Quantitative non-destructive nanoscale characterisation of advanced materials

Lead Research Organisation: University of Strathclyde
Department Name: Physics

Abstract

To satisfy the performance requirements for near term developments in electronic and optoelectronic devices will require pioneering materials growth, device fabrication and advances in characterisation techniques. The imminent arrival of devices a few atoms thick that are based on lighter materials such as graphene or boron nitride and also advanced silicon and diamond nano-structures. These devices pose new challenges to the currently available techniques for producing and understanding the resulting devices and how they fail. Optimising the performance of such devices will require a detailed understanding of extended structural defects and their influence on the properties of technologically relevant materials. These defects include threading dislocations and grain boundaries, and are often electrically active and so are strongly detrimental to the efficiency and lifetimes of nano-scale devices (a single badly-behaved defect can cause catastrophic device failure). These defects are especially problematic for devices such as silicon solar cells, advanced ultraviolet light emitting diodes, and advanced silicon carbide and gallium nitride based high power devices (used for efficient switching of large electrical currents or for high power microwave telecoms). For graphene and similar modern 2D materials, grain boundaries have significant impact on their properties as they easily span the whole size of devices.

Resolving all of these problems requires new characterisation techniques for imaging of extended defects which are simultaneously rapid to use, are non-destructive and are structurally definitive on the nanoscale. Electron channelling contrast imaging (ECCI) is an effective structural characterisation tool which allows rapid non-destructive visualisation of extended crystal defects in the scanning electron microscope. However ECCI is usually applied as a qualitative method of investigating nano-scale materials, has limitations on the smallest size features that it can resolve, and suffers from difficulties in interpreting the resulting images. This limits this technique's ability to work out the nature of defects in these advanced materials.

We will make use of new developments in energy resolving electron detectors, new advances in the modelling of electron beams with solids and the knowledge and experience of our research team and partners, to obtain a 6 fold improvement in the spatial resolution of the ECCI technique. This new energy-filtered way of making ECCI measurements will radically improve the quality of the information that can be obtained with this technique. We will couple our new capabilities to accurately measure and interpret images of defects to other advanced characterisation techniques. This will enable ECCI to be adopted as the technique of choice for non-destructive quantitative structural characterisation of defects in a wide range of important materials and provide a new technique to analyse the role of extended defects in electronic device failure.

Planned Impact

Our research programme will impact on researchers in both academia and industry who require information on the crystalline quality of their materials and subsequent electronic and optoelectronic devices, and on researchers developing new detectors and software tools for electron microscopy. Our research will result in new quantitative methods for materials characterisation, enabling for example optimisation of 2-D materials and improved performance of nitride-based electronic devices. Our project partners span researchers working on a diverse range of materials including nitride semiconductors, silicon, silicon carbide, diamond, graphene and ultrathin boron nitride thin films. While some of our co-investigators and project partners are working at the leading edge of electronic and optoelectronic device development, others are engaged in the development of next generation radiation detectors. Three of our project partners are international companies who are well placed to exploit advances we produce in electron microscopy techniques (Bruker Nano) and in materials characterisation (NXP Semiconductors UK Limited and IQE Plc). Throughout the grant period we will actively seek out new collaborators who would benefit from our new detectors and materials analysis expertise.

Where appropriate we will pursue the commercial development of our research through our industrial project partners in materials, instrumentation and software development. For example, in collaboration with Glasgow University and an industrial collaborator, we are presently preparing patents and are negotiating the licensing of our recent
novel applications of digital imaging direct electron detectors. From the simulation and analysis components of the proposal we will produce open source materials. Professional software will be packaged with associated tests and documentation and made available on a public open source repository such as GitHub or bitbucket. Bristol works closely with major semiconductor manufacturers, in particular NXP Stockport, MACOM Belfast, Element Six Didcot, ONSemi Belgium, Infineon Austria, Qorvo USA. The approaches and results
developed in this project will be discussed with these partners to feed back into their production processes. NXP is directly involved in this project and will be updated in project meetings; the other partners Bristol works with will be updated in meetings of other programmes such as the European ECSEL, EcoGaN and PowerBase events or US DARPA in one-to-one meetings to enable commercialisation.

We will engage with the wider public through participation in events held in the Glasgow and Bristol Science Centres and will continue, evolve and expand our involvement with public engagement, including work promoting science in local schools and contributions to the Glasgow and Bristol Science Festivals and European Researchers' Night. The team have a track record of giving lectures, writing articles, running workshops and quizzes, building exhibits, street busking, leading science street tours and providing kits to
schools. Specifically, to promote the research being undertaken in this project, we will provide resources on our website for teachers, school pupils and the public ranging from basic information on the physics and applications of semiconductors, through to instructions on how to make your own models of crystals and crystal defects via 3-D printing. We will also develop a Careers workshop, in collaboration with the Glasgow Science Centre, on the applications of microscopy.

