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TMS 2013 , March 6, San Antonio, Texas

TMS 2013 , March 6, San Antonio, Texas. Structural Characterization and Mechanical Evaluations of Abalone Nacre-inspired Multilayer Coatings Synthesized by RF Sputtering and Pulsed Laser Deposition.

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TMS 2013 , March 6, San Antonio, Texas

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  1. TMS 2013,March 6, San Antonio, Texas Structural Characterization and Mechanical Evaluations of Abalone Nacre-inspired Multilayer Coatings Synthesized by RF Sputtering and Pulsed Laser Deposition Chang-Yu Sun1, Yu-Chen Chan1, Hsi-Ming Yang1, Tsung-Hao Hsu1, I. Lopez2, Gustavo A. Hirata3, Joanna McKittrick2, Jenq-Gong Duh1, Po-Yu Chen1 1Department of Materials Science and Engineering, National TsingHua University, Hsinchu 30013, Taiwan 2Mechanical and Aerospace Engineering, University of California, San Diego, La Jolla, CA 92093, USA 3Center for Nanoscience and Nanotechnology-UNAM, Ensenada 22860, México Research support: National Science Council, Taiwan (NSC100-2218-E-007-016-MY3)

  2. Outline • Abalone nacre • Hierarchical structure • Toughening mechanisms • Role of the organic layer • Hybrid PVD system design for bio-inspired coatings • Structural characterization and mechanical evaluations of multilayer nacre-inspired films • Future work • Conclusions

  3. 10:1 2:1 4:1 B4C/Al 4 0 0 3 5 0 3 0 0 Work of fracture 1000X higher for nacre than aragonite. Why? 2 5 0 Specific Flexural Strength [MPa/(g/cc)] Al2O3/Al 2 0 0 1 5 0 B4C nacre Al2O3 1 0 0 CaCO3 5 0 0 non laminate laminate Abalone Nacre • Biological composite: 95 wt.% mineral (CaCO3: aragonite/calcite) 5 wt.% biopolymer (proteins and chitin) + ? = Red abalone (Haliotisrufescens) F. Heinemann, et al. BiophysChem 2011;153:126-53. Adapted from M. Sarikaya, University of Washington

  4. 5µm Abalone Nacre • Hierarchical structure: From macro- to nano-scale Mineral Bridges Mesolayers Abalone Shell: Nacre Aragonite Tiles Chitin fibril network M. A. Meyers, et al. Mater SciEng C (2010) 29:2398–410. M. A. Meyers, et al. J MechBehavBiomed Mater (2008) 1:76–85.

  5. Toughening Mechanisms • Macro-scale: crack deflection plastic microbuckling R. Menig, et al. Acta Mater (2000) 48:2383–98. A. Lin and M. A. Meyers. Mater SciEng A (2005) 390:27-41. • Micro-scale: tile pull out (inter-tile sliding) A. Lin and M. A. Meyers. Mater SciEng A (2005) 390:27-41.

  6. Toughening Mechanisms • Nano-scale: asperities organic layer acting as viscoelastic glue Combination mineral bridges M. A. Meyers, et al. J MechBehav Biomed Mater (2011) 4:626-57. M. A. Meyers, et al. J MechBehav Biomed Mater (2008) 1:76–85. M.A. Meyers et al. Prog Mater Sci (2008) 53:1–206. Nanoscale features at the organic/inorganic interface are the key to the fracture resistance.

