Summary of NSF Surface Analysis Workshop

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Summary of NSF Surface Analysis Workshop

• Kettering University, Flint, Michigan
• 23-27 June 2003

Ronald Kumon Summer 2003
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Purposes of Workshop

• Provide an overview of a variety of surface
  analysis techniques and their applications
• Expose participants to cutting edge
  experimental equipment
• Share ideas for hands-on experiments that are
  primarily suitable for inclusion in an
  undergraduate curriculum

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Schedule

• Monday Overview, facilities tour,
  optical microscopy
• Tuesday Vibrational spectroscopy
  (Raman and IR)
• Wednesday Electron spectroscopy
  (ESEM, ESCA/XPS)
• Thursday Scanning probe microscopy
  (STM, AFM)
• Friday Conclusion and evaluation

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Participants

• 9 participants 6 chemistry, 3 physics
• Professors, postdocs, graduate students
• Universities, colleges, community colleges

Instructors

• Prof. Bahram Roughani, Physics
• Prof. Diana Phillips, Chemistry
• Mr. Robert Cunningham, Lab Coordinator

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Information from Surfaces

• Elemental composition
• Chemical composition
• Morphology
• Surface homogeneity
• Crystalline structure
• Elastic properties
• Electrical properties

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Examples of Applications

• Microelectronics
• Catalysis
• Nanotechnology
• Drug Delivery
• Fuel Cells
• Corrosion
• Coatings and Adhesion

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Applicable Courses

• Modern Physics
• Materials Characterization
• Physical Chemistry
• Polymer Chemistry
• Surface Analysis (special topics)
• Undergraduate Research
• Graduate Research

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Experimental Considerations

• What do you want to know?
• How fast do you need the answer?
• How much do you want to spend?
• Is the sample vacuum compatible?
• Does the sample absorb radiation?
• Do you need certain temperatures, pressures, or
  chemical environment?
• How stable is the samples surface?

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Vibrational Spectroscopy

• Infrared (IR) absorption
• Provides information about chemical bonding
• Done in transmission or reflection
• Raman scattering
• Provides information about chemical bonding,
  crystalline structure, etc.
• Weaker than dominant Rayleigh scattering

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Comparison of Spectra
Water vibrations

• Spectra are typically complementary

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IR Laboratory
Example of IR spectrum
Thermo Nicolet Avatar 360 FT-IR
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Raman Laboratory
Side view of Raman spectrometer
Sample holder and microscope
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Electron Micro-/Spectroscopy

• Environmental Scanning Electron Microscopy
  (ESEM)
• Electron Spectroscopy for Chemical Analysis
  (ESCA), a.k.a., X-ray Photoelectron Spectroscopy
  (XPS)

ESEM
ESCA
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ESEM Laboratory
Sample images
Environmental SEM and EDX system
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ESCA Laboratory
Front view of ESCA system
Top view of ESCA system
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Scanning Probe Microscopy

• Scanning Tunneling Microscopy (STM)
• Probability of electron tunneling varies
  exponentially from tip
• Atomic Force Microscopy (AFM)
• Sensitive to force between surface and tip
• Tip deflection measured by laser beam deflection
  of cantilever

STM
AFM
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STM Demonstration
View of probe tip through magnifier
Top view of STM
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AFM Demonstration
AFM probe tips
Pacific Nanotechnology AFM system
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AFM NDE Imaging
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Magnetic F.M. with Legos
Laser beam deflection changes when arm moves over
magnets
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Polymer Applications

• IR, Raman for uncured adhesive samples
• IR, Raman, ESCA, ESEM, AFM for cured adhesive
  samples
• Several samples of uncured and cured epoxy left
  at Kettering for further analysis
• Examples of various techniques shown on the next
  slides

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IR analysis of adhesion
Identification of adhesive material
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Raman imaging of epoxy
Raman image of thin film of rubber-toughened
epoxy resin at 1665 cm-1 Garton et al., Appl.
Spectrosc. 47, 922-927 (1993)
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ESCA of adhesion

• Painted plastic parts were glued to body of
  vehicle
• Samples with more Si tended to fail more often

(from U. W. Ontario Surface Science web site)
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ESEM and EDX analysis of cured epoxy
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AFM Imaging of Polymers
LFM
Structured polymer (topoLFM)
PCM
Block co-polymer (topoPCM)
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Conclusion

• Learned about surface analysis techniques
• Exposed to ideas for adding surface analysis
  methods into undergraduate and graduate
  curriculum
• Met other physicists and chemists
• Obtained some ideas about potential directions
  for future research

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Acknowledgments

• National Science Foundation
• Georgia State University
• Kettering University
• University of Windsor

Presentation archived at
http//ron.kumonweb.com/pro/research.html