Wednesday, 27 July 2011

TOP 10 AM papers: Grant et al. 1976, Scanning Electron Microscopy/1976 (III)

1982 prototype of QEM*SEM with mini-computer to the right at CSIRO Melbourne

Review of Grant et al. 1976, Scanning Electron Microscopy/1976 (III)

In the 70's, it was not uncommon to publish outstanding geoscientific research in workshop proceedings. This groundbreaking paper on "Multicompositional particle characterization using the SEM-microprobe" by Grant, Hall, Alan Reid and Martin Zuiderwyk is published in the Proceedings of the Workshop on Techniques for Particulate Matter Studies in SEM held at the IIT Research Institute in 1976. Over three decades ago, the authors - listed in alphabetical order - demonstrated the first computer-controlled automated mineralogy system and outlined a number of principle functions in mapping particles which changed little over the years despite the revolution in computational power and software languages since.

Grant et al.'s vision, as outlined in the introduction, is to determine sizes and composition of complex particles, and to "measure rather than infer" areas and perimeters to derive shape functions to better understand physical and chemical behaviors of particles in industrial and mineral treatment processes, i.e. mineral flotation and the degree of liberation during grinding processes.

The original instrument design consists of a mini-computer controlled e-beam which is automatically moved across the sample along a user-defined pattern. An initial "fast scan" locates the particles for detailed scanning. The dwell time for x-ray acquisition at each point can be defined. In addition, an "event acceptance filter" is in place to only record changes in material composition. Composition and e-beam coordinates are saved in form of digital maps composed of line segments and points.

The original system is setup to accept secondary and backscattered electron signals, absorbed specimen current, as well as energy-dispersive x-ray counts from either EDS detectors or microprobe. The measurement mode outlined is a proto-type for what is to become the Particle Mineral Analysis (PMA) in the QEM*SEM and later QEMSCAN solution. It uses either rapid BSE or SE signals to locate the edges of particles which are in turned scanned in detail using x-ray signals. The software includes algorithms linking particles extending across multiple frames, similar to the "field stitch" pre-processor in iDiscover. In addition, mixed signals between particle and mounting medium, referred to as "boundaries" are resolved, a first step in the development of Species Identification Program (SIP) boundary phase definitions and the award-winning "Boundary Phase" pre-processor by Paul Gottlieb in the iDiscover software package. Touching particles are discussed beyond shape parameters using secondary electron images to discriminate same phases in the discussion with reviewers at the end of the paper.

The boundary coordinates are saved allowing for a visual display of the data and basic image analysis functions, including the particle-by-particle calculation of area, perimeter, centroid and even the option to report phase contributions to the perimeter. Particular consideration is given the stereological challenges of reporting unbiased particle size, shape and composition from 2-D data. Interestingly, the authors point out to future investigations in mounting particles onto surfaces and using a second set of detectors providing biaxial views to better estimate particle sizes in three dimensions.

It can be fairly said that the authors laid the foundation for automated mineralogy and future software developments. It is a testimony to their visional capacity that they discus ways to move forward in 3-D particle analysis and even applications of their algorithms beyond rock particles, such as the analysis of pore space or images of macro-scale objects.

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