  7. Role of the Organic Layer • Nanoscratch test Organic fibers holding the tiles together can be seen in untreated samples Deproteinized sample show debris and brittle fracture of the tiles M. I. Lopez et al., to be published

  8. Role of the Organic Layer • Nanoscratch test: Untreated Opening at tile interface Applied Load Crack deflection Trans-tile & Inter-tile fracture Penetration through multiple layers & Complete tile fracture M. I. Lopez et al., to be published

  9. Role of the Organic Layer • Nanoscratch test: Deproteinized Trans-tile & Inter-tile fracture Applied Load Crack Propagation Unobstructed Fracture Propagation Complete shattering (Debris) Mineral bridges Asperities/roughness M. I. Lopez et al., to be published

  10. Role of the Organic Layer • Nanoscratch test Mesolayer also plays a role in crack resistance (deflection) M. I. Lopez et al., to be published

  11. Nacre-inspired composites • Multiple routes have been developed to synthesize nacre-inspired composites Laminated ceramics Freeze casting S. Deville, et al. Science (2006) 311:515-8. E. Munch, et al. Science (2008) 322:1516-20. nacre ABS/epoxy M. E. Launey, et al. J R Soc Interface (2010) 7:741–753. H. D. Espinosa, et al. Nat Commun (2011) 2:173

  12. Nacre-inspired composites • Nacre-inspired thin films and coating applications Layer-by-layer deposition (LbL) Dip coating A. Sellinger, et al. Nature (1998) 394:256-60. Pros: simple, inexpensive, easy to control Cons: hard to be scaled up, weaker mechanical properties Z. Tang, et al. Nat Mater (2003) 2:413-8. Electrophoretic deposition Sputtering yields much better mechanical properties and quality of the deposited film, with the ability to scale up. However, it cannot deal with organic materials… T. H. Lin, et al. Chem Mater (2009) 21:2039–2044.

  13. Hybrid PVD System • A hybrid system combining RF sputtering and PLD was established to deposit inorganic and organic layers sequentially without breaking the vacuum chamber. Nd:YAG Laser Convergent Lenses Turbo Pump PLD Target Chamber Sputter Gun

  14. Hybrid PVD System • A hybrid system combining RF sputtering and PLD was established to deposit inorganic and organic layers sequentially without breaking the vacuum chamber. (a) RF sputtering

  15. Hybrid PVD System • A hybrid system combining RF sputtering and PLD was established to deposit inorganic and organic layers sequentially without breaking the vacuum chamber. (b) Pulsed Laser Deposition

  16. Multilayer Coatings • Several materials systems have been investigated:

  17. Multilayer Coatings ZrN PMMA • Preliminary results ZrN/PMMA Hirata et al., 2010 MRS Proceeding Compare: Al2O3/Polyimide Al2O3 polyimide Al2O3 Hardness and elastic modulus from nano-indentation tests showed no significant dependence on the number of polymer layers. Abalone nacre XPS O 1s KLL C 1s film MVV target PMMA

  18. Multilayer Coatings • Preliminary results ZrO2/Polyimide SEI BEI ZrO2 ZrO2 polyimide ZrO2 ZrO2 Polyimide The preferred c-axis columnar growth of RF-sputtered ZrO2 may become beneficial for mimicking the mineral bridges.

  19. Future Work 1. Thickness 2. Organic/inorganic volume fraction 3. Interfacial roughness 4. Mineral bridges

  20. Conclusions • Abalone nacre developed a “brick and mortar” microstructure to enhance its toughness. The nanoscale features are the key factors. • The organic layers play important roles on crack resistance. • A hybrid PVD system combining RF-sputtering and PLD have been established to deposit novel organic-inorganic multilayer coatings. • Many multilayer systems have been successfully deposited. • Mechanical properties and microstructures of the films have been preliminarily characterized.

  21. Acknowledgements • Technical work and advice provided by Hsien-Wei Chen, Li-Chi Hsu, and Prof. Jyh-Wei Lee • Department of MSE, National TsingHua University and Department of MSE, Ming Chi University of Technology • Financial support: • National Science Council, Taiwan (NSC-100-2218-E-007-016-MY3) • National Science Foundation, USA (DMR 1006931) • East Asia and Pacific Summer Institutes – NSF-NSC Summer Institute in Taiwan Scholarship

  22. Thank you for your attention !!

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