Abstract
Laser sintering (LS) of polyamide 12 (PA12) is increasingly being adopted for industrial production of end-use parts, yet the complexity of this process coupled with the lack of organized, rigorous, publicly available process-structure-physical property datasets exposes manufacturers and customers to risks of unacceptably poor part quality and high costs. Although an extensive scientific literature has been developed to address some of these concerns, results are distributed among numerous reports based on different machines, materials, process parameters, and users. In this study, a single commercially important LS PA12 feedstock has been processed along four build dimensions of a modern production LS machine, characterized by a wide range of physical techniques, and compared to the same material formed by conventional melt processing. Results are discussed in the context of the literature, offering novel insights including distributions of particle size and shape, localization of semicrystalline phase changes due to LS processing, effect of chemical aging on melt viscosity, porosity orientation relative to LS build axes, and microstructural effects on tensile properties and failure mechanisms. The resulting datasets will be made publicly available to modelers and practitioners for the purpose of improving certifiability and repeatability of end-use parts manufactured by LS.
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Notes
Identification of specific commercial equipment or materials in this publication is not intended to imply recommendation or endorsement by the Army Research Laboratory, nor is it intended to imply that the materials or equipment identified are necessarily the best available for the purpose
Certain commercial equipment, instruments, or materials are identified in this paper in order to specify the experimental procedure adequately. Such identification is not intended to imply recommendation or endorsement by the National Institute of Standards and Technology, nor is it intended to imply that the materials or equipment identified are necessarily the best available for the purpose.
References
(2014) ASTM F3091-14 standard specification for powder bed fusion of plastic materials. ASTM International: West Conshohocken
Tofail SAM, Koumoulos EP, Bandyopadhyay A, Bose S, O’Donoghue L, Charitidis C (2018) Additive manufacturing: scientific and technological challenges, market uptake and opportunities. Mater Today 21(1):22–37
Huang Y, Leu MC, Mazumder J, Donmez A (2015) Additive manufacturing: current state, future potential, gaps and needs, and recommendations. J Manuf Sci Eng 137(1):014001–014001-10
Gao W, Zhang Y, Ramanujan D, Ramani K, Chen Y, Williams CB, Wang CCL, Shin YC, Zhang S, Zavattieri PD (2015) The status, challenges, and future of additive manufacturing in engineering. Computer Aided Design 69:65–89
Hopkinson N (2006) Production economics of rapid manufacture. In: Hopkinson N, Hague RJM, Dickens P (eds) Rapid manufacturing: an industrial revolution for the digital age. Wiley, West Sussex, pp 147–158
Goodridge RD, Tuck CJ, Hague RJM (2012) Laser sintering of polyamides and other polymers. Prog Mater Sci 57(2):229–267
Yuan S, Shen F, Chua CK, Zhou K (2018) Polymeric composites for powder-based additive manufacturing: materials and applications. Prog Polym Sci 91:141–168
Schmid M (2018) Laser sintering with plastics. Carl Hanser Verlag GmbH & Co. KG, Munich
Fox B (2006) Rapid manufacture in the aeronautical industry. In: Hopkinson N, Hague RJM, Dickens P (eds) Rapid manufacturing: an industrial revolution for the digital age. Wiley, West Sussex, pp 221–232
