This page contains application notes showing how our equipment was applied to solve real-life situations.

 

EDS Application Notes

EBSD Application Notes

 

New EBSD Detector Symmetry: Application Notes

Rapid Characterisation of Steel and Ni

The Symmetry detector is ideal for the routine characterisation of metal samples at speeds up to 3000 pps. Here it is used to characterise a deformed Ni superalloy and a large area across a welded duplex steel.

PDF 8.30MB
High Resolution EBSD Mapping of Martensitic Steel

Martensitic structures are traditionally challenging to measure with EBSD. Here, the sensitivity and pattern detail provided by Symmetry enables exceptional results from a martensitic stainless steel.

PDF 3.10MB
Transmission Kikuchi Diffraction (TKD) of Metals

Successful TKD analyses require an EBSD detector with both high speed and high sensitivity. The suitability of Symmetry for TKD is demonstrated here on both deformed Al alloys and nanocrystalline Ni.

PDF 11.99MB
Symmetry High Sensitivity for Beam sensitive Materials

In this application, Symmetry is used to characterise a challenging biomaterial, shell nacre, and its performance is compared to conventional CCD-based detectors.

PDF 4.11MB
Characterising Complex Rock Samples using Symmetry

An eclogite sample containing 10 phases has been rapidly analysed using integrated EBSD and EDS. The performance of Symmetry enables high pattern resolution and good indexing, even at 250 pps.

PDF 3.77MB
Fast Characterisation of Deformed Quartz Rocks

A relatively simple geological sample, a quartz mylonite, is here characterised in a matter of minutes using Symmetry, collecting data at almost 1000 pps.

PDF 13.15MB
Detailed Study of a Bivalve Shell

An in-depth look at the structures of a mussel shell, characterised using Symmetry. Both calcite and nanostructured aragonite nacre are measured with an unprecedented level of detail and speed.

PDF 7.07MB
The Symmetry Advantage High Angular Resolution at High Speeds

This technical bulletin looks at the effect of collecting high resolution patterns at high speeds on metals: astonishing angular resolution, even at 3000 pps.

PDF 3.22MB

Find out more about Symmetry

 

 

 

EDS Application Notes

Nanometre scale EDS analysis using low-kV FEGSEM and a windowless EDS detector

The combination of X-Max Extreme with GeminiSEM 500 provides a uniquely convenient and powerful imaging and analysis tool for investigating the morphology and chemistry of nano-structures down to less than 10nm. Using the example of ferrocerium nano-particles and GaInAs quantum dots this capability is demonstrated in practice…

PDF 4.86MB
Mapping Semiconductor Devices in the SEM

As semiconductor devices continue to decrease in size to improve performance and take advantage of advances in fabrication techniques, there is a need to analyse both their structure and chemistry at ever increasing resolution. Typically this requires the use of TEM for metrology and failure analysis. Using ultrahigh resolution FEG-SEM, low kV imaging and the new X-Max Extreme EDS detector we demonstrate the ability to retain some of this high resolution analysis in the SEM. This allows for better targeting of resources and increased throughput of analysis.

PDF 4.31MB
Tru-Q – Making Accurate Analysis a Reality for All

Tru-Q is a unique combination of new and existing technologies that make the promise of automatic, real-time element identification and composition determination a reality.

PDF 407KB
Large Area EDS Mapping: Phase distribution in archaeological samples

Detailed surface analysis of samples which are extremely large in size and contain a distribution of object sizes from micro- to nano-scale can pose a challenge when faced with a limited analysis time.

Obtaining elemental maps at low magnifications by conventional analysis at relatively low pixel density can misrepresent the chemical and structural composition. This is particularly true in areas such as archaeology, geology, and materials science where micro- and nano-structure can have important implications, and samples are often of unknown morphology and chemistry. In this application note we describe how AZtecEnergy Large Area Mapping solves these challenges

PDF 7.81MB
Materials Analysis of Flexible Thin Films

Research and development of electronic circuitry mounted on plastic substrates is gathering pace. In order to assess the structural properties of the electronic components, they have to be analysed while on the plastic substrate without compromising their structural integrity. LayerProbe enables the analyst to separate the contributions of the substrate and the structures and enables measurements of the thickness and composition at high resolution and in a non-destructive manner.

