High-resolution DIC analysis of in situ strain and crack propagation in coated AZ31 magnesium alloys under mechanical loading
Source abstract
Abstract
Abstract Biodegradable magnesium (Mg) alloys are promising for various biomedical applications but their susceptibility to corrosion poses significant challenges. This study systematically examines the microstructural integrity and failure mechanisms of electrochemically deposited phosphate- and fluorine-rich coatings on AZ31 Mg alloy subjected to three-point bending (3 PB) in both non-corrosive and physiological (HBSS) environments. High-resolution digital image correlation (HR-DIC) combined with scanning electron microscopy (SEM) enables in situ visualization and quantitative analysis of crack initiation, evolution, and propagation within the coatings. Our findings reveal that thinner (5 µm) coatings are prone to forming dense networks of fine cracks, while thicker (15 µm) coatings display fewer but wider cracks, with both morphologies strongly governed by localized shear strain. Importantly, cross-sectional analyses after load-holding demonstrate that, while surface cracks initially remain confined within the coating, cracks generated under higher mechanical loading can propagate through the entire coating thickness. These through-thickness cracks create direct pathways for corrosive fluids to access the underlying alloy, serving as initiation sites for stress corrosion cracking within the substrate. Furthermore, our results indicate that fluoride in the coating mitigates rapid corrosion. Overall, the study reveals that coating failure and the formation of through-thickness cracks play a critical role in facilitating localized corrosion and crack initiation within the alloy under combined mechanical and corrosive environments. Graphical Abstract
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Magnesium Alloys: Properties and Applications · Bone Tissue Engineering Materials · Titanium Alloys Microstructure and Properties
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (49)
Show source-provided references
1. Niranjan C, Raghavendra T, Rao MP, Siddaraju C, Gupta M, Jain VKS, Aishwarya R (2023) Magnesium alloys as extremely promising alternatives for temporary orthopedic implants—a review. J Magnes Alloys 11:2688–271810.1016/j.jma.2023.08.002 ↗
2. Xing F, Li S, Yin D, Xie J, Rommens PM, Xiang Z, Liu M, Ritz U (2022) Recent progress in Mg-based alloys as a novel bioabsorbable biomaterials for orthopedic applications. J Magnes Alloys 10:1428–145610.1016/j.jma.2022.02.013 ↗
3. Gutiérrez Púa LDC, Rincón Montenegro JC, Fonseca Reyes AM, Zambrano Rodríguez H, Paredes Méndez VN (2023) Biomaterials for orthopedic applications and techniques to improve corrosion resistance and mechanical properties for magnesium alloy: a review. J Mater Sci 58:3879–390810.1007/s10853-023-08237-5 ↗
4. Zhao D, Witte F, Lu F, Wang J, Li J, Qin L (2017) Current status on clinical applications of magnesium-based orthopaedic implants: a review from clinical translational perspective. Biomaterials 112:287–302. https://doi.org/10.1016/j.biomaterials.2016.10.01710.1016/j.biomaterials.2016.10.017 ↗
5. Vujović S, Desnica J, Stanišić D, Ognjanović I, Stevanovic M, Rosic G (2022) Applications of biodegradable magnesium-based materials in reconstructive oral and maxillofacial surgery: a review. Molecules 27:5529. https://doi.org/10.3390/molecules2717552910.3390/molecules27175529 ↗
