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NanoMEGAS Precession Electron Diffraction
Precession Enhanced Electron Diffraction application
The beam Precession in Transmission Electron Microscopes (TEMs) is a well-known technique to enhance dramatically the quality of the electron diffraction patterns, mitigating dynamical effect, increasing dps resolution, enhance bending and thickness effect, etc
Based on Precession Electron Diffraction (PED), NanoMEGAS offers since 2004 several automated and robust unique applications. A hardware (DigiSTAR P2010) to control specifically the coils of any TEM, is a scan and precession generator simultaneously, that is used either for static acquisition of ED, or scanning ED, suitable also for precession enhanced 4D-STEM (named 4D-SPED).
Additionally, NanoMEGAS offers acquisition platforms for static or scanning data collection,
together with dedicated software depending on the user application(s) preference.
Thus, full packages of the following applications is available:
- Orientation & Phase mapping
- Strain Mapping
- Precession enhanced 3D-ED for crystal structure determination
- Electron Pair Distribution Function (ePDF) for amorphous materials characterisation
- Electron Pair Distribution Function (ePDF) mapping
- Electric Field mapping
- Enhanced EELS and EDX Spectroscopy
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DigiSTAR P2010: Scan and Precession generator
The first commercially available precession and scan control globally, available for several applications and ideal for precession enhanced 4D-STEM application, as several detectors can be triggered, and data can be automatically saved in a ready-to-analyzed format.
P2010 has been completely redesigned from 1st principles resulting in low distortion lower emissions product with full NRTL certification. Additional external synchronisation outputs have been added for hardware synchronising with on column accessories such as cameras and detectors. The standard installation now supports a distance of 10 m from the column with extension options available for remote installations up to 30 m. The new Digistar comes complete with 14 core IE9 processors and 32 GB of RAM with options of upgrading to 128 GB of RAM.
DigiSTAR P2010-Features
- Compatible with any TEM 120-200-300 Kv (LaB6 /W- FEG)
- Galvanic Isolation system (GIS) via optical fibre for TEM connection
- Retrofit between multiple TEMs in same lab
- High precession frequency >1kHz (depending on TEM)
- High Scanning speed >20kHz(depending on TEM)
- Precession semi-angle variable from 0- 85 mrad(TEM dependent), spot distortion correction-compensation at high angles ( > 15 mrad
- Simultaneous Scanning and Precession control
- Compatible with several high-end detectors (please ask)
- Dedicated straightforward automated software to control experimental settings
- Suitable for 4D-STEM and 4D-SPED acquisition
ASTAR: Orientation and Phase mapping
Automated orientation and phase mapping analysis of a variety of materials (metals, semiconductors, oxides etc.) by TEM using 4D-SPED technique consists of a successful application based on PED, called ASTAR. The major benefit of the technique is the high spatial resolution that can be down to 1-3 nm resolution (in case of FEG-TEM). Beam Precession is essential to improve data quality, in terms of dynamical effect reduction, and diffraction patterns increased resolution improving significantly the results reliability due to the present of higher order reflection. This application allows the user to further analyse their samples in nm scale, by Virtual Dark Field images, Texture analysis, Grain boundaries, Grain size distribution, etc
ASTAR-Features
- Orientation and Phase mapping of several kind of materials (alloys, metals, nanoparticles, nanowires, semiconductors, ceramics, batteries, etc)1
- Orientation (and phase) color maps that each color correspond to certain accurate crystal orientation (and phase) according to the crystal inverse pole figure colour map.
- Spatial resolution down to 1-2nm (TEM & sample depending)
- Precession: Mitigates dynamical effect (disappears possible Kikuchi lines) and enhance the reliability of the orientation and phase map, as higher order reflections are recorded.
TopSPIN strain: Strain and Deformation analysis
The 4D-SPED acquisition method can also be applied to obtain strain mapping analysis (TopSPIN strain) of semiconductor materials at 1-4 nm resolution (sensitivity 0.02%), based on comparison of PED- patterns of strained areas with a reference (non-strained) area. The use of a precessing beam is essential for observing diffraction spots further away from the central spot, enhancing the strain sensitivity detection, and furthermore, improving any sample bending or thickness effect. Strain mapping analysis in TEM by 4D-SPED technique is a straightforward method that can be applied at any TEM and provides rapid and accurate data (same order of magnitude as dark field holography) without any requirement to index diffraction patterns, is critical to monitor the designed and unintended strain distributions.