Publications

10 25 50
 
Title Data for: "Determining GaN nanowire polarity and its influence on light emission in the scanning electron microscope" 
Description Electron backscatter diffraction (EBSD) patterns and backscatter electron (BSE) intensity image derived from EBSD patterns, BSE and secondary electron (SE) images and cathodoluminescence (CL) hyperspectral images 
Type Of Art Image 
Year Produced 2019 
URL https://pureportal.strath.ac.uk/en/datasets/b152a121-3495-4235-b9cd-985bf1355cd8
 
Title Data for: "Luminescence behaviour of semi-polar (10-11) InGaN/GaN 'bow-tie' structures on patterned Si substrates" 
Description This dataset provides the experimental data used to generate the figures in the paper entitled "Luminescence behaviour of semi-polar (10-11) InGaN/GaN 'bow-tie' structures on patterned Si substrates". The room temperature cathodoluminescence (CL) data was recorded using a variable pressure field emission scanning electron microscope (SEM, FEI Quanta 250) which is equipped with a custom-built CL hyperspectral imaging system. The CL system collects the emitted light at an angle of 45° with respect to the incident electron beam using a Cassegrain reflecting objective. The light is then dispersed using a 125 mm focal length spectrograph (Oriel MS125) and detected using an electron-multiplying charge-coupled device (Andor Newton). Low temperature CL was performed in a field emission gun SEM (Zeiss LEO DSM 982) equipped with custom-built liquid helium flow cryostage (CryoVac). The light was collected using a UV-enhanced glass fibre placed in close contact with the sample, dispersed with a 90 cm focal length monochromator (SPEX 1702) and detected using a liquid nitrogen-cooled, UV-optimised CCD. As the electron beam scans across the sample surface, a whole CL spectrum is recorded per pixel building up the 3D hyperspectral data set. 2D CL images can then be extracted from the hyperspectral data set, such as peak energy, intensity or half width. The room temperature and low temperature (12 K) measurements were acquired with a beam voltage of 5 kV. Electron channelling contrast imaging is a non-destructive, diffraction technique performed in the SEM. ECC images are generally constructed by measuring the intensity of the backscattered electrons (BSEs) as the electron beam scans across the surface of a suitably-orientated sample. Any changes in crystallographic orientation and local strain can be monitored by the variation in the BSE intensity causing a change in contrast in an ECC image. This allows the imaging of low-angle tilt and rotation boundaries, atomic steps and extended defects (e.g. TDs). ECCI is carried out in a forward scattering geometry in a field emission SEM (FEI Sirion 200), equipped with an electron-sensitive diode and a custom-built signal amplifier. Electron backscatter diffraction (EBSD) measurements were performed using a Nordlys EBSD detector from Oxford Instruments attached to an FEI Quanta 250 variable pressure field emission SEM. The EBSD data was acquired at 20 kV and at a sample tilt of 70° with respect to the normal of the incident electron beam. For the analysis of the EBSD data, the electron backscatter pattern (EBSP) from each pixel was compared to simulated dynamical Kikuchi patterns using a Bloch wave approach. Abstract of the paper: In this work, we report on the innovative growth of semi-polar 'bow-tie'-shaped GaN structures containing InGaN/GaN multiple quantum wells (MQWs), and on their structural and luminescence characterisation. We investigate the impact of growth on patterned (113) Si substrates which results in the bow-tie cross-section with upper surfaces having the (10-11) orientation. Room temperature cathodoluminescence (CL) hyperspectral imaging reveals two types of extended defects: black spots appearing in intensity images of the GaN near band edge emission; and dark lines running parallel in the direction of the Si stripes in MQW intensity images. Electron channelling contrast imaging (ECCI) identifies the black spots as threading dislocations (TDs) propagating to the inclined (10-11) surfaces. Line defects in ECCI, propagating in the [1-210] direction parallel to the Si stripes, are attributed to misfit dislocations (MDs) introduced by glide in the basal (0001) planes at the interfaces of the MQW structure. Identification of these line defects as MDs within the MQWs is only possible because they are revealed as dark lines in the MQW CL intensity images, but not in the GaN intensity images. Low temperature CL spectra exhibit additional emission lines at energies below the GaN bound exciton emission line. These emission lines only appear at the edge or the centre of the structures where two (0001) growth fronts meet and coalesce (join of the bow-tie). They are most likely related to basal-plane or prismatic stacking faults or partial dislocations at the GaN/Si interface and the coalescence region. 
Type Of Art Image 
Year Produced 2019 
URL https://pureportal.strath.ac.uk/en/datasets/c71c237d-a544-4bf5-b7d3-1432ea22608e
 
