CHAPTER 3 DIFRACTION OF X-RAY IN CRYSTALS

3.1 X-Ray This chapter will discuss the determination of the crystal structure through the analysis of the diffraction patterns of the radiation wave in the crystal. Ray diffraction occurs only in a certain direction, such as the light fractted by the cracks. By measuring the direction associated with the intensity of diffraction and can be obtained information of crystal structure that responsible for the diffraction. There are three types of radiation that can be used for diffraction, namely: x-ray, neutron radiation and electron radiation. Treatment of three types of diffraction is similar, therefore only discuss in this discussion of x-ray diffraction. X-rays are electromagnetic waves with a wavelength close to 1 , this wavelength is short enough, x-rays have properties similar to other electromagnetic waves, such as optical waves. Thus the wavelength of an x-ray of the order sma with the crystal lattice constant, and therefore is used in x-ray crystal structure analysis. Photon energy of the x-ray revealed the Einstein equations E = h., by h Planck constant and is X-Ray frequency. By value of h = 6,6 x 10-27 erg-s and = 1 so the energy of X-Ray E 104 eV. Basic experimental arrangement to produce x-ray ray is depicted in Figure 2.1 below. Electrons emitted by the cathode of a vacuum tube is accelerated by a high potential acting between the cathode and anode. Therefore, the electrons gain kinetic energy was great and when mashing metal anode as a target, then the X-rays emitted from the target, then some of the x-ray is separated from the tube by the intensity for a particular purpose. X-rays have a continuous wave spectrum, which is composed by a series of discrete spectral lines. Continuous spectrum is produced by the emission of electrons emit radiation is deflected by the charges the target nucleus, whereas discrete emission lines produced by electron emission from the target atoms after they are excited by electrons coming. The maximum frequency of continously spectrum o depend to the potential acceleratter by relationship eV = h. o which is the maximum energy of a photon can not
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be larger than the kinetic energy of the electron ray. The wavelength of the x-ray spectra obtained from;
=
12,3 o A V

3.1

Wheres V in kilovolt. When a ray of x-rays passing through a medium, the x-rays will be absorbed in part, so intensiatas of the x-ray ray attenuation experienced by the equation:
.x I =I o .e

3.2

Wheres Io is intensiats initially on the surface of the medium and x is the distance entry of x-ray ray on the medium. The parameter is known as the absorption coefficient. Attenuation of the x-ray ray intensiats expressed by equation 3.2 scattering and absorption by the atom-atom medium.

V K A
Target cathode heating Vacuum tubes X-Ray

Electron

3.2 Bragg Difraction When a monochromatic x-ray ray is on the surface of a crystal, the x-ray ray is reflected, but reflection only occurs when the incident angle x-ray ray has certain prices. The prices of these angles depend on the wavelength and the lattice constants of the crystal, so that could explain the selective reflection occurs through interference effects, such as in optical physics. Selective reflectance models described by Figure 3.2, in which the crystal is expressed by pairs of parallel fields related to atomic crystal fields. X-ray
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ray that is reflected in part in each of these fields, which works like a mirror, and the reflected rays are then collected together on a detector. At detector files reflected x-rays interfere. Based on the physics of optical pattern is constructive interference occurs only when the path difference between two consecutive parallel ray is an even multiple of the wavelength of x-rays, namely; Different Path = n. n = 1,2,3,...... 3.3 Where is the wavelength of x-rays and n are positive integers.

Initial Ray

Figure 3.2 a. X-ray reflection from a crystal Reflected Ray b. The intensity of light reflected from the sample crystal KBr

Different path between light rays 1 and 2 in Figure 3.2a are:

= AB + BC - AC' = 2AB AC'

By equating it can be assumed that the specular reflectance of the angle of incidence is equal to the reflection angle. When the distance between the parallel planes (interplanar) expressed by the "d" from the picture above it is obtained;
AB = d sin 2d . cos tan

and AC' = AC cos =

Intensity of reflacted ray

3.4

Where is the angle between the light rays come with reflective beam. By inserting equation 3.4 into equation 3.3 and by establishing some manipulatted trigonometry then obtained following requirements constructive interference.
2d . sin = n.

