TEM imaging

Imaging of the sample using scanning electron microscopy (SEM). Typically, several images are taken with varying magnifications to get a good overview of the sample. Non-conductive samples can be prepared with a metallic coating to allow imaging. For cross-section measurement, additional preparation might be needed: FIB, BIB or freeze fracturing. If compositional analysis is also needed, please see the SEM-EDX measurement.

Imaging of the sample with transmission electron microscopy (TEM) and determination of the elemental composition of the sample using electron dispersive X-ray spectroscopy (EDX or EDS). Several images with varying magnifications are taken to get a good overview of the sample. An EDX mapping, line scan, or point measurement is collected to measure the sample composition (elemental at.% or wt.%). For solid samples, the analysis often requires FIB preparation, which is priced separately. HR-TEM can also be provided. Contact us for more details about the analysis options.

Imaging of the sample using a scanning electron microscope (SEM) with energy-dispersive X-ray spectroscopy (EDX or EDS). Typically, several images are taken with varying magnifications to get a good overview of the sample. An EDX mapping, line scan, or point measurement is collected to measure the sample composition (elemental at.% or wt.%). Non-conductive samples can be prepared with a metallic coating. For cross-section measurement, additional preparation might be needed: FIB, BIB, or freeze fracturing.

Nondestructive 3D analysis of internal structures by X-ray computed tomography. The method visualizes voids, cracks, density, and phase differences within solid structures. The method is most suitable for powdered materials, such as pharmaceutical and cosmetic ingredients. The resolution can go down to 2-3 µm for powders. Please contact us for more information about the analysis options for different materials and material dimensions.

Qualitative or comparative analysis of crystalline powders using X-ray diffraction (XRD). The analysis is only suitable for materials with at least one crystalline phase.

Particle size distribution (PSD) is determined from transmission electron microscopy (TEM) images. The method is most suitable for small particles of 50 nm or smaller. Depending on particle shapes, the method includes calculating the diameters or lengths and widths of particles. In addition to size, TEM provides qualitative information about the surface morphology of the particles. TEM is a good option for irregularly shaped and non-spherical particles such as fibers, rods, and crystals that cannot be characterized meaningfully with traditional methods, including laser diffraction (LD) and dynamic light scattering (DLS). As a result of the analysis, TEM images and the determined particle size distribution for diameter (or length and width) are delivered. Dry samples are suitable for TEM as is. If the particles are wet or dispersed in a solvent, the sample may be dried with a suitable sample preparation method before imaging.

Phase identification and quantification (Rietveld analysis) of a crystalline powder material using X-ray diffraction (XRD). The analysis can also provide unit cell dimensions. The analysis is only suitable for materials with at least one crystalline phase. The quantification accuracy is roughly 0.1 %, depending on the sample matrix and the phase in question. The available temperature range for XRD measurements is 25-1100 °C and the crystallinity can be studied as a function of temperatures. The measurements can be done under a normal atmosphere, inert gas, or vacuum. Please contact our experts to discuss the available temperature and atmosphere combinations. Please mention which crystalline phases your material contains and which ones are you interested in quantifying when requesting testing. However, the method can be applied to unknown phases as well. Either a tabletop or a synchrotron XRD can be used to perform the measurements.

Auger Electron Spectroscopy (AES) is a surface-sensitive technique (3-9 nm) used for compositional analysis and depth profiling, providing data on the elemental composition in depth. Secondary electron images can also be provided. AES is a very useful technique to measure patterns since it has a beam size that can go down to a few nm.

Hot-stage microscopy (HSM) analysis enables the direct visualization of materials under controlled temperature conditions. Capabilities include: Examining compound morphology and particle characteristics., Observing solid-solid transformations, melting/liquefaction, solidification, sublimation, and evaporation., Monitoring how different compounds interact, dissolve, or react with each other., Tracking crystal growth and growth rates., Utilizing the Kofler mixed fusion method for salt/co-crystal screening., Observing oxidation and other chemical reactions as they occur under heat.. The results will include microscope pictures and video showing the transitions during heating. Measurement specifications: Temperature range: 25 °C to 375 °C, Humidity control: 5–90% RH. Instrument details: The instrument set-up comprises a heating stage (hot stage) with a sample holder, coupled with a polarized-light microscope and a system that allows temperature measurements and video/picture recording.

X-Ray Reflectometry (XRR) analysis is used to measure the density (g/cm3), thickness (nm), and roughness (nm) of thin films. The method is applicable to the characterization of single- or multilayered thin films, as it provides information on the thickness and density of individual layers of the sample material as well as the roughness of the interphases. Greatest accuracy for XRR thickness measurements is generally achieved for samples containing 1-150 nm thick surface layers with under 5 nm RMS roughness. Thicker films and coatings with rougher surfaces can also be characterized, but the accuracy of thickness determination decreases as the thickness and roughness of the film or film stack increase. >150 mm wafers are typically cut to fit the sample holder. Please let us know if you need testing for larger wafers that cannot be cut into pieces. The available temperature range for XRR measurements is 25-1100 °C, and crystallinity can be studied as a function of temperature. The measurements can be performed under a normal atmosphere, inert gas, or vacuum. Measurements are typically performed using one of the following instruments: Rigaku SmartLab, Panalytical X'Pert Pro MRD, Bruker D8 Discover. Please let us know if you have a preference for a specific instrument.