Title Data for: "Subgrain structure and dislocations in WC-Co hard metals revealed by electron channelling contrast imaging" 
Description This dataset contains the experimental data used to generate the figures in the journal article, "Subgrain structure and dislocations in WC-Co hard metals revealed by electron channelling contrast imaging". The electron channelling contrast imaging data was recorded using a Zeiss Auriga FIB SEM using the Zeiss supplied quadrant diode backscattered electron detector which is inserted beneath the pole piece. The sample was tilted by around 20° away from the horizontal to increase the intensity of the backscattered signal, as the number of backscattered electrons increases as you increase the tilt of the sample. A series of images of single WC grains with the sample at different tilts or for different rotations were then acquired. In the case of the tilt series, ECCI images were acquired for tilts between 17° and 22° with the sample tilt changed by 0.2° between image acquisitions. For the rotation series, the sample was tilted at 20° and rotated 10° between image acquisitions, with the sample rotated by 180? for each grain. ECCI is a SEM based diffraction technique which can be used to detect small orientation changes or changes in lattice constant in a material. ECCI micrographs may be produced when a sample is placed so that a plane or planes are at, or close to, the Bragg angle with respect to the incident electron beam. Any deviation in crystallographic orientation or in lattice constant due to local strain will produce a variation in contrast in the resultant ECCI micrograph. Extremely small changes in orientation and strain are detectable, revealing subgrains and extended defects such as dislocations and stacking faults. We can also investigate the contrast exhibited by a defect for different diffraction conditions, ultimately identifying the nature of the defect. EBSD data in this study was collected in a Zeiss Auriga FIB SEM outfitted with an Oxford NordlysNano system. EBSD maps were acquired at 20 or 30 kV accelerating voltage with a 10 nA beam and the sample tilted at 70° from the horizontal. In EBSD the sample is tilted at around 70? to the normal of the incident electron beam. The impinging electrons are scattered inelastically through high angles forming a diverging source of electrons which can be diffracted. The resultant electron backscatter diffraction pattern (EBSP) consists of a large number of overlapping bands, known as Kikuchi bands, which are closely related to a 2-D projection of the crystal structure. Acquiring EBSPs over a grid of points on a sample allows mapping of the sample's microstructure. Abstract of the paper: In this study, electron channelling contrast imaging (ECCI) and electron backscatter diffraction (EBSD) have been used to examine the substructure and dislocations in tungsten carbide (WC) grains in tungsten carbide-cobalt (WC-Co) hardmetals. These complimentary scanning electron microscopy (SEM) diffraction techniques provide quantifiable information of the substructure without the difficulty of transmission electron microscopy (TEM) sample preparation and examination. Subgrain structures in WC grains have rarely been reported previously because of the sample preparation difficulty, but this study has found they can occur frequently and may provide information on grain growth during sintering. ECCI has also shown for the first time complex dislocation networks across large grains, indicating accumulation of stress in as-sintered materials. To identify the defects revealed by ECCI more precisely, WC grains with surface normals [0001],[11 ¯00] and [112 ¯0], were identified using inverse pole figure orientation maps generated from EBSD data. ECC images from these grains reveal defects intersecting the surface and subgrains bound by dislocations. The combination of ECCI and EBSD allows for new insights into dislocation networks in a WC-Co hardmetal sample over a large, in this case 75 µm × 75 µm, field of view. 
Type Of Art Image 
Year Produced 2019 
URL https://pureportal.strath.ac.uk/en/datasets/c80a3a0c-a718-4941-ac82-8981d21799ce
 
Description A novel method to resolve signals, by using interactions between scattered electrons and low pressure gas in the microscope has been developed. Gaseous detectors show promise (DOI: https://doi.org/10.1016/j.ultramic.2020.112977) for electron channelling contrast imaging in environmental scanning electron microscope configurations, with the potential for separation of signals from different scattering processes and energy ranges.

EBSD, a related technique to the main methods of the grant, has been demonstrated to capable of resolving and characterising extended defects. This new 'virtual diode' approach, which will be the focus of future work in this area, shows strong potential for energy resolved measurements that can distinguish, for example, between surface topography and channelling in characterising samples.

The developed high precision stage is working, and will be used in research for many years. The design can be adapted by other groups, for example we have discussed plans a Polish group have to implement similar technology, and the stage itself will be taken to Kraków in a couple of months as part of this collaboration.
Exploitation Route As mentioned, the stage design will influence work in other academic groups. Additionally there has been approach from a company regarding characterisation tools, along with other industrial requests to characterise materials.
Sectors Electronics,Energy,Manufacturing, including Industrial Biotechology

 
Description This grant's research has led to approaches from a several companies interested in applying the results of our work. In turn this has resulted in collaborations with companies developing the next generation of detector technologies for scanning electron microscopes. Additionally there are approaches and also agreements by and with companies wanting to commercialise the new applications of EBSD and electron channelling contrast imaging we have developed. For example this work has led to a successful impact acceleration bid (Sept-Nov 2021, 3 months, £13k + £21.5k in-kind): Collaboration between Dr Carol Trager-Cowan and Dr Jochen Bruckbauer (Strathclyde) and Dr Andrea Pinos (Plessey Semiconductor Ltd). This project supported Plessey in developing the next generation of micro-light-emitting diodes (microLEDs) for innovative display solutions through advanced electron microscopy characterisation.
First Year Of Impact 2020
Sector Electronics,Energy,Manufacturing, including Industrial Biotechology
Impact Types Economic

