Natural Ageing of PLA Filaments, Can It Be Frozen?

Polymers (Basel). 2022 Aug 17;14(16):3361. doi: 10.3390/polym14163361.

Abstract

The physical ageing of polylactic acid (PLA) is a phenomenon that changes the material's properties over time. This ageing process is highly dependent on ambient variables, such as temperature and humidity. For PLA, the ageing is noticeable even at room temperatures, a process commonly referred to as natural ageing. Stopping the ageing by freezing the material can be helpful to preserve the properties of the PLA and stabilise it at any time during its storage until it is required for testing. However, it is essential to demonstrate that the PLA's mechanical properties are not degraded after defrosting the samples. Four different methods for stopping the ageing (anti-ageing processes) are analysed in this paper-all based on freezing and defrosting the PLA samples. We determine the temperature and ambient water vapor influence during the freezing and defrosting process using desiccant and zip bags. The material form selected is PLA filaments (no bulk material or scaffold structures) printed at 190 °C with diameters between 400 and 550 µm and frozen at -24 °C in the presence or absence of a desiccant. The impact of the anti-ageing processes on PLA's ageing and mechanical integrity is studied regarding the thermal, mechanical and fractographical properties. In conclusion, an anti-ageing process is defined to successfully stop the natural ageing of the PLA for an indefinite length of time. This process does not affect the mechanical properties or the structural integrity of the PLA. As a result, large quantities of this material can be produced in a single batch and be safely stored to be later characterised under the same manufacturing and ageing conditions, which is currently a limiting factor from an experimental point of view as polymeric filament properties can show significant variety from batch to batch.

Keywords: PLA; ageing; desiccant; freezing; fused filament fabrication; thermal and mechanical properties.