PDF 2.38MB
Mineral Liberation Analysis - Large Area Mapping

Geological samples contain large amounts of information much of which may be gathered using an SEM equipped with EDS and EBSD analytical detectors and software. The combined suite of information gathered using both mapping and dedicated mineral analysis software enables a far deeper understanding of the specimen and the processes which have contributed to its formation than the individual methods alone.

PDF 3.04MB
Mineral Liberation Analysis - Mn Nodule Analysis

By using a range of solutions within Oxford Instruments’ AZtec and INCA software suite, detailed qualitative and quantitative information can be gained on the chemistry and mineralogy of geological samples of a wide range of types. INCAMineral and AZtec Energy have been used in the study of a Mn nodule suspected of containing economically viable quantities of valuable metals.

PDF 2.18MB
Biological EDS and Large Area SDD

Until recently, X-Ray Energy Dispersive Spectroscopy (EDS) in biological samples was limited to very basic analysis. Analysis often required higher beam currents than were acceptable: the mapping of small nanostructures could not even be considered due to sample drift and the beam damage that prolonged exposure would cause. The introduction of X-MaxN Very Large Area SDDs is revolutionising biological analysis by maximising count rates even at low accelerating voltages and small spot sizes.

PDF 4.89MB
Biological EDS with Multiple Detectors

The X-MaxN series of large area SDD detectors are revolutionising the EDS analysis of biological samples. With sensor active area up to 150 mm2, and the possibility to combine multiple detectors to make an effective area of up to 600 mm2, counts from samples are maximised even at low kV and small spot sizes. At last, ultra-fast analysis and nano-scale accurate mapping on biological materials are not only possible, but practical too.

PDF 5.26MB
LayerProbe - All Oxide Solar Cell Characterisation

Photovoltaic (PV) cells are an attractive option for generating low carbon renewable energy but traditional designs often include undesirable toxic compounds and must be manufactured under special conditions. The all-oxide approach to photovoltaic cells is thus very attractive as it circumvents many of these issues and offers a potential method of creating a lower cost, more widely used product. AZtec LayerProbe was used to characterise a combinatorial library sample with varying layer thicknesses and compositions in order to determine which combination is most effective.

PDF 1.15MB
AutoPhaseMap

AutoPhaseMap compendium

  • Phase characterisation of an aluminium alloy
  • Phase characterisation of an igneous rock and validation by EBSD
  • Automatic discovery of minor phases
  • Characterisation of nanoscale intermatallic phases
  • Classification of igneous rocks by AZtecEnergy
PDF 22.02MB
Gunshot Residue Analysis in AZtecGSR

This four page note discusses the use of AZtecGSR, a dedicated implementation of the AZtecFeature particle analysis system, for the analysis of a GSR sample.

PDF 3.03MB
Asbestos characterisation in the SEM

The automated analysis of asbestos in the SEM by EDS is a powerful technique that enables the quantity, composition, and morphology of suspected asbestos fibres to be quickly characterised. This application note discusses the use of AZtecFeature to perform the analysis of these challenging samples.

PDF 2.27MB
Particle and feature analysis in the SEM

AZtecFeature is a SEM software solution for particle analysis that offers increased speed, a significantly enhanced user experience and the highest possible accuracy. Here we consider AZtecFeature in the context of engine wear monitoring, geology and air cleanliness and pollution. We discuss how key improvements in AZtec Feature in combination with recent advances in EDS detector hardware make it a compelling proposition for a much wider group of researchers and practitioners in industry and academia.

PDF 7.03MB
Steel analysis using EDS

This technical bulletin describes the use of AZtecSteel to classify steel inclusions, including the data processing and reporting.

PDF 4.72MB
Analysis of Highly Insulating Ceramic Boron Nitride at 1.5 kV using X-Max Extreme

In this study we focus on the unique capability of X-Max Extreme to deliver meaningful analytical data at very low energies which, for insulators such as Boron Nitride ceramics, means that samples can be analysed without coating.

PDF 3.54MB

AutoPhaseMap: Phase Characterisation of an Aluminium Alloy

The AutoPhaseMap module in the Oxford Instruments’ EDS software, AZtecEnergy, automatically finds areas of different characteristic composition from X-ray map data, and determines the distribution, area, constituent elements and composition of each of these areas or phases. This application note examines how this can be used to characterise an aluminium alloy and its inter-metallic phases.