 
Description RSE Saltire International Collaboration Award
Amount £12,000 (GBP)
Organisation Royal Society of Edinburgh (RSE) 
Sector Charity/Non Profit
Country United Kingdom
Start 09/2021 
End 11/2021
 
Title DFTB+ 2020 release 
Description Software release associated with Hourahine et al. (J. Chem. Phys. DOI: 10.1063/1.5143190 included in the 2020 researchfish submission). Computational resources attached to this grant we used in development and testing. 
Type Of Material Computer model/algorithm 
Year Produced 2020 
Provided To Others? Yes  
Impact Software in use iin ~2000 research groups. This is a major release with significant extensions of functionality. 
URL https://github.com/dftbplus/dftbplus/tree/20.1
 
Title Data for: "Correlation between deep-level defects and functional properties of ß-(SnxGa1-x)2O3 on Si photodetectors" 
Description Data associated with research paper. The dataset contains CL hyperspectral imaging data, XRD, I-V curves, photocurrent as a function of time for Tin-gallium-oxide photodetectors. 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
Impact Too early for notable impact. 
URL https://pureportal.strath.ac.uk/en/datasets/data-for-correlation-between-deep-level-defects-and-func...
 
Title Data for: "Determining GaN nanowire polarity and its influence on light emission in the scanning electron microscope" 
Description Electron backscatter diffraction (EBSD) patterns and backscatter electron (BSE) intensity image derived from EBSD patterns, BSE and secondary electron (SE) images and cathodoluminescence (CL) hyperspectral images 
Type Of Material Database/Collection of data 
Year Produced 2019 
Provided To Others? Yes  
Impact Supporting data for paper in Nano Letters (included in submission), will be used in future presentations (acknowledging this award). 
URL https://pureportal.strath.ac.uk/en/datasets/b152a121-3495-4235-b9cd-985bf1355cd8
 
Title Data for: "High Figure-of-Merit Gallium Oxide UV Photodetector on Silicon by Molecular Beam Epitaxy: A Path toward Monolithic Integration" 
Description This data is for room temperature cathodoluminescence (CL) of beta gallium oxide thin films grown on Si (111) substrate by MBE. Room Temperature (RT) CL is performed in a JEOL JXA-8530F field emission EPMA with an electron beam energy of 4 kV and a beam current of 40 nA. The CL spectra were acquired by a spectrometer with a focal length of 163 mm with 300 grooves mm-1 grating blazed at 500 nm, a 105 µm entrance slit (fiber size), and a 1024-element charge-coupled device. 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
Impact Too early for impact from this data set. 
URL https://pureportal.strath.ac.uk/en/datasets/data-for-high-figureofmerit-gallium-oxide-uv-photodetect...
 
Title Data for: "High-degeneracy Potts coarsening" 
Description I examine the fate of a kinetic Potts ferromagnet with a high ground-state degeneracy that undergoes a deep quench to zero-temperature. I consider single spin-flip dynamics on triangular lattices of linear dimension 8 = L = 128 and set the number of spin states q equal to the number of lattice sites L×L. The ground state is the most abundant final state, and is reached with probability ˜ 0.71. Three-hexagon states occur with probability ˜ 0.26, and hexagonal tessellations with more than three clusters form with probabilities of O(10-3 ) or less. Spanning stripe states-where the domain walls run along one of the three lattice directions-appear with probability ˜ 0.03. "Blinker" configurations, which contain perpetually flippable spins, also emerge, but with a probability that is vanishingly small with the system size. Further details on the data can be found in the readme file provided. 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
Impact No significant impact so far. 
URL https://pureportal.strath.ac.uk/en/datasets/a79b861a-6b9b-4508-b44e-e4b6a00a3fb1
 
