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.
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.
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.
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.
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.
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.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.
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.
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.
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.
SAXS, GI-SAXS/WAXS are available on Bruker D8D+
The nanoFAB is pleased to announce that advanced Small-Angle X-ray Scattering (SAXS), Grazing-Incidence Small-Angle and Wide-Angle X-ray Scattering (GI-SAXS/WAXS) techniques are fully commissioned on the Bruker D8 DISCOVER Plus X-Ray Diffractometer and now open for user training.
SAXS utilizes small-angle x-ray scattering to quantify nano-scale density differences in a sample, which enables characterization of nanostructures in terms of the averaged particle sizes, shapes, distribution, pore sizes, characteristic distances of partially ordered materials, and much more. This is achieved by analyzing the elastic scattering behavior of X-rays when traveling through the material, recording their scattering at small angles (typically 0.1 - 10°).
The materials for SAXS analysis can be solid or liquid and they can contain solid, liquid or gaseous domains (so-called particles) of the same or another material in any combination. Not only particles, but also the structure of ordered systems like lamellas, and fractal-like materials can be studied. For thin films supported on solid substrates (such as glass or Si), derivatives of SAXS, namely GI-SAXS/WAXS can be used to characterize ordered structure/alignment within the films relative to the substrate surface, particularly molecular alignment/arrangement of polymer films. These methods are accurate, non-destructive and usually require a minimum of sample preparation. Applications are very broad, including colloids of all types, metals, cement, oil, polymers, plastics, proteins, foods and pharmaceuticals.
If you are interested in the SAXS, GI-SAXS/WAXS analysis, please submit a request (training or sample type) with sample details on LMACS. Our XRD team (Drs. Xuehai Tan and Nas Yousefi) will follow up and arrange sample analysis and training. If you have any questions, please feel free to contact Peng Li (Peng.Li@ualberta.ca) – the Characterization Group Manager.
Application Examples
Sample: 20 nm Au NPs Sample preparation: in water (capillary tube) Analysis: SAXS Application: Size distribution analysis
Among several techniques to measure particle size, SAXS provides accurate, reliable and high throughput analysis with simple sample preparation. While TEM imaging based analysis provides direct visualization with very high spatial resolution, it requires proper sample preparation (well dispersed particles) and the result accuracy relies on the quality of particle intensity thresholding. SAXS analysis is less dependent on sample preparation and probes a large volume of samples, providing the most statistically relevant results.
Figure 1: (A) Bright-Field TEM image and (B) measured size distribution of the Au nanoparticles, diameter = 19.2 ± 4.0 nm. (C) 2D SAXS data measured with an evacuated flight tube (EFT) filled with vacuum. (D, E) SAXS data integrated into 1D and background subtraction: A model-free analysis based on Pair Distance Distribution Function (PDDF). The obtained result is indicative of an overall spherical particle shape with approximated diameter of 18.9 nm. (F) PDDF P(r) functions for geometric bodies, adapted from DOI 10.1088/0034-4885/66/10/R05
Sample: 3 nm Si QDs Sample preparation: in toluene (capillary tube) Analysis: SAXS Application: Size distribution analysis Sample Courtesy: Chuyi Ni and Prof. Jon Veinot, Department of Chemistry, University of Alberta
TEM imaging analysis can be very challenging to characterize particle size when particles are difficult to disperse and/or the particles give poor contrast, such as light-element quantum dots (QDs), e.g., Si or carbon QDs. SAXS can provide reliable size and shape structure determination, empowered by several data analysis / modelling methods and further advances in instrumentation.
Figure 2: (A) Dark-Field STEM image and (B) measured size distribution of Si QDs, diameter = 3.7 ± 0.7 nm. (C) 2D SAXS data measured with an evacuated flight tube (ETF) filled with vacuum. SAXS analysis results with model free and model fitting: (D) Model free PDDF, diameter = 3.52 nm; (E) a model-based fitting assuming polydisperse spheres with Schultz size distribution and no interaction, diameter = 3.68 nm; (F) model-free Guinier analysis, diameter = 3.64 nm.
