Back to News
characterization  |  featured

Advanced TEM Sample Preparation

Peng Li
2023-10-19
The ThermoFisher Helios Hydra Plasma FIB offers advanced, damage-free TEM lamella preparation with enhanced flexibility and high throughput for various materials.
characterization | featured

Focused Ion Beam (FIB) provides preparation of site-specific, high-quality S/TEM samples for a wide range of materials. Unlike the conventional Ga-FIB, which has slow milling rate, results in Ga damage/implantation, the ThermoFisher Helios Hydra Plasma FIB (equipped with multiple inert ion species - Xe and Ar) overcomes those unwanted effects and produces damage free TEM lamellas./

The latest technological innovations on the Hydra PFIB microscope, such as flexible control of micro-manipulator and stage, multi-precursor gas injection system (GIS), along with well integrated software solutions, enable fast and easy lamella preparation with high throughput for TEM analysis, less dependent on the operators’ experience.

Our Characterization team is pleased to announce that all advanced processing for TEM lamella preparation on the Hydra PFIB have been successfully commissioned, including:

  • Low voltage Xe and Ar beams to produce damage free samples
  • Micro-manipulator (EasyLift) with continuous axial rotation, enabling flexible pluckouts, such as 90-degree / inverted pluckouts for both cross-sectional and plan-view preparation.
  • Multiple precursors for Gas Injection System (GIS): C, Pt, W, providing flexible capping films for materials with different hardness and backfilling for porous materials.
  • Automatic Lamella Sample preparation: fully automatic site preparation and software-assisted pluckout and final polishing.

Our user groups have utilized those techniques to produce TEM samples for their characterization needs. If you are interested in preparing TEM lamellas on the Hydra PFIB system, user training and staff analysis are available. Please submit a request (training or sample type) with sample details on LMACS. If you have any questions, please feel free to contact Dr. Shihong Xu (shihongx@ualberta.ca) - PFIB, Xuehai Tan (xtan@ualberta.ca) - TEM or Peng Li (peng.li@ualberta.ca) – the Characterization Group Manager.

Standard Lamella Preparation

Series of six images illustrating stages in advanced TEM sample preparation: capping film deposition, trench milling and undercutting, manipulator welding, plucking out, rough polishing, and final polishing.
Series of six images illustrating stages in advanced TEM sample preparation: capping film deposition, trench milling and undercutting, manipulator welding, plucking out, rough polishing, and final polishing.

Application Examples

Sample: Semiconducting Oxide Film on Si
FIB Application: Low voltage 2kV Ar polishing to produce damage free sample for HR-STEM imaging
Sample Courtesy: Avalon Holographics Inc., Edmonton

Microscopic images reveal the Si substrate (upper panel) and a textured semiconducting oxide film (lower panel), featuring distinct nano-scale structures and electron diffraction patterns, achieved through advanced TEM sample preparation techniques.
Microscopic images reveal the Si substrate (upper panel) and a textured semiconducting oxide film (lower panel), featuring distinct nano-scale structures and electron diffraction patterns, achieved through advanced TEM sample preparation techniques.

Sample: Rapidly solidified Al-10Si-0.4Sc droplets (atomized using Impulse Atomization)
FIB Application: Flexible micromanipulation to pluckout samples from spheres
Sample Courtesy: Akki Sahoo, Dr. Jonas Valloton and Prof. Hani Henein, Faculty of Engineering, University of Alberta; Abdoul-Aziz Bogno, Equispheres Inc., Ottawa

A collage of microscopic images, prepared with advanced TEM techniques, showcases various materials' textures and compositions with scale bars. The top right image features a color map, highlighting elements labeled as Al, Si, and Sc.
A collage of microscopic images, prepared with advanced TEM techniques, showcases various materials' textures and compositions with scale bars. The top right image features a color map, highlighting elements labeled as Al, Si, and Sc.

Sample: Al-Cr-Fe-Ni medium-entropy alloy (MEA)
FIB Application: Mixed Pt/C capping film for effective protection for HEA/MEA materials
Sample Courtesy: Guijiang Diao and Prof. Dongyang Li, Faculty of Engineering, University of Alberta

A series of SEM and color maps displaying material composition, with elements Cr (green), Fe (blue), Ni (red), Al (yellow) on a patterned surface. Focus is on a circular area, highlighting the precision in sample preparation for Advanced TEM analysis.
A series of SEM and color maps displaying material composition, with elements Cr (green), Fe (blue), Ni (red), Al (yellow) on a patterned surface. Focus is on a circular area, highlighting the precision in sample preparation for Advanced TEM analysis.