Title Data for: "Improving EBSD precision by orientation refinement with full pattern matching" 
Description This dataset contains the experimental data used to generate the figures in the journal article, "Improving EBSD precision by orientation refinement with full pattern matching". The data includes the original electron channeling contrast images and the raw electron backscatter diffraction patterns, all saved as tiff files. These were the basis for analysis presented in this paper. The electron channelling contrast imaging data was recorded using a Zeiss Auriga FIB SEM using the Zeiss supplied quadrant diode backscattered electron detector which is inserted beneath the pole piece. The sample was tilted by around 20° away from the horizontal to increase the intensity of the backscattered signal, as the number of backscattered electrons increases as you increase the tilt of the sample. Single WC grains were rotated by 10° between image acquisitions, for 180° per grain. ECCI is a SEM based diffraction technique which can be used to detect small orientation changes or changes in lattice constant in a material. ECCI micrographs are produced when a sample is placed so that a plane or planes are at, or close to, the Bragg angle with respect to the incident electron beam. Any deviation in crystallographic orientation or in lattice constant due to local strain will produce a variation in contrast in the resultant ECCI micrograph. Extremely small changes in orientation and strain are detectable, revealing subgrains and extended defects such as dislocations and stacking faults. We can also investigate the contrast exhibited by a defect for different diffraction conditions, ultimately identifying the nature of the defect. EBSD data in this study was collected in a Zeiss Auriga FIB SEM outfitted with an Oxford NordlysNano system. EBSD maps were acquired at 20 or 30 kV accelerating voltage with a 10 nA beam and the sample tilted at 70° from the horizontal. In EBSD the sample is tilted at around 70° to the normal of the incident electron beam. The impinging electrons are scattered inelastically through high angles forming a diverging source of electrons which can be diffracted. The resultant electron backscatter diffraction pattern (EBSP) consists of a large number of overlapping bands, known as Kikuchi bands, which are closely related to a 2-D projection of the crystal structure. Acquiring EBSPs over a grid of points on a sample allows mapping of the sample's microstructure. Abstract of the paper: We present a comparison of the precision of different approaches for orientation imaging using electron backscatter diffraction (EBSD) in the scanning electron microscope. We have used EBSD to image the internal structure of WC grains, which contain features due to dislocations and subgrains.We compare the conventional, Hough-transform based orientation results from the EBSD system software with results of a high-precision orientation refinement using simulated pattern matching at the full available detector resolution of 640 × 480 pixels. Electron channelling contrast imaging (ECCI) is used to verify the correspondence of qualitative ECCI features with the quantitative orientation data from pattern matching. For the investigated sample, this leads to an estimated pattern matching sensitivity of about 0.5 mrad (0.03°) and a spatial feature resolution of about 100 nm. In order to investigate the alternative approach of postprocessing noisy orientation data, we analyse the effects of two different types of orientation filters. Using reference features in the high-precision pattern matching results for comparison,we find that denoising of orientation data can reduce the spatial resolution, and can lead to the creation of orientation artefacts for crystallographic features near the spatial and orientational resolution limits of EBSD 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
Impact Data from research paper associated with this award. 
URL https://pureportal.strath.ac.uk/en/datasets/0757bccc-5df8-43ac-92a6-2e758d8952a5
 
Title Data for: "Influence of an InGaN superlattice pre-layer on the performance of semi-polar (11-22) green LEDs grown on silicon" 
Description This dataset provides the cathodoluminescence (CL) data used to generate figure 5 in the paper entitled "Influence of an InGaN superlattice pre-layer on the performance of semi-polar (11-22) green LEDs grown on silicon". The cathodoluminescence (CL) data discussed and presented in the paper was recorded using a variable pressure field emission scanning electron microscope (SEM, FEI Quanta 250) which is equipped with a custom-built CL hyperspectral imaging system. The CL system collects the emitted light at an angle of 45° with respect to the incident electron beam using a Cassegrain reflecting objective. The light is then dispersed using a 125 mm focal length spectrograph (Oriel MS125) and detected using an electron-multiplying charge-coupled device (Andor Newton). As the electron beam scans across the sample surface, a whole CL spectrum is recorded per pixel building up the 3D hyperspectral data set. 2D CL images can then be extracted from the hyperspectral data set, such as peak energy, intensity or half width. The room temperature CL measurements were acquired with a beam voltage of 5 kV. Abstract of the paper: It is well-known that it is crucial to insert either a single InGaN underlayer or an InGaN superlattice (SLS) structure (both with low InN content) as a pre-layer prior to the growth of InGaN/GaN multiple quantum wells (MQWs) served as an active region for a light-emitting diode (LED). So far, this growth scheme has achieved a great success in the growth of III-nitride LEDs on c-plane substrates, but has not yet been applied in the growth of any other orientated III-nitride LEDs. In this paper, we have applied this growth scheme in the growth of semi-polar (11-22) green LEDs, and have investigated the impact of the SLS pre-layer on the optical performance of semi-polar (11-22) green LEDs grown on patterned (113) silicon substrates. Our results demonstrate that the semi-polar LEDs with the SLS pre-layer exhibit an improvement in both internal quantum efficiency and light output, which is similar to their c-plane counterparts. However, the performance improvement is not so significant as in the c-plane case. This is because the SLS pre-layer also introduces extra misfit dislocations for the semi-polar, but not the c-plane case, which act as non-radiative recombination centres. 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
Impact Data set for paper associated with this project. 
URL https://pureportal.strath.ac.uk/en/datasets/a30b848c-c99e-43b6-89e8-0c5b939b64fc
 
