The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion

Powder bed fusion (PBF) is an additive manufacturing (AM) technique which offers efficient part-production, light-weighting, and the ability to create complex geometries. However, during a build cycle, multiple aging and degradation processes occur which may affect the reusability of the Polyamide 1...

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Main Authors: Benjamin Sanders, Edward Cant, Hoda Amel, Michael Jenkins
Format: Article
Language:English
Published: MDPI AG 2022-06-01
Series:Polymers
Subjects:
Online Access:https://www.mdpi.com/2073-4360/14/13/2682
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author Benjamin Sanders
Edward Cant
Hoda Amel
Michael Jenkins
author_facet Benjamin Sanders
Edward Cant
Hoda Amel
Michael Jenkins
author_sort Benjamin Sanders
collection DOAJ
description Powder bed fusion (PBF) is an additive manufacturing (AM) technique which offers efficient part-production, light-weighting, and the ability to create complex geometries. However, during a build cycle, multiple aging and degradation processes occur which may affect the reusability of the Polyamide 12 (PA-12) powder. Limited understanding of these phenomena can result in discarding re-usable powder unnecessarily, or the production of parts with insufficient properties, both of which lead to significant amounts of waste. This paper examines the thermal, chemical, and mechanical characteristics of PA-12 via an oven storage experiment that simulates multi jet fusion (MJF) conditions. Changes in the properties of PA-12 powder during oven storage showed two separate, time-dependent trends. Initially, differential scanning calorimetry showed a 4.2 °C increase in melting temperature (T<sub>m</sub>) and a rise in crystallinity (X<sub>c</sub>). This suggests that secondary crystallisation is occurring instead of, or in addition to, the more commonly reported further polycondensation process. However, with extended storage time, there were substantial reductions in T<sub>m</sub> and X<sub>c</sub>, whilst an 11.6 °C decrease in crystallisation temperature was observed. Fourier transform infrared spectroscopy, a technique rarely used in PBF literature, shows an increased presence of imide bonds—a key marker of thermo-oxidative degradation. Discolouration of samples, an 81% reduction in strength and severe material embrittlement provided further evidence that thermo-oxidative degradation becomes the dominant process following extended storage times beyond 100 h. An additional pre-drying experiment showed how moisture present within PA-12 can also accelerate degradation via hydrolysis.
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spelling doaj.art-8b48be15955940deac962d8dcb0fbb982023-11-30T22:21:45ZengMDPI AGPolymers2073-43602022-06-011413268210.3390/polym14132682The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed FusionBenjamin Sanders0Edward Cant1Hoda Amel2Michael Jenkins3School of Metallurgy and Materials, University of Birmingham, Elms Road, Birmingham B15 2SE, UKThe Manufacturing Technology Centre, Ansty Park, Coventry CV7 9JU, UKThe Manufacturing Technology Centre, Ansty Park, Coventry CV7 9JU, UKSchool of Metallurgy and Materials, University of Birmingham, Elms Road, Birmingham B15 2SE, UKPowder bed fusion (PBF) is an additive manufacturing (AM) technique which offers efficient part-production, light-weighting, and the ability to create complex geometries. However, during a build cycle, multiple aging and degradation processes occur which may affect the reusability of the Polyamide 12 (PA-12) powder. Limited understanding of these phenomena can result in discarding re-usable powder unnecessarily, or the production of parts with insufficient properties, both of which lead to significant amounts of waste. This paper examines the thermal, chemical, and mechanical characteristics of PA-12 via an oven storage experiment that simulates multi jet fusion (MJF) conditions. Changes in the properties of PA-12 powder during oven storage showed two separate, time-dependent trends. Initially, differential scanning calorimetry showed a 4.2 °C increase in melting temperature (T<sub>m</sub>) and a rise in crystallinity (X<sub>c</sub>). This suggests that secondary crystallisation is occurring instead of, or in addition to, the more commonly reported further polycondensation process. However, with extended storage time, there were substantial reductions in T<sub>m</sub> and X<sub>c</sub>, whilst an 11.6 °C decrease in crystallisation temperature was observed. Fourier transform infrared spectroscopy, a technique rarely used in PBF literature, shows an increased presence of imide bonds—a key marker of thermo-oxidative degradation. Discolouration of samples, an 81% reduction in strength and severe material embrittlement provided further evidence that thermo-oxidative degradation becomes the dominant process following extended storage times beyond 100 h. An additional pre-drying experiment showed how moisture present within PA-12 can also accelerate degradation via hydrolysis.https://www.mdpi.com/2073-4360/14/13/2682powder bed fusionpolyamide 12DSCrecyclabilitythermo-oxidationsecondary crystallisation
spellingShingle Benjamin Sanders
Edward Cant
Hoda Amel
Michael Jenkins
The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
Polymers
powder bed fusion
polyamide 12
DSC
recyclability
thermo-oxidation
secondary crystallisation
title The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
title_full The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
title_fullStr The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
title_full_unstemmed The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
title_short The Effect of Physical Aging and Degradation on the Re-Use of Polyamide 12 in Powder Bed Fusion
title_sort effect of physical aging and degradation on the re use of polyamide 12 in powder bed fusion
topic powder bed fusion
polyamide 12
DSC
recyclability
thermo-oxidation
secondary crystallisation
url https://www.mdpi.com/2073-4360/14/13/2682
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