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Environment and Mining

In the past two decades, environmental sciences have increased their share in the research portfolios of synchrotrons in general, and at the ESRF more specifically. Shaping a sustainable development, imagining renewable materials, improving energy management, understanding and mitigating pollution, etc, require a coordinated, shared and multifaceted approach. 

The ESRF offers a whole array of techniques to investigate environment-related materials, mainly X-ray absorption spectroscopy, X-ray fluorescence microscopy and X-ray microtomography:

  • Tracing of elements, including those in petrochemical products or identification of toxic concentrations of heavy metals.
  • Analysis of air pollution filters
  • Mineral characterisation
  • Geological studies
  • Soil analysis for environmental remediation.
  • Permeability and determination of microstructure of rocks, hardening of cement.

CASE STUDIES

Company or institute

University of Oslo, Norway

Challenge

The characteristics of shale reservoirs are closely related to their potential for shale gas production, which is of particular interest in energy exploration and resource exploitation. Researchers wanted to look inside samples of shale rock to identify the location and types of porosity and to discover whether the samples contain microfractures that could facilitate the onset of primary migration of hydrocarbon. Concerning porosity, the aim was to distinguish inorganic pores with capacity for gas storage from pores containing organic matter (kerogen).

Sample

The samples of shale were collected from a depth of around 1.8 km, from the Permian period in the northeastern part of the Ordos Basin, China. The shales had been formed in a transitional sedimentary environment, and the pore types are dominated by inorganic pores whose volumes are often larger than that of organic pores.

Solution

Multi-scale tomography at beamlines BM05 and ID16B was used to scan the samples with voxel sizes from 4 micrometres to 25 nanometres. Microtomography permitted imaging of a cubic centimetre sample volume to study the microstructure while nanotomography permitted imaging of regions smaller than 100 micrometres wide to study porosity at the nanoscale.

 

Tomographic reconstruction from the lowest resolution images (4 micrometre voxel size) collected at BM05.

 Figure 1: Tomographic reconstruction from the lowest resolution images (4 micrometre voxel size) collected at BM05. The 3D image was segmented to show microfractures that are oriented parallel to sedimentary layering. Each colour indicates a connected cluster of microfractures. Image credit: Chunqi Xue, Benoît Cordonnier and François Renard, University of Oslo.

 

High-resolution imaging with 50 nm voxel size collected at ID16B.

 Figure 2: High-resolution imaging with 50 nm voxel size collected at ID16B. Tomographic reconstruction coloured to show kerogen (organic matter) and porosity, blue and purple respectively. Chunqi Xue, Benoît Cordonnier and François Renard, University of Oslo.

 

Benefits

Microtomography at BM05 revealed microfractures oriented parallel to sedimentary layering (Figure 1). Nanotomography at ID16B (Figure 2) allowed the different types of pores to be visualised in 3D both for organic and inorganic pores. Analysis of the pore shapes from the nanotomographic reconstructions enabled quantification of various parameters such as porosity, coordination number and pore size distribution.

Reference

This work is part of the PhD thesis of Chunqi Xue, visiting researcher at the University of Oslo, Norway. Elodie Boller, Paul Tafforeau, Kudakwashe Jakata, Pauline Gravier and Benoît Cordonnier participated in the X-ray imaging studies.

 

Company

CNRS, MIT and the University of Haute-Alsace

Challenge

Limited petrol reserves are pushing oil companies to try to find new access to oil and gas. Drilling companies claim that trillions of cubic feet of shale gas may be recoverable, just in the UK. Accessing the rock is complicated. Kerogen is the organic matter which hosts hydrocarbons in gas shale structures. It is compressed within rocks a million times less permeable than in conventional hydrocarbon reservoirs. Hydraulic fracturing, or fracking, consists of drilling down into the earth and then directing a high-pressure water mixture to the rock that contains gas or oil inside. Researchers still don’t know much about kerogen. More knowledge could open doors to more environmentally-friendly extraction techniques.

