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LINAC
BRIGHT Beamlines

X-ray Fluorescence Nanoprobe beamline (Nanoprobe)

The Nanoprobe beamline it similar to a Scanning Electron Microscope (SEM) that uses hard X-rays instead of electrons.  Hard X-rays give the Nanoprobe unique analytical capabilities, revealing elemental, chemical and structural information and the ability to interrogate specimens from a diverse range of scientific fields.

The core capability of the Nanoprobe beamline is to deliver an intense and highly focussed beam to a specimen.  The design of the Nanoprobe beamline is such that intensity and resolution can be traded, enabling improved elemental sensitivity at the cost of spatial resolution.

The focussed beam illuminates a narrow column through a specimen, and multiple detectors around the specimen will collect various X-ray signals including fluorescence, scattering or diffraction.  Scanning of the specimen through the beam enables sequential sampling, which can be used to build up maps of the specimen’s structure and composition.

The Nanoprobe endstation will be optimised for the use of an energy-dispersive detector to determine the energy of secondary X-rays (fluorescence) emitted by the specimen.  The energies of these secondary X-rays provide fingerprints to enable elemental identification with spatial resolution down to 60 nm and very high sensitivity (low parts per million).

nanoprobe endstation

Elemental mapping using the Nanoprobe instrument.

An X-ray beam is focussed onto a specimen using a KB mirror pair.  In this figure, the focussed beam passes through a Maia detector, positioned to capture the maximum amount of secondary photons emitted by the specimen.  The specimen is scanned through the beam, and at each position the Maia energy dispersive detector will be used to determine the energy of characteristic fluorescence X-rays emitted by the specimen, as well as Rayleigh and Compton scattered X-rays. 

An on-axis photon-counting camera will be used to measure the specimen’s transmission and differential phase.  Along with techniques such as ptychography (aka Scanning X-ray Diffraction Microscopy, SXDM), these techniques can build up structural images of the specimen at a resolution substantially better than that of the focussed beam (down to around 15 nm).

Radiation-induced specimen damage will be mitigated using cryogenics, although this will compromise the special resolution of the system under study.

A precision rotation stage will enable acquisition of rotation series for tomographic data acquisition for most measurement modes.

  • Ultimate spatial resolution: best effort: 60 nm (~1x109 ph/s @ 10 keV).  Targeting 100 nm (~1x1010 ph/s @ 10 keV) for routine operations.
  • Ultimate sensitivity of ~µM per 0.1 sec dwell will be achieved with a 350 nm beam size and broad-bandpass beam (~1x1011 ph/s @ 10 keV).
  • Elemental mapping; elements heavier than silicon (Z > 14), except for elements between yttrium and iodine.
  • XANES Spectroscopy: elements from chromium to strontium (24 < Z < 38), and heavier than caesium
    (Z > 54)
  • Ptychography / SXDM for phase / absorption contrast at ~15 nm resolution
  • Tomography enabled
  • Cryogenics available at reduced resolution
  • Off-line characterisation capabilities, enabling pre-alignment of specimens using optical fluorescence microscopy

Samples

  • Typical specimen maximum dimensions will be 3 mm across.
  • Typical specimen thickness will be ~10 µm, although thicker may be possible depending on the material.
  • High-resolution positioning range will be around 300 µm.
  • We are planning for a small Physical Containment (PC-1) / Biosecurity Containment (BC-1) laboratory to be connected to the endstation.  PC-2 / BC-2 certification will not possible at the Nanoprobe endstation.  We are pursuing the possibility of a quarantine Approved Arrangement certification for the endstation.

The Nanoprobe beamline will enable core techniques including:

  • Elemental mapping for elements heavier than silicon (Si),
  • X-ray Absorption Near Edge Spectroscopy (XANES) Chemical state analysis and mapping of elements ranging from chromium (Cr) to strontium (Sr),
  • Scanning Transmission and Differential Phase Contrast @ native beam resolution, and
  • Ptychography @ around 5 times better than native beam resolution.

At the same time, the Nanoprobe beamline will provide a launching pad for the development of further techniques including:

  • Elemental Tomography
  • Scanning nano-Small- and Wide Angle X-ray Scattering (nano-SAXS/WAXS)
  • Scanning nano-diffraction. 

