nano- and micromechanics - mrl.illinois.edu and... · the right tool for the job •sensitive...
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© 2015 University of Illinois Board of Trustees. All rights reserved.
Nano- and Micromechanics
Kathy Walsh, Ph.D.
Frederick Seitz Materials Research Laboratory University of Illinois at Urbana-Champaign
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How does stuff respond when you poke it, squeeze it, or stretch it?
Sample
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Sample
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The Right Tool for the Job
• Sensitive enough to measure the sample
– Appropriate force resolution
• Spatial resolution on an interesting scale
– Lateral resolution: 10s of nm, 100s of µm, mm
– Displacement: nm, µm, mm
Choose the Right Technique for Your Sample
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Small-Scale Mechanical Testing
• Nanoscale – AFM
– Nanoindenter
• Microscale – Nanoindenter
– Microindenter
• Milliscale – Rheometer (twisting)
– DMA (stretching, compressing)
DMA
Nanoindenter
AFM
Small-scale Mechanical Testing
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Why Measure Nano- or Micromechanical Properties?
• Mechanical properties help define materials
– Optimize applications
– Flexibility, biomechanical compatibility
– Crack formation, wear resistance
• Local composition variations in samples
– Spatially-resolved mechanical testing
• Samples may be inherently small
– Thin films, MEMS devices, nanopillars
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What Mechanical Properties Do People Measure?
• Quasistatic
– Elastic modulus
– Hardness
• Dynamic
– Time-dependent (viscoelastic) properties
– Storage modulus, loss modulus, tan delta
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What Mechanical Properties Do People Measure?
• Quasistatic
– Stress vs. strain curves
– Load (force) vs. displacement curves
• Dynamic
– Properties as a function of time or frequency
– Creep or stress relaxation
Load
Displacement
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How do People Measure Mechanical Properties?
• Quasistatic
– AFM force curves
– Nanoindentation, microindentation
– Stress vs. strain curves
• Dynamic
– AFM dynamic measurements
– nanoDMA, Modulus Mapping
– Dynamic Mechanical Analysis
nan
oscale m
icroscale m
illiscale
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How do People Measure Mechanical Properties?
• Quasistatic
– Nanoindentation, microindentation
• Elastic (Young’s) modulus
– Related to sample stiffness
• Hardness
– Related to amount of plastic deformation
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Micro- vs. Nanoindentation
• (Instrumented) microindentation is sometimes more useful
– Indents to greater depths
– Cares less about • Surface roughness
• Surface forces (adhesion)
Micro- vs. Nanoindentation
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Nanoindenter
Microindenter
Optical microscope (indent positioning)
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Instrumented Indentation
• Different names, same technique
– Nanoindentation
• Indentation depths shallower than a few µm
• Microindentation if deeper (some instruments)
– Instrumented Indentation
– Depth-Sensing Indentation
Record applied load and indent depth
Poke a sample and record its response
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Nanoindenter Basic Parts
Tip Transducer
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Nanoindenter Basic Parts
Tip Transducer
Stiff frame
Nanopositioning
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Why Does the Instrument Frame Stiffness Matter?
Tip
Stiff frame © 2015 University of Illinois Board of Trustees. All rights reserved.
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It’s Basically About the Tip and Sample
Tip Transducer
Stiff frame
Nanopositioning
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Nanoindenter Tips
• Tips are made of diamond or sapphire
– Tip characteristics are well-known
– Tip compliance is negligible
• Variety of shapes for different applications
– Induce different deformation mechanisms
– Berkovich, Vickers, cube corner
– Flat punch, conospherical (bending, soft materials)
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Nanoindenter Tips
• Nanoindentation
– Up to a few µm deep
– Up to several mN
• Most popular tip shape for nanoindentation:
– Berkovich 3-sided pyramid
Nanoindentation residual imprint Berkovich tip on aluminum foil (atomic force microscopy image)
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Microindenter Tips
• Microindentation
– Many µm deep
– Up to several N
• Most popular tip shape for microindentation:
– Vickers 4-sided pyramid
– Soft materials: sphere
Microindentation residual imprints Vickers tip on steel (bright field and dark field optical microscopy images)
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Contact Area
• Contact area between tip and sample
– Very, very important (crucial calibration)
– How much of your tip is applying force on how much of your sample?
– Depends on depth indented into sample
– Depends on roughness
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Vickers indent on steel (AFM image)
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Contact Area
• To ensure well-defined contact area between tip and sample…
• make your sample as smooth as possible
– Polishing
– But beware of work hardening
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vs.
smooth rough
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The 5% Rule
• Contact area between tip and sample
• Sample roughness should be ≤ 5% of indent depth…
• … indent 20x deeper than surface roughness
• Can get tricky for thin samples because of the 10% rule
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This indent is not deep enough to get good data
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The 10% Rule
• The substrate effect
• Indent depth should be ≤ 10% of sample thickness
• Indent too deep, start measuring the substrate
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feels like foam feels stiffer
vs.
