Sample preparation for analysis by electron microscopy and electron spectroscopy

Discover the innovative technology and software for electron microscopy sample preparation offered by Thermo Fisher Scientific. Our comprehensive solutions include FIB-SEM and PFIB-SEM tools and advanced automation software. These innovations streamline the preparation of high-quality, ultra-thin samples for SEM, TEM, and APT analysis, ensuring precise results and accelerating research in materials science. Explore our versatile DualBeam instruments and software packages designed for high-resolution imaging, 3D characterization, and in situ experiments, catering to a wide range of materials and applications.


How are samples prepared for scanning electron microscopy?

The scanning electron microscope (SEM) is a powerful tool for imaging and analyzing micro and nanostructures. Modern SEMs, such as the Thermo Scientific Quattro SEM with its unique Environmental SEM capability, can assess samples in any condition - wet, oily, or outgassing. For the best performance, SEM chambers typically operate under high vacuum, which requires dedicated sample preparations.

How are samples prepared for transmission electron microscopy?

Sample preparation for scanning/transmission electron microscopy (S/TEM) is a challenging and time-consuming task in materials characterization labs. Traditional methods for creating ultra-thin samples demand extensive time and expertise, hindering research progress. Thermo Fisher Scientific has pioneered sample preparation instruments and software for over 30 years, facilitating in situ TEM sample preparation, which accelerates research and innovation. 

 

DualBeam microscopes now enable the preparation of high-quality, ultra-thin samples for (S)TEM analysis. 

TEM preparation

FIB-SEM instruments should possess a number of essential characteristics to produce high quality samples. First is a high-resolution FIB column for fast and precise chunking step. Low kV FIB performance is extremely important as well for the final polishing step, to make sure amorphous layer produced by FIB milling is minimal in the prepared sample. Then, there are other critical components, like gas injection system and high precision manipulator that glue the steps of the lamella prep workflow together.  Finally, automation makes expert-level results accessible to users of all experience levels across various materials.

 

Thermo Scientific DualBeam instruments employ state of the art technologies to deliver users high quality results and ensure reliable and smooth experience while preparing S/TEM samples.

How are samples prepared for atom probe tomography?

Atom probe tomography (APT) provides atomic-resolution 3D compositional analysis of materials. Focused ion beam (FIB) microscopy uniquely allows for orientation and site-specific sample preparation for atom probe tomography characterization. Atom probe technique imposes strict requirements on sample size and shape, necessitating the production of sharp tips with 50-100 nm diameter and well-controlled shank angles to ensure efficient data collection. In many cases, cryogenic conditions are necessary to minimize structural changes in the sample during fabrication. 

 

FIB-SEM preparation of atom probe tomography tips enables precise control of sample shape, ensuring the inclusion of specific features. Thermo Scientific DualBeam instruments, equipped with a cryo stage and vacuum transfer, support further investigations. Sample quality can also be directly assessed during fabrication using scanning transmission electron microscopy (STEM) within the SEM.

APT showing Kappa Carbides in a high-Mn light-weight steel. Sample was prepared using Thermo Fisher Helios DualBeam APT showing Kappa Carbides in a high-Mn light-weight steel. Sample was prepared using Thermo Fisher Helios DualBeam

How are electron microscopy samples prepared for in situ characterization?

Electron microscopy tools offer a unique opportunity for in situ investigation of complex processes, including material responses to heating, biasing, or mechanical stress. This allows direct observation of structural and compositional changes within the microscope chamber using SEM imaging, EDS, and EBSD analyses. Alternatively, samples can be transferred to a transmission electron microscope for experimentation.

In situ characterization

FIB-SEM microscopes provide a versatile and site-specific approach for sample preparation for in situ techniques. They are used to fabricate various sample geometries, such as pillars, cantilevers, and dog-bone samples for mechanical testing, as well as lamellas for MEMS heating and other in situ TEM experiments. The precise stage with an extended tilt range (on PFIB and Hydra instruments) enables the creation of required sample geometries, while high-resolution SEM and FIB ensure precise manufacturing and control over sample dimensions. Sample size is often crucial, particularly for mechanical testing, where larger samples are needed to extrapolate results to macroscopic scales. Plasma FIB and laser technology are essential for efficiently preparing larger samples. Thermo Scientific's Python-based AutoScript Software offers custom automation for preparing non-standard samples, saving operator time and ensuring reproducible results.