Title Data for: "Influence of micro-patterning of the growth template on defect reduction and optical properties of non-polar (11-20) GaN" 
Description This dataset provides the experimental data used to generate the figures in the paper entitled "Influence of micro-patterning of the growth template on defect reduction and optical properties of non-polar (11-20) GaN". The cathodoluminescence (CL) data discussed and presented in the paper was recorded using a variable pressure field emission scanning electron microscope (SEM, FEI Quanta 250) which is equipped with a custom-built CL hyperspectral imaging system. The CL system collects the emitted light at an angle of 45° with respect to the incident electron beam using a Cassegrain reflecting objective. The light is then dispersed using a 125 mm focal length spectrograph (Oriel MS125) and detected using an electron-multiplying charge-coupled device (Andor Newton). As the electron beam scans across the sample surface, a whole CL spectrum is recorded per pixel building up the 3D hyperspectral data set. 2D CL images can then be extracted from the hyperspectral data set, such as peak energy, intensity or half width. The room temperature CL measurements were acquired with a beam voltage of 5 kV. For the variable temperature photoluminescence (PL) measurements the samples were placed inside a liquid helium flow cryostat. A monochromator (SPEX1704) with a 1 m focal length and liquid nitrogen-cooled CCD were used for the detection of the emitted luminescence, which was excited by the 325 nm line of a He-Cd laser. Abstract of the paper: We investigate the influence of different types of template micro-patterning on defect reduction and optical properties of non-polar GaN using detailed luminescence studies. Non-polar (11-20) (or a-plane) GaN exhibits a range of different extended defects compared with its more commonly used c-plane counterpart. In order to reduce the number of defects and investigate their impact on luminescence uniformity, non-polar GaN was overgrown on four different GaN microstructures. The micro-patterned structures consist of a regular microrod array; a microrod array where the -c-side of the microrods has been etched to suppress defect generation; etched periodic stripes and finally a subsequent combination of etched stripes and etched microrods (double overgrowth). Overall the presence of extended defects, namely threading dislocations and stacking faults (SFs) is greatly reduced for the two samples containing stripes compared with the two microrod samples. This is evidenced by more uniform emission and reduction in dark regions of non-radiative recombination in room temperature cathodoluminescence imaging as well as a reduction of the SF emission line in low temperature photoluminescence. The observed energy shifts of the GaN near band edge emission are related to anisotropic strain relaxation occurring during the overgrowth on these microstructures. A combination of stripes and microrods is a promising approach for defect reduction and emission uniformity in non-polar GaN for applications in light-emitting devices as well as power electronics. 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
Impact Data set for paper associated with project. 
URL https://pureportal.strath.ac.uk/en/datasets/feded221-778b-4eae-8cf3-5322a3aec763
 
Title Data for: "Luminescence behaviour of semi-polar (10-11) InGaN/GaN 'bow-tie' structures on patterned Si substrates" 
Description This dataset provides the experimental data used to generate the figures in the paper entitled "Luminescence behaviour of semi-polar (10-11) InGaN/GaN 'bow-tie' structures on patterned Si substrates". The room temperature cathodoluminescence (CL) data was recorded using a variable pressure field emission scanning electron microscope (SEM, FEI Quanta 250) which is equipped with a custom-built CL hyperspectral imaging system. The CL system collects the emitted light at an angle of 45° with respect to the incident electron beam using a Cassegrain reflecting objective. The light is then dispersed using a 125 mm focal length spectrograph (Oriel MS125) and detected using an electron-multiplying charge-coupled device (Andor Newton). Low temperature CL was performed in a field emission gun SEM (Zeiss LEO DSM 982) equipped with custom-built liquid helium flow cryostage (CryoVac). The light was collected using a UV-enhanced glass fibre placed in close contact with the sample, dispersed with a 90 cm focal length monochromator (SPEX 1702) and detected using a liquid nitrogen-cooled, UV-optimised CCD. As the electron beam scans across the sample surface, a whole CL spectrum is recorded per pixel building up the 3D hyperspectral data set. 2D CL images can then be extracted from the hyperspectral data set, such as peak energy, intensity or half width. The room temperature and low temperature (12 K) measurements were acquired with a beam voltage of 5 kV. Electron channelling contrast imaging is a non-destructive, diffraction technique performed in the SEM. ECC images are generally constructed by measuring the intensity of the backscattered electrons (BSEs) as the electron beam scans across the surface of a suitably-orientated sample. Any changes in crystallographic orientation and local strain can be monitored by the variation in the BSE intensity causing a change in contrast in an ECC image. This allows the imaging of low-angle tilt and rotation boundaries, atomic steps and extended defects (e.g. TDs). ECCI is carried out in a forward scattering geometry in a field emission SEM (FEI Sirion 200), equipped with an electron-sensitive diode and a custom-built signal amplifier. Electron backscatter diffraction (EBSD) measurements were performed using a Nordlys EBSD detector from Oxford Instruments attached to an FEI Quanta 250 variable pressure field emission SEM. The EBSD data was acquired at 20 kV and at a sample tilt of 70° with respect to the normal of the incident electron beam. For the analysis of the EBSD data, the electron backscatter pattern (EBSP) from each pixel was compared to simulated dynamical Kikuchi patterns using a Bloch wave approach. Abstract of the paper: In this work, we report on the innovative growth of semi-polar 'bow-tie'-shaped GaN structures containing InGaN/GaN multiple quantum wells (MQWs), and on their structural and luminescence characterisation. We investigate the impact of growth on patterned (113) Si substrates which results in the bow-tie cross-section with upper surfaces having the (10-11) orientation. Room temperature cathodoluminescence (CL) hyperspectral imaging reveals two types of extended defects: black spots appearing in intensity images of the GaN near band edge emission; and dark lines running parallel in the direction of the Si stripes in MQW intensity images. Electron channelling contrast imaging (ECCI) identifies the black spots as threading dislocations (TDs) propagating to the inclined (10-11) surfaces. Line defects in ECCI, propagating in the [1-210] direction parallel to the Si stripes, are attributed to misfit dislocations (MDs) introduced by glide in the basal (0001) planes at the interfaces of the MQW structure. Identification of these line defects as MDs within the MQWs is only possible because they are revealed as dark lines in the MQW CL intensity images, but not in the GaN intensity images. Low temperature CL spectra exhibit additional emission lines at energies below the GaN bound exciton emission line. These emission lines only appear at the edge or the centre of the structures where two (0001) growth fronts meet and coalesce (join of the bow-tie). They are most likely related to basal-plane or prismatic stacking faults or partial dislocations at the GaN/Si interface and the coalescence region. 
Type Of Material Database/Collection of data 
Year Produced 2019 
Provided To Others? Yes  
Impact Data set associated with paper, contents have been presented at several international meetings. 
URL https://pureportal.strath.ac.uk/en/datasets/c71c237d-a544-4bf5-b7d3-1432ea22608e
 