Wooten J (2006) Aeronautical case studies using rapid manufacture. In: Hopkinson N, Hague RJM, Dickens P (eds) Rapid manufacturing: an industrial revolution for the digital age. Wiley, West Sussex, pp 233–240
Lyons B (2012) Additive manufacturing in aerospace: examples and research outlook. The Bridge: Linking Engineering and Society 42(1):13–19
Khajavi SH, Partanen J, Holmström J (2014) Additive manufacturing in the spare parts supply chain. Comput Ind 65(1):50–63
Spielman R (2006) Space applications. In: Hopkinson N, Hague RJM, Dickens P (eds) Rapid manufacturing: an industrial revolution for the digital age. Wiley, West Sussex, pp 241–248
Reuters, world’s biggest truck maker turns to 3D printing for spare parts. Fortune 2016, http://fortune.com/2016/07/13/daimler-trucks-3d-printing-spare/. Accessed 31 Oct 2018
LS allows 928 motorsports to improve Porsche 928 performance. Stratasys. https://www.stratasysdirect.com/resources/case-studies/3d-printing-selective-laser-sintering-porsche-engine-928-motorsports. Accessed 31 Oct 2018
Jin Y-a, Plott J, Chen R, Wensman J, Shih A (2015) Additive manufacturing of custom orthoses and prostheses—a review. Procedia CIRP 36:199–204
Deckers JP, Vermandel M, Geldhof J, Vasiliauskaite E, Forward M, Plasschaert F (2017) Development and clinical evaluation of laser-sintered ankle foot orthoses. Plast, Rubber Compos 47(1):42–46
Faustini MC, Neptune RR, Crawford RH, Stanhope SJ (2008) Manufacture of passive dynamic ankle-foot orthoses using selective laser sintering. IEEE Trans Biomed Eng 55(2 Pt 1):784–790
Harper NG, Russell EM, Wilken JM, Neptune RR (2014) Selective laser sintered versus carbon fiber passive-dynamic ankle-foot orthoses: a comparison of patient walking performance. J Biomech Eng 136(9):091001–091001–7
South BJ, Fey NP, Bosker G, Neptune RR (2009) Manufacture of energy storage and return prosthetic feet using selective laser sintering. J Biomech Eng 132(1):015001–015001-6
Idaho steel embraces 3D printing to deliver superior-quality parts faster. 3D Systems. https://www.3dsystems.com/learning-center/case-studies/idaho-steel-embraces-3d-printing-deliver-superior-quality-parts-faster. Accessed 31 Oct 2018
Balzereit S, Proes F, Altstädt V, Emmelmann C (2018) Properties of copper modified polyamide 12-powders and their potential for the use as laser direct structurable electronic circuit carriers. Addit. Manuf. 23:347–354
Beta LAYOUT—multi-dimensional circuit carriers using additive manufacturing. EOS. https://www.eos.info/case_studies/beta-layout-3d-printed-multidemsional-circuit-carriers. Accessed 31 Oct 2018
New Balance pushes the limits of innovation with 3D printing (2013) New Balance. https://www.newbalance.com/press-releases/id/press_2013_New_Balance_Pushes_Limits_of_Innovation_with_3D_Printing.html. Accessed 31 Oct 2018
Nike debuts first-ever football cleat built using 3D printing technology (2013) Nike News. https://news.nike.com/news/nike-debuts-first-ever-football-cleat-built-using-3d-printing-technology. Accessed 31 Oct 2018
Nike football accelerates innovation with 3D printed “Concept Cleat” for Shuttle (2014) Nike News. https://news.nike.com/news/nike-football-accelerates-innovation-with-3d-printed-concept-cleat-for-shuttle. Accessed 31 Oct 2018
The future of running is here (2016) New Balance. https://www.newbalance.com/article?id=4041. Accessed 31 Oct 2018
Kinematics dress (2014) Nervous System. https://n-e-r-v-o-u-s.com/projects/sets/kinematics-dress/. Accessed 31 Oct 2018
SLS design guide. 3D Systems. https://www.3dsystems.com/sites/default/files/2017-01/3dsystems-sls-designguide-2016.pdf. Accessed 31 Oct 2018
Bourell DL, Watt TJ, Leigh DK, Fulcher B (2014) Performance limitations in polymer laser sintering. Phys Procedia 56:147–156
Niino T, Sato K (2009) Effect of powder compaction in plastic laser sintering fabrication. Proceedings of the Solid Freeform Fabrication Symposium, pp 193–205