Scientific Applications

The Nanoprobe beamline will be able to address questions across a wide variety of scientific disciplines, including:

Human health and biology

First-row transition metals including manganese (Mn), iron (Fe), copper (Cu) and zinc (Zn) play key roles in biological systems, and are a co-factor in an estimated 30% of proteins.  The Nanoprobe will provide a unique ability to map the distribution of these elements with high sensitivity and organelle-level resolution within biological systems such as cells and tissues to deliver insights into a range of questions in inorganic biochemistry with applications in eg mechanisms, pathology, and treatment of neurodegenerative diseases and other diseases of aging.

Food, agriculture, and plant biology

Micronutrients such as iron (Fe), copper (Cu), zinc (Zn) and selenium (Se) are essential to human nutrition. Simultaneously, toxic elements such as arsenic (As), cadmium (Cd) and lead (Pb) can be taken up by plants and so enter the food chain.  Mapping the distributions of these elements within soils, fertilisers, root systems, stems and leaves will deliver insights into uptake, storage and biological fate of these metals and so enable improvements to the food chain with the potential to impact global food security.

Advanced materials and manufacturing

Nanomaterials technology is a key driver for manufacturing industry, and the Nanoprobe will provide a cutting-edge technique known as ptychography to provide high sensitivity imaging of larger nanoparticles at the 15 nm length scale.  In addition, the ~60 nm X-ray probe will enable studies employing fluorescence, diffraction and scattering from small volumes within a specimen.  The ability to employ both methods on a specimen within the one instrument will enable insights into nanostructure and function.

Environmental studies

Nanoscale distributions of environmental toxins are elucidated using the Nanoprobe.  Examples include

  • Distribution and speciation of toxic metals such as lead (Pb), mercury (Hg), and arsenic (As) in mine tailings and groundwater
  • Uptake pathways afforded by plants
  • Remediation pathways afforded by both plants and mineralogy
Earth Science and minerals formation

Mineralogy occurs across length-scales ranging from the nanometre to the kilometre.  Providing insight bridging from the nanoscale to the microscale, the Nanoprobe will complement the XFM beamline (itself bridging the microscale to the decimetre scale) to provide a combination of detail and context that illuminates mineralogy and thus geological processes.  Strategies for mining and exploration will be improved through studies of gold (Au), platinum (Pt), and uranium (U) bearing ore deposits, with the ability to probe chemical speciation providing key insights difficult if not impossible to obtain using other methods.

Cultural Heritage, Archaeology, and Arts

Understanding of the distribution and speciation of elements within art and artefacts can provide essential clues into origin, provenance, history, and genesis.  Examples include:

  • Chemical fingerprinting of ochres provides insights into the early Australian trading routes and so the extent of relations between aboriginal tribes.
  • Chemical speciation studies of pigments in older paintings can greatly assist understanding of painting degradation and remediation

The applications of the Nanoprobe are very broad – this reflects the both the importance of metals to life and technology and the fact that you can put just about anything under a microscope!  The unique capabilities of the Nanoprobe – exquisite elemental sensitivity, high resolution, high penetration – make it a key instrument for addressing nanoscale structure – function relations across a broad range of science.  Taken from operating international facilities, specific examples of the kinds of measurements that we aim to deliver are listed below.

Elemental mapping at high resolution
Elemental mapping nanoprobe beamline

Elemental distributions in frozen-hydrated Chlamydomonoas (green algae) measured using the Advanced Photon Source BioNanoprobe, alongside complementary ptychographic imaging.
From Deng et al, Scientific Reports (2017).
 

 

Ptychography for advanced nano-manufacturing and materials science: integrated circuits

Ptychography is a computationally-intensive method that provides access to high-resolution imaging, and will be able to resolve features down towards 15 nm with the Nanoprobe beamline.

Nanoprobe science applications circuits

Ptychography of an integrated circuit fabricated with 16 nm technology. The apparent ‘hatching’ is due to these 16-nm vias and interconnects within the chip.  Brighter colours indicate higher projected electron density. 
Deng et al; Review of Scientific Instruments, 90, 083701 (2019)

Elemental Mapping and Tomography
elemental mapping and tomography

Elemental tomography of a diatom at 400-nm resolution reveals distribution of elements at micro-molar concentrations.  We anticipate that such a measurement could be completed in one shift (8 hours) using the Nanoprobe.  From de Jonge et al, PNAS (2010). 

 

Mapping chemical co-ordination using XANES spectroscopy and imaging.

