polyamides. Crystallization from the melt gave rise to negative birefringent spherulites with a morphology (axialitic, speckled or ringed) that was dependent on the crystallization temperature. Kinetic analysis indicated that melt crystallization took place according to two growth mechanisms (Regimes II and III), which reflect distinct secondary nucleation rates. A complex polymorphic behavior on heating and cooling processes was evidenced by real time synchrotron experiments, being determined an intermediate crystalline structure as well as the typical pseudohexagonal arrangement associated to the Brill transition. Polymorphic transitions were highly dependent on the initial crystalline structure, being enhanced the structural transition from the low temperature structure to the intermediate one when traces of the latter were initially present. Calorimetric and infrared studies supported also the detected thermal transitions of nylon 4 9.