PDF 5.96MB
AutoPhaseMap: Phase Characterisation of an Igneous Rock and Validation by EBSD

This application note examines how the AutoPhaseMap technique can be used to determine and characterise the phases present in an igneous rock.The results are compared to the phase mapping results calculated from an EBSD dataset collected simultaneously with the EDS acquisition, to validate the result of the AutoPhaseMap method.

PDF 6.12MB
AutoPhaseMap: Automatic Discovery of Minor Phases

This application note examines how the AutoPhaseMap technique can uncover previously missed minor phases - even when their constituent elements are not known to be present in advance.

PDF 2.43MB
AutoPhaseMap: Characterisation of Nanoscale Intermetallic Phases

This application note examines how AutoPhaseMapcan be used to investigate the chemistry and distribution of nanoscale intermetallic phases in a Ni-based alloy which are on the scale of 150-1000 nm.

PDF 5.63MB
AutoPhaseMap: Classification of Igneous Rocks

This application note examines how AutoPhaseMap can be used to determine the modal percentages of different minerals in an igneous rock, and from this result classify its type.

PDF 3.41MB
Mineral liberation Analysis - An Overview

Mineral liberation is a critical stage in the production of high quality mineralogical concentrates from their ores. The products(concentrates) must be of a suitable degree of purity for the downstream processes in which they will be used.  This application note gives an overview into the process of mineral liberation analysis in a scanning electron microscope.

PDF 1.45MB

EDS in the TEM Application Notes

AZtecTEM solutions brochure

A 16 page brochure showing why AZtecTEM is the most powerful solution for EDS on the TEM. It comprises software and hardware sections (inc X-Max 100TLE and X-Max TSR).

PDF 4.63MB
Semiconductor analysis in the TEM

Development and testing of semiconductor devices requires extensive knowledge of local structure and elemental composition. With feature sizes of <5 nm, it is often necessary to perform imaging and EDS analysis in a S/TEM.

Once in the TEM, there are still many difficulties to be overcome to acquire accurate elemental maps. Elemental analysis of semiconductors is typically difficult due to strong overlaps of X-ray lines between commonly used elements and low concentrations of dopants. Not only are concentrations of dopants small but their X-ray lines often overlap with other materials used in semiconductor processing. This brief shows how AZtecTEM solves these overlaps to achieve an accurate elemental analysis.

PDF 3.27MB
Simultaneous EDS & EELS in the TEM

In Transmission Electron Microscopy (TEM) there are two ‘go to’ techniques for elemental analysis: Energy Dispersive X-ray Spectroscopy, (EDS), and Electron Energy Loss Spectroscopy, (EELS). Simultaneous acquisition of both signals is a powerful tool for materials analysis...

PDF 4.26MB
EDS for TEM Explained

This 12 page document gives an introduction to EDS applications in the Transmission Electron Microscope (TEM). It covers the theory of the SDD operation and X-ray analysis.

This document is available in bulk free of charge to universities and other institutions giving a course on the subject.

PDF 4.04MB

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EBSD Application Notes

EBSD Characterisation of high-strength lightweight steel

Understanding microstructure is fundamental to producing steels with specific mechanical properties for automotive applications. The integration of EBSD & EDS is a powerful microanalytical solution for monitoring microstructure, which aids the understanding of the relationship between materials processing, microstructure and performance...

PDF 18.29MB
AZtec Reclassify: Discriminating phases in steels

Austenite, ferrite, martensite and bainite are common phases in different steel alloys and the relative proportions of these different phases impact how the steel will behave in different regimes. Distinguishing martensite, bainite and ferrite is a challenge as the crystal structure of these three phases is essentially the same...

PDF 4.83MB
Grain characterisation of a steel wire by EBSD

EBSD is the ideal technique for determining grain size, here we report on the application to a steel wire.

PDF 2.80MB
Addressing pseudo-symmetric mis-indexing

This application note describes an application of AZtec Refined Accuracy in solving pseudosymmetry problems in gamma-TiAl.

PDF 8.19MB
Discriminating compounds with similar crystal structures

This application note illustrates the application of AZtec Synergy-TruPhase solution to accurate identifying critical phases in an alloy during EBSD mapping, even if different phases have very similar crystal structure.  Phase identification of this type is essential in a number of industries, typically where discriminating second phase particles or precipitates is important in understanding materials behaviour.

