Physical Principles of Electron Microscopy: An Introduction to TEM ...
Physical Principles of Electron Microscopy: An Introduction to TEM ...
Physical Principles of Electron Microscopy: An Introduction to TEM ...
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106 Chapter 4<br />
4.5 Diffraction Contrast from Polycrystalline Specimens<br />
Many inorganic materials, such as metals and ceramics (metal oxides), are<br />
polycrystalline: they contain small crystals (crystallites, also known as<br />
grains) within which the a<strong>to</strong>ms are arranged regularly in a lattice <strong>of</strong> rows<br />
and columns. However, the direction <strong>of</strong> a<strong>to</strong>mic alignment varies randomly<br />
from one crystallite <strong>to</strong> the next; the crystallites are separated by grain<br />
boundaries where this change in orientation occurs rather abruptly (within a<br />
few a<strong>to</strong>ms).<br />
<strong>TEM</strong> specimens <strong>of</strong> a polycrystalline material can be fabricated by<br />
mechanical, chemical or electrochemical means; see Section 4.10. Individual<br />
grains then appear with different intensities in the <strong>TEM</strong> image, implying that<br />
they scatter electrons (beyond the objective aperture) <strong>to</strong> a different extent.<br />
Because this intensity variation occurs even for specimens that are uniform<br />
in thickness and composition, there must be another fac<strong>to</strong>r, besides those<br />
appearing in Eq. (4.15), that determines the amount and angular distribution<br />
<strong>of</strong> electron scattering within a crystalline material. This additional fac<strong>to</strong>r is<br />
the orientation <strong>of</strong> the a<strong>to</strong>mic rows and columns relative <strong>to</strong> the incident<br />
electron beam. Because the a<strong>to</strong>ms in a crystal can also be thought <strong>of</strong> as<br />
arranged in an orderly fashion on equally-spaced a<strong>to</strong>mic planes, we can<br />
specify the orientation <strong>of</strong> the beam relative <strong>to</strong> these planes. To understand<br />
why this orientation matters, we must abandon our particle description <strong>of</strong> the<br />
incident electrons and consider them as de Broglie (matter) waves.<br />
A useful comparison is with x-rays, which are diffracted by the a<strong>to</strong>ms in<br />
a crystal. In fact, intera<strong>to</strong>mic spacings are usually measured by recording the<br />
diffraction <strong>of</strong> hard x-rays, whose wavelength is comparable <strong>to</strong> the a<strong>to</strong>mic<br />
spacing. The simplest way <strong>of</strong> understanding x-ray diffraction is in terms <strong>of</strong><br />
Bragg reflection from a<strong>to</strong>mic planes. Reflection implies that the angles <strong>of</strong><br />
incidence and reflection are equal, as with light reflected from a mirror. But<br />
whereas a mirror reflects light with any angle <strong>of</strong> incidence, Bragg reflection<br />
occurs only when the angle <strong>of</strong> incidence (here measured between the<br />
incident direction and the planes) is equal <strong>to</strong> a Bragg angle �B that satisfies<br />
Bragg’s law:<br />
n � = 2 d sin�B<br />
(4.20)<br />
Here, � is the x-ray wavelength and d is the spacing between a<strong>to</strong>mic planes,<br />
measured in a direction perpendicular <strong>to</strong> the planes; n is an integer that<br />
represents the order <strong>of</strong> reflection, as in the case <strong>of</strong> light diffracted from an<br />
optical diffraction grating. But whereas diffraction from a grating takes place<br />
at its surface, x-rays penetrate through many planes <strong>of</strong> a<strong>to</strong>ms, and diffraction<br />
occurs within a certain volume <strong>of</strong> the crystal, which acts as a kind <strong>of</strong> three-