Aharoni SM (1997) n-Nylons: their synthesis, structure, and properties. Wiley, Chichester
Puffr R, Raab M, Dolezel B (1991) Properties. In: Puffr R, Kubanek V (eds) Lactam-based polyamides volume I: polymerization, structure, and properties. CRC Press, Boca Raton, pp 187–260
Holmes DR, Bunn CW, Smith DJ (1955) The crystal structure of polycaproamide: nylon 6. J Polym Sci 17(84):159–177
Bradbury EM, Brown L, Elliott A, Parry DAD (1965) The structure of the gamma form of polycaproamide (nylon 6). Polymer 6(9):465–482
Rhee S, White JL (2002) Crystal structure and morphology of biaxially oriented polyamide 12 films. J Polym Sci B Polym Phys 40(12):1189–1200
Inoue K, Hoshino S (1973) Crystal structure of nylon 12. J Polym Sci Polym Phys Ed 11(6):1077–1089
Schmid M, Amado A, Wegener K (2014) Materials perspective of polymers for additive manufacturing with selective laser sintering. J Mater Res 29(17):1824–1832
Kruth JP, Vandenbroucke B, Van Vaerenbergh J, Mercelis P (2005) Benchmarking of different SLS/SLM processes as rapid manufacturing techniques. Int Conf Polymers & Moulds Innovations
Seepersad CC, Govett T, Kim K, Lundin M, Pinero D (2012) A designer’s guide for dimensioning and tolerancing SLS parts. Proceedings of the Solid Freeform Fabrication Symposium, pp 921–931
Akande SO, Dalgarno KW, Munguia J, Pallari J (2016) Assessment of tests for use in process and quality control systems for selective laser sintering of polyamide powders. J Mater Process Technol 229:549–561
Pavan M, Craeghs T, Verhelst R, Ducatteeuw O, Kruth J-P, Dewulf W (2016) CT-based quality control of laser sintering of polymers. Case Studies in Nondestructive Testing and Evaluation 6:62–68
Schmid M, Kleijnen R, Vetterli M, Wegener K (2017) Influence of the origin of polyamide 12 powder on the laser sintering process and laser sintered parts. Appl Sci 7(5):462
Jacobi E, Schuttenberg H, Schulz RC (1980) A new method for gel permeation chromatography of polyamides. Makromol. Chem., Rapid Commun 1(6):397–402
Cureton LT, Napadensky E, Annunziato C, La Scala JJ (2017) The effect of furan molecular units on the glass transition and thermal degradation temperatures of polyamides. J Appl Polym Sci 134(46):45514
ISO/ASTM 52921-13 (2013) Standard terminology for additive manufacturing-coordinate systems and test methodologies. ASTM International, West Conshohocken
Usher JS, Gornet TJ, Starr TL (2013) Weibull growth modeling of laser-sintered nylon 12. Rapid Prototyp J 19(4):300–306
Tamari S (2004) Optimum design of the constant-volume gas pycnometer for determining the volume of solid particles. Meas Sci Technol 15(3):549–558
Taylor MA, Garboczi EJ, Erdogan ST, Fowler DW (2006) Some properties of irregular 3-D particles. Powder Technol 162(1):1–15
Van den Eynde M, Verbelen L, Van Puyvelde P (2015) Assessing polymer powder flow for the application of laser sintering. Powder Technol 286:151–155
Scholten H, Christoph W (1997) Use of a nylon-12 for selective laser sintering. US6245281B1, Evonik Degussa GmbH, EOS GmbH Electro Optical Systems
Meyer K-R, Hornung K-H, Feldmann R, Smigerski H-J (1979) Method for polytropically precipitating polyamide powder coating compositions where the polyamides have at least 10 aliphatically bound carbon atoms per carbonamide group. US4334056A, Huels AG
Baumann F-E, Monsheimer S, Grebe M, Christoph W, Heinrich D, Renners H, Scholten H, Schiffer T, Muegge J, Chiovaro J (2002) Polyamide powder with long-lasting, consistently good flowability. US7211615B2, Evonik Degussa GmbH
Dickens ED, Lee B-L, Taylor GA, Magistro AJ, Ng H, McAlea KP, Forderhase PF (1992) Sinterable semi-crystalline powder and near-fully dense article formed therewith. USRE39354E1, 3D Systems Inc.