3.5
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Equation 3.5 is known as Bragg diffraction requirement. Angles obtained from equation 3.5 for the price d and are the angles at which reflection occurs. In another angle shrinkage then reflected rays undergo destructive interference and consequently did not appear reflective beam-beam on the detector. The prices of n = 1, 2, ... of reflection related to the first order, second order, and so on. The intensity of the reflected beam is reduced with increasing orede reflection. That's why in this case would be more appropriate to replace the concept of reflection here as the concept of diffraction as part of the process. The basic idea underlining use Bragg law in studying the crystal structure is what is obtained from equation 3.5. Since can ditenteukan freely, and can be measured directly from the experiment (it is the half of the angle between the light beam diffracted beams come up with, as shown in Figure 3.2a), then by applying equation 3.5 can be calculated that the amount of distance between field interplanar d. It should be noted that according to equation 3.5 diffraction is only possible if and only if <2d, which shows why the optical wave can not be used to study the crystal structure, it is also noted that if the crystal is rotated a diffraction would occur associated with the occurrence of a pair interplanar field that new, as shown in Figure 3.2b for KBr crystals. Model of the Bragg law used above is very simplified, the fact that the event occurs scattering (scattering) of the x-ray beam caused by sifar discrete properties of the atom-atom crystal itself, so due to the contribution of the scattering atoms then the following fields must be seen as an atom pairs interplanar continuous field. With such treatment should be considered the interference caused by the diffraction of the x-rays are scattered all atoms of the crystal lattice. Thus the crystal lattice must be seen as a threedimensional diffraction grating. 3.3 Scattering of An Atom Diffraction process can be divided naturally into two stages: 1) scattering by individual atoms, and 2) build mutual interference between the scattered rays. Since the two phases are separated from each other, then both processes should be treated separately.

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Why does an atom scatter x-ray beam? Each atom is surrounded by electrons moving with an acceleration in the electric field of work which was brought by the x-ray beam. Since the electric charges are accelerated diffuse radiation (as described in the electromagnet) thus happens to the electrons of atoms. As a result, the electron absorbs the energy of the x-ray beam and toss it in all directions. Thus, when viewed from the beam scattering of atoms, it is necessary to consider the phase difference between the rays terhanbur for different regions of the cloud charge. Review the scattering by an electron as shown in figure 3.3a. flat wave field is expressed by;
u = A.e i (ko .r .t )

3.6

where A is the amplitude and wave vector ko (and angular frequency . wave flat expressed by equation 3.6 comes apada an electron. then came the wave scattered by electrons in the form of spherical waves are expressed;
u' = f A i (k .D .t ) .e eD

3.7

By fe a parameter known as the electron scattering length, D is the radial distance of an electron to the point at which the electric field is measured. Magnitude k is the number of scattered waves that have the same major ko. Equation 3.7 found that the scattered wave amplitude decreases with the distance to 1 / D, so the nature of the waves generated by spherical.
Scattered light Incident light M P2 N Electron (c) S k 2 Incident light (a) Electron So P1 (b) ko S

Fidure 3.3

a. Scattering by an electron b. Scattering by two electrons c. Wave vectors

Further review the scattering by two electrons as shown 3.3b. In this case both the scattered electron emits a spherical wave, and the scattered field observed at tsebuah

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point is the sum of two separate fields in which the phase difference between the two fields considered in the summation. Thus electron waves are scattered by the second;

A i[ k.D + k.( D + )] u = fe .e D
'
(

3.8

where is the phase lag of the electron wave terhabur 1terhadap waves scattered by electrons 2. of the second phase difference picture 3.3b scattered waves can be expressed;
= P 1N P 1M . ) 2 = ( r.S r.S
o

