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- Dual Nature of Matter
- Fred Alan Wolf - Quantum Consciousness
- ch14
- Manual Xrd 6100
- 11-03-Paper.pdf
- A Study on Size and Shape of Erythrocytes of normal and malarial blood using Laser Diffraction Technique1 by amar alansi
- Thermal Radiation lab rep.doc
- Minerals explained 37
- lab_ads
- UT Dallas Syllabus for phys5322.001 05f taught by (axh049000)
- 145659210-Solutions-Hw01.pdf
- Diffraction Crystal Structure
- solid state IIT
- V. Zhurbenko Passive Microwave Components and Antennas 2010
- Electron Scattering and Diffraction
- Absorption
- (1) Crystal Structure
- Ch-3 Compatibility Mode
- Vorlaender Mommertz Scattering
- Update Rrtm

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beams

Contents

1 Introduction 1

2 Scattering by an electron 3

3 Scattering by an atom 6

4 Scattering by an unit cell 6

5 Structure factor with single atom basis 9

5.1 Simple cubic . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

5.2 Body centered cubic . . . . . . . . . . . . . . . . . . . . . . . 10

5.3 Face centered cubic . . . . . . . . . . . . . . . . . . . . . . . . 10

5.4 Hexagonal close packed . . . . . . . . . . . . . . . . . . . . . . 11

6 Structure factor with multi-atom basis 11

7 X-ray intensity 12

7.1 Multiplicity factor . . . . . . . . . . . . . . . . . . . . . . . . . 12

7.2 Lorentz-polarization factor . . . . . . . . . . . . . . . . . . . . 12

7.3 Absorption factor . . . . . . . . . . . . . . . . . . . . . . . . . 13

7.4 Temperature factor . . . . . . . . . . . . . . . . . . . . . . . . 13

1 Introduction

Consider the X-ray diraction pattern of Fe (bcc) and Al (fcc) shown in

gures 1 and 2 Certain crystallographic planes are missing in the patterns,

e.g 100 is missing in both while 110 is missing in fcc Al. Also, the intensities

of the lines are all dierent. We understand the position of the lines is given

1

MM3030: Materials Characterisation

Figure 1: X-ray diraction pattern from bcc Fe

Figure 2: X-ray diraction pattern from fcc Al

2

MM3030: Materials Characterisation

Figure 3: Body centered and base centered orthorhombic structure. Taken

from Elements of X-ray diraction - B.D. Cullity.

by Braggs law and knowing the lattice constant and the crystal structure

it is possible to calculate the 2 values but what decides the intensity and

the presence/absence of some lines? This is dictated by the position of the

atoms in the lattice. Thus the crystal structure plays a role and also the

number and type of each atom. If we have a compound or intermetallic the

intensities will depend on the position and amount of each of the constituent

atoms. Similarly, in the case of intermetallics order-disorder transformations

can also aect the XRD patterns (we will see this later).

To give and example of how atom positions aect the presence/absence of

peaks in the XRD pattern consider gure 3 which shows the base centered

and body centered orthorhombic structures. For the base centered structure,

in the c axis, the interplanar spacing is c and the plane is 001. For the body

centered structure the interplanar spacing is c/2 and the plane is 002. Thus,

001 diraction will be present in the base centered structure but for the

body centered structure it will be out of phase with the 002 planes and will

be absent, shown in 4. Thus, the presence of the extra atom in the unit cell

at the center can cause a dierence in the XRD pattern of a material. This

same argument is true for a simple cubic and body centered cubic lattice.

Thus 100 reection is possible in the simple cubic lattice but not in the body

centered cubic lattice. To understand how intensities vary for the dierent

peaks we need to look at the interaction of x-rays with the crystal. This can

be understood by considering the interaction of x-ray with an electron, then

an atom (group of electrons since X-rays do not interact with the nucleus),

and nally a crystal (group of atoms with added periodicity).