Sample: textured PVDF film Sample preparation: Freestanding film Analysis: SAXS Application: Internal periodical structures and orientation Sample Courtesy: Amanuel Abay and Prof. Anastasia Elias, Faculty of Engineering, University of Alberta
SAXS is useful not only for characterizing the size and shape of particles, but also for measuring structural information of partially or completely disordered systems. In the following example, SAXS analysis is utilized to study the internal repeating structure of a free-standing PVDF film.
Figure 3: (A) a photo of the SAXS setup, including X-ray collimator, the vertically mounted free-standing PVDF film, and the evacuated flight tube (EFT) that is attached to the 2D detector. (B) The orientation of the sample with respect to the 2theta and gamma directions of the 2D detector. (C) Illustration of the internal lamella orientation confirmed by the SAXS analysis. (D) 2D SAXS data marked with q values in both 2𝛉 and 𝞬 directions. (E) SAXS data integrated into 1D and background subtraction. (F) The measured q value suggests a repeated distance of 11.6 nm for the internal lamella.
Sample: Organic Photovoltaic (OPV) films (30 nm PEDOT + 250 nm P3HT:PCBM) Sample preparation: Spin-coated on ITO-coated glass substrate Analysis: GI-SAXS Application: Internal periodical structures and orientation Sample Courtesy: Prof. Jillian Buriak, Department of Chemistry, University of Alberta
GI-SAXS is particularly useful to analyze domain size, interplanar spacings and orientation of small molecule/polymer thin films for photovoltaics, block copolymer thin films and inorganic/metal thin films for batteries. GI-SAXS analysis of an organic Photovoltaic film (P3HT:PCBM) measured an interplanar spacing d = 1.61 nm and their 2D distribution (both in-plane 2𝛉 and out-of-plan β).
Figure 4: (A) 2D GI-SAXS data marked with q values in both 2𝛉 and gamma directions; (B) Integrated profile in 2𝛉 direction and (C) Integrated profile in β direction.
Sample: PBTTT film (30 nm) Sample preparation: spin-coated on ITO-coated glass substrate Analysis: GI-WAXS Application: Internal periodical structures and orientation Sample Courtesy: Prof. Loren Kaake, Department of Chemistry, Simon Fraser University
Semiconducting polymers play an important role in advancing the field of printed and mechanically flexible electronics, such as flat panel displays and photovoltaic cells. Thin film transistors with thiophene-based polymer layers have demonstrated good field-effect carrier mobilities that are considered highly valuable across various applications. It is widely recognized that achieving high carrier mobility in these materials hinges on the precise molecular ordering, as charge movement depends on effective intermolecular electronic coupling. While the spacing of the molecular ordering and crystalline domains is too small for GI-SAXS, GI-WAXS provides an effective analysis.
As shown in the figures below, typical GI-WAXS setups on the Bruker D8D plus (0.1 mm slit and a 0.3 mm Goebel mirror collimator, 0.17° incidence angle, and 145 mm sample-to-detector distance) effectively confirms the edge-on orientation of the polymer lamellas in a 30 nm PBTTT film on glass.
Compared to the results (available here) obtained from the Synchrotron Hard X-ray MicroAnalysis (HXMA) beamline (at the Canadian Light Source), the GI-WAXS analysis on the Bruker D8D plus provides equally informative results, but more accessible to general users.
Figure 5: GI-WAXS results of PBTTT thin films measured on the Bruker D8D + and the Synchrotron Hard X-ray MicroAnalysis (HXMA) beamline of the Canadian Light Source. (A) Two-dimensional WAXS scattering data (B) 1D profile of the scattering intensity. (C) Azimuthal dependence of the scattering intensity. (D) The molecular structure of PBTTT and the schematic depicting PBTTT different molecular alignment within thin layers relative to the substrate surface: Edge-On and Face-On orientations. The arrangement of molecules within the cell is primarily qualitative and is not intended to provide a quantitative representation of the precise molecular packing specifics.
Broad Ion Beam (BIB) polishing for SEM/EDX/EBSD
The RES 102 system features:
Ion energy: 0.8 to 10 keV
Source current: Up to 4.5 mA
Stage Rotation: 0.6 to 10 rpm
Sample size SEM holder: max. Ø 25 mm × 12 mm
Prepared area SEM holder: max. Ø 25 mm
RES102 BIB Ion Milling System equipped with two Ar guns
Among general electron microscopy applications, Electron Backscatter Diffraction (EBSD) is a surface technique – typical probing depth is in the range of a few tens nm for a beam energy of 20 kV. Smooth and damage-free surface is critically important to obtain high quality EBSD data. Compared to conventional mechanical polishing techniques, which can result in very rough surfaces and a thick damaged layer, low energy beam at grazing incident angle and rotating stage on the RES102 can effectively polish the surface to reduce roughness and remove the damaged layer.