).k

3.9 where r adalan radius vector of the electron relative to the electron 2 1, and S and So the unit vector in the direction of the incident wave and scattered waves. Statement for can be expressed in the form
= s .r

3.10 3.11 3.12

where the scattering vector is defined as s = k (S So) = k - ko as can be seen in Figure 3.3c of the scattering vector is given by s = 2k sin obtained
u' = f A ik .D .e 1 + eis.r eD

with is half the scattering angle. By entering 3.10 into the equations 3.8 equations

3.13

At 3.13 deriving equations selected as the reference coordinate elektron1 position, but for the incompatibility as a reference point chosen point, so the two electrons are treated on an equal footing. With the scattered wave equation becomes;
u' = f A ik .D is.r1 is.r .e e +e 2 eD

3.14

with r1 and r2 is the vector of the electron relative to the second position of the new point of reference. Equation 3.13 constitute special condition of the equation 3.14 for r1 = 0,

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that is, when the reference point is at the position of electron 1. Generalization of the equation 3.14 for a scattering of crystal atoms is;
u' = f A ik .D is.r .e e i eD i

3.15

where ri position vector of the ith electron and the sum done for all the electrons. By analogy to the case of a single electron equation 3.7 the scattering length for many electron system is obtained by summing;
f = f e e
i

is.ri

3.16

Which is the total scattering length, ie the number of individuals taking into account the length haburan phase. The intensity I of the beam scattering depends on the square of the magnitude of the wave field, therefore I~
f 2 =f 2

e
i

is.ri

3.17

The results obtained by the equation 3.16 and 3.17 is the basic equation in enacting the scattering and diffraction. By using the important aspects of the scattering process is the coherence properties contained in the scattering which means that in the process of scattering occurs a particular phase relationship of each beam scattering allowing terjadinnya interference, resulting in the intensity of the scattered wave can be simplified into I~
N. f 2 e

3.18

where N is the number of electron scattering. Furthermore, the results obtained above can be applied to the case of a single atom in a free state. In applying equation 3.18 electrons is deemed not in the position of discrete but scattered electrons as a continuous charge cloud meets the atomic volume. Thus summation 3.16 discrete equations can be transformed into the integral form;
f = f e i is.r e i
f e

(r ).eis.r d 3 r

3.19 With (r) is the electron cloud density (in electrons per stuan volume) and integral to the entire volume of the atom. Atomic scattering factor fa defined as a form of integral equations arising from 3:16 in the.
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= (r ).eis.r d 3 r

3.20

fa a scale without units. Forms of integral equations 3.20 can be simplified when (r) is a spherical symmetry around the nucleus, because the next equation can diintegral to all corners of the volumen element, which produces;
R

sin sr f = 4 .r 2 ( r ). dr a sr o

3.21

where R is the atomic faint. As shown in equation 3.21 scattering factor depends on the scattering angle (s = 2 k sin ) coming from the oscillating factor (sin sr)/sr the integral. Ossilasi wavelength is inversely proportional to s as depicted in Figure 3.4a ossilasi shorter wavelength then fa smaller due to the interference between the scattered beam to differences in the area of cloud charge. By taking back the equation s = 2 k sin it can be shown that the increase in the scattering angle 2 s also raise the price and yield reduction in atomic scattering factors fa.

S = 2k.sin

Figure 3.4

a. Factors oscillation sin (sr)/sr b. Scattering factor as a function of scattering angle for the carbon atom

Furthermore, to calculate fa need to know the density of atoms (r). There is a special way to where fa can be calculated, which is = 0, s = 0 and subsequent oscillation factor sin sr/sr to 1, so the equation becomes 3.21
R o

f a = 4 .r 2 ( r ).dr
3.22 And the integral becomes simple is the same as the total number of electrons in the atom. For example, atoms with atomic number Z generate
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fa ( = 0) = Z phase, so that the resulting interference is constructive.

3.23

Physical interpretation of the equation 3.23 is that all parts of the file are scattered in

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