Nano Indentation Lecture2

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  • 1. Do Kyung Kim Department of Materials Science and Engineering KAIST, Korea Nanoindentation Lecture 2 Case Study
  • 2. Applications of nanoindentation
    • Mechanical characterization of nanostructures
    • Pressure-induced phase transformation
    • Thin film and MEMS structure – mechanical properties
    • Biomechanics
    • Newly Developed Technique
  • 3. Mechanical Characterization of Nanostructures
  • 4. Carbon Nanotube (1)
    • Vertically aligned carbon nanotubes were prepared using PECVD method with different nickel catalyst thickness.
    • The nanoindentation on a VACNT forest consecutively bends nanotubes during the penetration of the indenter.
    Sample A Sample B Sample C Gleason, J Mech Phys Solids, 2003
  • 5. Carbon Nanotube (2)
    • The resistance of a VACNT forest to penetration is due to successive bending of nanotubes as the indenter encounters nanotubes
    • Superposition of interaction between the indenter and nanotubes encountered by the indenter during nanoindentation gives the total penetration resistance.
    Gleason, J Mech Phys Solids, 2003
  • 6. Carbon Nanotube (2)
    • Average f-p curve for the three samples from experiements
    • Sample C (high density, small length) Sample A, B (Same density) Sample A (Larger diameter and smaller length)
    Gleason, J Mech Phys Solids, 2003
  • 7. Silver Nanowire (1)
    • Silver nanowire-not single crystal but twinned-prepared from two silver solutions (AgNO3 and NaOH) and adhered onto glass slide.
    • Nanoindentation and imaging with same Berkovich indenter.
    • Penetration depth as low as 15 nm. (30 % of diameter)
    Caswell, Nano Letters, 2003
  • 8. Silver Nanowire (2)
    • Hardness 0.87 GPa / Elastic modulus 88 GPa
    • In good agreement with the nanoindentation value of bulk single crystal, 2 times higher than macroscale indentation results (indentation size effect)
    • This approach permits the direct machining of nanowires.
    Caswell, Nano Letters, 2003
  • 9. ZnO and SnO2 nanobelt (1)
    • The nanobelts were synthesized by thermal evaporation of oxide powder.
    • Indentation with maximum 300  N with loading rate 10  N/s
    Wang, APL, 2003
  • 10. ZnO and SnO2 nanobelt (2)
    • ZnO is a little softer than bulk single crystal.
    • The crack propagates along [101] and cleavage surface is (010).
    Wang, APL, 2003
  • 11. Pressure-induced Phase Transformation
  • 12. Silicon (1)
    • Single crystal silicon undergoes phase transformation during indentation
    • A sudden displacement discontinuity referred to as a pop-in
    • Upon unloading, pop-out or kink pop-out happen, resulting from a sudden material expansion
    Gogotsi, J Mater Res, 2004
  • 13. Silicon (2)
    • The average pop-in pressure is determined from pure elastic loading assumption.
    Gogotsi, J Mater Res, 2004
  • 14. Silicon (3)
    • Single and multiple pop-in events occurred during indentation
    • These events could be due to either subsurface cracking, squeezing out of ductile materials or sudden dislocation burtst
    1 mN/s 5 mN/s Gogotsi, J Mater Res, 2004
  • 15. Silicon (4)
    • A great amount of a-Si, Si-III, or Si-XII is at deeper rather than shallower depths for a number of unloading conditions.
    • The results from different wavelength spectrum show a-Si, Si-III, or Si-XII exist below the surface.
    • Pop-in, out  Si-III or Si-XII and No pop-in, out  a-Si
    Gogotsi, J Mater Res, 2004
  • 16. Germanium (1)
    • Nanoindentation experiments were performed using Berkovich and cube-corner indenters
    • The unloading pop-out or elbow phenomena was not observed in loading curve.
    • A number of displacement discontinuities in the loading curve are caused by discontinuous crack extension and chipping.
    Pharr, APL, 2005
  • 17. Germanium (2)
    • SEM observation of the cube corner hardness impressions revealed a thin layer of extruded material.
    • The micro-Raman spectra for cube-corner indentation exhibits distinct narrow Ge-IV and a-Ge peaks.
    • Ge-IV phased vanishes within 20 hours of removing pressure.
    Pharr, APL, 2005
  • 18. Thin Film and MEMS Structure – Mechanical Properties
  • 19. MEMS structure (1)
    • Silicon nanobeam fabricated by micromachining process
    • Load applied by indentation loading machine
    • Si strength-17.6 GPa (bulk single crystal strength 6 GPa)
    • Similar elastic modulus
    Li, Ultramicroscopy, 2003
  • 20. MEMS structure (2)
    • SiO2 microbeam fabrication by micromachining process
    • SiO2 strength 68 Gpa (18.5  m sample) / 2.5 Gpa (58.5  m sample)
    Lee, J Kor Ceram Soc, 2003
  • 21. Thin films – Al (1)
    • Aluminum single crystal (111) showing pop-in behavior
    • The maximum critical load 22  N  a mean pressure 14.7 GPa which is equivalent to a simplified estimate of the theoritical shear stress.
    • Dislocation is responsible for pop-in events.