Title Data for: "Metrology of crystal defects through intensity variations in secondary electrons from the diffraction of primary electrons in a scanning electron microscope" 
Description ECCI micrographs shown in Figs. 2 to 5 were acquired using the FEI (now Thermo Fisher) Quanta 250 FEG-SEM. Typically, electron beam energy of 30 keV, beam currents between 2 - 4 nA, working distances between 10 - 16 mm and gas pressures between 0.5 - 1 mbar were used to perform ECCI in a low vacuum mode. ECCI micrographs shown in Figs. 6 and 7 were acquired using the Zeiss Auriga 60 with the Gemini column in high vacuum at 2 keV and 20 keV respectively. In order to achieve an acceptable signal to noise, the ECCI micrographs obtained using the gaseous secondary electron detector was acquired with a resolution of 2048 × 1768 pixels with a 100 µs dwell time and a detector bias set between +230 V to +250 V. An Oxford instruments forescatter detector was used to acquire the images shown in Figs. 2b, 3b, 5c, 5d and an Oxford Instruments Nordlys electron backscatter diffraction camera was used to acquire the electron backscatter diffraction pattern shown in Fig. 3d. An FEI quadrant backscattered electron detector was used to collect the image shown in Fig. 2c whereas Figs. 3a, 3c, and Fig. 4 were captured using the off-axis large field of view detector and on-axis gaseous secondary electron detector respectively. We used an Everhart-Thornley detector to acquire the ECCI micrographs displayed in Figs. 5a and 5b. 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
Impact Supporting data set for associated paper. 
URL https://pureportal.strath.ac.uk/en/datasets/d40c3955-5ca9-4464-9d7f-a8a1db31051a
 
Title Data for: "Origin of Red Emission in ß-Ga2O3 Analysed by Cathodoluminescence and Photoluminescence Spectroscopy" 
Description This data is for room temperature cathodoluminescence and temperature dependent photoluminescence of Fe, Sn, Si and un doped beta gallium oxide crystals. Room temperature CL is performed in an FEI Quanta 250 Schottky variable pressure FEG-SEM using a custom-built CL system. A Cassegrain reflecting objective is used to collect the emitted light, which is dispersed with a 1/8 m focal length spectrometer (Oriel MS125) onto a 1600-channel electron-multiplying charge-coupled device (Andor Newton). The CL is excited by an electron beam energy of 5 keV. The CL spectra were obtained using a 400 lines/mm grating and a dwell time of 10 seconds. The CL spectra for the Fe doped sample were recorded in low vacuum mode since the sample was charging under the electron beam. Low-temperature PL spectroscopy is performed using a custom-built PL system with a closed cycle He cryostat and a 355nm CW laser (Cobolt Zouk) with a maximum power of 20mW as the excitation source. The light emitted from the sample was collected into a 0.67m spectrometer (McPherson 207) with a diffraction grating with 300 lines/mm and dispersed over a cooled CCD (Andor Technology) where each spectrum is collected for 10 seconds. 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
URL https://pureportal.strath.ac.uk/en/datasets/2a356523-baa7-4776-80ef-a9e6519af352
 
