Combining Rheology and Raman Spectroscopy: Following an Epoxy Resin Curing Reaction

The combination of a MCR series rheometer and a Cora 5X00 Fiber or 7X00 series Raman spectrometer offers unique opportunities in measuring both physical and chemical properties of a system simultaneously. For this report we will monitor an epoxy curing reaction to demonstrate the capabilities of the combination of the instruments.

Introduction

Rheometers are excellent tools for following the change in physical parameters during some process in a rigid and defined way. In the case of a chemical reaction, further insight can be gained by simultaneous acquisition of chemical information using a Raman spectrometer.

An example for a process during which both the physical and chemical properties of a sample change simultaneously is the curing reaction of an epoxy resin. It involves the gradual changes in viscosity and elasticity as a direct consequence of the chemical reaction in which the epoxy and hardener are converted into a three-dimensional network of the desired properties.

The combination of rheology and Raman spectroscopy presented here offers the advantage of simultaneous measurements. Thus, both viscoelastic and spectroscopic data share a common time axis. Therefore, it is straightforward to correlate the information gain between the two techniques.

When comparing chemical and physical data on the same reaction, it becomes evident that the chemical reaction progress precedes changes in the physical properties of the material. Only after a substantial amount of epoxy has reacted does the transition between the liquid and gelatinized solid phase occur.

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