TopSPIN strain-Features
- Strain analysis software for semiconductor materials and single crystal uniformly oriented systems.
- Strain sensitivity down to 0.1-0.01%
- Spatial resolution down to 1-5nm (TEM & sample depending)
- Precession: Facilitates the zone axis orientation of the sample, reduces the sensitivity of the sample thickness and bending effect, increase the number of higher order reflections, reduces dynamical scattering.
ADT-3D: PED tomography (Precession 3D-ED)
PED was firstly applied in electron crystallography, which in combination with 3D diffraction tomography (or 3D-ED, MicroED) in TEM, has become a critical method for structure determination of various nanocrystals, from minerals and alloys to complex zeolites, MOFs, organic compounds and proteins. In the conventional PED tomography method, a series of ED patterns are collected in a TEM every 1degree of tilting around the goniometer axis. Acquired data are automatically processed by specific software (ADT-3D). Specifically, the diffraction patterns are merged towards the reciprocal space 3D reconstruction, cell parameters determination, indexing and intensities measurement used for ab initio crystal structure determination .
ADT-3D-Features
- Ab-initio structure determination of (any nanostructure) metals, ceramics, polymers, semiconductors, pharmaceuticals, organics, proteins etc
- Cell parameters determination
- Symmetry determination for nanocrystals (space and point group)
- Merging several ED data sets
- Reflections integrations by Precession
- Increased resolution in ED patterns through Precession
- Analysis of twin crystal datasets
- Diffuse scattering for further disorder modelling
ePDF basic: Amorphous Materials Characterisation
Precession electron diffraction in TEM is reported to provide high quality data for analysis of amorphous or nanocrystalline materials. Typical total scattering patterns are acquired in TEM in a few seconds, a speed only matched by synchrotron radiation (lab X-ray acquisition is a much more time-consuming approach for such materials (2-20 hours). The total scattering data are processed by a specific software (ePDF) using the well-known Pair Distribution Function method. Amorphous and/or nanocrystalline materials can not only be identified but furthermore can be characterised through the interatomic distances from the PDF diagram.
ePDF basic-Features
- ePDF calculation using PED data
- Interatomic distances identification
- Simulations of ePDF from know crystal structures
- Pearson Correlation
- Pattern summation (new feature)
- Automatic beam stopper determination
- Automated diffraction centre determination and position adjustment
- Automatic calculation of peak positions for any calculated ePDF from experimental data
- Overlay of bond distances or simulated PDFs calculated using any CIF file on the experimental ePDF
- Normalisation of ePDF during overlay
ePDF advanced: Amorphous Materials Mapping
The latest (introduced spring 2025) software expands the basic ePDF version to analyse 4D-SPED data, obtaining ePDF maps, which is particularly useful for studying amorphous, nanocrystalline, and disordered systems, with applications in semiconductor materials, amorphous glass, amorphous solid dispersions and polymers. The ePDF is automatically computed for every pixel/step of the electron diffraction data series. The computed ePDFs are used to determine the Pearson correlation function, enabling a rapid assessment of similarities and differences across the scanned area. Additionally, peak positions, widths, and heights of the ePDF profiles can be plotted as a function of the x-y position in the map to identify structural variations.
ePDF mapping-Features ( additional to ePDF basic)
- VBF/VDF map generation for a quick overview of structural variations in scanned 4DTSEM data
- Selection of specific areas for further ePDF processing
- Automated masking to remove unwanted spots in diffraction patterns
- Mapping of peak position, width, or height in the experimental ePDF
- Pearson Correlation map of experimental ePDF
- Relative to any reference point in the experimental or simulated PDF
- Can compare with externally generated PDFs
eEF mapping: Electric Field Studies
Detailed characterisation of local Electric Fields and built-in potentials in functional materials is NanoMEGAS’ recent application, combining 4D-SPED acquisition together with dedicated data processing software. During scanning over the sample, the transmitted beam is deflected by the local electric field (Coulomb force). The strength and direction of the local electric field translates into the shift of the intensity distribution in the transmitted central electron beam. Beam Precession is essential to get rid of dynamical effects which prevent accurate determination of the COM (Centre of Mass) and obtain ED patterns with less noise leading to enhanced results [5]. Electric field calculations are of high interest to study properties of many materials and devices, e.g. (P-N junctions, quantum wells, semiconductors, batteries, nanowires, etc)
eElectric Field Mapping-Features
- Apparent electric field (MV/cm) and apparent potential (V) calculation
- Centre of mass (COM) and template matching (TM) codes for the calculation of beam deflection and electric field.
