Introduction to EBSD

Electron backscatter diffraction (EBSD), also known as backscatter Kikuchi diffraction (BKD), is an SEM based microstructural-crystallographic technique to measure the crystallographic orientation. In EBSD a stationary electron beam strikes a tilted crystalline sample and the diffracted electrons form a pattern on a fluorescent screen. This pattern is characteristic of the crystal structure and orientation of the sample region from which it was generated. It provides the absolute crystal orientation with submicron resolution. It is a very powerful tool for microstructural characterisation. EBSD can be used to index and identify the seven crystal systems, and as such it takes typical measurements to Crystal orientation Misorientation Grain size Global texture Local texture Recrystallise/deformed fractions Substructure analysis Strain analysis Grain boundary characterisation CSL boundary distribution Slip system activity Phase identification Phase distribution Phase transformations Fracture analysis... It has been applied to many industries such as Metals processing Aerospace industry Nuclear industry Automotive industry Microelectronics Earth sciences... Many materials have been investigated by using EBSD, such as Metals, Alloys Intermetallics Ceramics Thin films Geological minerals Semiconductors

Superconductors... EBSD has become a well established technique for the SEM, and obtaining crystallographic information from samples is now both routine and easy. This online tutorial explains how an EBSD system works, describes the experiments that can be performed, and how to undertake them.

Principal system components

An EBSD detector system will typically consist of following: A phosphor screen which is fluoresced by electrons from the sample to form the diffraction pattern. A sensitive charge coupled device (CCD) camera together with optics for viewing the diffraction pattern on the phosphor screen. A lead glass window behind the phosphor screen to block the radiation. Vacuum seals which allow the camera to operate at atmospheric pressure without degrading the chamber pressure. Movement control which allows the detector to be positioned at different positions; retracted position will be so that the detector doesnt interfere with normal SEM work. An interface in order to mount the detector onto the relevant SEM port. A computer to control EBSD experiments; collect and analyse the diffraction patterns as well as display results and do further processing. Optional FSD detectors mounted around the phosphor screen. Electronic hardware that controls the SEM scanning. Communication control of SEM stage and column.

Figure 1 The experimental set up for EBSD VIEW ALL VIEW ALL

Pattern formation
For EBSD, a beam of electrons is directed at a point of interest on a tilted crystalline sample approximately 70 relative to normal incidence of the electron beam in the SEM (Figure 2). The mechanism by which the diffraction patterns are formed is complex, but the following model describes the principal features. The atoms in the material inelastically scatter a fraction of the electrons with a small loss of energy to form a divergent source of electrons close to the surface of the sample. Some of these electrons are incident on atomic planes at angles which satisfy the Bragg equation:

(Equation 1) where n is an integer, is the wavelength of the electrons, d is the spacing of the diffracting plane, and is the angle of incidence of the electrons on the diffracting plane. These electrons are diffracted to form a set of paired large angle cones corresponding to each diffracting plane. When used to form an image on the fluorescent screen the regions of enhanced electron intensity between the cones produce the characteristic Kikuchi bands of the electron backscatter diffraction pattern (Figure 3).

Figure 2 Formation of the electron backscattered diffraction pattern. Electrons from a divergent source incident on crystal planes at the Bragg angle are diffracted into a pair of cones to form Kikuchi bands in the diffraction pattern ENLARGE

Figure 3 A diffraction pattern from nickel collected at 20 kV accelerating voltage ENLARGE

Interpreting the diffraction pattern

The centre lines of the Kikuchi bands correspond to the projection of the diffracting planes on the phosphor screen. Hence, each Kikuchi band can be indexed by the Miller indices of the diffracting crystal plane which formed it. Each point on the phosphor screen corresponds to the intersection of a crystal direction with the screen. In particular, the intersections of the Kikuchi bands correspond to the intersection of zone axes in the crystal with the phosphor screen. These points can be labelled by the crystal direction for the zone axis (Figure 4).

Figure 4 Relationship between diffraction pattern and the crystal VIEW ALL VIEW ALL VIEW ALL VIEW ALL VIEW ALL The pattern is a gnomonic projection of the diffracted cones of electrons onto the phosphor screen. The semi-angle of the diffracted cones of electrons is (90 - ) degrees. For EBSD this is a large angle so the edges of the Kikuchi bands approximate to straight lines. For example, the wavelength of 20 kV electrons is 0.00859 nm and the spacing of the (111) plane in aluminium is 0.233 nm making the cone semi-angle 88.9. The width w of the Kikuchi bands close to the pattern centre is given by:

(Equation 2) where l is the distance from the sample to the screen (Figure 5). Hence, planes with wide d-spacings give thinner Kikuchi bands than narrow planes.

