Maniaci, Frank F.. The analysis of degree of polymerization for photocurable ceramic suspensions through Raman spectroscopy. Retrieved from https://doi.org/doi:10.7282/t3-ea8q-jb88
DescriptionA process for determining the degree of polymerization (DOP) of photocurable ceramic suspension using Raman spectroscopy was developed in this work. It was compared to the commonly used method of Fourier transform infrared spectroscopy.
Photocuring involved using free radical photoinitiators to break acrylate bonds in uncured photocurable ceramic suspensions. This propagates polymer chains, and the suspension turns into a solid. In the process of stereolithography, this process was repeated to create layers to form complex shapes. The acrylate bonds were measured using FTIR and Raman spectroscopy at the wavenumber region of 1600-1650 cm⁻¹ for both methods. This was normalized with a carbonyl peak in the 1660-1720 cm⁻¹ region.
Various curing methods were tested, including single layered and multi-layered samplers were tested. Parameters including varying energy dose, varying power, and multiple exposure were tested for single layered samples. Multi-layered samples of 20 and 50 µm were also tested, using varying energy doses depending on depth of cure.
FTIR and Raman results showed a general increase in DOP as energy dose increased, with a higher DOP for the side that was directly exposed to UV light when compared to the side that was not exposed. Samples cured at varying powers showed a DOP that was generally within the same range as each other. Samples exposed multiple times showed a higher DOP when compared to the control sample, but there was little DOP increase between the sample exposed three times and seven times. Multi-layered samples showed an increase in DOP with higher energy dose, but the differences in layer thickness did not appear to cause any major differences in DOP.
Raman was found to be a more efficient method to work with as it allowed for sample analysis through the depth of a sample that was not available with FTIR. This could allow for pinpoint DOP analysis on any part of a cured sample and allow for a better idea of the ideal printing parameters.