Characterization Approaches for Solid Materials

This lecture covers the fundamental characterization approaches for solid materials, focusing on elemental analysis, inductively coupled plasma optical emission spectroscopy (ICP OES), mass spectrometry (MS), energy dispersive X-ray analysis (EDX), prompt gamma neutron activation analysis (PGAA), thermal analysis techniques like differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), and microscopy methods including scanning electron microscopy and transmission electron microscopy. The instructor explains the importance of elemental analysis in verifying material composition, the use of ICP OES and MS for different concentration ranges, and the surface sensitivity of EDX. Additionally, the lecture delves into the principles of neutron-based spectroscopies like inelastic neutron scattering (INS) and quasi-elastic neutron scattering (QENS), highlighting their role in studying vibrations and rotations within materials.

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Thermal analysis

Thermal analysis is a branch of materials science where the properties of materials are studied as they change with temperature.

Differential thermal analysis

Differential thermal analysis (DTA) is a thermoanalytic technique that is similar to differential scanning calorimetry. In DTA, the material under study and an inert reference are made to undergo identical thermal cycles, (i.e., same cooling or heating programme) while recording any temperature difference between sample and reference. This differential temperature is then plotted against time, or against temperature (DTA curve, or thermogram). Changes in the sample, either exothermic or endothermic, can be detected relative to the inert reference.

Thermogravimetric analysis

Thermogravimetric analysis or thermal gravimetric analysis (TGA) is a method of thermal analysis in which the mass of a sample is measured over time as the temperature changes. This measurement provides information about physical phenomena, such as phase transitions, absorption, adsorption and desorption; as well as chemical phenomena including chemisorptions, thermal decomposition, and solid-gas reactions (e.g., oxidation or reduction). Thermogravimetric analysis (TGA) is conducted on an instrument referred to as a thermogravimetric analyzer.

Transmission electron microscopy

Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through a specimen to form an image. The specimen is most often an ultrathin section less than 100 nm thick or a suspension on a grid. An image is formed from the interaction of the electrons with the sample as the beam is transmitted through the specimen. The image is then magnified and focused onto an imaging device, such as a fluorescent screen, a layer of photographic film, or a sensor such as a scintillator attached to a charge-coupled device.

Cryogenic electron microscopy

Cryogenic electron microscopy (cryo-EM) is a cryomicroscopy technique applied on samples cooled to cryogenic temperatures. For biological specimens, the structure is preserved by embedding in an environment of vitreous ice. An aqueous sample solution is applied to a grid-mesh and plunge-frozen in liquid ethane or a mixture of liquid ethane and propane. While development of the technique began in the 1970s, recent advances in detector technology and software algorithms have allowed for the determination of biomolecular structures at near-atomic resolution.