Development of a phase diagram to control composite manufacturing using Raman spectroscopy

Fiber reinforced epoxy resins manufactured in autoclaves are expected to continue to dominate the composites market through 2010. However, the ability to obtain consistent mechanical properties from product-to-product remains difficult. This is largely due to the inability to monitor and control epoxy cure, loosely defined as the process of chain extension and cross-linking. Current autoclave process control employs a heat schedule based on a time-temperature-transformation (TTT) phase diagram that is determined by dynamic mechanical rheology. The phase diagram defines epoxy cure in terms of gelation and vitrification. We have been using an FT-Raman spectrometer to develop correlations between molecular (chain extension and cross-linking) and macroscopic (gelation and vitrification) data. The basis of a TTT phase diagram using Raman kinetic data for process control will be presented for several reactions.

[1]  Stuart Farquharson,et al.  Characterization of polymer composites by fiber optic Fourier transform Raman spectroscopy , 1999, Other Conferences.

[2]  Wayne W. Smith,et al.  Characterization of polymer composites during autoclave manufacturing by Fourier transform Raman spectroscopy , 2001, SPIE Optics East.

[3]  Douglas Wilson,et al.  PMR‐15 processing, properties and problems—a review , 1988 .

[4]  D. Uhlmann,et al.  Ultrastructure processing of ceramics, glasses, and composites , 1992 .

[5]  Bor Z. Jang,et al.  Advanced polymer composites , 1994 .

[6]  R. Dickie,et al.  Cross-linked polymers : chemistry, properties, and applications , 1988 .

[7]  J. Schlup,et al.  In situ Near-Infrared Spectroscopic Investigation of Epoxy Resin-Aromatic Amine Cure Mechanisms , 1994 .

[8]  Terry Ford,et al.  High Performance Composites , 1993 .

[9]  S. Senturia,et al.  Monitoring the cure of a composite matrix resin with microdielectrometry , 1989 .

[10]  S. Farquharson,et al.  On-Line Analysis Of Extruded Polymers Via Fiber-Optic Coupled Fourier Transform Near-Ir Spectroscopy. , 1990, Other Conferences.

[11]  B. Bulkin,et al.  Applications of Raman spectroscopy , 1980 .

[12]  Richard D. Driver,et al.  Fourier Transform Infrared (FTIR) Fiber Optic Monitoring Of Composites During Cure In An Autoclave , 1990, Other Conferences.

[13]  J. K. Gillham,et al.  Time–temperature–transformation (TTT) cure diagram: Modeling the cure behavior of thermosets , 1983 .

[14]  Henry Lee,et al.  Handbook of Epoxy Resins , 1967 .

[15]  Stuart Farquharson,et al.  Applications of Raman spectroscopy to industrial processes , 1992, Other Conferences.

[16]  Michael L. Myrick,et al.  Raman and Near-Infrared Studies of an Epoxy Resin , 1993 .

[17]  Hubertus F.J.M. Koopman,et al.  Contemporary polymer chemistry , 1981 .