Towards the Reuse of Fire Retarded Polyamide 12 for Laser Sintering
Abstract
:1. Introduction
2. Materials and Methods
- Warm-up temperature: 151 °C
- Printing temperature: 153 °C
- Laser scan speed: 2.85 m·s−1
- Laser power: 3.64 W
- Layer height: 0.1 mm
- Time to ignition (TTI)
- Peak of rate release rate (pHRR)
- Mass loss rate
- Total heat released (THR)
- Maximum of average rate of heat emission (MARHE) as a function of time.
3. Results and Discussions
3.1. DSC Thermograms
3.1.1. Analysis of Initial and Reused Powder Blends
3.1.2. Analysis of Specimens as Function of Reuse Cycles and Compositions
3.2. Porosity of Specimens
3.3. EDX of Powders
3.4. Properties of LS Parts
3.4.1. Scanning Electron Microscopy (SEM)
3.4.2. Thermal Stability (Thermogravimetric Analysis—TGA)
3.4.3. Fire Behavior at Microscopic Scale—PCFC
3.4.4. Fire Behavior—Cone Calorimeter
3.4.5. Fourier Transform Infrared Spectra of LS Samples
3.4.6. Polyamide 12 Phase Analysis—XRD
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Sample | Tic (°C) | Tc Peak (°C) | Tim (°C) | Tm Peak (°C) | ΔHc (J/g) | Processing Window ΔT (°C) | ΔHF (J/g) |
---|---|---|---|---|---|---|---|
PA-0 | 153.8 | 148.2 | 182.4 | 183.9 | 45.0 | 29.1 | 88.1 |
PA-1 | 154.1 | 148.8 | 182.3 | 183.4 | 46.0 | 28.7 | 83.3 |
PA-2 | 153.2 | 148.6 | 183.5 | 183.5 | 46.1 | 30.3 | 86.6 |
PA-3 | 153.2 | 148.4 | 182.5 | 182.5 | 45.4 | 29.3 | 85.6 |
PA-4 | 153.2 | 148.3 | 182.1 | 182.1 | 45.7 | 28.9 | 88.8 |
AP30-0 | 155.7 | 152.7 | 181.0 | 184.8 | 45.9 | 25.3 | 80.2 |
AP30-1 | 155.6 | 149.4 | 181.2 | 184.2 | 45.7 | 25.6 | 79.9 |
AP30-2 | 158.2 | 151.6 | 183.4 | 185.0 | 45.1 | 25.2 | 78.0 |
AP30-3 | 158.0 | 152.0 | 182.6 | 186.2 | 47.7 | 24.6 | 78.9 |
AP30-4 | 156.8 | 150.4 | 181.8 | 185.6 | 46.6 | 25.0 | 76.3 |
ZB30-0 | 153.0 | 148.5 | 180.5 | 186.0 | 47.8 | 27.5 | 76.8 |
ZB30-1 | 154.2 | 149.0 | 182.0 | 187.6 | 47.1 | 27.8 | 76.8 |
ZB30-2 | 154.5 | 150.0 | 182.6 | 188.2 | 47.7 | 28.0 | 76.5 |
ZB30-3 | 153.2 | 149.4 | 182.6 | 186.5 | 47.8 | 29.4 | 80.0 |
ZB30-4 | 153.0 | 150.5 | 181.9 | 187.1 | 46.8 | 28.9 | 78.2 |
Sample | Tic (°C) | Tc Peak (°C) | Tim (°C) | Tm Peak (°C) | ΔHc (J/g) | ΔHF (J/g) |
---|---|---|---|---|---|---|
PA-0 | 152.6 | 148.7 | 173.3 | 183.3 | 50.2 | 58.0 |
PA-1 | 153.0 | 149.4 | 172.4 | 182.6 | 49.5 | 56.9 |
PA-2 | 153.1 | 149.3 | 173.0 | 181.9 | 49.7 | 57.0 |
PA-3 | 153.1 | 149.6 | 174.9 | 182.2 | 46.6 | 55.5 |
PA-4 | 154.0 | 149.8 | 176.7 | 184.2 | 49.2 | 50.9 |
AP30-0 | 159.2 | 153.4 | 175.9 | 182.9 | 45.5 | 57.3 |
AP30-1 | 158.9 | 153.8 | 177.1 | 183.3 | 40.1 | 54.9 |
AP30-2 | 158.6 | 153.7 | 176.4 | 184.4 | 42.5 | 57.7 |
AP30-3 | 158.5 | 153.6 | 177.3 | 183.1 | 41.1 | 58.4 |
AP30-4 | 158.8 | 154.0 | 177.1 | 183.1 | 42.4 | 56.5 |
ZB30-0 | 159.3 | 154.2 | 176.1 | 183.4 | 46.0 | 58.0 |
ZB30-1 | 160.1 | 152.7 | 175.1 | 183.6 | 46.8 | 46.3 |
ZB30-2 | 160.0 | 152.5 | 176.2 | 183.5 | 45.4 | 52.2 |
ZB30-3 | 160.0 | 153.2 | 175.8 | 183.0 | 47.7 | 49.8 |
ZB30-4 | 160.0 | 153.2 | 176.0 | 183.7 | 46.9 | 48.0 |
Sample | Theoretical P Content (%) | P (%) | Theoretical Zn Content (%) | Zn (%) |
---|---|---|---|---|