Figure 5 EBSD Geometry ENLARGE

Figure 6 Changes in the crystal orientation result in movement of the diffraction pattern. The simulated diffraction pattern is from a sample tilted 70 to the horizontal and the crystal orientation is viewed along the direction perpendicular to the sample. Because the diffraction pattern is bound to the crystal structure of the sample, as the crystal orientation changes the resultant diffraction pattern also changes. The positions of the Kikuchi bands can therefore be used to calculate the orientation of the diffracting crystal (Figure 6). Click here for an interactive Java applet showing the relationship between the crystal structure and the diffraction pattern. This animation shows the relationship between the crystal orientation and simulated diffraction pattern for a face centred cubic crystal. As the crystal rotates the diffraction pattern moves. (The simulated diffraction pattern is from a sample tilted 70 to the horizontal and the crystal orientation is viewed along the direction perpendicular to the sample). VIEW ANIMATION

Calibrating the EBSD system

To collect accurate EBSD data you have to accurately calibrate the projection parameters of your pattern, and these will be dependent on the geometry of the acquisition (i.e. the working distance and detector distance). In older EBSD systems this data is typically extracted from a single pattern. Historically, this not only requires a certain level of expertise but it was also a source of inaccuracy in the data. In AZtecHKL there is an AutoCalibration routine which works seamlessly to correct for changes in the geometry of the system. Now you can use any working distance or any detector position without having to worry about or change the calibration. This innovative method enhances the productivity and ease of use associated with EBSD. This autocalibration is based on a procedure performed once then the system is installed. This procedure automatically collects a series of EBSD patterns at known working distance and detector distance. It then uses an image correlation technique to find the pattern centre (The pattern centre is the point on the screen closest to the generation point of the diffraction pattern on the sample.) at each geometry set up, as shown in the figure 7 below. This information is then used during normal working conditions. Coupled with this there is a calibration refinement so the user can check and be satisfied that the calibration is good.

Figure 7 AZtecHKL Autocalibration geometry

Automated indexing and orientation measurement

The crystal orientation is calculated from the Kikuchi band positions by the computer processing the digitised diffraction pattern collected by the CCD camera. The Kikuchi band positions are found using the Hough transform. The transform between the coordinates (x,y) of the diffraction pattern and the coordinates (, ) of Hough space is given by (Figure 8):

(Equation 3)

Figure 8 The Hough Transform transforms lines into points in Hough space. A straight line is characterised by , the perpendicular distance from the origin and the angle made with the x-axis and so is represented by a single point (, ) in Hough space. Kikuchi bands transform to bright regions in Hough space which can be detected and used to calculate the original positions of the bands (Figure 9).

Figure 9 Finding the position of the Kikuchi bands in the diffraction pattern using the Hough transform VIEW ALL VIEW ALL VIEW ALL VIEW ALL VIEW ALL Using the system calibration, the angles between the planes producing the detected Kikuchi bands can be calculated. These are compared with a list of inter-planar angles for the analysed crystal structure to allocate Miller indices to each plane. The final step is to calculate the orientation of the crystal lattice with respect to coordinates fixed in the sample. This whole process takes less than a few milliseconds with modern computers.

Band Intensity
The mechanisms giving rise to the Kikuchi band intensities and profile shapes are complex. As an approximation, the intensity of a Kikuchi band for the plane (hkl) is given by:

(Equation 4) Where fi() is the atomic scattering factor for electrons and (xi yi zi) are the fractional coordinates in the unit cell for atom i. An observed diffraction pattern should be compared with a simulation calculated using equation 4, to ensure only planes that produce visible Kikuchi bands are used when solving the diffraction pattern (Figure 10). This is especially important when working with materials with more than one atom type.

Figure 10 Diffraction pattern band intensities. VIEW ALL VIEW ALL VIEW ALL

Summary
When an electron beam is incident on a tilted crystalline sample, electron backscatter diffraction patterns are formed on a suitably placed phosphor screen. The diffraction pattern consists of a set of Kikuchi bands which are characteristic of the sample crystal structure and orientation. The centre line of each Kikuchi band corresponds to the intersection with the phosphor screen of the diffracting plane responsible for the band. The position of the Kikuchi bands can be found automatically with the Hough transform and used to calculate the crystal orientation of the sample region that formed the pattern.

EBSD and other techniques

EBSD is unquestionably the fastest and most reliable way in which to acquire data for crystalline structure and orientation in a solid crystalline phase. Traditionally these types of microstructural characterisation studies have been carried out using optical metallography, X-ray diffraction (XRD), neutron diffraction, synchrotron radiation, electron diffraction in a TEM, Kossel Patterns, Channelling Patterns. Several strength and limitation have been concerned for each tool as following: Electron Backscatter Diffraction (EBSD) Good spatial resolution (~10nm) Good angular resolution (~0.2) Visualization of phases, grain size and grain/subgrain distribution Visualization of local texture and local crystal orientations from mm to 20nm Accurate identification for minor phases Reasonable statistics with automation Good availability 2-D and 3-D Variation crystalline characterization measurements Sample preparation can be time consuming and requires a level of expertise Sample size needs to be able to fit in a SEM tilt to 70 degrees Optical metallography Easy sample preparation Poor spatial resolution (~200nm) Phase identification (depends on experience) X-ray Easy sample preparation Powerful and rapid technique for unknown phase identification No information of phase distribution Difficult to extract information on size Low volume fraction (~ 2%) phases missed Peak overlay may occur and worsens for high angle reflections Spatial resolution limited to beam size Data interpretation can be complex and requires a level of expertise Synchrotron Radiation Good statistics 3-D information Low Spatial Resolution (5m) Moderate angular resolution (1-2)

Difficult mathematical reconstruction Poor availability TEM Diffraction (Kikuchi patterns, Spot patterns, CBED) High spatial resolution to atomic level (~0.08nm) Good accuracy Extremely limited area Difficult sample preparation Limited automation Some 3-D information Poor statistics Electron Channelling Poor spatial resolution (5-10m) Moderate accuracy (0.5) 2-D No automation Poor statistics. Kossel X-Ray Diffraction Good accuracy (0.1) Poor spatial resolution (10m) 2-D Limited materials No automation Poor statistics