Zarringhalam H, Hopkinson N, Kamperman NF, de Vlieger JJ (2006) Effects of processing on microstructure and properties of SLS nylon 12. Mater Sci Eng A 435-436:172–180
Garboczi EJ, Bullard JW (2013) Contact function, uniform-thickness shell volume, and convexity measure for 3D star-shaped random particles. Powder Technol 237:191–201
Amado A (2016) Characterization and prediction of SLS processability of polymer powders with respect to powder flow and part warpage. Ph.D. Thesis, ETH Zürich, Zürich, Switzerland
Wudy K, Drummer D (2019) Aging effects of polyamide 12 in selective laser sintering: molecular weight distribution and thermal properties. Additive Manufacturing 25:1–9
Dupin S, Lame O, Barrès C, Charmeau J-Y (2012) Microstructural origin of physical and mechanical properties of polyamide 12 processed by laser sintering. Eur Polym J 48(9):1611–1621
Haworth B, Hopkinson N, Hitt D, Zhong X (2013) Shear viscosity measurements on polyamide-12 polymers for laser sintering. Rapid Prototyp J 19(1):28–36
McAninch IM, Palmese GR, Lenhart JL, La Scala JJ (2015) DMA testing of epoxy resins: the importance of dimensions. Polym Eng Sci 55(12):2761–2774
Launay A, Marco Y, Maitournam MH, Raoult I (2013) Modelling the influence of temperature and relative humidity on the time-dependent mechanical behaviour of a short glass fibre reinforced polyamide. Mech Mater 56:1–10
Zarringhalam H, Majewski C, Hopkinson N (2009) Degree of particle melt in nylon-12 selective laser-sintered parts. Rapid Prototyp J 15(2):126–132
Zhao M, Wudy K, Drummer D (2018) Crystallization kinetics of polyamide 12 during selective laser sintering. Polymers 10(2):168
Paolucci F, Baeten D, Roozemond PC, Goderis B, Peters GWM (2018) Quantification of isothermal crystallization of polyamide 12: modelling of crystallization kinetics and phase composition. Polymer 155:187–198
Kline DB, Wool RP (1988) Polymer welding relations investigated by a lap shear joint method. Polym Eng Sci 28(1):52–57
Seppala JE, Hoon Han S, Hillgartner KE, Davis CS, Migler KB (2017) Weld formation during material extrusion additive manufacturing. Soft Matter 13(38):6761–6769
Majewski C, Zarringhalam H, Hopkinson N (2008) Effect of the degree of particle melt on mechanical properties in selective laser-sintered nylon-12 parts. Proc Inst Mech Eng B J Eng Manuf 222:1055–1064
Dencheva N, Nunes TG, Oliveira MJ, Denchev Z (2005) Crystalline structure of polyamide 12 as revealed by solid-state13C NMR and synchrotron WAXS and SAXS. J Polym Sci B Polym Phys 43(24):3720–3733
Monobe K, Fujiwara Y (1967) A study on single crystals of nylon 12. Memoirs of the School of Engineering, Okayama University, 2(1):88–92
Ishikawa T, Nagai S, Kasai N (1980) Effect of casting conditions on polymorphism of nylon-12. J Polym Sci Polym Phys Ed 18(2):291–299
Ishikawa T, Nagai S, Kasai N (1981) The γ → α partial transformation in nylon 12 by drawing. Die Makromolekulare Chemie 182(3):977–988
Nobuyasu H, Kazunao H, Susumu H (1983) Study of transformations among α, γ and γ' forms in nylon 12 by X-ray and DSC. Jpn J Appl Phys 22(2R):335
Li LB, Koch MHJ, de Jeu WH (2003) Crystalline structure and morphology in nylon-12: a small- and wide-angle X-ray scattering study. Macromolecules 36(5):1626–1632
Ramesh C (1999) Crystalline transitions in nylon 12. Macromolecules 32(17):5704–5706
Dadbakhsh S, Verbelen L, Verkinderen O, Strobbe D, Van Puyvelde P, Kruth J-P (2017) Effect of PA12 powder reuse on coalescence behaviour and microstructure of SLS parts. Eur Polym J 92:250–262
Xu F, Yan C, Shyng Y-T, Chang H, Xia Y, Zhu Y (2014) Ultra-toughened nylon 12 nanocomposites reinforced with IF-WS 2. Nanotechnology 25(32):325701
