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Scanning Electron Microscopy (SEM) and X-Ray Microanalysis

Hitachi SU 3500 scanning electron microscope (SEM)

The Sandberg Geomaterials Department has its own in-house Hitachi SU 3500 scanning electron microscope (SEM) fitted with a state of the art Oxford Instruments energy dispersive X-Ray microanalysis system and X-Max X-ray detector capable of light element detection.  The equipment is supervised by staff with over 30 years’ experience in SEM and associated petrographic/analytical techniques.  Sandberg is UKAS accredited for the SEM analysis of concrete and crushed rock fill.

Hitachi Scanning Electron Microscope (SEM) fitted with a state of the art Oxford Instruments INCA energy dispersive X-Ray microanalysis system.

Hitachi Scanning Electron Microscope (SEM) fitted with a state of the art Oxford Instruments INCA energy dispersive X-Ray microanalysis system.

Capabilities

The Sandberg SEM is able to carry out very high-resolution imaging but also has the additional ability to examine samples at low vacuum enabling easily damaged materials or fragile hydrated samples, such as clays or polymers, to be examined. High-resolution, low vacuum imaging in secondary electron, as well as backscattered electron mode, is possible using the Hitachi UVD secondary electron detector.

The microscope has a maximum resolution of 7nm (0.000007mm) and can operate at magnifications of up to x100,000 enabling the morphology of cement hydrates in concrete and clays to be revealed in great detail. The microscope also has a large sample chamber allowing samples of up to 70mm in diameter to be examined.

Typical X-ray spectrum from a GGBS particle in concrete. Spot chemical analysis measuring about 0.01mm in diameter

Typical X-ray spectrum from a GGBS particle in concrete. Spot chemical analysis measuring about 0.01mm in diameter.

The SEM is fitted with a backscattered electron detector that can be used to provide images of samples that show variation in chemical composition. Materials containing elements with a high atomic mass, such as iron, appear brighter d electron images than materials containing elements with predominantly low atomic masses, such as magnesium or carbon.

Chemical analysis / X-ray Microanalysis

The Oxford Instruments INCA analysis system coupled with an X-Max 50 dry X-ray detector allows for the simultaneous analysis of multiple elements and can provide a cost-effective solution to establishing general information about the chemical composition. A typical analysis would commence with the identification of the elements present which are then analysed simultaneously and expressed as either elements or oxides.

The ability to undertake chemical analyses is indispensable for most types of SEM-based analysis. With the Sandberg SEM, it is possible to make spot chemical analysis of particles as small as 1 µm (0.001mm) in diameter. Much larger areas of up to 4mm x 4mm can also be analysed. X-ray mapping can be used to show the spatial distribution of elements.

Working at low accelerating voltages it is possible to obtain chemical compositions of very thin surface coatings that are less than 0.001mm thick. This ability is vital for staining investigations.

Image Analysis and X-phase Mapping

The SEM has the ability to carry out image analysis based either on contrast/ brightness or on chemical or mineral phase composition. This technique has many applications and can be useful for quantifying proportions of morphological features such as microscopic voids/pores, for examining the distributions of elements such as chloride around a crack in concrete or for investigating the distribution of specific compounds on a crack surface such as the image shown below:

image analysis

For more information contact our in-house expert:

avatar

Mike Eden

Direct Tel: 020 7565 7077
Email: mike.eden@sandberg.co.uk
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