Cryo-SEM-EDX 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. Cryo preparation is available for biological materials and other sensitive sample types. If compositional analysis is also needed, please see the SEM-EDX measurement. We also offer high-temperature SEM analyses at temperatures up to 1400 °C. Do not hesitate to ask for a quote.

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.

XPS is a semi-quantitative technique used to measure the elemental composition of material surfaces. In addition, it can also determine the binding state of the atoms. XPS is a surface-sensitive technique. Typical probing depth is 3-9 nm, and detection limits range roughly between 0.1 and 1 atomic %. XPS can measure elements from Li to U. The elemental composition is reported in at.% and measured on 1 area of a few 100 µm. Upon request, we can measure smaller areas or depth profiles, and a binding state determination can also be provided. Measurements are typically performed using one of the following instruments: PHI Genesis, Thermo Fisher ESCALAB 250Xi, PHI Quantum 2000. Synchrotron XPS is also available. Contact us for more information and a quote for your project.

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 with a transmission electron microscope (TEM). Typically, several images with varying magnifications are taken to get a good overview of the sample. TEM allows nm-resolution images. Solid samples often require FIB preparation before analysis. HR-TEM and cryo-TEM can also be provided. Contact us for more details.

The focused ion beam (FIB) technique is used to prepare samples for electron microscopy. It allows very precise cutting of samples to observe them by TEM or SEM imaging. We are happy to provide a quote for FIB preparation on its own, as well as FIB-TEM or FIB-SEM analysis.

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.

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.

In XPS depth profiling, ion gun etching cycles and XPS analysis cycles are alternated to obtain semi-quantitative information on the elemental composition (at.%) of the sample as a function of depth. The binding states of atoms can also be analyzed as a function of depth to determine the chemistry of the sample and its variations with depth. XPS depth profiling is a destructive technique with an analysis area diameter ranging from 10 µm to several 100 µm. Sputtering is done with an Ar-cluster GCIB ion beam or Ar monoatomic ions, and XPS measurements are typically performed using one of the following instruments: PHI Genesis, Thermo Fisher ESCALAB 250Xi, PHI Quantum 2000.