Sample: Intel Core i7 processor
FIB Application: Inverted pluckout to reduce curtaining and damage in the regions of interest.

Advanced TEM images reveal semiconductor structures with ion beam detection, highlighting inverted pluck-out areas. Color coding indicates elements: Cu, Si, Ti, ensuring precise TEM sample preparation for detailed analysis.
Advanced TEM images reveal semiconductor structures with ion beam detection, highlighting inverted pluck-out areas. Color coding indicates elements: Cu, Si, Ti, ensuring precise TEM sample preparation for detailed analysis.

Sample: AlGaAs multilayers
FIB Application: 90-degree pluckout (ion beam parallel to the layer stacks) to produce uniform thin thickness across all layers.

A semiconductor cross-section reveals layers of Al₀.₃Ga₀.₇As and Al₀.₄₅Ga₀.₅₅As on Si, with advanced TEM images and a diffraction pattern presented on the right, highlighting meticulous sample preparation techniques.
A semiconductor cross-section reveals layers of Al₀.₃Ga₀.₇As and Al₀.₄₅Ga₀.₅₅As on Si, with advanced TEM images and a diffraction pattern presented on the right, highlighting meticulous sample preparation techniques.
Advanced TEM nanobeam diffraction images reveal crystallographic mismatch in Al[_x]Ga[_{1-x}]As/Al[_y]Ga[_{1-y}]As layers, complemented by a selected area electron diffraction pattern.
Advanced TEM nanobeam diffraction images reveal crystallographic mismatch in Al[_x]Ga[_{1-x}]As/Al[_y]Ga[_{1-y}]As layers, complemented by a selected area electron diffraction pattern.
Microscopic image of AlGaAs/AlGaAs multilayers displaying 30 repeating stacks. Includes HAADF and EDS mapping with highlighted elements: Al in red, As in green, Ga in blue. Advanced TEM sample preparation showcases intricate layer details for accurate analysis.
Microscopic image of AlGaAs/AlGaAs multilayers displaying 30 repeating stacks. Includes HAADF and EDS mapping with highlighted elements: Al in red, As in green, Ga in blue. Advanced TEM sample preparation showcases intricate layer details for accurate analysis.

Sample: Nano-composite material (Ni nanoparticles in anodized Al)
FIB Application: Flexible miro-manipulation to produce cross-sectional and plan-view lamellas
Sample Courtesy: Dr. Matthew Nickel and Prof. Todd McMullen, Faculty of Medicine & Dentistry, University of Alberta

Advanced TEM cross-sectional and plan-view microscopy images reveal distributions of Ni, Al, and O with remarkable clarity. The cross-section shows stratified layers, while the plan-view features patchy clusters. Scale bars are set at 200 nm and 50 nm respectively.
Advanced TEM cross-sectional and plan-view microscopy images reveal distributions of Ni, Al, and O with remarkable clarity. The cross-section shows stratified layers, while the plan-view features patchy clusters. Scale bars are set at 200 nm and 50 nm respectively.

Sample: Porous solid oxide fuel cell
FIB Application: Back-filling with in-situ GIS to prepare high quality samples from porous materials.
Sample Courtesy: Prof. Douglas Ivey, Faculty of Engineering, University of Alberta

Microscopic images using advanced TEM reveal pores, element concentration maps, and overlays; highlighting small carbon-filled pores and unfilled, damaged pores.
Microscopic images using advanced TEM reveal pores, element concentration maps, and overlays; highlighting small carbon-filled pores and unfilled, damaged pores.

Sample: Intel Core i7 processor
FIB Application: Fully automatic/unattended site preparation of 25 locations

A grayscale image showcasing a zoomed-in view of microstructures highlights an inset detailing a close-up of one microstructure, prepared using Advanced TEM techniques, featuring a rectangular shape inside a square cavity.
A grayscale image showcasing a zoomed-in view of microstructures highlights an inset detailing a close-up of one microstructure, prepared using Advanced TEM techniques, featuring a rectangular shape inside a square cavity.