Correlative Mapping of Crystal Orientation and Chemistry at the Nanoscale

Lead Research Organisation: University of Manchester
Department Name: Materials


Advanced materials lie at the heart of a huge number of key modern technologies, from aerospace and automotive industries, to semiconductors through to surgical implants. Central to the study of materials is the ability to analyse the structure of materials from the atomic scale, up through the microscopic structure and on to the size of individual components and devices. Only by understanding this hierarchy of structure can the properties and performance of devices and components be optimised.
Transmission electron microscopy (TEM) is a key technique for characterising the local structure and chemistry of a wide range of materials. It is possible to gain information about the arrangement of atoms through imaging and electron diffraction patterns, and also to study composition via complementary spectroscopic measurements. One of the greatest strengths of the TEM is the ability to study tiny volumes of material, and hence to uncover information about the local defects and interfaces which often control the macroscopic properties of modern devices and materials.

In this proposal we aim to install a state-of-the-art TEM with a dedicated electron diffraction camera that enable ultra-fast and large area analysis of the crystal structure, orientation and strain in engineering materials, alloys, ceramics and coatings. Furthermore, the high sensitivity of the new detector will also allow the same range of experiments using low electron doses. Excitingly this will open up new opportunities to study the atomic arrangement and microstructure of materials that are traditionally not suited to electron microscopy methods. These include organic materials (such as polymers, composites and pharmaceuticals) and also the variety of novel hybrid organic-inorganic materials that are showing great potential for technologies such as solar cells, gas storage and targeted catalysis. This new advance is particularly important as such organic and hybrid materials are difficult to characterise using traditional X-ray diffraction methods and the microstructure of ordered and disordered domains, defects and interfaces is often poorly understood for these materials. Only by understanding such structural complexity can we hope to control and harness their amazing breadth of properties.

Combined with this diffraction capability will be high efficiency X-ray spectroscopy compositional analysis allowing the simultaneous analysis of the local atomic structure and chemistry of samples. Such correlative experiments will allow a better understanding of the macroscopic behaviour of materials and device, for example understanding how trace impurities affects the way cracks extend through barrier coatings or the structure changes that occur when hybrid framework materials absorb gas molecules. This will include the incorporation of advanced data science methods (often referred to as big-data approaches) to help process and understand the huge quantities of data that such a system can generate. In this way it should be possible to unlock secrets of material structure that would be impossible to ascertain by the isolated study of either crystal structure or composition.

This new analytical power will be used in conjunction with a range of in-situ experimental methods that will allow materials and devices to be subjected to conditions such as temperature, fields, stress or chemical attack during the studies. By mimicking realistic operating conditions the true behaviour of materials can be explored and optimised for the benefit of all.

Planned Impact

The proposed instrument will provide a state-of-the-art facility for characterising advanced materials and allowing improved understanding of materials performance. Advanced materials characterisation enables the development of new and improved technologies, which provides economic benefit through industrial partnerships and new products and services; as well as providing improvements in day-to-day life as technologies become cleaner, cheaper, more efficient and more reliable.

There is a wide variety of areas where the development of advanced materials is key if we are to solve the scientific and technical issues facing UK industry and the rest of the world. Examples include:

- The development of improved aerospace and automotive alloys is essential to reduce the cost of foreign travel while reducing the carbon footprint of transport.
- The development of improved pharmaceuticals could reduce the frequency patients have to take medication and reduce the cost of public medicine.
- Addressing the corrosion and degradation of materials during their operating lifetime, this can not only save on repair and replacement of infrastructure but also lead to safer transport, industry and power networks.
- Developing new framework materials for gas storage, allowing safer nuclear technologies or producing more efficient filters leading to cleaner air and water around the world have clear environmental impact.
- Understanding the interaction between nanomaterials and biological systems to allow new medical technologies and to manage issues of toxicity.

