Electron Microscopy

Introduction

In accordance with the NINT mandate, the Electron Microscopy (EM) Lab engages in collaborative scientific research projects; continually develops and expands the capabilites of the instruments in order to position NINT at the forefront of nanoscience and nanoengineering; and delivers technical services on a fee for service basis;.

All of the NINT microscopes are situated in specially-designed characterization suites that minimize environmental disturbances and ensure optimal performance.

A staff of seven professional microscopists are available to assist clients with their projects.

Accessing The Facility

Our client-driven projects vary in scope from small fee for service contracts to large research and development collaborations. Preference is given to extensive high-impact projects that are well-aligned with the NINT goals.

Charges apply for most activities. Clients may negotiate for inkind support in order to cover beam time costs. For further information please contact the NINT business office at NINT-request@nrc-cnrc.gc.ca.

Quantitative Electron Microscopy Research at NINT

The Quantitative Electron Microscopy (QEM) Project led by Dr. Marek Malac endeavors to extend the boundaries of practical electron microscopy. One of the goals the QEM Project is the development of new instrumentation and methods for EM data interpretation. Dr Malac’s team works closely with the facilties staff to transfer this knowledge to client projects.

Hitachi Electron Microscope Products Development Centre

Established in 2011, NINT’s $15 million Hitachi Electron Microscopy Products Centre (HEMiC) was created in order to accelerate the commercialization of NINT microscope innovations by utilizing Hitachi’s product development and technical sales expertise. HEMiC was made possible through collaboration involving NINT, the Alberta Ingenuity Fund’s nanoWorks program, the University of Alberta, and Hitachi High Technologies Canada Inc.

Through the HEMiC agreement, three microscopes were installed in the Facility: the H-9500 ETEM; the S-5500 SEM; and the NB-5000 FIB/SEM. Prior to the installations, extensive modifications were made to the existing building to create an environment with extremely low mechanical, acoustic, electromagnetic, and thermal disturbances. This environment is ideal for conducting materials science research at the nanoscale, and provides an optimal venue for potential clients to experience and explore the latest Hitachi instruments prior to purchase.

Instrumentation

The facility is home to 3 transmission electron microscopes (TEMs), 3 scanning electron microscopes (SEMs), and 2 focused ion beam (FIB) microscopes.

As a general rule, the TEMs, FIBs, and the S-5500 SEM operate in an assisted access mode. This is done in order to ensure optimal performance of the instruments and minimize the risks associated with expensive and delicate multi-user equipment. Training and self-use on these instruments is considered on a case by case basis.

The S-4800 and S-3000N SEMs operate in both self-use and assisted access modes.

JEOL 2200 FS Soft Materials TEM

photo_jeol_2200This is a 200kV Schottky field emission instrument is equipped with an in-column filter, which allows acquisition energy filtered images and diffraction patterns to be collected both on image plates and slow scan CCD camera. The Schottky source of this instrument is sufficiently robust to allow analysis of organic samples.

Techniques that can be used include:

  1. Cryogenic TEM imaging in both conventional parallel beam and scanning modes
  2. Electron Energy Loss Spectroscopy (EELS) at moderate energy resolution, and convenient energy filtering, diffraction and imaging
  3. Energy-filtering Electron Diffraction, both with parallel beam and convergent beam modes
  4. Cryogenic and high-tilt imaging and electron tomography at ~ 0.3 nm resolution
  5. Energy dispersive chemical analysis and mapping

A wide range of holders and detectors are available for this instrument.

Materials Science Transmission Electron Microscope Hitachi HF 3300

HF3300This advanced 300kV TEM/STEM instrument is equipped with a post-column Gatan Tridiem Image Filter (GIF).

Its cold field emission gun (CFEG) technology delivers superior spectroscopic performance with outstanding electron interferometry capabilities.

The combination of quantitative electron microscopy techniques sets this instrument apart from the rest.

The excellent flexibility and stability of the microscope – mechanical and electrical – allows researchers to push the limits of electron microscopy and analyze extremely difficult samples and problems.