2 Scattering by an electron

X-ray are electromagnetic radiation i.e. they have mutually perpendicular

electric and magnetic elds. Electrons are negatively charged particles that

3

MM3030: Materials Characterisation

Figure 4: Diraction from 001 and 002 orthorhombic planes. For the body

centered the 001 lines are absent. Taken from Elements of X-ray diraction

- B.D. Cullity.

are aected by these electric and magnetic elds. When X-rays interact with

electrons it causes it to oscillate. The oscillating electron will in turn emit

X-rays - this is called scattering. There are 2 kinds of scattering

1. Coherent scattering - emitted X-rays have the same wavelength

(same energy) as the incident X-rays. This is also called elastic scatter-

ing and the scattered radiation has a denite phase relation with the

incident X-rays.

2. Incoherent scattering - the X-rays lose some energy during scatter-

ing so that the nal energy is lower (wavelength is higher) than the

incident energy. There is no denite phase relation to the incident

radiation. This is also called inelastic scattering.

In the case of X-ray diraction we are interested in the elastic scattering com-

ponent. Any inelastic scattering will only add to the background. Another

component to the background is x-ray uorescence so the choice of the x-ray

source depends on the type of material (Cu is not normally used for Fe due

to strong x-ray uorescence). For elastic scattering the scattered radiation

is phase shifted from the incident beam by

2

or has a path dierence of

2

.

The scattering takes place in all directions but the intensity depends on the

angle of scattering. The expression for this is given by J.J. Thompson.

I

r

= I

0

e

4

r

2

m

2

c

4

sin

2

(1)

where, I

r

is the intensity at a distance r from the electron and is the

angle between the recoiling electron and the scattered x-ray. In the case of

diraction we want the intensity in terms of the angle between the incident

4

MM3030: Materials Characterisation

Figure 5: Coherent scattering of x-rays from a single electron. Taken from

Elements of X-ray diraction - B.D. Cullity.

and scattered radiation (2). This is given by (schematically shown in gure

5

I

r

= I

0

e

4

r

2

m

2

c

4

(1 +

cos

2

2

2

) (2)

This is the Thompson equation for the scattering of x-rays by a single elec-

tron. The intensity decreases as square of the distance from the electron.

Scattering is high in the forward or backward direction (2 = 0

or 180

).

The term (1 +

cos

2

2

2

) is called the polarization factor.

The x-ray can also undergo inelastic interaction with the electron. This is

called the Compton eect and is shown schematically in gure 6. Compton

scattering is usually observed for x-ray interaction with loosely bound elec-

trons in an atom i.e. the valence electrons. The X-rays lose energy to the

electron so that the nal wavelength is higher than the initial wavelength.

The change in wavelength is given by the scattering angle by

=

2

1

(1 cos2) (3)

The radiation obtained is called Compton modied radiation and there is

no phase relation with the incident radiation i.e. incoherent radiation. As

mentioned earlier, Compton scattering only adds to the background.

5

MM3030: Materials Characterisation

Figure 6: Compton eect - scattering of x-rays from a single electron with

loss of energy. Taken from Elements of X-ray diraction - B.D. Cullity.

3 Scattering by an atom

An atom consists of electrons (loosely and tightly bound) and a nucleus.

Nucleus is not involved in x-ray scattering since its extreme mass means that

x-ray dont have sucient energy to oscillate it and produce other x-rays. So

scattering by an atom refers to scattering by the electrons in the atom. One

simple way to think about this is that the scattering by all the individual

electrons of the atom add up so that the total scattering by the atom is

directly proportional to the atomic number (Z). Then, the total amplitude

is Z times the amplitude from one electron. This is true only for the forward

scattering direction (2 = 0) since the scattering from all the electrons are in

phase. For other directions this need not be true. For scattering of x-rays by

an atom, a scattering factor, f, is dened which is called atomic scattering

factor. This is given by

f =

amplitude of wave scattered by atom

amplitude of wave scattered by electron

Z (4)

For 2 = 0 f = Z, while it is lower for other angles. The scattering factor

also depends on the wavelength of the X-rays. For shorter wavelength, f is

lower since the path dierence will be higher with respect to the wavelength.

