lescc presentation 2 16-2010
TRANSCRIPT
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Expert Vision for a Changing World
AFM Applications for Polymer and Particle Systems
PolyInsight LLC526 South Main Street, Suite 414
Akron, Ohio 44311(330) 777-0025
[email protected]://polyinsight.com
Michael P. Mallamaci, Ph.D.
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 2 of 30
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
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 3 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 4 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 5 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 6 of 30
Atomic-Force Microscopy (AFM)
Change in amplitudeChange in amplitudeprovides topographyprovides topography
Lag in phase relatedLag in phase relatedto viscoelasticityto viscoelasticity
or material stiffnessor material stiffness
Free amplitude = Free amplitude = AAooDamped amplitude atDamped amplitude atsetpoint S = setpoint S = AAss
AAoo AAssPhase lag
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 7 of 30
Atomic-Force Microscopy (AFM)
Veeco Dimension 3000 AFM(large sample sizes)
Veeco MultiMode AFM(highest spatial resolution)
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 8 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 9 of 30
Surface Characterization via AFM
Roughness Analysis – Surface of Polymer Stent
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 10 of 30
Surface Characterization via AFM
NIST Gold –
30nm spheres
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 11 of 30
Surface Characterization via AFM
Nano-drug particles –
unknown size
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 12 of 30
Particle size analysis using Veeco Nanoscope
software
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 13 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 14 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 15 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 16 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 17 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 18 of 30
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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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 19 of 30
Particulate gels in polymer modifiers
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 20 of 30
Particulate gels in polymer modifiers
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 21 of 30
Particulate gels in polymer modifiersBadGood
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 22 of 30
Surface structure of different nail polishesClear top coat
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 23 of 30
Surface structure of different nail polishes“Metallic silver” pigment in top coat
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 24 of 30
Structure of Hair
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 25 of 30
Surface structure of human hair
Scales
Deposit
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 26 of 30
Surface structure of human hair
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 27 of 30
Internal structure of human hair
Cuticle
Cortex
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 28 of 30
Internal structure of human hair
Cuticle
Cortex
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 29 of 30
Internal structure of human hair
Cortex
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February 16, 2010Society of Cosmetic ChemistsLake Erie Chapter
Slide 30 of 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