With the programmable recipes of flexible parameters (beam energy, beam current, incident angle, stage rotating speed), the RES102 BIB has produced very nice results for our users for EBSD analysis. See recent examples below.
Application Examples (EBSD)
Sample: 3D printed Alumina for structural applications
Sample Courtesy: Cass (Haoyang) Li, Dr. James Hogan, Mechanical Engineering Department, Faculty of Engineering, University of Alberta
Ion Milling process:
8 kV, 3 mA, 3.5 degrees, 1.5 rmp for 120 mins
8 kV, 2 mA, 2.5 degrees, 1.5 rmp for 60 mins
EBSD mapping: 175 µm x 175 µm, stepsize 50 nm
(A) SEM image; (B) Orientation map; (C) Phase maps of Alumina and Aluminium; (D) Grain size distribution
Sample: Rail Steel
Sample Courtesy: Stephen Okocha, Drs. Ben Jar and Michael Hendry, Mechanical Engineering Department, Civil and Environmental Engineering Department, Faculty of Engineering, University of Alberta
Ion Milling process:
8 kV, 3 mA, 2.5 degrees, 1.5 rmp for 60 mins
6 kV, 2 mA, 2.5 degrees, 1.5 rmp for 60 mins
EBSD mapping: 300 µm x 300 µm, stepsize 250 nm
(A) SEM image; (B) Orientation map; (C) Grain size distribution
Sample: Al-Cr-Fe-Ni medium-entropy alloy (MEA)
Sample Courtesy: Guijiang Diao, Dr. Dongyang Li, Chemical and Materials Engineering Department, Faculty of Engineering, University of Alberta
Ion Milling process:
8 kV, 3 mA, 3.5 degrees, 1.5 rmp for 60 mins
5 kV, 2 mA, 2.5 degrees, 1.5 rmp for 60 mins
EBSD mapping: 2500 µm x 1500 µm, stepsize 500 nm
(A) Orientation map; (B) Crystal unit cell orientation and (C) Grain Size Distribution
The RES102 ion milling system is now available to general users for both staff analysis and user training. Any users interested in getting trained on this tool or staff analysis should submit a request on LMACS. If you have any questions, please contact the tool managers Drs. Nas Yousefi and Shihong Xu or Peng Li – the Characterization Group Manager
In-situ heating S/TEM is available
The nanoFAB is pleased to announce that the DENS solutions In-Situ Lightning TEM holder is fully commissioned and in-situ heating TEM analysis is available on the JEOL JEM-ARM200CF S/TEM Microscope.
The DENS lightning in-situ heating platform utilizes the state-of-the-art MEMS technology to create the lab-on-chip environment that replicates the real-life heating conditions inside the TEM, which provides unprecedented control and accuracy over temperature:
8 contacts for simultaneous heating and biasing analysis
Double tilted holder
Maximum heating temperature of 1100 °C
Flexible and customizable heating profiles
Compatible with EDX analysis
All these unique features enable dynamic analysis of morphological (imaging), structural (diffraction) and compositional (EDX) changes of materials at very high spatial resolution on the JEOL ARM S/TEM.
The in-situ heating TEM analysis is now available to all users. If you have needs for these analysis, please submit a sample analysis request with sample details on LMACS. If you have any questions, please feel free to contact Dr. Xuehai Tan (xtan@ualberta.ca) – the primary TEM staff member or Peng Li (Peng.Li@ualberta.ca) – the Characterization Group Manager.
Images show (A) double tilted Dens Lightning holder, (B) heating chip being heated at 1100°C, (C) (D) heating chip and (E) (F) sample areas on the chip.
Application Examples
Recrystallization and melting of polycrystalline Au film heated up to 1100 °CMorphological analysis by DF-STEM images: formation of particles up to 800 °CCompositional analysis by EDX: confirming the composition of the particles. Despite the influence of infrared radiation emitted from the heating device, EDS elemental mapping is acquired at elevated temperature (800 °C) during the in-situ heating.
