Transmission and Scanning Transmission Electron Microscopy

Instruments for TEM and STEM

Background

Determine the microstructure of materials such as grain size, defect density and type, and dislocation distribution; study the local microstructure including heterointerface and individual nanostructures; examine crystalline and amorphous structures; determine the composition of materials from micrometer level down to atomic level. Six instruments with complementary capabilities include atomic resolution (0.19 nm) TEM and analytical scanning TEM with 0.2 nm beam for atomic number (Z-contrast) imaging, EDS, EELS and nanodiffraction. Traditional sample preparation such as ion millers, Cryo TEM with cryomicrotomy, vitreous ice sample preparation and cryo-transfer are also available.

JEOL 2200FS (S)TEM

Staff Contacts:

Jim Mabon
(217) 333-4265

CQ Chen
(217) 300-4837

Honghui Zhou
(217) 300-3934

Location
B70C Materials Research Laboratory (217) 244-2137

General:
The aberration-corrected JEM-2200FS, a state-of-the-art analytical electron microscope, is equipped with a 200kV field emission gun (FEG), a CEOS probe Cs-corrector, and an in-column energy filter (Omega Filter) that allows elemental analysis and chemical analysis of specimens. It is also equipped with an Energy Dispersive X-ray Spectrometer (EDS) and a CCD-camera. With an available small probe size of ~0.1 nm, atomic level high-resolution high-angle annular dark-field (Z-contrast) images, and high resolution EELS spectrum imaging can be obtained. With the low background Be specimen holder, large (50mm2) detector area, and the hard X-ray aperture, high-quality EDS analysis and mapping is available.

Specifications:

  •     Cs = 0.5mm Cc = 1.1mm
  •     Energy 200kV
  •     Tilt 25 degrees on both axes
  •     HAADF Resolution = 0.1nm
  •     HREM Point resolution = 0.19nm
  •     Information Limit better than 0.1nm
  •     Sample loading-Side entry
  •     Energy Spread better than 0.8eV

Attachments:

  •     Corrector - CEOS Cs-corrector system
  •     Image Filter - In-column Omega Filter
  •     EDS - Oxford INCA 50mm2 detector
  •     Digital Imaging - 2k Gatan CCD
  •     Digital Scan - Gatan Digiscan
  •     Video - Hamamatsu cameras
  •     HAADF Detector
  •     BF Detector
  •     Low-background double tilt holder

Hitachi H-9500 Dynamic Environmental TEM

Staff Contacts:

Jim Mabon
(217) 333-4265

CQ Chen
(217) 300-4837

Wacek Swiech
(217) 244-9532

Location

B66A Materials Research Laboratory

General

Hitachi H-9500 DETEM (Dynamic Environmental TEM)
Hitachi H-9500 DETEM (Dynamic Environmental TEM)

The H-9500 is a high resolution 100-300 kV ETEM with a LaB6 electron gun equipped for study of dynamic material reactions down to the atomic scale. This is a user-friendly TEM for atomic-resolution TEM imaging and routine structural characterization. It is equipped with the Gatan Orius SC200 2kx2k CCD Camera and the Gatan K2-IS 4kx4k direct electron detection CMOS high speed camera capable of imaging and recording at up 400 full frames per second (up to 1600 fps for sub-frames). Together with the inherent differential pumping system and an add-on gas injection system for windowless environmental conditions up to ~0.1 Pa at the sample, a gas injection heating holder (to 1500 C), and a Hummingbird liquid electrochemistry cell holder; This makes it a high performance in-situ characterization TEM, with capabilities of resolving dynamic details in heating, catalysis, TEM diffraction, electrical testing, and chemical reaction experiments with high spatial and time resolution.

Increasing time resolution and adding in situ capabilities have been among the prime goals in TEM development.  Towards furthering this capability, pulse laser systems are being developed for dynamically exciting the electron source as a photocathode and the specimen for performing dynamic pump-probe experiments at very high temporal resolution from current 2.5 milliseconds to ~250 femto-seconds.

Features:

User-friendly operation: High specimen throughput, requiring 1 minute for specimen exchange and 5 minutes for voltage ramp-up (300 kV) and beam-on.

High-resolution microscopy: Point-to-point resolution of 0.18 nm and lattice resolution of 0.1 nm.A stable 5-axis eucentric goniometer stage.

  • Accelerating voltage: 300 kV, 200 kV, 100 kV
  • Electron gun: Filament: LaB6 (DC heating)
  • Resolution: 0.10 nm (lattice), 0.18 nm (point-to-point)
  • Illumination system: 4-stage lens system
  • Probe size: Micro mode: 0.05 - 0.2 µm (4 steps), Nano mode: 1 - 10 nm (4 steps)
  • Imaging system: 5-stage lens system
  • Stage translation Motor drive by CPU control
    X/Y = ±1 mm, Z = ±0.3 mm, tilt α = ±15°, β = ±15°
  • Orius SC200 CCD Camera and the K2 IS direct electron detection CMOS high speed camera
  • Vacuum system: Electron gun: Ion pump: 60 L/s; Column: TMP: 260 L/s; Viewing/camera chamber: Diffusion pump: 280 L/s
  • Hitachi single tilt holder
  • Hitachi standard double tilt holder
  • Hitachi in-situ gas injection heating holder
  • Hummingbird liquid cell electrochemistry holder

JEOL 2010F (s)STEM

Staff Contacts:

CQ Chen
(217) 300-4837

Honghui Zhou
(217) 300-3934

Jim Mabon
(217) 333-4265

Location
0026 Materials Research Laboratory (217) 244-6116

General:
The 2010F is an energy filtering, field-emission analytic TEM/STEM. It is ideal for small probe work including: HAADF STEM, nanodiffraction, and spatially resolved EELS and EDS. It operates at 200kV and uses a Schottky field emitter. The 2010F is equipped with an energy filter to filter both images and diffraction patterns as well as act as a energy-loss spectrometer. The system is capable of EDS/EELS mapping, holography, and in-situ heating and cooling. Both intensified video rate and slow-scan CCD cameras are available. The system is controlled by the JEOL FasTEM system allowing total computer control of the system.

