Precession electron diffraction

Precession electron diffraction (PED) is a specialized method to collect electron diffraction patterns in a transmission electron microscope (TEM). By rotating (precessing) a tilted incident electron beam around the central axis of the microscope, a PED pattern is formed by integration over a collection of diffraction conditions. This produces a quasi-kinematical diffraction pattern that is more suitable as input into direct methods algorithms to determine the crystal structure of the sample. Precession electron diffraction (PED) is a specialized method to collect electron diffraction patterns in a transmission electron microscope (TEM). By rotating (precessing) a tilted incident electron beam around the central axis of the microscope, a PED pattern is formed by integration over a collection of diffraction conditions. This produces a quasi-kinematical diffraction pattern that is more suitable as input into direct methods algorithms to determine the crystal structure of the sample. Precession electron diffraction is accomplished utilizing the standard instrument configuration of a modern TEM. The animation illustrates the geometry used to generate a PED pattern. Specifically, the beam tilt coils located pre-specimen are used to tilt the electron beam off of the optic axis so it is incident with the specimen at an angle, φ. The image shift coils post-specimen are then used to tilt the diffracted beams back in a complementary manner such that the direct beam falls in the center of the diffraction pattern. Finally, the beam is precessed around the optic axis while the diffraction pattern is collected over multiple revolutions. The result of this process is a diffraction pattern that consists of a summation or integration over the patterns generated during precession. While the geometry of this pattern matches the pattern associated with a normally incident beam, the intensities of the various reflections approximate those of the kinematical pattern much more closely. At any moment in time during precession, the diffraction pattern consists of a Laue circle with a radius equal to the precession angle, φ. It is crucial to note that these snapshots contain far fewer strongly excited reflections than a normal zone axis pattern and extend farther into reciprocal space. Thus, the composite pattern will display far less dynamical character, and will be well suited for use as input into direct methods calculations. PED possesses many advantageous attributes that make it well suited to investigating crystal structures via direct methods approaches: Precession electron diffraction is typically conducted using accelerating voltages between 100-400 kV. Patterns can be formed under parallel or convergent beam conditions. Most modern TEMs can achieve a tilt angle, φ, ranging from 0-3°. Precession frequencies can be varied from Hz to kHz, but in standard cases 60 Hz has been used. In choosing a precession rate, it is important to ensure that many revolutions of the beam occur over the relevant exposure time used to record the diffraction pattern. This ensures adequate averaging over the excitation error of each reflection. Beam sensitive samples may dictate shorter exposure times and thus, motivate the use of higher precession frequencies. One of the most significant parameters affecting the diffraction pattern obtained is the precession angle, φ. In general, larger precession angles result in more kinematical diffraction patterns, but both the capabilities of the beam tilt coils in the microscope and the requirements on the probe size limit how large this angle can become in practice. Because PED takes the beam off of the optic axis by design, it accentuates the effect of the spherical aberrations within the probe forming lens. For a given spherical aberration, Cs, the probe diameter, d, varies with convergence angle, α, and precession angle, φ, as Thus, if the specimen of interest is quite small, the maximum precession angle will be restrained. This is most significant for conditions of convergent beam illumination. 50 nm is a general lower limit on probe size for standard TEMs operating at high precession angles (>30 mrad), but can be surpassed in Cs corrected instruments. In principle the minimum precessed probe can reach approximately the full-width-half-max (FWHM) of the converged un-precessed probe in any instrument, however in practice the effective precessed probe is typically ~10-50x larger due to uncontrolled aberrations present at high angles of tilt. For example, a 2 nm precessed probe with >40 mrad precession angle was demonstrated in an aberration-corrected Nion UltraSTEM with native sub-Å probe (aberrations corrected to ~35 mrad half-angle).