AP30-0 | 9.57 | 9.3 ± 0.3 | - | - |
AP30-1 | 9.57 | 9.6 ± 1 | - | - |
AP30-2 | 9.57 | 10.1 ± 0.8 | - | - |
AP30-3 | 9.57 | 10.4 ± 0.3 | - | - |
AP30-4 | 9.57 | 9.5 ± 0.4 | - | - |
ZB30-0 | - | - | 15.5 | 15.5 ± 0.5 |
ZB30-1 | - | - | 15.5 | 11.8 ± 2 |
ZB30-2 | - | - | 15.5 | 12.5 ± 1.3 |
ZB30-3 | - | - | 15.5 | 12.8 ± 1.2 |
ZB30-4 | - | - | 15.5 | 12.6 ± 0.9 |
Sample | T5% | T20% | T50% | Residue at 750 °C (%) |
---|---|---|---|---|
PA-0 | 395.2 | 432.8 | 451.3 | 0 |
PA-1 | 399.9 | 427.9 | 448.2 | 0.4 |
PA-2 | 396.0 | 424.9 | 443.7 | 0.7 |
PA-3 | 397.3 | 425.1 | 443.9 | 0.9 |
PA-4 | 398.7 | 425.4 | 443.7 | 1.0 |
AP30-0 | 354.1 | 378.5 | 389.9 | 20.0 |
AP30-1 | 352.3 | 374.7 | 386.5 | 22.5 |
AP30-2 | 352.6 | 376.6 | 387.4 | 21.9 |
AP30-3 | 355.2 | 377.5 | 389.0 | 23.0 |
AP30-4 | 355.0 | 377.0 | 388.0 | 20.9 |
ZB30-0 | 405.8 | 447.3 | 466.1 | 25.1 |
ZB30-1 | 398.9 | 441.3 | 463.6 | 23.5 |
ZB30-2 | 406.4 | 452.1 | 468.9 | 25.9 |
ZB30-3 | 408.1 | 443.7 | 462.5 | 26.1 |
ZB30-4 | 406.2 | 443.5 | 462.9 | 24.6 |
Sample | THR (kJ/g) | pHRR (W/g) | Peak Temperature (°C) |
---|---|---|---|
PA-0 | 34.7 | 699 | 454.5 |
PA-1 | 33.6 | 573 | 460.4 |
PA-2 | 35.2 | 586 | 454.7 |
PA-3 | 34.2 | 575 | 466.6 |
PA-4 | 34.3 | 592 | 461.7 |
AP30-0 | 24.7 | 951 | 393.4 |
AP30-1 | 24.1 | 958 | 381.9 |
AP30-2 | 24.4 | 987 | 381.8 |
AP30-3 | 25.7 | 968 | 380.4 |
AP30-4 | 24.1 | 935 | 390.5 |
ZB30-0 | 24.5 | 588 | 477.3 |
ZB30-1 | 22.8 | 569 | 478.7 |
ZB30-2 | 23.8 | 521 | 479.8 |
ZB30-3 | 23.7 | 577 | 474.6 |
ZB30-4 | 24.0 | 550 | 483.8 |
Sample | TTI (s) | pHRR (kW/m²) | THR (MJ/m²) | MAHRE (kW/m²) | Residue (%) |
---|---|---|---|---|---|
PA-0 | 154 ± 10 | 1416 ± 200 | 131 ± 5 | 337 ± 25 | - |
PA-1 | 94 ± 3 | 942 ± 37 | 117 ± 3 | 328 ± 7 | - |
PA-2 | 80 ± 5 | 893 ± 98 | 120 ± 1 | 345 ± 15 | - |
PA-3 | 88 ± 5 | 827 ± 95 | 115 ± 5 | 324 ± 23 | - |
PA-4 | 193 ± 20 | 1037 ± 102 | 115 ± 4 | 320 ± 15 | - |
AP30-0 | 122 ± 10 | 351 ± 5 | 92 ± 6 | 196 ± 4 | 31 ± 2 |
AP30-1 | 118 ± 3 | 347 ± 14 | 105 ± 5 | 197 ± 5 | 30 ± 3 |
AP30-2 | 144 ± 1 | 373 ± 2 | 81 ± 6 | 180 ± 10 | 27 ± 1 |
AP30-3 | 139 ± 3 | 363 ± 15 | 88 ± 8 | 192 ± 8 | 26 ± 1 |
AP30-4 | 143 ± 2 | 374 ± 14 | 86 ± 5 | 180 ± 10 | 27 ± 1 |
ZB30-0 | 115 ± 20 | 125 ± 15 | 95 ± 8 | 120 ± 10 | 38 ± 3 |
ZB30-1 | 214 ± 6 | 163 ± 70 | 92 ± 13 | 115 ± 15 | 35 ± 3 |
ZB30-2 | 189 ± 5 | 175 ± 61 | 98 ± 6 | 130 ± 14 | 33 ± 1 |
ZB30-3 | 252 ± 20 | 204 ± 19 | 101 ± 8 | 65 ± 8 | 25 ± 1 |
ZB30-4 | 180 ± 20 | 220 ± 22 | 95 ± 5 | 72 ± 5 | 29 ± 2 |
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Seigler, D.; Batistella, M.; Lopez-Cuesta, J.-M. Towards the Reuse of Fire Retarded Polyamide 12 for Laser Sintering. Materials 2024, 17, 4064. https://doi.org/10.3390/ma17164064
Seigler D, Batistella M, Lopez-Cuesta J-M. Towards the Reuse of Fire Retarded Polyamide 12 for Laser Sintering. Materials. 2024; 17(16):4064. https://doi.org/10.3390/ma17164064
Chicago/Turabian StyleSeigler, Dylan, Marcos Batistella, and José-Marie Lopez-Cuesta. 2024. "Towards the Reuse of Fire Retarded Polyamide 12 for Laser Sintering" Materials 17, no. 16: 4064. https://doi.org/10.3390/ma17164064