Developing Applications of Mineral-Specific X-ray Diffraction

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

Abstract

Dr Graeme Hansford has invented a novel X-ray diffraction (XRD) technique which enables the enhancement of the diffraction signal from a specific mineral within a mixture. This technique has multiple potential commercial applications, primarily in metallurgy and mining. It can be implemented using relatively low-cost X-ray technology as a handheld or portable device or in a production line configuration. The technique is suited to applications in which the user is interested in one key mineral or phase, such as an important impurity. The method can be used to determine the presence or absence of this phase, and for quantification.

The primary targeted application at this stage is the quantification of retained austenite in steel production. The heat treatment of steels is mainly aimed at producing martensite which is an iron phase supersaturated with carbon. Martensite has generally desirable properties for steel applications, for example it is has a high tensile strength. Any austenite which does not convert to martensite (hence 'retained') may have benefits to the intended application or, more commonly, it may be deleterious. Measurement of the amount of retained austenite is therefore crucial for process and quality control purposes in the manufacture of steel. XRD methods are standard for retained austenite quantification, but current instruments cost in excess of £100k and either require destructive preparation of the sample or have a cumbersome measurement head which must be carefully positioned relative to the analysis area. In contrast, an instrument based on the phase-specific XRD technique can have a point-and-shoot format similar to handheld X-ray fluorescence instruments and is likely to cost ~£30k. This novel technique has the potential to disrupt the existing market in retained austenite measurement.

Another application example is the detection and quantification of quartz in iron ores. Quartz is commonly present as an impurity in iron ores and determines the optimum processing method because it is a hard mineral. A quick and accurate estimate of the quartz content in ores would allow rapid decision making at mines and mineral processing plants, saving costs through streamlining of operations and avoiding costly and wasteful errors. The mineral-specific XRD technique offers a compact and low-cost method of making such measurements.

Publications

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Hansford GM (2016) Phase-targeted X-ray diffraction. in Journal of applied crystallography

 
Description The primary aim of this research project was the development of an analytical technique, based on X-ray diffraction, to enhance the detection sensitivity to a specific crystallographic phase within a sample. Although the research showed that such enhancement is possible, the balance of advantages and disadvantages of the technique was shown to be not particularly favourable. It is possible that the developed technique may find niche applications in the future.
Exploitation Route There remains some potential for industrial applications of this research. The PI holds a Royal Society Industry Fellowship, working with Rolls-Royce, and the company is currently assessing whether to take forward a specific application that takes advantage of the experimental technique that was the subject of this research project.
Sectors Aerospace, Defence and Marine,Manufacturing, including Industrial Biotechology

 
Description Industry Fellowship
Amount £117,551 (GBP)
Funding ID IF170021 
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 05/2018 
End 04/2022
 
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 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 X-RAY ANALYSIS DEVICE 
Description An X-Ray analysis device comprising an X-Ray source and an X-ray detector and a method of analysis are disclosed. The X-ray source is arranged to emit a first characteristic X-Ray line and a second characteristic X-Ray line both incident on the sample. The X-Ray detector is adapted to detect X-rays diffracted by the sample. Each of the first and second characteristic X-Ray lines is diffracted at a distinct diffraction angle determined by each of the first and second lattice spacings to produce four diffraction angles, and two of the diffraction angles correspond to one another. 
IP Reference WO2016193687 
Protection Patent application published
Year Protection Granted 2016
Licensed No
Impact None. This patent application has now been allowed to lapse.
 
Description Geo.Rep.Net Meeting 3 Presentation 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Multi-disciplinary meeting to discuss the challenges surrounding geological repositories for storing nuclear waste and for carbon capture and storage, including the transfer of technology from high technology sectors (space, high energy physics) into this application.
Year(s) Of Engagement Activity 2015
URL http://www.georepnet.org/news.html?news_id=28
 
Description International Innovation article 
Form Of Engagement Activity A magazine, newsletter or online publication
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact An article which gives an in-depth snapshot of my research, including the X-ray diffraction techniques I am developing, their applications and my collaborations. I believe this is an excellent advert for further possible collaborators.

No impacts yet - publication due in late November 2014.
Year(s) Of Engagement Activity 2014
 
Description Spectroscopy Magazine Handheld XRD article 
Form Of Engagement Activity A magazine, newsletter or online publication
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Media (as a channel to the public)
Results and Impact An article devoted to the description of my research was written and published in the Spectroscopy magazine. The article is entitled "Handheld X-ray Diffraction for Remote, Field-Based Applications".
Year(s) Of Engagement Activity 2015
URL http://www.spectroscopyonline.com/handheld-x-ray-diffraction-remote-field-based-applications