X-ray microscopy (XRM) image of an untreated sample of gas shale, showing inclusions of pyrite, clay, organic matter and other minerals. Copyright: M. Hubler (MIT) and J. Gelb (Carl Zeiss X-ray Microscopy).
 

Sample

The international group of scientists studied four different kerogen samples of different origin and degree of maturation.

Solution

The X-ray scattering technique on beamlines ID11 andID27 at the ESRF gave them access to the chemical composition of the kerogen, its texture and density. At ID27, the sample was placed in a diamond anvil cell with a pressure of up to 5.1 GPa to reconstruct the conditions underground. 

Benefits

Using a hybrid method, combining an arsenal of experiments and molecular simulations, the team developed molecular models of kerogen with different maturities. These atomistic models were then validated by comparing them with experimentally accessible kerogen properties. They unravelled the adsorption, mechanical, and transport properties of this organic matter. The new findings should now help understand the microscopic behaviour of this disordered and heterogeneous matter and open doors to improved extraction technology.

Nature Materials, doi: 10.1038/nmat4541.

Company

iRock Technology Co., Ltd. is a rock-core analysis company with headquarters in Beijing, China. iRock offers integrated services and software to the oil and natural gas industry to provide a better understanding of their reservoirs and to improve recovery in conventional and unconventional reservoirs. A key technology to provide these services is called digital rock analysis.

The challenge

Digital rock analysis is a pore-scale imaging and numerical modelling technology to extract nanometre to centimetre scale geological and petrophysical information, as well as multi-phase fluid-flow data based on pore-scale displacement processes from digitized rock samples. One of the benefits of this technology is the capability to provide a large number of rock properties within a very short time compared to traditional physical laboratory experiments.

A prerequisite for calculating representative rock properties are high-quality 3D multi-scale images of a rock sample that capture the representative elementary volume (centimetre-millimetre) and at the same time resolve the finest structures, such as the smallest pores (micrometre-nanometre scale). Computed tomography is currently the best-suited technique to acquire 3D images of rock samples over several decades of length scales.

Due to the fulminant development of benchtop CT and micro-CT hardware during the past decade, it is nowadays possible to image decimetre to millimetre-sized rock samples at voxel sizes of few hundred microns down to one micron at good quality and within an acceptable time of minutes to several hours per sample. However, CT imaging with benchtop micro-CT machines below 1-micron voxel size are of lower quality and are extremely time consuming (>1 day/sample); imaging below 0.5 microns/voxel is not possible at all, in a reasonable time and with acceptable quality.

The crux is that approximately more than 60% of the reservoirs worldwide consist of rocks with very small pore systems, which require imaging at voxel sizes (far) below 1 micrometre with ideal scanning resolutions between 100 and 300 nanometres/voxel.

A partial solution is to use a dedicated nano-CT device for imaging but these machines are delicate with respect to stability, maintenance, flexibility in sample and voxel size and scanning times. So is the maximum sample diameter around 60-70micrometres and the voxel size is fixed to 65 nanometres.

Even if this machine is used in conjunction with micro-CT we are left with a gap in scanning resolution between 65 nanometres and approx. 1 micrometre per voxel. This is unfortunately exactly the voxel-size range required for the majority of reservoirs rocks.

irock1.png
3D digital rock model and geological, petrophysical and fluid-flow data that are commonly extracted.

 

Solution

With their flexibility in energy ranges, spot sizes and detection architecture, beamlines at ESRF can CT-scan our rock samples with varying sample diameters at resolutions ranging from micro- to nano-scale. Due to this capability it is possible to close the resolution gap, which is essential to investigate many reservoir rocks.

A regular micro-CT, imaged at 1 micrometre voxel size, shows that a large proportion of the pore space in the rock is unresolved. On ID19, by imaging at 280 nanometres per voxel the results do not show partial volume effects and resolve the entire pore space (Fig. 2).

