1. Expert Vision for a
Changing World
AFM Applications for Polymer and
Particle Systems
Michael P. Mallamaci, Ph.D.
PolyInsight LLC
526 South Main Street, Suite 414
Akron, Ohio 44311
(330) 777-0025
mike@polyinsight.com
http://polyinsight.com

2. Agenda
• Brief History of PolyInsight
• Atomic-Force Microscopy (AFM)
– Surface characterization technique
– Internal structure technique
• Using AFM in Cosmetic Science
– Particulate gels in polymer modifiers
– Surface structure of different nail polishes
– Surface structure of human hair
– Internal structure of human hair
• Summary / Q & A
Society of Cosmetic Chemists February 16, 2010 Slide 2 of 30
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3. PolyInsight
• Small team of experts in the physical and
chemical structure of rubber and plastics
• Laboratory operation with several
microscopes and related sample
preparation equipment in-house
• Located in Akron, Ohio at the Akron Global
Business Accelerator
• Partnerships with The University of Akron
and other regional laboratories providing
additional instrument access
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4. PolyInsight (cont’d)
• Continuous operation since July 2003
• Services include:
– Failure Analysis
– Atomic-Force Microscopy (AFM)
– Polymer and Chemical Analysis
– Consulting and Litigation Support
• Developed a portfolio of over 50 clients
nationally and overseas
• Medical/Healthcare, Automotive, Industrial
Coatings, and Consumer Products
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5. Atomic-Force Microscopy (AFM)
• High spatial resolution
imaging of surface
topography
• Similar to stylus
profilometry, except 1 nm
resolution
• Probe interacts with surface
to reveal mechanical
properties at high resolution
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6. Atomic-Force Microscopy (AFM)
Change in amplitude Lag in phase related
provides topography to viscoelasticity
or material stiffness
Free amplitude = Ao
Damped amplitude at
setpoint S = As
Ao As
Phase lag
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7. Atomic-Force Microscopy (AFM)
Veeco Dimension 3000 AFM Veeco MultiMode AFM
(large sample sizes) (highest spatial resolution)
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8. Surface Characterization via AFM
• The height of surface features can be
measured quantitatively with 0.1 nm
resolution
• Atomic step heights on crystals, DNA
molecules, proteins, semiconductor
lithography applications
• Maximum height of features allowed is ~
6 µm, so surfaces must be “smooth”
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9. Surface Characterization via AFM
Roughness Analysis – Surface of Polymer Stent
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10. Surface Characterization via AFM
NIST Gold – 30nm spheres
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11. Surface Characterization via AFM
Nano-drug particles – unknown size
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12. Particle size analysis using Veeco Nanoscope software
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13. Internal Structure via TEM
• Classic technique for
examining the structure of
composite materials is
Transmission-Electron
Microscopy (TEM)
• Materials must be thinned to
~ 100 nm or less to be
electron transparent
• Image contrast is based on
either electron diffraction
(crystalline materials) or
mass-density (amorphous
materials)
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14. Internal Structure of Soft Materials via TEM
• Sample preparation technique for obtaining
electron transparent thin sections is
cryoultramicrotomy
• Mass-density image contrast is enhanced by
using heavy-metal stains, such as RuO2 or OsO4
• TEM offers highest spatial resolution possible at
< 0.1 nm, plus chemical ID techniques
• Time-consuming sample preparation ($$$)
• Difficulty with complex multi-component systems
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15. Internal Structure of Soft Materials via AFM
• Probe interaction with the surface can
image “mechanical property” distribution
with high spatial resolution (1-5 nm)
• Cryoultramicrotomy must be used to
expose the internal structure – cut open in
cross-section and look at the surface
• Relies on surface structure being
representative of internal structure (just
like polished sections)
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16. Internal Structure of Soft Materials via AFM
• Incompatible 4
component
polymer blend
can be imaged
– PP (brightest)
– PA (round, less
bright)
– PE (dark orange)
– SEBS (black,
surrounds PA)
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17. Review of AFM Capabilities
• High spatial resolution imaging of surfaces
• Quantitative measurement of surface
roughness and particles on substrates
• Imaging of internal structure based on
mapping of mechanical properties
• Complex structures can be imaged, no
stains required
• Environmental control possible: air, inert
gas, temperature
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18. Using AFM in Cosmetic Science
• Particulate gels in polymer modifiers
– Appearance, processing
• Surface structure of different nail polishes
– Reflectivity, composition
• Surface structure of human hair
– Damage, deposits
• Internal structure of human hair
– Dyeing
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19. Particulate gels in polymer modifiers
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20. Particulate gels in polymer modifiers
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21. Particulate gels in polymer modifiers
Good Bad
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22. Surface structure of different nail polishes
Clear top coat
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23. Surface structure of different nail polishes
“Metallic silver” pigment in top coat
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24. Structure of Hair
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25. Surface structure of human hair
Deposit
Scales
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26. Surface structure of human hair
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27. Internal structure of human hair
Cuticle
Cortex
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28. Internal structure of human hair
Cortex
Cuticle
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29. Internal structure of human hair
Cortex
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30. Summary
• AFM has unique strengths as a high
resolution microscopy technique
• Routine use as a tool for cosmetic
chemists is possible: can “see” things that
other techniques cannot
• Offers quantitative microscopic
measurement tool for “soft” cosmetic
systems
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