Kurt J. Lesker 150LX ALD system now open for training
The nanoFAB is pleased to announce that our newly installed and commissioned KJLC 150LX Atomic Layer Deposition system is now fully operational and available for training to all nanoFAB users. The ALD offers excellent uniformity and controlled growth of a variety of films on an atomic scale. Its high-vacuum load-lock and UHV-type sealing, combined with near-constant high-purity Ar flow, enable high-purity process conditions and excellent quality films.
Main system features include:
Single wafer transfer load-lock
Substrate heating up to 500 °C
150 mm platen, with an available carrier for samples <150 mm
Thermal and plasma-enhanced (PE-ALD) processes available
In situ film growth monitoring using Film Sense FS-1EX multiwavelength ellipsometer
The KJLC 150LX ALD is available to users for self-use (after training) and fee-for-service work. Any users interested in getting trained on this tool should submit a training request via LMACS. If you have any questions, please contact Aaron Hryciw (ahryciw@ualberta.ca) or Scott Munro (smunro@ualberta.ca).
nGauge AFM is now Available at nanoFAB
The nanoFAB is pleased to announce that the new Atomic Force Microscopy system, the ICSPI nGauge AFM, has been successfully installed and is operational now. This benchtop AFM allows nanoscale topography data collection with 3 easy steps: automatic sweep, approach, and scan. The nGauge AFM is a laserless system, based on a patented AFM-on-a-chip technology. In this new technology, all of the sensors and scanners of a traditional AFM have been integrated onto a single chip, so you can capture routine scans in just over a minute.
The nGauge AFM operates in the tapping mode and generates topography, phase, and error images simultaneously for any solid samples (including conductive and non-conductive, but not liquid samples). nGauge AFM tips are made of durable materials like diamond-like carbon (DLC) and aluminum oxide, which are also integrated onto the AFM chip, enabling hundreds (or thousands) of scans possible with each tip.
(a) The benchtop nGauge AFM. (b) AFM chip and its integrated components. (c) Front view of the Diamond-Like Carbon and Aluminum tips. (d) 3-step scan collection via nGauge AFM
nGauge AFM Specifications:
Max scan area: 20 x 20 μm
Z Range: 10 μm
Scan speed: 80 seconds (256 x 256 pixel, 20 x 20 μm)
Max scan resolution: 1024 x 1024 pixels (5 minutes)
Noise floor: <0.5 nm rms
XY Scanner resolution: <0.5 nm
Images: Topography, Phase, Error
Approach: Automatic
Max sample size: 100 mm x 50 mm x 16 mm
Sample: Shale (before and after ion milling processes) Sample courtesy of Graham Spray, M.Sc., P.Geo., AGAT Laboratorie.
Diamond-Like Carbon (DLC) Tip Specification:
nGauge AFM tips are made of diamond-like carbon materials with high aspect ratio offering excellent lateral resolution and excellent contamination resistance.
Tip radius: <20 nm
Tip height: >1 μm
Cone angle: <10°
Aspect ratio: >3
Tilt compensation: 15°
Tip post height: 3 μm
Tip shape: Conical
Tip material: Diamond-like carbon\
Sample: Patterned Cr + Au / Ti on Si chip
Cantilever Specifications:
nGauge AFM tips are located at the very end of the cantilever beam and are integrated onto a micro-electro-mechanical systems (MEMS) chip. The chip features integrated lateral and vertical actuators and piezoresistive sensors.
Shape: Beam
Length: 30 μm
Width: 6 μm
Thickness: 3 μm
Resonant Frequency: 8 kHz (typical: 7.3–8.7 kHz)
Stiffness: 0.1 N/m
The nGauge AFM is now available to users for both staff analysis and self-use/user training provided they purchase own nGauge AFM chip. Any users interested in getting trained on this tool or staff analysis should submit a request via LMACS. If you have any questions, please contact Dr. Nas Yousefi or Peng Li – the Characterization Group Manager.
Sample: Polymeric Membrane Sample courtesy of Dr. Sadrzadeh, Mechanical Engineering Department, Faculty of Engineering, University of Alberta.
![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.](https://www.nanofab.ualberta.ca/wp-content/uploads/2025/02/06b-Al-Ga-As-1024x410.png)