    Moris Jr, J Mater Res, 2004
  • 22. Thin films – Al (2)
    • In situ nanoindentation
    • Approach  Contact  Plastic deformation  Extensive dislocation activity
    Moris Jr, J Mater Res, 2004
  • 23. Thin films – Al (3) Before indentation After indentation with same direction After indentation with tilted direction (dislocation in entire grain) Moris Jr, J Mater Res, 2004
  • 24. Residual stress (1)
    • Residual stress from
      • non-uniform cooling down from the processing temperature
      • deposition of a surface coating or a thin film on a substrate
    • Equal biaxial state of residual stress (tensile or compressive)
    Suresh, Acta Mater, 1998
  • 25. Residual stress (2)
    • Tensile
    • Compressive
    Suresh, Acta Mater, 1998
  • 26. Residual stress (3)
    • Implementation with ref. sample
    Suresh, Acta Mater, 1998
  • 27. Superlattice (1)
    • Nanscale multilayered coating
    • W/ZrN nanolayer
    • Superlattice period: 2.1 nm
    • Annealed at 1000  C for 1hr
    • AlN/VN nanolayer
    • Epitaxial stabilization of B1-AlN
    • Transformation to wurtzite
    Scott, MRS bulletin, 2003
  • 28. Superlattice (2)
    • Nanoindentation TiN/TiB2 superlattice
    Scott, MRS bulletin, 2003
  • 29. Biomechanics
  • 30. Dental hard tissue (1) Anisotropic structure of enamel Swain, J Mater Res, 2006
  • 31. Dental hard tissue (1)
    • Nanoindentation experiments on enamel with different orientation and indenter radius
    • Parallel to enamel rods, the hardness and modulus are 3.9 Gpa and 87.5 GPa, respectively , whereas perpendicular to enamel rods, they are 3.3 GPa and 72.2 GPa.
  • 32. Dental hard tissue (3)
    • The bacterial demineralization in enamel known as caries is simply detected through the changes in its mechanical properties.
  • 33. Dental hard tissue (4) Weihs, Archives of Oral Biology, 2002 Nanoindentation mapping of enamel tooth structure Lingual Buccal Pulp Dentin Hardness (GPa) 2.5 3 3.5 4.0 4.5 5 5.5 6 Lingual Buccal Pulp Dentin Elastic Modulus (GPa) 110 100 90 80 70 60 50 120
  • 34. Human bone (1)
    • Human Femur – cortical and trabecula bone lamellae
    Goldstein, J Biomech, 1999
  • 35. Human bone (2)
    • The mean elastic modulus was found to be significantly influenced by the type of lamella and by donor.
    • Hardness followed a similar distribution as elastic modulus among types of lamellae and donor.
    Goldstein, J Biomech, 1999
  • 36. Biocomposite (1)
    • Hydroxyapatite (HA) + polymethylmethacrylate (PMMA) + co-polymer coupling agent
    • In vitro interfacial mechanics of HA and PMMA cross section of the composite
    • Microscopic analysis
    • Indentation analysis (load-displacement curve)  more comprehensive local analysis
    • In vitro testing – a reduction of bulk bending, local elastic modulus, local hardness with increase of immersion time
    • The effect of coupling agent  improvement of the interfacial mechanics
    Marcolongo, IEEE Bioeng, 2004
  • 37. Biocomposite (2)
    • Human bone
      • 45-60% mineral: HA
      • 20-30% matrix: collagen
      • 10-20% water
    Marcolongo, IEEE Bioeng, 2004
  • 38. Biocomposite (3)
    • To determine the local mechanical properties of a bioactive composite a function of immersion period in simulated body fluid (SBF)  in vitro testing
    Marcolongo, IEEE Bioeng, 2004
  • 39. Biocomposite (4)
    • The “in vitro” local mechanical properties of the bioactive composite as a function of surface bioactivity
    Marcolongo, IEEE Bioeng, 2004
  • 40. Newly Developed Technique
  • 41. Cross-section of indentation damage(1) Indentation Pt Fast mill Tilt Markers Slow mill Lift-off Bradby, 2004
    • Focused ion beam TEM sample preparation
  • 42. Cross-section of indentation damage(2) Fast unloading Slow unloading Slip line Misc. defect Extended defect Bradby, 2004 Silicon
  • 43. Cross-section of indentation damage(3) GaAs InP Bradby, 2004
  • 44. Cross-section of indentation damage(4) GaN ZnO Bradby, 2004
  • 45. In-situ nanoindentation in SEM (1) Utke, 2006
  • 46. In-situ nanoindentation in SEM (2)
    • Vitreloy 105 (Zr 52.5 Cu 17.9 Ni 14.6 Al 10 Ti 5 )
    Partial correlation between shear band formation and displacement burst in P-h curve. Utke, 2006
  • 47. In-situ nanoindentation in SEM (3)
    • FEB deposited reference pattern for in situ measure of contact area
    Utke, 2006
  • 48. In-situ nanoindentation in SEM (4) Silicon pillar Median crack Basal crack Buckling Utke, 2006
  • 49. In-situ nanoindentation in TEM (1) Minor, 2002
  • 50. In-situ nanoindentation in TEM (2) Minor, 2002
  • 51. In-situ nanoindentation in TEM (3) Before After Minor, 2002
  • 52. Concluding remarks
    • Broad applications of Nanoindentation to investigate the mechanical properties!!!