This microscope is primarily designed for work on materials science samples using these techniques:

  1. High resolution TEM imaging (HR TEM) in both conventional (parallel beam) and scanning (STEM) modes
  2. High-energy Resolution Electron Energy Loss Spectroscopy (HREELS) with ~ 0.2 nm probe size and significant beam current
  3. Off-axis electron holography, three beam interferometry and STEM holography
  4. Electron diffraction both with parallel beam (the CFEG source allows for parallel beam work with very small probe sizes) and convergent beam modes
  5. Energy Dispersive Spectrometry (EDS) chemical analysis and mapping

A wide range of holders and detectors are available for this instrument.

Hitachi H-9500 Environmental Transmission Electron Microscope (ETEM)

H-9500This microscope allows the study in-situ chemical reactions of samples in liquids and gases.

Offering very low background pressure (in the 10-8 torr range), the ETEM can ensure low sample contamination rate and little effect of background gases on in-situ experiments.

The instrument can heat samples to temperatures exceeding 1500° C while exposed to various gases or study liquid samples at temperatures exceeding 300° C.

The analytical capabilities of the instrument include:

  • electron energy loss spectroscopy and
  • energy dispersive X-ray spectrometry for chemical analysis.

The ETEM also offers standard TEM imaging and diffraction capabilities allowing the investigation of sample structure and morphology.

Hitachi S-5500

photo_hitachi_s5500This is one of the world’s highest resolution SEMs, with a resolution of 0.4nm at 30kV and 1.6nm at 1kV.

It permits morphological observation down to the atomic or molecular structures of various materials, far surpassing the performance of any conventional SEM.

Aside from SE and BSE imaging modes, the Duo-STEM Bright Field/Dark Field Detector allows for simultaneous imaging and adjustable collection angle.

Hitachi S4800 High Resolution Scanning Electron Microscope

S4800The S-4800 is a cold field emission high resolution scanning electron microscope with many advanced features including operation at low landing energies and filtering of signals using an in-lens ExB filter.

The major advantage of this instrument is its ability to access many unprocessed signals – sample, reference and beam current monitor signals.

This microscope also allows separate access to each of its lenses and electrodes, facilitating the development of additional detectors and other improvements for semi-quantitative scanning electron microscopy.

Hitachi S-3000N Elevated Pressure Scanning Electron Microscope

photo_hitachi_s3000nThis variable pressure type SEM is capable of analyzing non-conductive and wet samples, which traditionally could not be analyzed using standard SEM methods.

This microscope is ideal for studying biological and polymeric samples when soft and sensitive nanostructures must be preserved during sample preparation or when using other conventional electron microscopy methods.

The 3000N is a tungsten filament SEM suitable for medium resolution imaging. It is set up for imaging at elevated pressures and is equipped with a four quadrants backscattered electron (BSE) detector along with an energy dispersive X-ray spectrometer (EDS) for chemical microanalysis.

Hitachi NB-5000 Dual (Focused Ion/Electron) Beam Microscope (FIB/SEM)

photo_fib_semThis instrument combines the capabilities of a focused ion beam (FIB) with a high resolution scanning electron microscope (SEM).

This microscope is used primarily for the following applications:

  1. Milling and extraction of lamellae and cylinders for transfer to and analysis by TEM
  2. FIB tomography (a sequence of alternating FIB slicing and SEM imaging steps, allowing 3D reconstruction of a sample volume)
  3. FIB-assisted lithography

Zeiss NVision 40 Dual (Focused Ion/Electron) Beam Microscope (FIB/SEM)

photo_hitachi_s5500This microscope is currently used for the following applications:

  1. FIB-assisted milling, imaging, and EDS analysis under cryo conditions
  2. Preparation of samples for cryo-TEM
  3. FIB tomography (a sequence of alternating FIB slicing and SEM imaging steps, allowing 3D reconstruction of a sample volume)
  4. FIB-assisted lithography
  5. FIB-assisted prototyping of nanoelectromechanical devices

Sample preparation facility

This area of the facility typically operates in self-use mode and contains the following tools:

  • multi-target sputter coater
  • ion mill polisher
  • plasma and uv sample cleaners
  • cryo preparation area for FIB and TEM samples
  • grinders, dimplers and polishers for TEM sample preparation
  • fume hood stations for chemical work

Computation and Data Processing

This area contains a number of computer work stations featuring software for the analysis and interpretation of microscope data.