Typically, f is plotted as a function of angle and wavelength, as shown in

gure 7 for Cu. The maximum value is at 2 = 0 and is equal to 29 (atomic

number of Cu). Similar plots (or tables) are available for other elements.

The atomic scattering mentioned above is an example of coherent scattering

(Thompson scattering). There is also incoherent scattering from an atom

(Compton scattering), which increases as Z decreases. This is because with

decrease in atomic number the number of loosely bound electrons increases.

6

MM3030: Materials Characterisation

Figure 7: Atomic scattering factor for Cu. Taken from Elements of X-ray

diraction - B.D. Cullity.

7

MM3030: Materials Characterisation

Figure 8: X-ray interaction with matter. Taken from Elements of X-ray

diraction - B.D. Cullity.

So it is hard to get good x-ray intensities for the light elements since the

incoherent background is strong. The same is true for electron scattering as

well. Before we look at scattering from an unit cell, we can summarize x-ray

interaction with the electron and atom in gure 8.

4 Scattering by an unit cell

We started with one electron and them moved onto the atom, which was

considered as a group of electrons (as far as x-ray scattering is considered).

The next step is the unit cell. We can consider the unit cell as a group of

atoms arranged in a periodic fashion. Also we will focus only on the coherent

scattering since incoherent radiation will only add to the background. Given

that the atoms are arranged in a crystal with three dimensional periodicity x-

ray scattering only takes place at certain directions, diraction, which obeys

Braggs law. If Braggs law is not satised then there is no diraction and

hence no x-ray scattering. Thus, we only need to look at the x-ray intensity

in directions where Braggs law is satised and the intensity depends on the

types and positions of the atoms in the lattice. Also, we only have to consider

only one unit cell since the crystal is periodic.

Consider the one set of planes shown in gure 9. For simplicity let these

planes be of the form (h00) planes so that the d-spacing is equal to a\h.

This is from the denition of Miller indices where (hkl) gives the intercepts

of the planes with the axes. X-rays are incident on this plane at the Bragg

angle so that diraction condition is satised. Consider another set of atoms

located at position B, which is at a distance x from A. The path dierence

8

MM3030: Materials Characterisation

Figure 9: Eect of atom position on X-ray intensity. Taken from Elements

of X-ray diraction - B.D. Cullity.

between the x-rays reected from A and B is then given by (

AB

AC

) or (

x

a/h

).

This can be converted to phase dierence by multiplying with 2. Thus

the phase dierence is given by 2h

x

a

, which can be written as 2hu where

u represents the fractional coordinate for the atom at position B. We can

extend this argument to 3D for any general plane (hkl) with atoms located

at fractional coordinates (uvw). The total phase dierence is then given by

= 2(hu + kv + lw) (5)

This represents the phase dierence between x-rays reected from the unit

cell at dierent positions. Combining this with the atomic scattering factor

of the atoms located at the dierent positions we can dene a new term

called the structure factor, F. The structure factor with an atom located

at position (uvw) in an unit cell is given by

F = f exp 2i(hu + kv + lw) (6)

If there are N atoms in the unit cell and the n

th

atom has structure factor

f

n

and is located at (u

n

v

n

w

n

) then the structure factor for the unit cell, for

some plane (hkl) is given by

F =

N

n=1

f

n

exp 2i(hu

n

+ kv

n

+ lw

n

) (7)

9

MM3030: Materials Characterisation

Putting this in words the structure factor is given as

F =

amplitude of wave scattered by unit cell

amplitude of wave scattered by electron

(8)

This is an analogous denition to the atomic scattering factor from equation

4.

5 Structure factor with single atom basis

Using equation 7 it is possible to calculate the structure factor for a (hkl)

plane of an unit cell once the atom scattering factors and positions are known.