The effects of unresolved voxels in digital rock analysis are dramatic, since a clear segmentation of the rock phases is not possible. Every voxel layer that is classified into a wrong rock phase can offset subsequent calculations by orders of magnitude and leads to inadequate simulation results.

Access to the ESRF beamlines offers quick and high-quality imaging at flexible voxel sizes and a range of sample sizes, which is not achievable with laboratory CT machines. The acquired images provide a profound base to build representative 3D digital rock models and extract rock properties at a high confidence level.

Benefits

Next to the image quality, the higher sample throughput compared to laboratory devices helps iRock to plan and conduct projects for the oil and gas industry in shorter time. The oil and gas companies, in turn, benefit from great time savings in comparison to their traditional methods - weeks and months instead of several years for a typical project.

irock2.png

Comparison of a carbonate rock imaged with conventional micro-CT (upper panel; 2mm side length, 1 micro-metre voxel size) and synchrotron CT (lower panel; 0.5 mm side length, 280 nm voxel size). To the left are the 3D volumes, to the right are 2D slices across. Black colour is pore space, light grey indicates solid grains and intermediate grey shades are unresolved voxels (partial volume effect). 

 

Company or institute

Geological Survey of Finland

 

Challenge

The aim of the research was to decipher the spatial characteristics of ore-forming processes using high-resolution 3-D synchrotron techniques in complement to 2-D lab-based computed microtomography.

 

Sample

The samples were oriented drill core samples extracted from the Suurikuusikko orogenic gold deposit of northern Finland.

 

Solution

Much of our knowledge about the textural characteristics of orogenic gold deposits comes directly from laboratory-based two-dimensional (2-D) trace element mapping and analysis. A more detailed insight into ore-forming processes could be obtained through high-resolution synchrotron X-ray computed micro- and nano-tomography, which are versatile, non-destructive technologies for visualising ore textures at the micro- and nanoscales in 3-D.

The X-ray nanoprobe beamline ID16B was used to characterise the 3-D textural settings of gold from the micrometre down to the 50 nanometre scale. In particular, holotomography was used as the procedure for 3-D nano-tomography. Individual arsenopyrite crystals were separated and scanned with voxel sizes ranging from 50 nm to 150 nm.

3-D visuals of X-ray nanotomography data from an arsenopyrite (Apy) crystal.

3-D visuals of X-ray nanotomography data from an arsenopyrite (Apy) crystal. a) Backscattered electron image (BEI) of SEM showing rutile (Rt) and gold (Au) inclusions inside arsenopyrite. b) Nano-CT slice showing replicate of BEI for comparison. c) Surface rendering of arsenopyrite along with two orthogonal grayscale slices showing gold and rutile. d) Three horizontal slices showing location of gold at three different levels inside rutile. e) Inclusions of gold and rutile showing preferred alignment within arsenopyrite (from Sayab et al., Geology 44, 739-742 (2016), © 2016 Geological Society of America).

Benefits

Synchrotron X-ray computed microtomography and nanotomography make possible the visualisation and quantification of rock volumes in 3-D. This ultra-high-resolution technique illustrated the 3-D distribution of micro- to nanoscale gold inclusions, mostly associated with primary rutile or along secondary microfractures inside arsenopyrite.

 

The results show 3-D texture, mineralogy, mode, and relative timing of gold formation inside arsenopyrite. In addition, the size, shape, mode, and 3-D textural setting of gold at the submicron level inside sulphides revealed by nanotomography can be useful in evaluating the treatment of ores by different processing options, assay calculations, and effective recovery methods.

 

Reference

Three-dimensional textural and quantitative analyses of orogenic gold at the nanoscale, M. Sayab, J.-P. Suuronen, F. Molnár, J. Villanova, A. Kallonen, H. O’Brien, R. Lahtinen, M. Lehtonen, Geology 44, 739-742 (2016); DOI: 10.1130/G38074.1.