Indexed electron diffraction ring positions from a polycrystalline deposit identify candidate phases and give lattice parameters after camera-length calibration. Spot patterns from a small selected area establish zone axis directions, epitaxial orientation relationships or crystal twinning. Nanobeam mapping can reveal grain orientation changes, while systematic spot shifts can measure relative strain if lens distortions and scan drift are controlled. Spot or ring broadening can reflect finite coherent size, but also strain and instrumental broadening, so it is not an unqualified particle-diameter measurement. Use a calibration standard and an empty support region, vary dose to check electron beam damage, and combine spacing information with elemental analysis when chemically distinct phases have similar lattice parameters.
Choose cyclic reciprocal units, so the incident and elastically scattered wavevectors have magnitude . Place the reciprocal lattice origin at the end of the incident vector from the sphere centre . A reciprocal vector is excited when its endpoint lies on the Ewald sphere, because
A specimen tilt rotates the reciprocal lattice relative to this construction. The very short electron de Broglie wavelength makes the sphere nearly flat across several ordinary reciprocal-lattice spacings. In a thin foil, finite thickness broadens reciprocal points into reciprocal lattice rods approximately along the foil normal, with characteristic longitudinal extent . A rod may intersect the sphere even when its ideal point is slightly off it. Consequently several reflections can appear simultaneously near a zone axis, and thinning changes the excitation tolerance. A small particle has finite-size broadening in other directions too. This geometrical excitation condition does not guarantee a particular spot intensity: crystal basis structure factors, specimen thickness and dynamical diffraction still matter.
Figure 1.
Local Ewald sphere intersections and calculated fcc gold reflections
. Details.
For cubic lattice planes, . The face-centred cubic selection rule permits indices that are all odd or all even. Thus
The first two spacings exceed the quoted 0.19 nm real-space resolution, whereas does not. This restriction is for the resolved image and its transform; a diffraction instrument need not have the same cutoff.
A natural candidate is a beam near a local zone axis. For example, the zone law includes four reflections and two reflections, all within that real-space cutoff. Their reciprocal-space length ratio is . The angle between and reciprocal vectors is . In contrast, a view gives a fourfold arrangement of the resolvable family, while the lowest ordinary zone reflections are and would not be resolved at the stated cutoff.
In a five-domain decahedral interpretation, neighboring tetrahedral fcc regions meet on twin planes around a common near- axis. Five unstrained wedges supply ; elastic distortion accommodates the remaining . Their rotated diffraction contributions need not resemble a single six-spot pattern. Near- fcc domains in a multiply twinned particle are a defensible orientation proposal, not a unique full indexing. The printed transform has no reciprocal-space scale or indexed spot list, so it cannot establish every domain rotation or exclude an overlapping-particle contribution. Calibrated spacings and transforms from individual regions would settle those distinctions. The five-domain geometry is independently observed in atomic-resolution gold-particle measurements.[ref]
The upper island has lower contrast than the rod in HAADF imaging, consistent with a lighter Zn-containing region above a Ru-rich support. Thickness, orientation and detector conditions also affect contrast, so intensity alone is not a compositional assay. The island is a flattened supported cap, not an isolated regular bulk crystal.
Using the 2 nm scale bar as a ruler gives a projected lateral size of order 4–6 nm and height of order 1–2 nm, depending on placement of the diffuse edges. These are approximate image estimates, not a three-dimensional diameter or size distribution. The height/width ratio is roughly –, and only a few atomic rows span the height. Thus surface and interface atoms form a substantial fraction of the particle. The truncated, irregular cap and weak edge order depart from an infinite, fully coordinated, perfectly periodic wurtzite crystal.
Adhesion can favor spreading across the rod. epitaxy can orient ZnO against a compatible surface repeat of the rutile structure, despite the different bulk symmetries. Coherent growth initially introduces strain; free edges allow relaxation, while larger islands may develop misfit dislocations. Facet-dependent attachment, polar surface energies, ligand coverage and unequal precursor delivery can further alter the cap. A final image does not uniquely reveal which kinetic pathway operated.
To measure strain, first index the zone axis and projected lattices. For pixel spacing and scale-bar length , . Compare an indexed spacing with its unstrained reference:
The latter is the hexagonal wurtzite relation. An ideal tetrahedral geometry has and internal coordinate ; real bulk ZnO itself need not attain those ideal values. Measure several periods and compare interface and free-edge regions to distinguish strain from tilt and calibration errors.
A unique numerical lattice strain, vacancy concentration or phase assignment is not established by this unindexed single projection. Oxygen columns are weak, so a missing bright spot does not prove an oxygen vacancy. Tilted images, electron diffraction, chemical mapping and thickness-aware simulations would test those claims. The full rutile structure is primitive tetragonal with a basis: its metal positions can appear body-centered in a conventional cell, but the oxygen basis prevents calling the entire structure a body-centered tetragonal Bravais lattice.
Use high-resolution transmission electron microscopy with a coherent, well-aligned beam and an objective aperture admitting the direct beam and the spatial frequencies required at the interface. Orient a crystalline region near a suitable zone axis so that useful lattice fringes are excited; minimize drift, vibration and astigmatism. Choose defocus and aberration correction to transfer the target frequencies, rather than treating the image as a direct map of atoms at arbitrary defocus.
An aberration-corrected scanning transmission electron microscopy probe with high-angle annular dark-field imaging can instead resolve an interface with more directly interpretable atomic-number contrast. A nominal thickness may be too great for clean atomic-resolution interpretation: thin the interface further if necessary, finish focused ion beam milling at lower ion energy to reduce damaged surface layers, and check for curtaining and implantation. The best mode depends on crystallinity and damage sensitivity; an amorphous interface calls for resolving its boundary and composition rather than inventing lattice fringes.
Zone axis 2026-10-20
A crystallographic direction shared by a set of planes. Aligning a transmission electron microscopy beam along a suitable zone axis can excite multiple useful lattice reflections.