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Introduction to Nano-scale Mechanical Properties Testing

Introduction to Nano-scale Mechanical Properties Testing. Micro Materials Ltd. Wrexham, UK. Outline. Depth-sensing indentation The NanoTest system Case studies Nanoindentation – bond pads Nano-impact – fatigue of DLC films Polymer nanoindentation Summary.

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Introduction to Nano-scale Mechanical Properties Testing

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  1. Introduction to Nano-scale Mechanical Properties Testing Micro Materials Ltd. Wrexham, UK.

  2. Outline • Depth-sensing indentation • The NanoTest system • Case studies • Nanoindentation – bond pads • Nano-impact – fatigue of DLC films • Polymer nanoindentation • Summary

  3. What is depth-sensing indentation? • elastic and plastic properties • of the sample determine the • shape of the unloading curve loading unloading coating substrate • force, displacement and time are recorded • throughout the indentation of a test sample • by a diamond probe Scanning = transverse sample movement during loading Impact = sample oscillation at constant load

  4. Where does depth-sensing indentation fit in? SPM Nanoindentation Macro-hardness • Surface • Friction • Adhesion (local) • (Wear) • Topography • Role of specific chemical interactions? • Surface/near-surface • Mechanical properties of thin films and coatings • Hardness • Modulus • Creep • Depth-profiling • Wear resistance • Interfacial adhesion • Fracture toughness • Bulk • Hardness of thick coatings and bulk materials • Fracture toughness of bulk materials

  5. Micro Materials Limited - growing market share in a fast growing market... Source: British Library on-line database. Keyword search on “nanoindentation”.

  6. The most versatile nanomechanical property testing centre... The NanoTest system 2 loading heads: Nano - 10 mN - 500 mN Micro - 0.1 N - 20 N 3 modules: Indentation Scanning Impact 10 options including: High temp testing Continuous compliance Pin-on-disk wear Microscopes

  7. The NanoTest pendulum • Advantages of the pendulum over vertical loading instruments include… • large samples possible • calibrated contact load • high temperature stage • sample oscillation • options such as pin-on- disk wear testing and 2D levelling stage Original design - University of Lancaster, UK, Newey, Wilkins and Pollock, J Phys E, 1982, pp119-122. Micro Materials formed 1988 by Dr Jim Smith, first instruments sold 1992.

  8. nickel plating passivation layer Si wafer Al pad Indentation Quantitative measurement of the mechanical properties of thin films Comparison of load ranges Technique Applied Force SPM nN-mN NanoTest 10 mN-500 mN MicroTest 100 mN - 20 N Hardness N-kN Aim: determine the hardness and modulus of top layer in IC bond pad without substrate influence

  9. Indentation NanoTest indentation module • Techniques • Nanoindentation • Microindentation • Load-partial-unload • High temperature testing • Continuous compliance • Properties • Hardness • Elastic modulus • Fracture toughness • Adhesion • Creep • Elastic and plastic work • Elastic recovery parameter • Stress-strain

  10. Indentation

  11. Indentation Depth-profiling of mechanical property variation Load-partial-unload technique 20-cycle load-partial-unload Depth controlled 50-1000 nm Experiment time 30 min Analysis time 30 sec • rapid and quantified • variation in hardness • and modulus with depth

  12. Indentation Hardness of 5 mm Ni-based top-layer of bond pad coating + substrate coating coating + substrate decreasing hardness constant hardness • “1/10 rule” - for a hard coating on softer substrate

  13. Indentation How homogeneous is my coating? An example of nanoindentation as a QA tool • rapid, automatic scheduling • of arrays of indentations

  14. Indentation Mapping variations in hardness and elasticity at the nanoscale Precise indent placement with a 4-objective high resolution metallurgical microscope NOTE: 1 objective can be replaced by contact/AC mode SPM Indentations along 10 mm alloy interface between stainless steel surfaces • studies of nano- and micro- scale phase separation

  15. Indentation Nanoindentation-induced adhesion failure DLC on Si Adhesion failure • indentation + residual stress = coating failure

  16. Scanning NanoTest scanning module • for… • Scratch testing • Nano- and micro- friction • Adhesion • Profilometry • Acoustic Emission • Fatigue wear “Nanotribometer”

  17. Scanning Ramped load scratch testing (1) Film failure at critical normal load Lc is revealed by... • Depth change • Acoustic Emission • Friction Force • Topography Scan • Optical Microscopy Adhesion failure at critical load of 3.2 mN

  18. Scanning Ramped load scratch testing (2) • qualitative ranking of test coatings and multilayers at the development stage

  19. dplast dtotal Scanning Multi-pass sub-critical load scratch testing 2, 4, 6 1, 3, 5, 7 Experimental parameters: 25 mm Rockwell probe scratch load:- ramped to 1 mN topography load 0.1 mN scan speed 0.5 mm/s Nano-scratching wear of polymer film • fatigue behaviour • cohesive failure (fracture) • adhesive failure (delamination) Repeat scratches over the same wear track reveal...

  20. Impact NanoTest impact module • for… • Impact testing • Contact fatigue testing • Erosive wear testing • Fracture toughness • Adhesion testing • Dynamic hardness The only commercial nano-impact tester available

  21. Impact Impact testing - simulating fatigue wear and failure • adhesion failure • fracture

  22. Impact Impact Testing of a brittle TiN coating 100 mN applied load is on throughout test 80 Hz oscillation frequency Oscillation on 30 s after start Oscillation off 30 s before end Film failure after 250 s • For bulk materials wear rates are determined from changes in probe depth • For coatings, time-to-failure is related to the bonding strength to the substrate

  23. To summarise…. 1. Nanoindentation techniques are essential in the optimisation of the mechanical properties of thin films and coatings 2. The NanoTest has large range of testing techniques, and therefore offers a complete testing capability 3. These techniques are possible due to the unique pendulum design 4. The high temperature option and impact module allow testing under contact conditions that can closely simulate those in service 5. The versatility and wide range of options have resulted in the system finding applications in….

  24. NanoTest systems are in regular use in… MIT USA Eastman Kodak USA Philips Netherlands HP Singapore Gintic Singapore Cambridge Uni UK Barcelona Uni Spain VITO Belgium NPL UK Enterprise Ireland Salford Uni UK Cranfield Uni UK Timken USA RPI NY USA AGFA DE LOT Oriel DE Paisley UK Loughborough UK TU Clausthal DE UMIST UK DERA UK Leeds Uni UK ICM Madrid Spain Trivandrum India ...and many more - over 75 sites worldwide

  25. Current NanoTest application areas include… • Automotive • Bearings • Biomedical Devices • Ceramics • Composites • Contact Lenses • Cutting Tools • Hard Coatings • Laminates • Magnetic Disks • Microelectronics • Optical Coatings • Optical Disks • Packaging Materials • Paints • Paper Coatings • Pharmaceuticals • Photographic Film • Polymers • Powders • Printing Plates • Semiconductors • Thin Film Adhesion • Turbine Blades ...future application areas will be in?

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