6. Bonithon R, Kao AP, Fernández MP, Dunlop JN, Blunn GW, Witte F, Tozzi G (2021) Multi-scale mechanical and morphological characterisation of sintered porous magnesium-based scaffolds for bone regeneration in critical-sized defects. Acta Biomater 127:338–352. https://doi.org/10.1016/j.actbio.2021.03.06810.1016/j.actbio.2021.03.068 ↗
7. Espiritu J, Meier M, Seitz J-M (2021) The current performance of biodegradable magnesium-based implants in magnetic resonance imaging: a review. Bioact Mater 6:4360–4367
8. Dubey VP, Kopec M, Kowalewski ZL (2021) Insight of magnesium matrix nanocomposites for biomedical applications: a synthetic review. XXII Polish Conference on Biocybernetics and Biomedical Engineering (PCBBE), Abstract Book, Warsaw, May 19–21, 2021. Available from: https://www.researchgate.net/publication/351839663
9. Zhang X, Mao J, Zhou Y, Ji F, Chen X (2021) Mechanical properties and osteoblast proliferation of complex porous dental implants filled with magnesium alloy based on 3D printing. J Biomater Appl 35:1275–128310.1177/0885328220957902 ↗
10. Li D, Zhang D, Yuan Q, Liu L, Li H, Xiong L, Guo X, Yan Y, Yu K, Dai Y (2022) In vitro and in vivo assessment of the effect of biodegradable magnesium alloys on osteogenesis. Acta Biomater 141:454–46510.1016/j.actbio.2021.12.032 ↗
11. Wang Y, Huang H, Jia G, Zeng H, Yuan G (2021) Fatigue and dynamic biodegradation behavior of additively manufactured Mg scaffolds. Acta Biomater 135:705–72210.1016/j.actbio.2021.08.040 ↗
12. Tkacz J, Slouková K, Minda J, Drábiková J, Fintová S, Doležal P, Wasserbauer J (2017) Influence of the composition of the hank’s balanced salt solution on the corrosion behavior of AZ31 and AZ61 magnesium alloys. Metals 7:1–17. https://doi.org/10.3390/met711046510.3390/met7110465 ↗
13. Zehra T, Kaseem M, Hossain S, Ko Y-G (2021) Fabrication of a protective hybrid coating composed of TiO2, MoO2, and SiO2 by plasma electrolytic oxidation of titanium. Metals 11:1182. https://doi.org/10.3390/met1108118210.3390/met11081182 ↗
14. Liu J, Liu B, Min S, Yin B, Peng B, Yu Z, Wang C, Ma X, Wen P, Tian Y (2022) Biodegradable magnesium alloy WE43 porous scaffolds fabricated by laser powder bed fusion for orthopedic applications: process optimization, in vitro and in vivo investigation. Bioact Mater 16:301–319
15. Sankara Narayanan TSN, Park IS, Lee MH (2014) Strategies to improve the corrosion resistance of microarc oxidation (MAO) coated magnesium alloys for degradable implants: prospects and challenges. Progr Mater Sci 60:1–71. https://doi.org/10.1016/j.pmatsci.2013.08.00210.1016/j.pmatsci.2013.08.002 ↗
16. Jiang P, Blawert C, Bohlen J, Zheludkevich ML (2020) Corrosion performance, corrosion fatigue behavior and mechanical integrity of an extruded Mg4Zn0.2Sn alloy. J Mater Sci Technol 59:107–116. https://doi.org/10.1016/j.jmst.2020.04.04210.1016/j.jmst.2020.04.042 ↗
17. L. Prawin Babu, R. Radha (2024) Advancements in magnesium-based alloys for orthopedic implants: balancing corrosion, mechanical properties, and biological effects (part 1)–a review. Can Metall Q, pp 1–2610.1080/00084433.2024.2427455 ↗
18. Matykina E, Garcia I, Arrabal R, Mohedano M, Mingo B, Sancho J, Merino MC, Pardo A (2016) Role of PEO coatings in long-term biodegradation of a Mg alloy. Appl Surf Sci 389:810–823. https://doi.org/10.1016/j.apsusc.2016.08.00510.1016/j.apsusc.2016.08.005 ↗
19. Hornberger H, Virtanen S, Boccaccini AR (2012) Biomedical coatings on magnesium alloys—a review. Acta Biomater 8:2442–2455. https://doi.org/10.1016/j.actbio.2012.04.01210.1016/j.actbio.2012.04.012 ↗
