The many experimental methods, originally designed to study the chemical and physical behavior of solids and liquids, have grown into a new field known as Materials Characterization (or Materials Analysis). During the past 30 years a host of techniques aimed at the study of surfaces and thin films has been added to the many tools for the analysis of bulk samples. The field has benefited particularly from the development of computers and microprocessors, which have vastly increased the speed and accuracy of the measuring devices and the recording of their output. Materials characterization was and is a very important tool in the search for new physical and chemical phenomena. It plays an essential role in new applications of solids and liquids in industry, communications, and medicine. Many of its techniques are used in quality control, in safety regulations, and in the fight against pollution.
In most Materials Characterization experiments the sample is subjected to some kind of radiation: electromagnetic, acoustic, thermal, or particles (electrons, ions, neutrons, etc.). The surface analysis techniques usually require a high vacuum. As a result of interactions between the solid (or liquid) and the incoming radiation a beam of a similar (or a different) nature will emerge from the sample. Measurement of the physical and/or chemical attributes of this emerging radiation will yield qualitative, and often quantitative, information about the composition and the properties of the material being probed.
The modern tendency of describing practically everything in this world by a combination of a few letters (acronyms) has also penetrated the field of Materials Characterization. The table below gives the meaning of the acronym for every technique listed, the form and size of the required sample (bulk, surface, film, liquid, powder, etc.), the nature of the incoming and of the emerging radiation, the depth and the lateral spatial resolution that can be probed, and the information obtained from the experiment. The last column lists one or two major references to the technique described.
Technique | Sample | In | Out | Depth | Lateral resolution | Information obtained | Ref. | |
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Optical and Mass Spectroscopies for Chemical Analysis | ||||||||
1. | AAS Atomic Absorption Spectroscopy | Atomize (flame, electro, thermal, etc.) | Light, e.g., glow discharge | Absorption spectrum | – | – | Concentration of atomic species (quantitative, using standards) | 1,2 |
2. | ICP-AES Induct. Coupled Plasma – Atomic Emission Spectroscopy | Atomize (flame, electro, thermal, ICP, etc.) | – | Emission spectrum | – | – | Concentration of atomic species (quantitative, using standards) | 3 |
3. | Dynamic SIMS Dynamic Secondary Ion Mass Spectroscopy | Surface | Ion beam (1–20 keV) | Secondary ions; analysis with mass spectrometer | 2 nm–1 µm (or deeper: ion milling) | 0.50 nm | Elemental and isotopic analysis; depth profile (all elements); detection limits: ppb-ppm | 4 |
4. | Static SIMS Static Secondary Ion Mass Spectroscopy | Surface | Ion beam (0.5–20 keV) | Secondary ions, analysis with mass spectrometer | 0.1–0.5 nm | 10 µm | Elemental analysis of surface layers; molecular analysis; detection limits: ppb-ppm | 4 |
5. | SNMS Sputtered Neutral Mass Spectroscopy | Surface, bulk | Plasma discharge; noble gases: 0.5–20 keV | Sputtered atoms ionized by atoms or electrons; then mass analyzed | 0.1–0.5 nm (or deeper: ion milling) | 1 cm | Elemental analysis Z ≥ 3; depth profile; detection limit: ppm | 4,6 |
6. | SALI Surface Analysis by Laser Ionization | Surface | e-beam, ion-beam, or laser for sputtering | Sputtered atoms ionized by laser; then mass analyzed | 0.1–0.5 nm up to 3 µm in milling mode | 60 nm | Surface analysis; depth profiling | 7 |
7. | LIMS Laser Ionization Mass Spectroscopy | Surface, bulk | u.v. laser (ns pulses) | Ionized species; analyzed with mass spectrometer | 50–150 nm | 5 µm–1 mm | Elemental (micro)analysis; detection limits: 1–100 ppm | 8 |
8. | SSMS Spark Source Mass Spectroscopy | Sample in the form of two electrodes | High voltage R.F. spark produces ions | Ions – analyzed in mass spectrometer | 1–5 µm | – | Survey of trace elements; detection limit: 0.01–0.05 ppm | 9 |
9. | GDMS Glow Discharge Mass Spectroscopy | Sample forms the cathode for a D.C. glow discharge | Sputtered atoms ionized in plasma | Ions – analyzed in mass spectrometer | 0.1–100 µm | 3–4 mm | (Bulk) trace element analysis; detection limit: sub-ppb | 9,10 |
10. | ICPMS Induct. Coupled Plasma Mass Spectroscopy | Liquid-dissolved sample carried by gas stream into R.F. induction coil | Ions produced in argon plasma | Ions – analyzed in quadrupole mass spectrometer | – | – | High-sensitivity analysis of trace elements | 11 |
Photons — Absorption, Reflection, and Electron Emission | ||||||||
11. | IRS Infrared Spectroscopy | Thin crystal, glass, liquid | I.R. light (W-filament, globar, Hg-arc) | I.R. spectrum | – | – | Electronic transitions (mainly in semiconductors and superconductors); vibrational modes (in crystals and molecules) | 12,13,14 |
12. | FTIR Fourier Transform I.R. Spectroscopy | Solid, liquid; transmission or reflection | White light (all frequencies) | Fourier transform of spectrum (interferometer) | – | – | Spectra obtained at higher speed and resolution | 15 |
13. | ATR Attenuated Total Reflection | Surface or thin crystal | – | – | µm’s | – | Atomic or molecular spectra of surfaces and films | 16 |
14. | (µ)-RS (Micro-) Raman Spectroscopy | Solid, liquid (1 µm–1 cm) | Laser beam, e.g., Ar-line, YAG-line | Raman spectra | 0.5 µm | 0.5 µm | Molecular and crystal vibrations | 12,14,17 |
15. | CARS Coherent Anti-Stokes Raman Spectroscopy | Solid, liquid (50 µm–3 cm) | Pump beam (ω0)+ probe beam (ωs) | Anti-Stokes spectrum | – | – | High-resolution Raman spectra | 14 |
16. | Ellipsometry | Transparent films, crystals, adsorbed layers | Polarized light | Change in polarization | 0.05 nm–5 µm | 25 µm (or sample thickness) | Refractive index and absorption | 18,19 |
17. | UPS Ultraviolet Photoelectron Spectroscopy | Surfaces, adsorbed layers | u.v. light, 10–100 eV; 200 eV (synchrotron) | Electrons | 0.2–10 nm | 0.1–10 nm | Energies of electronic states of surfaces and free molecules | 20,21 |
18. | PSD Photon Stimulated Desorption | Surfaces with adsorbed species | Far u.v. light E > 10 eV | Ions – analyzed with mass spectrometer | 0.1–2 nm | – | Structure and desorption kinetics of adsorbed atoms and molecules | 22 |
X-Rays | ||||||||
19. | XRD X-Ray Diffraction | Single crystals, powders films | x-rays: λ = 0.05–0.2 nm (6–17 keV) | Diffracted x-ray beam | 1–1000 µm | 0.1–10 mm | Identification of crystallographic structures; all elements (low Z difficult) | 23,24 |