- No need for pixelated detector
- Increased sensitivity compared to other methods, as there is an average on incident beam reduction
- Spatial resolution down to 1-2nm (TEM & sample depending)
- Precession: Facilitates the zone axis orientation of the sample, minimise dynamical contrast, uniformise the transmitted beam and reduce the thickness variation and sample bending effect.
A range of side entry camera mounts which optimise the signal quality from a stingray camera. This mechanism features faster decay phosphor, optimised optical coupling, special lens and reduced background light contamination. Additionally, the camera is mounted perpendicular to the image plane resulting in distortion free diffraction images. These are available for side entry ports (35mm) on most columns.
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Strain Measurement
Measurement of strain with high spatial resolution and high precision in semiconductor devices is critical to monitor the designed and unintended strain distributions. Use of spot diffraction patterns with nanobeam illumination gives higher spatial resolution than other TEM techniques.
Structure of Intriguing Meso-Microporous Zeolites
Zeolites are crystals that are mainly created from aluminium and silicate. They have small pores which make them interesting for the field of energy and environmental technology due to their potential use as adsorbers, ion exchangers or catalysts.
Architecture of Hybrid Nanocrystalline Microporous Materials
The synthesis of aluminosilicate hybrids with organic groups fused within a crystalline framework is a daunting mission which has eluded many workers. Hybrids add variable chemical modification to the repertoire of zeolites, which are well established as heterogeneous catalysts, ion exchangers, and molecular sieves with many different pore architectures.
From Clean Energy Cars to Structure of Metal-Organic Framework Materials (MOFs)
Fossil fuels are not renewable, which means that if the world uses them uncontrollably, fuel will be limited in the future. Hydrogen is an attractive energy carrier which could replace petroleum. However, hydrogen storage is a difficult problem which still has to be solved.
Inside the Structure of Dye-Sensitised Solar Cells
Dye-sensitised solar cells (DSSCs) belong to the family of thin film solar cells and are an attractive and considerably cheaper way of producing electricity. DSSCs are designed like a traditional alkaline battery and do not require tricky manufacturing process.
Towards Alternative Energy Sources: Structure of Thermoelectric Nanomaterials
Solar cells operating at 20% efficiency and covering 0.1% of the Earth's land area would be sufficient to supply the worldwide yearly energy requirement. The Sun as an energy source can also be used by thermoelectric (TE) modules which directly convert solar heat into energy.
Shed Light to Magma Genesis & Seismicity
The processes that give rise to arc magma at convergent plate margins have long been a subject of scientific research and debate. H2O-transfer from the subducted slab to the overlying mantle wedge has been largely recognised as one of the major processes driving rheological modifications of the upper mantle, affecting its petrological variablilty and promoting magma genesis.
Charoite: The Enigmatic Structure of "Unnaturally Beautiful" Gemstone
Charoite is a rare mineral first described in 1978 and named after the chara River. Charoite is translucent lavender to purple in colour with a pearly lustre. Charoite is strictly massive in nature, and fractures are conchoidal. It has an unusual swirling, fibrous appearance, sometimes chatoyant, and that along with its intense colour, can lead many to believe at first that it is synthetic or enhanced artificially.
Structure of New Sarrabusite Mineral
The new mineral Sarrabusite Pb5CuCl4(SeO3)4 has been discovered in Baccu Locci in southeastern Sardinia, Italy. This mineral was discovered in the late 90's and was tentatively assigned as Pb5CuCl4(SeO3)4OH) based on EDX. However, owing to the exceeding small dimensions, no structural study could be preformed using conventional X-ray diffraction and the nature of this possibly new species remained unknown for more than a decade.
Structure of Embedded Nanodomains in Intermetallics
Ni-Te is an intermetallic compound with possible applications in thermoelectric generators (TEGs) that convert heat into electrical power by exploiting a temperature gradient. The system is a two-solid phase mixture where nanodomains of modulated (layered) unknown phase were found inside the NiTe matrix.
