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

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
Lake Erie Chapter

February 16, 2010

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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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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PolyInsight (contd)
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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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Atomic-Force Microscopy (AFM)

Change in amplitude
provides topography

Lag in phase related

to viscoelasticity
or material stiffness

Free amplitude = Ao
Damped amplitude at
setpoint S = As
Ao

As
Society of Cosmetic Chemists
Lake Erie Chapter

Phase lag
February 16, 2010

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Atomic-Force Microscopy (AFM)

Veeco Dimension 3000 AFM
(large sample sizes)

Society of Cosmetic Chemists

Lake Erie Chapter

Veeco MultiMode AFM

(highest spatial resolution)

February 16, 2010

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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 m, so surfaces must be smooth
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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Surface Characterization via AFM

Roughness Analysis Surface of Polymer Stent

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Lake Erie Chapter

February 16, 2010

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Surface Characterization via AFM

NIST Gold 30nm spheres

Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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Surface Characterization via AFM

Nano-drug particles unknown size

Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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Particle size analysis using Veeco Nanoscope software

Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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)
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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)
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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)
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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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

Society of Cosmetic Chemists

Lake Erie Chapter

February 16, 2010

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Particulate gels in polymer modifiers

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Lake Erie Chapter

February 16, 2010

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Particulate gels in polymer modifiers

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Lake Erie Chapter

February 16, 2010

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Particulate gels in polymer modifiers

Good

Bad

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Lake Erie Chapter

February 16, 2010

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Surface structure of different nail polishes

Clear top coat

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Lake Erie Chapter

February 16, 2010

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Surface structure of different nail polishes

Metallic silver pigment in top coat

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Lake Erie Chapter

February 16, 2010

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Structure of Hair

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Lake Erie Chapter

February 16, 2010

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Surface structure of human hair

Deposit

Scales

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Lake Erie Chapter

February 16, 2010

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Surface structure of human hair

Society of Cosmetic Chemists

Lake Erie Chapter

February 16, 2010

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Internal structure of human hair

Cuticle

Cortex

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Lake Erie Chapter

February 16, 2010

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Internal structure of human hair

Cortex

Cuticle

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Lake Erie Chapter

February 16, 2010

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Internal structure of human hair

Cortex

Society of Cosmetic Chemists

Lake Erie Chapter

February 16, 2010

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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
Society of Cosmetic Chemists
Lake Erie Chapter

February 16, 2010

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