 

Thermo Scientific DualBeam instruments can be configured with various accessories, including in situ heating stages (e.g., uHeater), tensile or compression testing stages, cryo stages, and more, to facilitate a wide range of in situ experiments.

Electron microscopy sample preparation instruments

Helios 5 DualBeam

High performance FIB-SEM for automated sample preparation. The fifth generation of the industry-leading Thermo Scientific Helios DualBeam family features the latest electron and ion beam technology, along with automation capabilities to enable advanced workflows in materials science.

 

Key Features:

  • Fully automated, high-quality, ultra-thin TEM sample preparation 
  • High throughput, high resolution subsurface and 3D characterization 
  • Rapid nanoprototyping capabilities

Helios 5 PFIB DualBeam

High throughput PFIB-SEM DualBeam. Exceptional capabilities for large-volume 3D characterization, gallium-free sample preparation, and precise micromachining.

 

Key Features:

  • Gallium-free STEM and TEM sample preparation 
  • Multi-modal, large volume subsurface and 3D information 
  • Next-generation, high throughput 2.5 μA xenon plasma FIB column

Helios 5 Hydra DualBeam

Multi-ion species PFIB-SEM DualBeam for the most demanding materials science characterization tasks. Exceptional, fast switchable multi-ion PFIB-SEM providing optimized results for a broad range of materials and use cases.

 

Key Features:

  • 4 fast switchable ion species (Xe, Ar, O, N) for optimized PFIB processing of a wide range of materials
  • Ga-free TEM sample preparation
  • Extreme high resolution SEM imaging
Helios 5 Hydra DualBeam Helios 5 Hydra DualBeam

Helios 5 Laser System

TriBeam instrument combining (P)FIB, SEM and fs-Laser. Fully integrated fs-Laser enables excellent material removal rates for fast mm-scale characterization with nanometer resolution. 

 

Key Features:

  • All three beams have same coincident point for accurate and repeatable cut placement 
  • Millimeter-scale cross sections with up to 15,000x faster material removal than a typical FIB 
  • Statistically relevant deep subsurface and 3D data analysis

Scios 2 DualBeam

Versatile FIB-SEM for broad range of materials science samples and use cases. Non-immersion, ultra-high-resolution analytical FIB-SEM system with advanced ease of use and automation capabilities that provides high quality sample preparation, subsurface and 3D characterization for a wide range of materials.

 

Key Features:

  • Full support of magnetic and non-conductive samples 
  • High throughput, multi-modal subsurface and 3D characterization 
  • Optional Low Vacuum capability

Electron microscopy sample preparation software

AutoTEM Software - (S)TEM sample preparation software for automated, high productivity creation of high-quality TEM samples

Thermo Scientific AutoTEM Software offers a comprehensive solution for DualBeam systems, enabling fully automated in situ S/TEM sample preparation across diverse materials. Users, regardless of experience, can rely on the system's unattended operation to consistently generate top-quality TEM samples.

Spin Mill - Software package for large area planar milling and 3D imaging

Spin Mill Science is a package within Thermo Scientific Auto Slice & View Software that enables site-specific large area polishing. This facilitates high-quality surface preparation for applications like EBSD analyses and 3D characterization. Available on Thermo Scientific PFIB and Hydra DualBeam systems, this software automates sequential milling and imaging of areas up to 1 mm.

AutoScript Software - Python-based application programming interface (API) that offers control of Thermo Scientific SEM and DualBeam systems to enable custom automation

Thermo Scientific AutoScript Software provides comprehensive microscope control for automating diverse tasks, from sample preparation for in situ mechanical testing to advanced image processing, computation, AI, and more, using Python libraries.

For Research Use Only. Not for use in diagnostic procedures.