Structure of Pigment Yellow for the Car Industry
Some years ago, the automotive industry turned their interest from solvent-based to water-based coatings. This led to the requirement of novel water-dispersible pigments. Greenish-yellow shades appeared to be one of the most problematic, because all existing greenish-yellow pigments were either not dispersible in water or had an insuffienct weather fastness, i.e. they faded out after a few years.
Structure of Organic (CNBA) Molecules
The photo-optical properties of 9,9'-bianthracene-10-carbonitrile (CNBA) in solution are related to the angle between the two anthracene moieties. The 9,9'-bianthryl and its analogues are well-known systems whole excited state behavious and dynamical processes have been studied extensively in a range of conventional solvents.
Bio-Mineralisation Process in Sea Environment
Among the siliceous sponges, the spiculogenesis in the demosponge is best understood. It was suspected that the intial stages of spicule formation proceed intracellularly. Because the synthesis of the spicules is a rapid process, the earliest stages of spicule formation can be studied under in vitro conditions in the cell culture system, the primmorphs.
What is Stacking in Our Pipes: The Structure of Vaterite
Vaterite, one of the common natural CaCO3 polymorphs, plays a pivotal role in weathering and biomineralisation processes. Vaterite is important for the problems of scales in pipes, biomineralisation of mollusks and pearls. Differently from calcite and aragonite, vaterite can be found only in the form of nanosized crystals, not suitable for structure determination by X-ray diffraction.
Design Materials with Specific Applications
Titanium alloys are metals which contain a mixture of titanium and other chemical elements. Such alloys have very high tensile strength and durability (even at extreme temperatures). They are light weight, have extraordinary corrosion resistance and the ability to withstand extreme temperatures. However, the high cost of both raw materials and processing have limited so far their use in certain applications.
Better Steels with Improved Properties
Steel is an alloy made by combining principally iron and carbon; moreover other alloying elements are used to improve mechanical characteristics , such as manganese, or vanadium. The resulting steels are commonly known as High Strength Low Alloy Steels (HSLA). Carbon and other elements act as a hardening agent, preventing dislocations in the iron atom crystal lattice from sliding past one another.
Challenging Materials for Challenging Applications
Synthetic Sapphire is a single crystal form of corundum, Al2O3, also known as alpha-alumina, alumina, and single crystal Al2O3. Synthetic sapphire is the hardest of all known oxide crystals with a 9 on the Mohs scale. It is second in hardness only to diamond, and retains its strength at high temperatures. Synthetic sapphire crystals have good thermal properties, with excellent electrical and dielectric properties.
Steel Corrosion in Nuclear Plants
Generation IV reactors (Gen IV) are a set of theoretical nuclear reactor designs currently being researched. Most of these designs are generally not expected to be available for commercial construction before 2030. Current reactors in operation around the world are generally considered second- or third-generation systems, with most of the first-generation systems having been retired some time ago.
Metal Under Huge Stress
Silver and copper have a wide miscibility gap therefore special methodologies are needed to obtain a metastable alloy. The usual results of a Cu-Ag alloy synthesis is spinodal decomposition of Ag, Cu phases intergrown in bands some hundred nanometers wide. A way to push the spinodal decomposition to a smaller scale is given by the severe plastic deformation induced by a high pressure torsion (HPT).
Pavements of the Nanoworld
One effective method of producing nanocrystalline materials (grain size < 100 nm) is pulsed electrodeposition. It has been observed that electrodeposits form and grow in a nodular fashion each nodule representing a “colony” of nanosized grains. TEM has been used to investigate the local microtexture and Pole figures revealing ocal orientation measured at the interface between two colonies.
Nanoscale Reaction Models in Solid Oxide Fuel Cells
Solid oxide fuel cell (SOFC) technology is a promising energy conversion option at a time when efficient solutions are sought. During the electrochemical reaction of a fuel with an oxidant gas (usually air) at an operation temperature of ~ 800°C, SOFCs cogenerate heat and electricity with high efficiency: Electric efficiencies close to 60% are obtained now with a SOFC alone.
Next Generation Circuits for Semiconductor Industry
The scaling down to reach faster chip performances in electronic devices has pushed the dimensions of copper interconnect (CI) lines to the nanometre domain. This constant downscaling of CIs implies a change in their microstructure. A change in the grain boundary type distribution and local teture will strongly influence the resistivity and the mechanical reliability of downscaled CIS.