PDF 1.83MB
Colour Orientation Imaging

Microstructure imaging using Forescatter diodes (FSD) on the EBSD detector helps to highlight regions of interest for further investigation during an EBSD analysis. Traditionally, these images were presented in greyscale, but, by adding colour and mixing images from three diodes, a lot more insights can be gained. This note gives examples.

PDF 5.60MB
Grain Size Characterisation of a Steel Sample

Grain size is an important characteristic used in understanding the development, engineering and potential failure of steels. EBSD is an ideal technique for determining grain size, it offers microstructural characterisation including grain size, grain boundary characterisation and texture quantification. In this example, a galvanized steel wire is examined using AZtecHKL.

PDF 11.86MB
Determining optimum sample thickness for TKD using AZtec

This application note discusses the effect of sample thickness and density on TKD results.

PDF 7.75MB
AZtec Grain Analysis

This application note covers two examples: Grain characterisation through recovery and recrystallization of a folded Al alloy, and Grain size variation through a spot welded steel.

PDF 3.38MB
Integrating EBSD and magnetic susceptibility data

In this note, the authors demonstrate the robustness of using grain shape data obtained on the basis of crystallographic information from EBSD analysis to quantify shape preferred orientation (SPO) and strain in XZ section of deformed quartzite.

PDF 2.25MB
TKD Analysis in AZtec

The TKD technique has been proven to enable spatial resolutions better than 10 nm.  This technique is ideal for routine EBSD characterisation of both nanostructured and highly deformed samples.

This application note describes some of the challenges when using TKD and how application of the AZtec EBSD system overcomes them.

PDF 1.91MB
Strain analysis with AZtec EBSD

Strain in a material’s microstructure has a significant influence on its properties and behaviour. Therefore, characterising microstructural strain is now of increasing interest in engineering materials. The Oxford Instruments’ AZtec EBSD system is ideal for measuring strain on the micro- and nano- scale as it includes extensive functionality to examine and understand the state of strain in materials.

This technical note covers aspects of strain analysis by AZtec: from the importance of the quality of the initial Kikuchi pattern collection, to the application of a wide-ranging, comprehensive set of postacquisition data analysis tools specifically designed to study strain, including third party analysis and strain visualisation tools, such as BLG Crosscourt.

PDF 10.29MB
TruPhase: Solving phases with similar crystal structures but different chemistry

EBSD identifies crystalline phases on the basis of their particular crystallographic characteristics and allows the orientation of the mineral grains within a sample to be determined. However, it has traditionally been a challenge to differentiate between phases with very similar crystal structures.

AZtec TruPhase enables phases with very similar crystal structures to be differentiated by simultaneously collecting EBSD and Energy Dispersive X-ray Spectrometry (EDS) data.

PDF 5.17MB

Large area EBSD mapping of quartz-rich mylonites

Large-area EBSD mapping allows large quantities of information relating to microstructural deformation to be obtained, enabling the history and evolution of a geological sample to be revealed. This study investigates the microstructural response of quartz layers to flow around rigid secondary garnet porphyroclasts during ductile deformation.

PDF 6.76MB
Microcharacterisation of CIGS devices by EBSD and EDS

An important part of the research and development of thin-film solar cells is the characterisation of microstructural and compositional properties of the functional layers. For this purpose, energy-dispersive X-ray spectrometry (EDS) and electron backscatter diffraction (EBSD) represent techniques which exhibit spatial resolutions on the nanometer scale but can be, at the same time, applied on large areas of several square millimeters. The application of EDS and EBSD is demonstrated on this example of thin-film solar cells with Cu(In,Ga)Se2 absorber layers.

PDF 2.50MB
In-Situ EBSD: Tensile and Heating

In-situ experiments in the SEM combined with crystallographic data gathered using EBSD can provide insight into themechanisms operating during deformation and recrystallisation of materials. In order to conduct such experiments suitable EBSD systems are required that can handle infra red radiation emitted from hot samples and in-situ stages that can be inserted intostandard scanning electron microscope chambers.

PDF 9MB
In-Situ EBSD: Bent Al Alloy

This study presents changes in microstructure characterised by EBSD in the tensile region of a bent Al alloy 6063 sheet during in-situ isochronal heating. It has been shown that the bending process generates both a texture and strain gradient across the bent region [1,2]. This study takes this into account in order to follow the recovery and recrystallisation driven by strain gradient.
 

