Metallurgy Applications of Handheld X-ray Diffraction

Lead Research Organisation: University of Leicester
Department Name: Space Research Centre

Abstract

X-ray powder diffractometry is a well-established materials analysis technique which produces results directly linked to the microcrystalline structure of the sample material. It is the definitive method for the identification and quantification of the mineral content of rocks, and finds wide-spread application in other areas such as metallurgy and the development of novel materials. Many materials are crystalline in nature at the micron-scale - rocks, soils, many raw materials and building materials, metals - and so the technique has very wide applicability both in research and industrial contexts. Standard methods generally require careful, and destructive, preparation of the sample.

Dr Graeme Hansford has invented an innovative X-ray diffraction (XRD) technique which is suitable for implementation in a handheld instrument format. The unique feature of this XRD technique is tolerance to surface morphology on the mm-scale which allows non-destructive analysis of samples with no preparation of the sample at all. This technique is being developed at the University of Leicester and in conjunction with Bruker Elemental, a major manufacturer of scientific instruments. To date, there are no commercial handheld XRD instruments and its production would represent a global first. An earlier project focussed on developing mining applications of this technology, while this new project is aimed at developing the technique for application to a wide range of metals, alloys and coatings. It is anticipated that this technology will find application in steel manufacture, aerospace, marine, nuclear and power systems industrial sectors.

Publications

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Hansford G (2018) A prototype handheld X-ray diffraction instrument. in Journal of applied crystallography

 
Description The overarching aim of this research project was to investigate the efficacy of handheld XRD instrumentation (developed on an earlier grant) to the crystallographic analysis of metals and alloys. The following conclusions were reached:
1. The technique is capable of detecting only the major phases present in metals in the large majority of cases. For example, the technique is not sensitive to the presence of iron carbides in steel and iron alloys.
2. The technique is most likely to find application in the analysis of metals/alloys consisting of more than one major phase e.g analysis of ferrite and austenite phases in steels.
3. With further development, the technique can be applied to the analysis of texture (aka preferred orientation) in metals.
Exploitation Route The next step is to transfer the technology into industry. The PI and the University of Leicester are in active discussions with a US company which has identified a specific application. They are currently constructing an experimental mock-up in order to perform their own experimental assessment. In addition, the PI holds a Royal Society Industry Fellowship, working with Rolls-Royce plc and Tata Steel UK Ltd. The primary aim of this fellowship is to develop applications of handheld XRD in steel manufacture, and aerospace, marine, nuclear and power systems sectors. It is expected that use of handheld XRD in these sectors will serve to streamline a variety of manufacturing and inspection processes, resulting in substantial cost savings. This work will also serve to make the licencing proposition the University is able to offer more attractive.The fellowship also includes the remit to develop cultural heritage applications of the technology.
Sectors Aerospace, Defence and Marine,Energy,Manufacturing, including Industrial Biotechology,Culture, Heritage, Museums and Collections

 
Description Industry Fellowship
Amount £117,551 (GBP)
Funding ID IF170021 
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 04/2018 
End 04/2022
 
Description Non-Destructive High-Resolution X-ray Diffraction for Cultural Heritage
Amount £467,165 (GBP)
Funding ID EP/R024626/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 03/2018 
End 03/2021
 
Description Applications of Handheld XRD with an Industrial Partner: Rolls-Royce 
Organisation Rolls Royce Group Plc
Country United Kingdom 
Sector Private 
PI Contribution Investigation of the application of novel XRD methods, particularly handheld XRD, to the complex manufacturing processes involved in the production of jet engines. The aim is to streamline one or more processes and consequently save costs and reduce waste. The contribution is to test relevant samples using a prototype instrument, process and analyse the data and present the results to Rolls-Royce personnel for assessment.
Collaborator Contribution Rolls-Royce are providing material samples and imparting relevant knowledge of the manufacturing processes. They are also providing access to analytical facilities where appropriate.
Impact No impact yet. The collaboration is multi-disciplinary: advanced materials/metallurgy, X-ray diffraction, instrument design.
Start Year 2018
 
Description Corrosion analysis of Mary Rose cannonballs using handheld XRD and synchrotron XRD 
Organisation Mary Rose Trust
Country United Kingdom 
Sector Charity/Non Profit 
PI Contribution We are investigating the capabilities of a prototype handheld XRD instrument in the analysis of the corrosion of iron-based cultural heritage artefacts, specifically applied to cannonballs from the Mary Rose. The contribution has been the provision of the prototype instrument, data acquisition and processing. In addition, we are sourcing pure mineral samples to make up representative mixtures for comparative measurements. We have also conducted non-destructive synchrotron XRD measurements on the same samples (analysis yet to be done).
Collaborator Contribution Provision of samples in the form of Mary Rose cannonballs (or fragments).Interpretation of the results from a cultural heritage perspective, especially relating to the conservation of iron artefacts.
Impact No outcomes as yet. Highly multidisciplinary - X-ray physics, materials analysis by XRD and XRF (mineralogical and elemental analyses), cultural heritage and conservation.
Start Year 2017
 
Description Corrosion analysis of Mary Rose cannonballs using handheld XRD and synchrotron XRD 
Organisation University College London
Department Institute of Archaeology
Country United Kingdom 
Sector Academic/University 
PI Contribution We are investigating the capabilities of a prototype handheld XRD instrument in the analysis of the corrosion of iron-based cultural heritage artefacts, specifically applied to cannonballs from the Mary Rose. The contribution has been the provision of the prototype instrument, data acquisition and processing. In addition, we are sourcing pure mineral samples to make up representative mixtures for comparative measurements. We have also conducted non-destructive synchrotron XRD measurements on the same samples (analysis yet to be done).
Collaborator Contribution Provision of samples in the form of Mary Rose cannonballs (or fragments).Interpretation of the results from a cultural heritage perspective, especially relating to the conservation of iron artefacts.
Impact No outcomes as yet. Highly multidisciplinary - X-ray physics, materials analysis by XRD and XRF (mineralogical and elemental analyses), cultural heritage and conservation.
Start Year 2017
 
Description Tata Steel UK collaboration 
Organisation TATA Steel
Department Tata Limited UK
Country United Kingdom 
Sector Private 
PI Contribution Investigation of the utility of novel XRD methods to steel manufacture.
Collaborator Contribution Provision of relevant samples; know how concerning the production of steel and what XRD measurements would help to streamline operations.
Impact Publication: doi 10.1107/S1600576716011936 The relevant disciplines are: steel manufacture, X-ray diffraction, instrument design
Start Year 2015
 
Title Working handheld XRD prototype 
Description A prototype handheld X-ray diffraction (XRD) instrument has been developed by modifying a handheld X-ray fluorescence instrument from Bruker Elemental. The prototype gave the first successful results in September 2014. Results yielded by the instrument were improved by the addition of the capability to evacuate the sensorhead in March 2015. 
Type Of Technology Detection Devices 
Year Produced 2014 
Impact The prototype instrument has been tested with iron ore and limestone rock and powder samples, and many types of metals/alloys. More recently, the instrument has been applied to the analysis of iron corrosion in archaeological artefacts, specifically Mary Rose iron shot. Successful phase analysis has been demonstrated in each case. The University of Leicester is actively pursuing a licencing deal with an instrument manufacturer. In addition, projects are underway to transfer this technology into industry (aerospace and steel production applications) and to investigate its potential in the analysis of cultural heritage artefacts.