20. Koo Y, Jang Y, Yun Y (2017) A study of long-term static load on degradation and mechanical integrity of Mg alloys-based biodegradable metals. Mater Sci Eng B Solid-State Mater Adv Technol 219:45–54. https://doi.org/10.1016/j.mseb.2017.02.00910.1016/j.mseb.2017.02.009 ↗
21. Dorozhkin SV (2014) Calcium orthophosphate coatings on magnesium and its biodegradable alloys. Acta Biomater 10:2919–2934. https://doi.org/10.1016/j.actbio.2014.02.02610.1016/j.actbio.2014.02.026 ↗
22. Bonithon R, Lupton C, Roldo M, Dunlop JN, Blunn GW, Witte F, Tozzi G (2023) Open-porous magnesium-based scaffolds withstand in vitro corrosion under cyclic loading: a mechanistic study. Bioact Mater 19:406–417. https://doi.org/10.1016/j.bioactmat.2022.04.01210.1016/j.bioactmat.2022.04.012 ↗
23. Quan PH, Antoniac I, Miculescu F, Antoniac A, Manescu V, Robu A, Bița AI, Miculescu M, Saceleanu A, Bodog AD, Saceleanu V (2022) Fluoride treatment and in vitro corrosion behavior of Mg–Nd–Y–Zn–Zr alloys type. Materials 15:1–17. https://doi.org/10.3390/ma1502056610.3390/ma15020566 ↗
24. Yavuzyegit B, Karali A, De Mori A, Smith N, Usov S, Shashkov P, Bonithon R, Blunn G (2023) Evaluation of corrosion performance of AZ31 Mg alloy in physiological and highly corrosive solutions. ACS Appl Bio Mater. https://doi.org/10.1021/acsabm.3c0116910.1021/acsabm.3c01169 ↗
25. Denkena B, Köhler J, Stieghorst J, Turger A, Seitz J, Fau DR, Wolters L, Angrisani N, Reifenrath J, Helmecke P (2013) Influence of stress on the degradation behavior of Mg LAE442 implant systems. Procedia CIRP 5:189–195. https://doi.org/10.1016/j.procir.2013.01.03810.1016/j.procir.2013.01.038 ↗
26. Amer M, Hayat Q, Janik V, Jennett N, Nottingham J, Bai M (2022) A review on in situ mechanical testing of coatings. Coatings 12:299. https://doi.org/10.3390/coatings1203029910.3390/coatings12030299 ↗
27. Völker B, Du C, Fager H, Rueß H, Soler R, Kirchlechner C, Dehm G, Schneider JM (2020) How tensile tests allow a screening of the fracture toughness of hard coatings. Surf Coat Technol 390:125645. https://doi.org/10.1016/j.surfcoat.2020.12564510.1016/j.surfcoat.2020.125645 ↗
28. Ahmadi M, Salgın B, Kooi BJ, Pei Y (2021) Cracking behavior and formability of Zn–Al–Mg coatings: understanding the influence of steel substrates. Mater Des 212:110215. https://doi.org/10.1016/j.matdes.2021.11021510.1016/j.matdes.2021.110215 ↗
29. Chaieb HE, Maurel V, Ammar K, Forest S, Tanguy A, Héripré E, Nozahic F, Mataigne J-M, De Strycker J (2024) In-situ localization of damage in a Zn–Al–Mg coating deposited on steel by continuous hot-dip galvanizing. Scripta Mater 243:115960. https://doi.org/10.1016/j.scriptamat.2023.11596010.1016/j.scriptamat.2023.115960 ↗
30. Švec M, Nováková I, Solfronk P (2023) Determination of the effect of deformation on the corrosion resistance of Zn–Al–Mg coated sheets. Manuf Technol 23:709–716
31. Yavuzyegit B, Avcu E, Smith AD, Donoghue JM, Lunt D, Robson JD, Burnett TL, da Fonseca JQ, Withers PJ (2023) Mapping plastic deformation mechanisms in AZ31 magnesium alloy at the nanoscale. Acta Materialia 250:118876. https://doi.org/10.1016/j.actamat.2023.11887610.1016/j.actamat.2023.118876 ↗
32. Wu DJ, Mao WG, Zhou YC, Lu C (2011) Digital image correlation approach to cracking and decohesion in a brittle coating/ductile substrate system. Appl Surf Sci 257:6040–6043. https://doi.org/10.1016/j.apsusc.2011.01.11910.1016/j.apsusc.2011.01.119 ↗
33. Orozco-Caballero A, Lunt D, Robson JD, Da Fonseca JQ (2017) How magnesium accommodates local deformation incompatibility: a high-resolution digital image correlation study. Acta Mater 133:367–37910.1016/j.actamat.2017.05.040 ↗
