Section: 12 | Techniques for Materials Characterization |
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John R. Rumble, ed., CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), CRC Press/Taylor & Francis, Boca Raton, FL.
If a specific table is cited, use the format: "Physical Constants of Organic Compounds," in CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), John R. Rumble, ed., CRC Press/Taylor & Francis, Boca Raton, FL.


H. P. R. Frederikse

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.

Experimental Techniques Used to Determine the Composition, Structure, and Energy States of Solids and Liquids

 TechniqueSampleInOutDepthLateral resolutionInformation obtainedRef.
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Optical and Mass Spectroscopies for Chemical Analysis
Atomic Absorption Spectroscopy
Atomize (flame, electro, thermal, etc.)Light, e.g., glow dischargeAbsorption spectrumConcentration of atomic species (quantitative, using standards)1,2
Induct. Coupled Plasma – Atomic Emission Spectroscopy
Atomize (flame, electro, thermal, ICP, etc.)Emission spectrumConcentration of atomic species (quantitative, using standards)3
3.Dynamic SIMS
Dynamic Secondary Ion Mass Spectroscopy
SurfaceIon beam (1–20 keV)Secondary ions; analysis with mass spectrometer2 nm–1 µm (or deeper: ion milling)0.50 nmElemental and isotopic analysis; depth profile (all elements); detection limits: ppb-ppm4
4.Static SIMS
Static Secondary Ion Mass Spectroscopy
SurfaceIon beam (0.5–20 keV)Secondary ions, analysis with mass spectrometer0.1–0.5 nm10 µmElemental analysis of surface layers; molecular analysis; detection limits: ppb-ppm4
Sputtered Neutral Mass Spectroscopy
Surface, bulkPlasma discharge; noble gases: 0.5–20 keVSputtered atoms ionized by atoms or electrons; then mass analyzed0.1–0.5 nm (or deeper: ion milling)1 cmElemental analysis Z ≥ 3; depth profile; detection limit: ppm4,6
Surface Analysis by Laser Ionization
Surfacee-beam, ion-beam, or laser for sputteringSputtered atoms ionized by laser; then mass analyzed0.1–0.5 nm up to 3 µm in milling mode60 nmSurface analysis; depth profiling7
Laser Ionization Mass Spectroscopy
Surface, bulku.v. laser (ns pulses)Ionized species; analyzed with mass spectrometer50–150 nm5 µm–1 mmElemental (micro)analysis; detection limits: 1–100 ppm8
Spark Source Mass Spectroscopy
Sample in the form of two electrodesHigh voltage R.F. spark produces ionsIons – analyzed in mass spectrometer1–5 µmSurvey of trace elements; detection limit: 0.01–0.05 ppm9
Glow Discharge Mass Spectroscopy
Sample forms the cathode for a D.C. glow dischargeSputtered atoms ionized in plasmaIons – analyzed in mass spectrometer0.1–100 µm3–4 mm(Bulk) trace element analysis; detection limit: sub-ppb9,10
Induct. Coupled Plasma Mass Spectroscopy
Liquid-dissolved sample carried by gas stream into R.F. induction coilIons produced in argon plasmaIons – analyzed in quadrupole mass spectrometerHigh-sensitivity analysis of trace elements11
Photons — Absorption, Reflection, and Electron Emission
Infrared Spectroscopy
Thin crystal, glass, liquidI.R. light (W-filament, globar, Hg-arc)I.R. spectrumElectronic transitions (mainly in semiconductors and superconductors); vibrational modes (in crystals and molecules)12,13,14
Fourier Transform I.R. Spectroscopy
Solid, liquid; transmission or reflectionWhite light (all frequencies)Fourier transform of spectrum (interferometer)Spectra obtained at higher speed and resolution15
Attenuated Total Reflection
Surface or thin crystalµm’sAtomic or molecular spectra of surfaces and films16
(Micro-) Raman Spectroscopy
Solid, liquid (1 µm–1 cm)Laser beam, e.g., Ar-line, YAG-lineRaman spectra0.5 µm0.5 µmMolecular and crystal vibrations12,14,17
Coherent Anti-Stokes Raman Spectroscopy
Solid, liquid (50 µm–3 cm)Pump beam (ω0)+ probe beam (ωs)Anti-Stokes spectrumHigh-resolution Raman spectra14
16.EllipsometryTransparent films, crystals, adsorbed layersPolarized lightChange in polarization0.05 nm–5 µm25 µm (or sample thickness)Refractive index and absorption18,19
Ultraviolet Photoelectron Spectroscopy
Surfaces, adsorbed layersu.v. light, 10–100 eV; 200 eV (synchrotron)Electrons0.2–10 nm0.1–10 nmEnergies of electronic states of surfaces and free molecules20,21
Photon Stimulated Desorption
Surfaces with adsorbed speciesFar u.v. light E > 10 eVIons – analyzed with mass spectrometer0.1–2 nmStructure and desorption kinetics of adsorbed atoms and molecules22
X-Ray Diffraction
Single crystals, powders filmsx-rays: λ = 0.05–0.2 nm (6–17 keV)Diffracted x-ray beam1–1000 µm0.1–10 mmIdentification of crystallographic structures; all elements (low Z difficult)23,24

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