Title Data for: "Scanning electron microscopy as a flexible technique for investigating the properties of UV-emitting nitride semiconductor thin films" 
Description Scanning electron microscope images, electron channelling contrast micrographs, Electron backscatter diffraction data and cathodoluminescence data 
Type Of Material Database/Collection of data 
Year Produced 2019 
Provided To Others? Yes  
Impact Led to invited talks for the data-set (and associated paper) lead author. 
URL https://pureportal.strath.ac.uk/en/datasets/b5238863-a088-4f30-8b13-2625260eb73a
 
Title Data for: "Subgrain structure and dislocations in WC-Co hard metals revealed by electron channelling contrast imaging" 
Description This dataset contains the experimental data used to generate the figures in the journal article, "Subgrain structure and dislocations in WC-Co hard metals revealed by electron channelling contrast imaging". The electron channelling contrast imaging data was recorded using a Zeiss Auriga FIB SEM using the Zeiss supplied quadrant diode backscattered electron detector which is inserted beneath the pole piece. The sample was tilted by around 20° away from the horizontal to increase the intensity of the backscattered signal, as the number of backscattered electrons increases as you increase the tilt of the sample. A series of images of single WC grains with the sample at different tilts or for different rotations were then acquired. In the case of the tilt series, ECCI images were acquired for tilts between 17° and 22° with the sample tilt changed by 0.2° between image acquisitions. For the rotation series, the sample was tilted at 20° and rotated 10° between image acquisitions, with the sample rotated by 180? for each grain. ECCI is a SEM based diffraction technique which can be used to detect small orientation changes or changes in lattice constant in a material. ECCI micrographs may be produced when a sample is placed so that a plane or planes are at, or close to, the Bragg angle with respect to the incident electron beam. Any deviation in crystallographic orientation or in lattice constant due to local strain will produce a variation in contrast in the resultant ECCI micrograph. Extremely small changes in orientation and strain are detectable, revealing subgrains and extended defects such as dislocations and stacking faults. We can also investigate the contrast exhibited by a defect for different diffraction conditions, ultimately identifying the nature of the defect. EBSD data in this study was collected in a Zeiss Auriga FIB SEM outfitted with an Oxford NordlysNano system. EBSD maps were acquired at 20 or 30 kV accelerating voltage with a 10 nA beam and the sample tilted at 70° from the horizontal. In EBSD the sample is tilted at around 70? to the normal of the incident electron beam. The impinging electrons are scattered inelastically through high angles forming a diverging source of electrons which can be diffracted. The resultant electron backscatter diffraction pattern (EBSP) consists of a large number of overlapping bands, known as Kikuchi bands, which are closely related to a 2-D projection of the crystal structure. Acquiring EBSPs over a grid of points on a sample allows mapping of the sample's microstructure. Abstract of the paper: In this study, electron channelling contrast imaging (ECCI) and electron backscatter diffraction (EBSD) have been used to examine the substructure and dislocations in tungsten carbide (WC) grains in tungsten carbide-cobalt (WC-Co) hardmetals. These complimentary scanning electron microscopy (SEM) diffraction techniques provide quantifiable information of the substructure without the difficulty of transmission electron microscopy (TEM) sample preparation and examination. Subgrain structures in WC grains have rarely been reported previously because of the sample preparation difficulty, but this study has found they can occur frequently and may provide information on grain growth during sintering. ECCI has also shown for the first time complex dislocation networks across large grains, indicating accumulation of stress in as-sintered materials. To identify the defects revealed by ECCI more precisely, WC grains with surface normals [0001],[11 ¯00] and [112 ¯0], were identified using inverse pole figure orientation maps generated from EBSD data. ECC images from these grains reveal defects intersecting the surface and subgrains bound by dislocations. The combination of ECCI and EBSD allows for new insights into dislocation networks in a WC-Co hardmetal sample over a large, in this case 75 µm × 75 µm, field of view. 
Type Of Material Database/Collection of data 
Year Produced 2019 
Provided To Others? Yes  
Impact Reference data which may find re-use in later publications with the National Physical Laboratory. 
URL https://pureportal.strath.ac.uk/en/datasets/c80a3a0c-a718-4941-ac82-8981d21799ce
 
Title dftbplus/dftbplus: Release 20.1 
Description Release 20.1 
Type Of Technology Software 
Year Produced 2020 
Impact Open source software in use in ~2,000 research groups world wide. Resources from this grant were used for testing and development of new features and in supporting the associated open access paper (highlight article for the journal). 
URL https://zenodo.org/record/3956552