Specifications:

  •     Cs = 1.0mm Cc = 1.4mm
  •     Energy 200kV
  •     Tilt 40 degrees on one axis and 30 degrees on the other
  •     HAADF Resolution = 0.18nm
  •     HREM Point resolution = 0.24nm
  •     Information Limit > 0.12nm
  •     Lens Type-Side entry (Condenser/Objective)
  •     Energy Spread 0.7eV

Attachments:

  •     Image Filter - Gatan Image Filter (GIF) 2001
  •     EDS - Oxford INCA 30mm ATW detector
  •     Digital Imaging - 1k CCD on GIF
  •     Digital Scan - Gatan Digiscan and Oxford INCA
  •     Video - Intensified off-axis and GIF cameras
  •     Computer Control - FasTEM
  •     Biprism
  •     HAADF Detector
  •     1000ºC double tilt holder
  •     Liquid N2 double tilt holder

JEOL 2100 CryoTEM

Staff Contacts:

Wacek Swiech
(217) 244-9532

Jim Mabon
(217) 333-4265

CQ Chen
(217) 300-4837

Location
0011 Materials Research Laboratory (217) 244-0620

General:
The 2100 Cryo is a conventional TEM with large pole piece gap. It is optimized for BF/DF imaging, diffraction and high sample tilts. It operates at 200kV. The 2100 Cryo is equipped with a combined video rate/slow scan camera for real time imaging and final image recording. It has a low-dose mode. A high tilt is available with +/-70 degrees using a special tip for the single tilt holder. Cryo transfer stage, double tilt heating, and liquid N2 stages are available.

Specifications:

  •     Cs = 2.0mm
  •     Energy 200kV
  •     +/-70 degrees (special single tilt holder)
  •     Point resolution = 0.27nm
  •     Information Limit > 0.14nm
  •     Side Entry Goniometer - Cryo Pole Piece

Attachments:

  •     Digital Imaging - Gatan UltraScan 2kx2k CCD
  •     Computer Control - Digital Micrograph
  •     Free Lens Control
  •     Cryo transfer stage
  •     1000ºC double tilt holder
  •     Liquid N2 double tilt holder

JEOL 2010 LaB6 TEM

Staff Contacts:

Wacek Swiech
(217) 244-9532

Jim Mabon
(217) 333-4265

CQ Chen
(217) 300-4837

Location
0017 Materials Research Laboratory (217) 244-0620

General:
The 2010LaB6 is a conventional TEM. It is optimized for BF/DF imaging, diffraction and high sample tilts. It operates at 200kV. The 2010LaB6 is equipped with a combined video rate/slow scan camera for real time imaging and final image recording. A double tilt holder is available with +/-45 degrees of tilt. Double tilt heating and liquid N2 stages are available.

Specifications:

  •     Cs = 1.4mm
  •     Energy 200kV
  •     Tilt 40 degrees on two axes
  •     Point resolution = 0.28nm
  •     Information Limit > 0.14nm
  •     Lens Type-Side entry (Condenser/Objective)

Attachments:

  •     Digital Imaging - Gatan MatScan1kx1k progressive scan CCD
  •     Computer Control - Digital Micrograph
  •     Free Lens Control
  •     1000ºC double tilt holder
  •     Liquid N2 double tilt holder

Gatan Precision Ion Polishing System (PIPS)

Staff Contacts:

CQ Chen
(217) 300-4837

Jim Mabon
(217) 333-4265

Location: B59 Materials Research Laboratory

The Gatan 691 Precision Ion Polishing System (PIPSTM) is a user-friendly precision Argon ion beam polisher designed to produce high quality, TEM specimens with minimal effort.

Ion polishing is done by two variable-angle, miniature Penning ion guns. The operating angles of the guns, ± 10 deg., are independent of one another. Both guns accurately center the beam onto the specimen at any angle within this range. Theguns provide bright high current Argon ion beams and are capable of very high thinning rates. Easy alignment features are provided to accurately center the beams on the specimen. These features make it possible to thin specimens at very low angles in a reasonably short time.

An optical stereo microscope is used to inspect the specimen in its working position at any time during the thinning process to achieve precise control over the final stage of specimen thinning. This feature is especially important for insulators and semiconductors since these materials are transparent to light and the interference-fringe technique can be used to control the final specimen thickness in the region of interest to anaccuracy of about ±10 nm.

Several unique design features are incorporated into the Gatan PIPS:

  • High milling rates at shallow angles.
  • Milling angle +10° to -10°, Each gun independently adjustable
  • Milling voltage: - 100eV to 6.0KeV
  • Load lock for fast and simple specimen exchange.
  • Specimen holders for double sided, low angle milling.
  • Beam modulation offering both single and double sector milling.

Gatan Cryo-PIPS

Staff Contacts:

CQ Chen
(217) 300-4837

Jim Mabon
(217) 333-4265

Location: B59 Materials Research Laboratory

In addition to all the features of the normal Gatan PIPS, the Gatan Cryo-PIPS has extra capability of the following

  • Liquid nitrogen sample coolingduring milling for temperature sensitive materials
  • CCD imagery for "real-time" video imagingon a digital monitor