X-ray diffraction (XRD) is used to characterize the crystal structure of thin films and nanocrystals. XRD works by detecting constructive and destructive interference of x-rays scattered by the atomic structure of a material. The Bragg equation relates diffraction peak positions to atomic spacing. XRD analysis provides information on lattice constants, grain size, defects, and stress. The document describes how the Scherrer formula uses XRD peak broadening to estimate nanocrystal size from the number of coherent scattering domains.
X-ray diffraction (XRD) is used to characterize the crystal structure of thin films and nanocrystals. XRD works by detecting constructive and destructive interference of x-rays scattered by the atomic structure of a material. The Bragg equation relates diffraction peak positions to atomic spacing. XRD analysis provides information on lattice constants, grain size, defects, and stress. The document describes how the Scherrer formula uses XRD peak broadening to estimate nanocrystal size from the number of coherent scattering domains.
X-ray diffraction (XRD) is used to characterize the crystal structure of thin films and nanocrystals. XRD works by detecting constructive and destructive interference of x-rays scattered by the atomic structure of a material. The Bragg equation relates diffraction peak positions to atomic spacing. XRD analysis provides information on lattice constants, grain size, defects, and stress. The document describes how the Scherrer formula uses XRD peak broadening to estimate nanocrystal size from the number of coherent scattering domains.
X-ray diffraction (XRD) is used to characterize the crystal structure of thin films and nanocrystals. XRD works by detecting constructive and destructive interference of x-rays scattered by the atomic structure of a material. The Bragg equation relates diffraction peak positions to atomic spacing. XRD analysis provides information on lattice constants, grain size, defects, and stress. The document describes how the Scherrer formula uses XRD peak broadening to estimate nanocrystal size from the number of coherent scattering domains.
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Chapter 2 Synthesis and Characterization
2.2.1 X-ray Diffractometer (XRD)
X-ray diffraction (XRD) is a very important experimental technique in revealing the crystal structure of bulk solid microstructure of thin films. Apart from providing the structural phase of the nanocrystals, this technique also provides an estimate of the size of the nanocrystals, as discussed later in this section. The XRD methods are generally applied to films thicker than several angstroms on account of the strong penetrating power of the x-rays. Information related to the crystal structure of the films, including lattice constants, grain size, preferred orientation of polycrystals, defects, stress, etc. can be determined from the x-ray diffraction measurement. X-rays are electromagnetic waves. The phenomenon of the x-ray diffraction by crystals results from a scattering process in which x-rays are scattered by the electrons of the atoms without change in wavelength. As the wavelength of X-rays is close to atomic size (~ 1.5 Ǻ), they get diffracted by atoms and ions. If, as in the case of crystals, the atoms or ions are arranged in a particular fashion then the diffracted x-rays interfere constructively or destructively with each other depending on the path difference. W.L. Bragg formulated the condition for constructive interference as,
2d sin n
where, d is the spacing between two adjacent atomic planes, θ is the angle between the
atomic plane and the x-rays, n is the order of diffraction maximum, and λ is the wavelength of the x-rays. The resulting diffraction pattern comprising both the positions and intensities of the diffraction effects is a fundamental physical property of the substance. Analysis of the positions of the diffraction effect leads immediately to a knowledge of the size, shape and orientation of the unit cell. For our studies we have used the Bruker D8 Advance X-ray diffractometer as shown in Figure 2.4.
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Figure2.4: X-ray diffractometer
The finite size of the crystallites has a marked effect on the X-ray diffraction line widths. With reduction in the particle size, observed X-ray diffraction lines broaden significantly. This is due to the finite size of the nanocrystals. The particle size can be estimated from the width of the diffraction line corresponding to a particular (hkl) refection from the Scherrer formula [18]. The origin of such broadenings of the diffraction peaks due to the finite size effect can be understood by considering the effect of diffraction from a finite number of planes as shown schematically in Figure 2.5. Considering an ideal crystal having p atomic (hkl) planes of spacing d parallel to the surface, the approximate thickness of the crystal is close to pd. The amplitude of a diffracted ray will be maximum when the path difference between the rays reflected from successive planes is equal to a multiple of the wavelength
δl 2dsinθ nλ (2.1)
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A characteristic shift towards lower angle compared to the reflex of ideal crystals indicates a lattice expansion. The lattice distortion (∆d/d0) is defined as:
d d 0 ( d exp d hkl ) d hkl (2.2)
Figure 2.5: A schematic diagram of X-ray diffraction from finite number of planes.
When the incident angle differs from θ by a small amount , the resulting path difference is given by
l = 2d sin (θ + ) = 2d sin θ cos + 2d sin cos θ = n cos = 2d sin cos θ
(2.3)
Since, is small, the above expression can be written as
l n 2 d cos (2.4)
The corresponding phase difference between the first and the pth plane is given by
4p d cos (2.5) The resultant amplitude of the reflected wave is given by the vector sum of the amplitude
of each of the p vectors successively differing by increasing phase of , by
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2p d cos ap sin A 2p d cos (2.6)
The amplitude of the reflected ray is maximum when = 0; in this case A0 = ap. The full width at half maximum intensity can be calculated by 2 A 2 sin ( 2 ) 1 = (2.7) A02 2 2 ( ) 2
The above equation holds when
= 1.40 2 (2.8) or using equation, 4p d cos = 1.40 (2.9) 2 The full width at half maximum, hkl for the diffraction peak at 2 θ angle is then given by
0.89 (2.10) B cos
This expression is known as the Scherrer formula. We have used the above formula for determining the size of the nanocrystallites, as will be discussed in the subsequent chapters.