The structure factor is related to the intensity of the x-ray diracted from

that plane (there are other factors as well, which we will see below). Thus if

the structure factor for a given plane is zero then there will be no diracted

intensity, even though Braggs law is satised. Thus, Braggs law only decides

the 2 value for a given plane while structure factor decides the intensity.

5.1 Simple cubic

In a simple cubic unit cell there is only one atom per unit cell, located at

(000). So N = 1 and (uvw) is (000). So using equation 7 the structure factor

for a (hkl) plane simply becomes F

hkl

= f. Thus, for a simple cubic structure

diraction is possible for all possible planes since the structure factor is a

constant, equal to the atomic scattering factor. Thus, all planes can be seen

in the diraction pattern of a simple cubic structure. The intensities are still

not the same since there are other factors involved.

5.2 Body centered cubic

In a body centered cubic structure there are 2 atoms per unit cell, at (000)

and (

1

2

1

2

1

2

). These represent the fractional coordinates of the atoms in the

unit cell. substituting them in equation 7 we can get the expression for the

structure factor as

F

hkl

= f[1 + exp i(h + k + l)] (9)

From equation 9 it can be seen that when h+k+l is even (exp i(h + k + l))

is equal to 1 and when h + k + l is odd it is -1. So the structure factor is

h + k + l = even F = 2f

h + k + l = odd F = 0

(10)

10

MM3030: Materials Characterisation

Thus, diraction intensities are only found for specic hkl planes in bcc which

satisfy the condition in equation 10 i.e. h+k+l should be even. This can

be seen from gure 1 for bcc Fe. The rst line seen is (110) and not (100)

because of the rule in equation 10.

5.3 Face centered cubic

In the face centered cubic structure there are 4 atoms per unit cell, one at the

corner and 3 on the face centers. Once again using equation 7 the expression

for the structure factor simplies to

F

hkl

= f[1 + exp i(h + k) + exp i(k + l) + exp i(l + h)] (11)

The rules for diraction intensities for fcc is then

h, k, l all evenor all odd F = 4f

h, k, l mixed F = 0

(12)

Thus, for fcc structure diraction lines are seen for planes like (111), (200),

(220), (311), (222) where the indices are all even or odd. Other dirac-

tion lines are absent. The x-ray plot for Al in gure 2 conrm this rule.

5.4 Hexagonal close packed

In the case of the hcp structure, the fractional coordinates for the atoms are

(000) and (

1

3

2

3

1

2

). The equation for the structure factor then becomes

F

hkl

= f[1 + exp 2i(

h

3

+

2k

3

+

l

2

)] (13)

While this is a more complicated equation than the equations for fcc and

bcc, it is possible to derive rules for the values of (hkl) to obtain non zero

diraction intensities.

It is important to understand that the structure factor calculations do not

depend on the size and shape of the unit cell. The structure factor only

depends on the position and type of atoms in the unit cell. The

calculations derived above are for unit cells with only one type of atom. If

we have more than one type of atom then the atomic scattering factors are

also dierent and the structure factor rules are no longer valid.

11

MM3030: Materials Characterisation

6 Structure factor with multi-atom basis

For unit cells with more than one type of atom - compounds or intermetallics

the structure factor can be still calculated using equation 7 except that the

atomic scattering factor for each type of atom needs to be taken into account.

The consequence of this is that the intensities for some (hkl) planes will no

longer be zero but will have a nite value (since the f values are dierent).

To give and example consider the case of CsCl. This has a bcc structure

with the Cl

+

ion at the center of the unit cell.