The importance of access to high level TEM characterisation for UK industry is illustrated by the large volume of our facilities current research funding that is either directly from industry or associated with industrial support (estimated >60%).

The new TEM has a further goal to increase our ability to supply UK industry with highly skilled researchers. The human output of the facility will be scientists with cutting edge technical and problem solving abilities, who will provide evident benefit to the skills base of the wider UK workforce, especially given the current shortage of highly skilled candidates for engineering and technical roles in the UK economy. An example of this is that the instrument has the capability to produce very large and complex data sets and researchers with the skills required to analyse such big data systems are known to be of high demand for high tech companies such as google, IBM etc.


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Duran E (2020) The structure of a new nano-phase of lanthanum-doped strontium titanate in Journal of Solid State Chemistry

Description This grant purchased a new transmission electron microscope (TEM) with combined elemental mapping and high resolution structural imaging and diffraction capabilities. After extensive discussions with manufacturers we tendered and purchased the unique instrument. Installation started before the pandemic in March 2020 and the instrument was signed off and made available for first users in November 2020. In summer 2021 it was possible to get the engineer to visit from France to complete the precession diffraction part of the installation. The cryogenic-holder capabilities were purchased in February 2021 and commenced use in April 2021. However, with COVID impacting travel and staffing we have not completed all the planned 20 days free proof of principle access to external users. The university is committed to continuing to support this for the next 12 months despite the end of the grant.
Exploitation Route Over 50 new and existing TEM users have been trained on this instrument, impacting work on at least 15 UKRI grants.
Sectors Aerospace, Defence and Marine,Chemicals,Electronics,Energy,Pharmaceuticals and Medical Biotechnology

Description Mapping the microstructure of soft and complex materials with electron crystallography
Amount £359,731 (GBP)
Funding ID URF\R\191017 
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 09/2019 
End 09/2022
Description Departmental Seminar, University of Durham 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Other audiences
Results and Impact Delivered a departmental seminar introducing the techniques and capabilities specifically provided by the equipment acquired from this grant. The goal was to raise awareness of the unique experimental capabilities it provides and to introduce the main methods of data analysis used for crystallographic mapping of materials. Local users have since been in contact to start collaborations where the experiments will use this equipment to explore the nanostructure of thin film materials.
Year(s) Of Engagement Activity 2019
Description Departmental Seminar, University of York 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Other audiences
Results and Impact The seminar was intended to introduce the capabilities of crystallographic mapping to a wider academic audience at an institution outside the host institution, and to offer the possibility of utilising the unique capabilities of the equipment purchased with the grant for studying materials sstems being developed by other researchers. Since the talk there have been discussions about experiments to study the structure and composition of thermoelectric materials, and materials for spintronic application on the equipment. This will hopefully lead to the establishment of longer-term collaborations between the institutions.
Year(s) Of Engagement Activity 2020
Description Interview for Manchester's Covid Catalysts Campaign 
Form Of Engagement Activity A press release, press conference or response to a media enquiry/interview
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Media (as a channel to the public)
Results and Impact Interviews with members of the university discussing the impact of the pandemic on researcher progress, students and the bp-ICAM
Year(s) Of Engagement Activity 2020
Description Interviews and discussion with potential undergraduate students 
Form Of Engagement Activity Participation in an open day or visit at my research institution
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact Each Department Open Day (~15 dates per year) involves visits for 60-100 school pupils who are potential or actual university applicants. Prof Haigh regularly interviews candidates for these events. In 2020/2021 these have been operating online.
Year(s) Of Engagement Activity 2019,2020,2021
Description Seminar at St Andrews University 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Regional
Primary Audience Postgraduate students
Results and Impact Plenary presentation at St Andrew's Electron microscopy Workshop given by Prof Sarah Haigh. As part of this talk Prof Haigh advertised the potential of the new TEM to attendees (estimate as 120 participants from the region, including postgraduate and graduate researchers).
Year(s) Of Engagement Activity 2020