X-ray microprobes and nanoprobes are commonly used to perform local tests of chemical speciation (oxidation state), but the Nanoprobe will leverage world-leading expertise at the XFM beamline to deliver XANES imaging at the Nanoscale.

mapping chemical coordination

Imaging of chromium (Cr) speciation within a paint sample from van Gogh, showing alteration of Cr chemistry due to degradation. Data from the ESRF, ID21. From Monico et al, JAAS (2014). 

Technical Information and Specifications

The Nanoprobe beamline is designed to produce a tight, bright focus.  In diffraction-limited mode, it will deliver 108 ph/s into a 60-nm spot; more commonly, it is anticipated that sensitivity requirements will push operations towards 1010 ph/s into 100 nm, or 1011 ph/s into 300 nm.  Typical resolution for biological specimens (with µM concentrations) will be of order 150 nm.

In order to achieve this small focus, the Nanoprobe beamline will be around 100 m long and will be situated alongside the IMBL, as indicated in this aerial overlay:

Location layout nanoprobe

Several design decisions have been taken in order to maintain the focussed flux on the Nanoprobe beamline, including:

  • Use of a Double Multilayer Monochromator (DMM) to transport the entirety of the undulator harmonic to the endstation at around 1% bandpass.
  • Horizontal and vertical focussing to a Secondary Source Aperture (SSA) to enable flux tunability with high dynamic range.  This optical configuration has been demonstrated to improve vibration resilience of the beamline transport.  The Horizontal and Vertical Focussing Mirrors (HFM and VFM) are situated in the First Optical Enclosure (FOE), on the technical floor within the main synchrotron building.
  • Endstation focussing optics will employ KB mirrors due to their high focussing efficiency (>80%) and achromaticity (wavelength independence of the focal length)

Beamline layout

nanoprobe detailed design layout

Technical Specifications

View Nanoprobe Technical Specifications

Source

Undulator

CPMU or IVU, 3 m length

Monochromation

DCM (Si 111)

Monochromatic for spectroscopic resolution

DE/E ~ 1.4x10-4

 

DMM

Broad-band for mapping sensitivity

 DE/E ~ 1x10-2

Endstation focussing Optics

KB mirrors

60 nm diffraction-limited resolution

~ 1 mrad NA

3 mrad nominal incidence angle

100% reflectivity cut-off energy: 17 keV

50% reflectivity cut-off energy: 22 keV

Scanning stages

(Indicative and target performance)

 

Axes: xyzθ.

> 200 µm scan range (fine positioning); ~5 nm precision

> 5 mm range (coarse positioning)

> 100 mm z range (beam parallel); ~100 nm precision

Minimum dwell ~ 1 ms / pixel transit

Energy Dispersive Detectors

Silicon drift diode (SDD)

>1 Mcps overall count rate

< 200 eV energy resolution (Mn Kα) at 1 Mcps rate

Transmission camera(s)

 

Photon counting detector

> 500 Hz frame rate

< 80 µm pixels

Camera length adjustable from 0.1 – 7 m

Beamline status

View Beamline status

Date

Stage

2018 August

Preliminary design commences

2020 April

Investment Case (IC) endorsement

2020 March

Radiation enclosures (hutches) tender release

2020 March

External building conceptual design

2020 June

Conceptual Design Report

2020

Tender submitted for Insertion Device (ID)

2021

Photon Delivery System (PDS) design review

2021

PDS tender release

2022

Satellite building construction

2023

Delivery and installation of equipment

2023

Cold commissioning commences

2024

Hot commissioning commences, includes expert users

*2024 Q3

First User Experiments; Beamline fully commissioned over the next 12 months

* Delay due to covid-19 considered unlikely

Staff

Dr Phil Eliades – Project Manager

Dr Martin de Jonge – Lead Scientist

Ms Michela Semeraro – Lead Engineer

Mr Nader Afshar – Lead Controls Engineer

Beamline Advisory Panel

Prof. Hugh Harris [Chair] – University of Adelaide

Prof. Brian Abbey – La Trobe University

Dr Louise Fisher - CSIRO

Prof David Paganin – Monash University

Dr Fatima Eftekhari [Retired] - Melbourne Centre for Nanofabrication

Assoc Prof Mark Hackett – Curtin University

Dr Alessandra Gianoncelli [International Advisor] - Sincrotrone Elettra, Italy

Prof Stefan Vogt [International Design Advisor] - Argonne National Laboratory, USA

Contact

as-nano@ansto.gov.au