34. Wang L, Wang H, Di Y, Zhao Y, Wang L (2020) Research on strain distribution and damage behavior of thermal barrier coatings based on digital image correlation. Int J Appl Ceram Technol 17:2156–2161. https://doi.org/10.1111/ijac.1352310.1111/ijac.13523 ↗
35. Gazenbiller E, Mansoor S, Konchakova N, Serdechnova M, Zheludkevich ML, Blawert C, Höche D (2022) Computational damage modelling of PEO coated extruded magnesium tested in slow strain rate configuration. Surf Coat Technol 446:128758. https://doi.org/10.1016/j.surfcoat.2022.12875810.1016/j.surfcoat.2022.128758 ↗
36. Li Y, Gao J, Yang L, Shen J, Jiang Q, Wu C, Zhu D, Zhang Y (2019) Biodegradable and bioactive orthopedic magnesium implants with multilayered protective coating. ACS Appl Bio Mater 2:3290–329910.1021/acsabm.9b00313 ↗
37. Abràmoff MD, Magalhães PJ, Ram SJ (2004) Image processing with ImageJ. Biophotonics International 11:36–42
38. Thomas R (2021) MechMicroMan/DefDAP: v0. 93.610.1007/978-3-030-64865-7_5 ↗
39. Yavuzyegit B (2022) Investigation of the deformation mechanisms of magnesium alloys at room and elevated temperature. The University of Manchester (United Kingdom)
40. Santos-Coquillat A, Mohedano M, Martinez-Campos E, Arrabal R, Pardo A, Matykina E (2019) Bioactive multi-elemental PEO-coatings on titanium for dental implant applications. Mater Sci Eng C 97:738–752. https://doi.org/10.1016/j.msec.2018.12.09710.1016/j.msec.2018.12.097 ↗
41. Dehnavi V, Shoesmith DW, Luan BL, Yari M, Liu XY, Rohani S (2015) Corrosion properties of plasma electrolytic oxidation coatings on an aluminium alloy—the effect of the PEO process stage. Mater Chem Phys 161:49–58. https://doi.org/10.1016/j.matchemphys.2015.04.05810.1016/j.matchemphys.2015.04.058 ↗
42. Lin ASP, Fechter CM, Magill M, Wipf F, Moore T, Guldberg RE (2016) The effect of contouring on fatigue resistance of three types of fracture fixation plates. J Orthop Surg Res 11:1–7. https://doi.org/10.1186/s13018-016-0439-110.1186/s13018-016-0439-1 ↗
43. Yang H, Huang L, Zhan M (2010) Coupled thermo-mechanical FE simulation of the hot splitting spinning process of magnesium alloy AZ31. Comput Mater Sci 47:857–866. https://doi.org/10.1016/j.commatsci.2009.11.01410.1016/j.commatsci.2009.11.014 ↗
44. Rao H, Thompson WA, Katz JL, Harper RA (1976) Elastic constants of the composite system hydroxyapatite-dicalcium phosphate dihydrate. J Dent Res 55:70810.1177/00220345760550043501 ↗
45. Akao M, Aoki H, Kato K (1981) Mechanical properties of sintered hydroxyapatite for prosthetic applications. J Mater Sci 16:809–81210.1007/BF02402799 ↗
46. Harun WSW, Asri RIM, Alias J, Zulkifli FH, Kadirgama K, Ghani SAC, Shariffuddin JHM (2018) A comprehensive review of hydroxyapatite-based coatings adhesion on metallic biomaterials. Ceram Int 44:1250–1268. https://doi.org/10.1016/j.ceramint.2017.10.16210.1016/j.ceramint.2017.10.162 ↗
47. Gao Y, Yerokhin A, Matthews A (2015) Mechanical behaviour of cp-magnesium with duplex hydroxyapatite and PEO coatings. Mater Sci Eng C 49:190–200. https://doi.org/10.1016/j.msec.2014.12.08110.1016/j.msec.2014.12.081 ↗
48. Zheng Y, Li Y, Chen J, Zou Z (2015) Effects of tensile and compressive deformation on corrosion behaviour of a Mg–Zn alloy. Corros Sci 90:445–45010.1016/j.corsci.2014.10.043 ↗
49. Kirkland NT, Birbilis N, Staiger MP (2012) Assessing the corrosion of biodegradable magnesium implants: a critical review of current methodologies and their limitations. Acta Biomater 8:925–936. https://doi.org/10.1016/j.actbio.2011.11.01410.1016/j.actbio.2011.11.014 ↗