sample
indent here
substrate
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The 5% and 10% Rules
• 5% rule and 10% rule are just rules of thumb… the actual values are sample-dependent
– Compliant sample on stiff substrate: can probably go deeper than 10%
– Stiff sample on compliant substrate: probably see substrate effect at depths shallower than 10%
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Performing an Indent Th
is is actually a n
on
-instru
me
nted
micro
ind
enter
can hold to do a creep/stress relaxation test
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Example Nanoindentation Data (Quartz)
Load P (few µN to few mN)
Displacement h (few tens of nm to few µm)
“Load—displacement curve”
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Example Nanoindentation Data (Quartz)
“Load—displacement curve”
loading curve
unloading curve
(optional) hold segment
to measure creep
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Example Nanoindentation Data (Quartz)
“Load—displacement curve”
unloading curve
fit for analysis
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Getting “the Answer”
Reduced modulus Hardness
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(Actually, , but just look up “fundamental equation of nanoindentation.”)
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Contact area: area of tip in contact with sample at a given depth
Why Does Contact Area Matter, Again?
Reduced modulus
Hardness
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Elastic from Reduced Modulus
Elastic (Young’s) modulus
Already known (diamond tips)
Poisson’s ratio of the sample
Measure using nanoindentation
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Many people just quote this value
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(Quasi)static vs. Dynamic Testing
• Many materials are somewhat viscoelastic
– Time-dependent mechanical behavior
• Creep or stress relaxation
– Hold a constant load or displacement for a long time
– Beware of drift
• Dynamic testing
creep
relaxation
creep and stress relaxation tests on nitrile glove
(Quasi)static vs. Dynamic Testing
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Nanomechanical Properties as a Function of Depth
hardness
and
(reduced) modulus
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indentation depth (tens of nm to few µm typical)
5% rule
surface effects and calibrations matter more for shallower indents
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Nanomechanical Properties as a Function of Depth
hardness
and
(reduced) modulus
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indentation depth (tens of nm to few µm typical)
10% rule
may start to measure substrate properties
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Nanoindentation Gives Nanomechanical Properties as a Function of Depth and Location
hardness
and
(reduced) modulus
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These indents were done at different places on the sample as well as at different depths
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Nanoindenters Are (Usually) Not Made for Soft Materials
• Nanoindenters are usually made for the “engineering materials” community
– Metals, composites, non-porous materials
• Using a traditional nanoindenter to study soft, compliant, porous, or sticky materials
– Usually doesn’t go deep enough
– Usually doesn’t have awesome enough force resolution
Measurements are Harder on Soft Materials
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~MPa comfortable modulus for nanoindentation (try AFM-based techniques for more compliant samples)
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Practical Concerns for Biomaterials
• Fixative changes mechanical properties!
– Fixative makes things stiffer
– If that’s the only way you can study your sample…
• Do a comparative study (no absolute numbers)
• Make control samples with just the fixative
• May need a heating cell/stage to stay at biorelevant temperatures
• May need to work in fluid
Practical Considerations for Biomaterials
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Keeping the “Hydro” in Hydrogel
• Keep wet samples wet
– Drying and rewetting can change properties
– Samples may dry out during measurements
• Don’t get fluid (or vapors) into the instrument
• Petri dishes, closed fluid cells, special tips
Keeping the “Hydro” in Hydrogel
standard
fluid-compatible
the tip is at the end
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Sample Preparation
• Know what your surface looks like first
– Look at it under an optical microscope
– Check sample roughness
• Mounting the sample
– Can’t measure mechanical properties of something that’s floating
– Compliant glue affects results
Sample Preparation
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Sample Mounting
• Glue (usually superglue)
– Porous samples may get partially filled with glue
– Some glue is designed for biological use
• Alternative sample mounting strategies
– Cast gels directly onto substrate
• Glass slide, Petri dish
– Wrap or clamp samples
• Don’t stress the area you want to measure
Sample Mounting
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How to Approach Your Data
• Oliver—Pharr model
– Elastoplastic materials
• But your samples may be…
– Sticky, compliant
– Poroelastic
– Viscoelastic
– Poroviscoelastic
– Thin films
Try continuous stiffness measurements
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JKR model
Do dynamic testing, creep/relaxation tests
Most people start here
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TA Instruments Q800 DMA clamps: dual cantilever, tension
Nano/micromechanical Testing Facilities
Asylum Cypher 5µm z range
30µm x 30µm scan size
Asylum MFP-3D-SA (x2) 15µm z range
90µm x 90µm scan size
Hysitron TI-950 TriboIndenter transducers: standard, nanoDMA,
high load (2.8N), AE, nanoECR
Nano/micromechanical Testing Facilities at MRL
DMA (milliscale) AFM (nanoscale)
Nanoindentation and Microindentation (nano/microscale)
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Recommended Reading
• Nanoindentation (3rd ed., 2011) – Anthony C. Fischer-Cripps
– Classic text on nanoindentation
• Handbook of Nanoindentation with Biological Applications – Michelle L. Oyen
– Soft materials people: read this one
• Both books are available for free online through the U of I library
Useful Books about Nanoindentation
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