Nano-Characterization
SEM | TEM |
---|---|
Particle morphology | (maybe) |
surface morphology | 2D projection - internal structure |
elemental analysis (yes eds) | yes (eds) |
10nm-500micron | 1nm - 5micron (but sub Å resolution) |
electron backscatter diffraction | electron diffraction |
- | EELS |
Low energy BSE: imaging, topograhpic etc | Electron diffraction, crysstallography |
High energy BSE: atom number contrast (bulk analysis) | |
Characteristic X-rays (EDX) | EDX; STEM-EDX |
Rare: Transmitted e-, bright field imaging | Bright + 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