Jones NA, Atkins EDT, Hill MJ, Cooper SJ, Franco L (1996) Chain-folded lamellar crystals of aliphatic polyamides. Comparisons between nylons 4 4, 6 4, 8 4, 10 4, and 12 4. Macromolecules 29(18):6011–6018
Wu J, Xu X, Zhao Z, Wang M, Zhang J (2018) Study in performance and morphology of polyamide 12 produced by selective laser sintering technology. Rapid Prototyp J 24(5):813–820
Leigh DK (2012) A comparison of polyamide 11 mechanical properties between laser sintering and traditional molding. Proceedings of the Solid Freeform Fabrication Symposium:574–605
Stichel T, Frick T, Laumer T, Tenner F, Hausotte T, Merklein M, Schmidt M (2017) A round robin study for selective laser sintering of polyamide 12: microstructural origin of the mechanical properties. Opt Laser Technol 89:31–40
Osmanlic F, Wudy K, Laumer T, Schmidt M, Drummer D, Körner C (2018) Modeling of laser beam absorption in a polymer powder bed. Polymers 10(7):784
Murray BR, Leen SB, Semprimoschnig COA, Brádaigh CMÓ (2016) Helium permeability of polymer materials as liners for composite overwrapped pressure vessels. J Appl Polym Sci 133(29)
Hendra PJ, Maddams WF, Royaud IAM, Willis HA, Zichy V (1990) The application of Fourier transform Raman spectroscopy to the identification and characterization of polyamides—I. Single number nylons. Spectrochim Acta A: Mol Spectrosc 46(5):747–756
Verbelen L, Dadbakhsh S, Van den Eynde M, Kruth J-P, Goderis B, Van Puyvelde P (2016) Characterization of polyamide powders for determination of laser sintering processability. Eur Polym J 75:163–174
Brule B, Decraemer N (2014) Method for producing an object by melting a polymer powder in a powder sintering device. US20180001549A1, Arkema France
Greiner S, Wudy K, Wörz A, Drummer D (2019) Thermographic investigation of laser-induced temperature fields in selective laser beam melting of polymers. Opt Laser Technol 109:569–576
Craft G, Nussbaum J, Crane N, Harmon JP (2018) Impact of extended sintering times on mechanical properties in PA-12 parts produced by powderbed fusion processes. Addit Manuf 22:800–806
Rüsenberg S, Schmidt L, Schmid H-J (2011) Mechanical and physical properties—a way to assess quality of laser sintered parts. Proceedings of the Solid Freeform Fabrication Symposium, pp 239–251
Rouholamin D, Hopkinson N (2014) An investigation on the suitability of micro-computed tomography as a non-destructive technique to assess the morphology of laser sintered nylon 12 parts. Proc Inst Mech Eng B J Eng Manuf 228(12):1529–1542
Dewulf W, Pavan M, Craeghs T, Kruth J-P (2016) Using X-ray computed tomography to improve the porosity level of polyamide-12 laser sintered parts. CIRP Ann 65(1):205–208
Erdoğan ST, Garboczi EJ, Fowler DW (2007) Shape and size of microfine aggregates: X-ray microcomputed tomography vs. laser diffraction. Powder Technol 177(2):53–63
Majewski C, Hopkinson N (2011) Effect of section thickness and build orientation on tensile properties and material characteristics of laser sintered nylon-12 parts. Rapid Prototyp J 17(3):176–180
Starr TL, Gornet TJ, Usher JS (2011) The effect of process conditions on mechanical properties of laser-sintered nylon. Rapid Prototyp J 17(6):418–423
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The authors wish to thank Matt Bartucci, Daniel Cole, John La Scala, and Jian Yu for useful discussions.
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Bain, E.D., Garboczi, E.J., Seppala, J.E. et al. AMB2018-04: Benchmark Physical Property Measurements for Powder Bed Fusion Additive Manufacturing of Polyamide 12. Integr Mater Manuf Innov 8, 335–361 (2019). https://doi.org/10.1007/s40192-019-00146-3
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DOI: https://doi.org/10.1007/s40192-019-00146-3