Then the structure factor for this unit cell, using equation 7 is given by

F

h

kl = f

Cl

+ f

Cs

exp i(h + k + l) (14)

Using the same conditions for bcc the structure factor values are

h + k + l = even F = f

Cl

+ f

Cs

h + k + l = odd F = f

Cl

f

Cs

(15)

Thus, unlike a bcc unit cell with one atom basis, the intensity of the dirac-

tion line does not go to zero when h+k +l is odd but has a nite value (the

intensity will be low since it is proportional to the dierence of the atomic

scattering factors). Similarly, we can work out the structure factor for NaCl,

which has a fcc structure with a 2 atom basis Na at (000) and Cl at (

1

2

1

2

1

2

).

7 X-ray intensity

In the absence of all other factors the intensity of the diracted x-ray is equal

to the square of the structure factor. But there are a number of other factors

that aect the intensity.

7.1 Multiplicity factor

The multiplicity factor refers to the relative proportion of the planes con-

tributing to diraction. More the no. of planes greater is the intensity.

Compare diraction from the 100 and 111 set of planes of a cubic crystal.

The 100 family has 3 planes (100), (010), and (001) with the same d-spacing

(hence same 2) but dierent orientations. The 111 family has 4 planes

with the same d-spacing but dierent orientation - (111), (

111), (1

11), (11

1).

Thus, everything else being same, the ratio of the intensities from the 100

and 111 planes will be in the ratio of 3/4. Dierent planes have dierent mul-

tiplicity values, which are usually tabulated. The multiplicity factor depends

on the crystal structure since the planes must have the same d-spacing.

12

MM3030: Materials Characterisation

Figure 10: Lorentz-polarization factor as a function of Bragg angle. Taken

from Elements of X-ray diraction - B.D. Cullity.

7.2 Lorentz-polarization factor

The Lorentz factor is a trigonometric factor that relates to the distribution

of planes as a function of 2. For a powder sample, with randomly oriented

particles, the integrated intensity (area under the curve) of a reection at a

given Bragg angle depends on the no. of particles with that orientation. Even

though the particles are oriented at random this number is not a constant

but depends on the value of the Bragg angle. This dependence is called the

Lorentz factor and is given by

Lorentz factor =

1

4sin

2

cos

(16)

Usually, the Lorentz factor is combined with the polarization factor (seen in

the Thompson equation given in 2) to form the Lorentz-polarization factor.

Lorentz polarizationfactor =

1 + cos

2

2

sin

2

cos

(17)

The Lorentz-polarization factor as a function of Bragg angle is shown in

gure 10.

7.3 Absorption factor

The x-ray intensity also depends on the absorption of the specimen being

investigated. This also depends on the geometry of the setup. In the case

of the diractometer the absorption factor is independent of the Bragg angle

and does not aect the relative intensities of the dierent lines.

13

MM3030: Materials Characterisation

7.4 Temperature factor

Atoms in the lattice are constantly vibrating about their equilibrium posi-

tion. As the temperature increases, this vibration amplitude increases. One

eect of this vibration is that the lattice spacing constantly changes so that

the overall intensity of a line decreases with increasing temperature. At the

same time background scattering increases. For a given temperature the ef-

fect is pronounced at higher Bragg angles since the d-spacing is smaller. The

temperature eect is usually determined experimentally and written in the

form exp(2M).

Putting the various factors together the intensity of the x-ray diraction

line is given by

I = |F

2

|p(

1 + cos

2

2

sin

2

cos

) exp(2M) (18)

I here refers to the relative integrated intensity (area under the curve of

the diraction line), F is the structure factor for the (hkl) plane and p is

the multiplicity factor. The other factors are the Lorentz-polarization factor

and the temperature factor. The absorption factor is not included for the

relative intensities since it does not depend on Bragg angle. The intensity

given here assumes a random polycrystalline sample - powder or lm. If

there is any preferred orientation due to external conditions like growth or

stress than this equation is no longer valid. The ICDD (International Center

for Diraction Data) databases gives the d-spacing and the intensities of the

various diraction lines of a material. The intensities are given with respect

to the strongest line which has a value of 100. By comparing the experimental

ratios with the values given in the ICDD database it is possible to check if a

sample has a truly random orientation.

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