Structure of Magnetic Semiconductors
Magnetic Semiconductor materials have attracted widespread attention in recent years due to their potential application for the transport of information by exploiting both the intrinsic spin of the electron and its associated magnetic moment, in addition to its fundamental electronic charge.The new technology which emerged from discoveries in solid-state devices was called spintronics ("Spin Transport Electronics") also known as magnetoelectronics.
Hybrid Inorganic/Organic Systems for Optoelectronics In Daily Life
Nanocrystalline ZnO is provided in an inorganic/organic system of ZnO deposited on sexiphenyl (6P). Initially 6P was deposited on a-plane ZnO substrate at room temperature forming mesoscopic 1-dimensional islands of 6P. In a second step, the islands were capped with ZnO via molecular beam epitaxy at 373 K. Information on the nanostructure of ZnO grown atop 6P was provided by high-resolution TEM.
Atomic Scale of Nanolayer Composites
A stacking fault is a one or two layer interruption in the stacking sequence of the crystal structure. These interruptions carry a certain stacking fault energy (SFE). High SFE materials such as Al do not form twins easily. However, researchers have shown that it is possible to form Al layers in twin orientation to each other across polar TiN layers, if these are grown so that both the Al and TiN layers have a {111} surface as their growth front.
Understanding Li Insertion Mechanism for Next Generation Batteries
Lithium iron phosphate (LiFePO4) is a good candidate for positive electrodes in lithium-ion batteries to be installed in new electric vehicles. Its cost is low, it has an excellent life cycle and it is safe. To obtain the best performance in terms of electrical conductivity it is synthesised in nanocomposite with grain size between 50 and 300 nm.
Drug Delivery & Structure of Nanoparticles
Iron oxide nanoparticles (usually below 20 nm) are being investigated for biomedical applications because of their biocompatibility and unique physical properties. This biocompatibilty result from their capacity for metabolism, transportation and storage of human tissues. Magnetic iron oxide particles with diameter above 20 nm are ferromagnetic, which generates unstable particulate suspensions, as the particles aggregate together into biologically toxic, micron-sized clusters.
Inside the Nanowire Forest
III-V semiconductor nanowires are at the forefront of solid state physics and technology. Nanowires are quasi one dimensional crystals that can be heterostructured in different sectors having different chemical composition and crystal structure. They are grown by chemical beam epitaxy (CBE) from a III-V wafer with the Au-assisted growth method. In this method the wafer is coated with a thin layer film that by a dewetting thermal treatment in the CBE chamber transforms into small Au nanoparticles.
Texture Secrets of Nanoparticles
Nanoparticles are now a hot topic in several different fields for their astonishing and unusual properties compared to bulk materials. New sciences like nanochemistry, nanomedicine and nanotoxicology are born and an accurate knowledge of the nanoparticle structure is required to model properly their useful properties. Among these, the grain size, the defects and the particle shape are of major importance, since they easily correlate especially with optical properties.
Crystal Orientation Imaging of Organic Nanomagnets
The development and characterisation of nanometre-scaled functional molecular-based materials have recently attracted much attention. Molecular nano-objects offer the possibilty of tuning or combining magnetic, optical or electrical properties by a rational synthetic chemical approch. These materials present promising technological applications in molecular electronics, or magneto-optic memory devices providing that we can design single domain particles with hysteresis behavious in the future.
Inside a Roman Ceramic Factory in Ancient Gaul
Terra sigillata is certainly the most famous fine ware of the Roman period with characteristic decorations obtained by means of specially designed stamps (sigilla). This pottery was extensively produced in standardised shapes by a few specialised workshops and was widely distributed across the Roman Empire. The success of this pottery was mainly because of the brightness and red colour of the slip.
Shed Light to Earth Seismicity
The mineral olivine dominates the composition of the Earth's upper mantle and hence controls its mechanical behaviour and seismic anisotropy. Experiments at high temperature and moderate pressure, and extensive data on naturally deformed mantle rocks, have led to the conclusion that olivine at upper-mantle conditions deforms essentially by dislocation creep with dominant [100] slip.
The World of Mineral Polymorphs & Textures
Inorganic nanoparticles are widely used in catalysis. Research has led to control their morphology, crystallographic orientation and assembly. Metal oxide composites can be formed by heteroaggregation using electrostatic forces induced by the surface charges of the nanoparticles. It is important to understand the mechanisms of heteroaggregation and in particular the role of crystallographic facets.