PDF 6.86MB
EBSD Analysis of Industrial Materials

This note illustrates how Broad Beam Ion Milling has been used to produce improved quality of EBSD data from specimen such as aluminium, zirconium, magnesium, titanium alloys and galvanized zinc coatings - which are usually difficult to prepare by mechanical routes only.

PDF 6.22MB
EBSD Analysis of Large Sample Areas

AZtec Large Area Mapping has the capability to collect data with great detail over large sample areas at the fastest speeds. It is then possible to apply single field analysis tools to the large area data sets.  This application note will demonstrate the capability of large area mapping using two data sets to visualise the change in microstructure over the complete sample.

PDF 4.69MB

In-situ heating of an aluminium alloy

This technical note highlights the performance of the NordlysMax2 detector in combination with AZtecHKL software to acquire simultaneous EBSD/EDS data from tungsten heavy alloy (WHA). The highest acquisition speed achieved was 870Hz with a hit rate >98% at 20kV acceleration voltage and 16.6nA probe current.

PDF 449KB
TKD Analysis (aka t-EBSD)

Despite significant technological developments in recent years, the EBSD technique is still limited by the pattern source volume to resolutions in the order of 25-100nm; this is insufficient to measure accurately truly nanostructured materials (with mean grain sizes below 100nm). A new approach to SEM-based diffraction has emerged, namely using an electron transparent sample coupled with conventional EBSD hardware and software. This technique, referred to as transmission EBSD (t-EBSD: Keller and Geiss, 2012) or SEM Transmission Kikuchi Diffraction (TKD) has been proven to enable spatial resolutions better than 10nm, and is ideal for routine EBSD characterisation of both nanostructured and highly deformed samples.

PDF 612KB
Nanomanipulation and EBSD analysis of Au wire

As the trend towards miniaturisation and nanotechnology increases in microelectronic devices, a key growing requirement is the microstructural understanding of materials at the nanoscales to produce reliable products. This application note describes a method of combining Oxford Instrument’s OmniProbe tools and AZtec EBSD system for the manipulation and analysis of a 5μm diameter gold microelectronic wire sample.

PDF 5.43MB
EBSD and Microelectronics

This application note describes the use of AZtecHKL with a Nordlys EBSD detector in the characterisation of Through-Silicon Vias, or TSV.

PDF 1.60MB
Zirconium Hydride Analysis by EBSD

Zirconium alloys are used in nuclear reactors owing to their low capture cross-section for thermal neutrons and good mechanical and corrosion properties. However, they suffer from delayed hydrogen cracking (DHC) due to formation of hydride particles. This study shows how EBSD can be used to characterise hydrides in terms of their orientation relationship with the matrix and internal structure and local misorientation.

PDF 570KB
EBSD and EDS analysis of high entropy alloys

A high entropy alloy has been developed from an equiatomic AlCoCrCuFeNi alloy. Due to its promising properties, such as high corrosion and oxidation resistance and high thermal stability, it is a candidate for various applications at elevated temperature as, e.g., furnace parts, tools and moulds. The exploration of new metallic systems for high temperature applications is an important challenge in today’s materials science.

However, an increase of the strength of this alloy is desirable and requires further optimization. In order to improve these mechanical properties, knowledge of the microstructure is necessary. Therefore, Al8Co17Cr17Cu8Fe17Ni33 high entropy alloy has been studied by means of energy-dispersive X-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD).

PDF 4.02MB
EBSD Sample Preparation

Specimen preparation for EBSD is critical, because the diffracted electrons escape from within only a few tens of nanometres of the specimen surface. However, sample preparation requirements can typically be achieved following some simple recipes. Some broad guidelines are given here.

PDF 6.03MB
EBSD Analysis of a Crept Nickel Alloy

Microanalysis is a powerful tool in understanding potential failure mechanisms and potential life time of many materials. In this example, the microstructure and damage distribution following creep deformation of a nickel superalloy is studied using electron
backscatter diffraction (EBSD) and energy dispersive spectrometry (EDS).

PDF 4.22MB
Orientation Imaging

The Nordlys EBSD detector has the capability to be fitted with up to six forescattered detectors.This application note discusses their application to orientation imaging...

PDF 678KB

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