Specimen Heating for SEM with the Murano Heating Stage

Metallurgical and materials science studies can considerably benefit from directly observing specimen heating within the scanning electron microscope. Gatan’s MuranoTM heating stage makes it possible to dynamically observe a number of phenomena such as oxidation, phase transformations, grain growth, and recrystallization during heating.

The heating stage has been particularly designed to interface with traditional SEM stages, containing a thermally isolated interface which is perfect for electron backscatter diffraction (EBSD), SEM imaging, and focused ion beam (FIB milling).

The temperature range of the heating stage covers ambient to 950 °C. In order to aid catalysis, oxidation or reduction reactions, gas injection is achieved through a capillary (optional) adjoining the sample. Control over the external gas flow is achieved through a flange-mounted needle valve.

The internal SEM chamber, and the surrounding detectors, are protected by a water-cooled base and shield. A low vibration water chiller provided in each individual system interlocks with a PC-based temperature controller, a power supply, and a safety flow switch.

The specimen heater platform has been customized to facilitate easy loading. Logging software makes it possible to record time stamps against temperatures. Combined with an image processing system and a DigiScan™ digital beam control, temperature data from the Murano heating stage can be stamped on an experiment’s video recordings and images by means of the in-situ video software.


EBSD map of bronze specimen recrystallization taken in-situ at 800 ºC using Murano heating stage.

Advantages

In-situ heating and tensile testing stages can provide a better understanding of materials research and enable dynamic microstructural observations.

  • Modules are designed especially for the SEM environment
  • Custom designs facilitate fast fitting and removal from SEM stages so that normal SEM use can be restarted instantly
  • Compatible with geometrical requirements of a wide range of detectors, including EBSD for dynamic observations

Heating Stage Modules

  • Offline specimen mounting and storage is achieved through a proprietary design
  • Allows real-time crystallization and phase transformations analyses at elevated temperatures up to 950 °C
  • Murano stage available for heating to 1250 °C for SED imaging, and 950 °C for EBSD applications
  • Heat protective shielding and water cooling ensure excellent protection at increased temperatures
  • Bulk specimen support has been particularly designed to operate within SED/EBSD/FIB geometry limitations
  • Additional bias control to aid imaging at elevated temperatures

Key Features

The main features of the Murano heating stage are as follows:

  • Compact design: Small size accommodates the wide range of tilt needed for EBSD, and also allows easy insertion and removal of device
  • PC-based temperature controller: Temperature precision < 0.5 °C and stability <1 °C/h
  • Powerful, in-situ heating holder: Fast heating and cooling (>100 °C/min) of specimens up to several mm in size
  • Option for gas injection nozzle: Enables localized gas reaction studies at increased temperatures
  • Water-cooled module: Protects SEM chamber and enables specimen temperatures of 950 °C

Applications

The Murano heating stage is used in the following applications:

  • Gas reaction studies
  • Characterization of grain growth
  • Identification of phase transformation and eutectic temperatures
  • High temperature semiconductor failure analysis
  • Recrystallization of deformed structures

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