Nano-Characterization

SEMTEM
Particle morphology(maybe)
surface morphology2D projection - internal structure
elemental analysis (yes eds)yes (eds)
10nm-500micron1nm - 5micron (but sub Å resolution)
electron backscatter diffractionelectron diffraction
-EELS
Low energy BSE: imaging, topograhpic etcElectron diffraction, crysstallography
High energy BSE: atom number contrast (bulk analysis)
Characteristic X-rays (EDX)EDX; STEM-EDX
Rare: Transmitted e-, bright field imagingBright + dark + high angle annular dark field imaging
  • Particle size through imaging and image scanning of particles (not directly crystallite size)

X-Ray diffraction

  • mg amount of powders
  • not individual NP’s
  • Bulk and average data
  • needles and planes can have preferred orientation (might alter the intensities)
  • Particle size information (Scherrer equation) can deviate from sem/tem because XRD relates to crystallite size, not directly particle size
  • How to differentiate Solid solution, phase segregation and core shell?
    • Solid solution: Vegards law: Unit cell volume varies with linearly with degree of substitution
    • Segregation: two phases are present, which shows XRD peaks from both phases
    • Core-shell: Same as segregation but consider significant peak broadening if one of the constituents are thin. (if either shell or core is thin)

XPS: Photoelectron scattering

  • UHV
  • Only surface (electrons must be able to escape)
  • NAP-XPS (near ambient pressure XPS) need synchrotron radiation
  • ARPES: Angle resolved Photo Emission Spectroscopy generates band structure information
  • Can give information on oxidation state
  • Only surface 2-5nm depth

FTIR

(and raman) will provide excellent information on functional groups in metalorganic molecules.

XANES

  • Can give information on oxidation states
  • X-Ray is used, so atmospheric pressure can be used.
  • Get information about bulk

NMR

  • Nuclear Magnetic Resonance

Importance of operando

  • you want information while the process is happening