X-RAY DIFFRACTION

A lab report of an x-ray diffraction experiment

November 2 2020
Abstract

An x-ray diffraction experiment where theoretical knowledge is combined with equations in order to

identify unknown metals (using experimental data), determine silicon wafer orientation and draw

conclusions based on experimental x-ray diffraction data. Based on calculated crystal structure, metal 1

was found to be Iron and metal 2 was found to be Aluminum. The x-ray machine used Copper K-alpha

(Kα) radiation with wavelength 1.54 Angstroms and a copper target. A nickel filter was used.

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Contents
Abstract.......................................................................................................................................................1
Introduction.................................................................................................................................................3
Method........................................................................................................................................................4
Identification of unknown metals............................................................................................................4
Orientation of Si wafer............................................................................................................................5
Results.........................................................................................................................................................5
Graphs.....................................................................................................................................................5
Calculation Results...................................................................................................................................8
Discussion....................................................................................................................................................9
Sample Calculations...................................................................................................................................10

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Introduction

X-ray diffraction is an analytical technique in which x-rays (highly penetrative electromagnetic radiation)

of approximately one wavelength (monochromatic) are shot at a material. The x-rays are diffracted by

the crystal structure of the material and specific information about the crystal structure can be obtained

by measuring diffraction angles. X-rays are produced by phenomena followed by the rapid deceleration

of charged species (electrons). These electrons are usually produced from a filament and accelerated by

an extremely large voltage (about 30kV – 50kV) until they hit the target metal, causing the rapid

deceleration. There are many ways in which electrons may decelerate and this leads to many different

wavelengths of x-rays being generated. The result is a continuous spectrum of x-rays with a few

characteristic wavelengths with “peak” intensities. However, for diffraction, almost purely

monochromatic radiation is necessary. Therefore, a filter material is used to absorb some of the white

radiation but most importantly, to absorb most of the intensity of all characteristic peaks except one.

The peak with wavelength corresponding to Kα radiation. The result is a spectrum of x-rays that can be

considered to be monochromatic. A filter is made of another metal with certain absorption

characteristics such that it is able to selectively absorb radiation to increase the ratio of intensity of Kα

to all other radiation (i.e. make Kα the most intense and all other wavelengths negligible). In an x-ray

machine, a sample material is placed in the center of the machine and attacked by Kα radiation. There is

an x-ray source and an x-ray detector whose motion is synchronized and are placed opposite each other.

The detector starts at an angle of 0 degrees and keeps turning until it goes over 100 degrees. The

detector moves as the source moves so that any diffracted x-rays will be captured. A graph of intensity

against angle 2θ is plotted. This graph consists of certain peaks which correspond to atomic planes

which satisfy Bragg’s law. These peaks are characteristic for specific metal structures and therefore the

graphs can be used for identification. In this lab, experimental data from the explained x-ray diffraction

method is combined with theoretical knowledge such as Bragg’s Law and Structure Factor calculation in

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order to differentiate between two unknown metals, determine the orientation of a silicon wafer and

provide explanations for the data. The radiation used by the machine was Copper Kα radiation with

wavelength of 1.54 Angstroms. 2 main equations were used:

2 d sinθ=nλ

Bragg’s Law

Equation 1: The relationship between planar spacing (d), diffracted angle (θ) and wavelength (λ) that

must be satisfied in order to have diffraction peak

a
d=
√ h +k 2+l2
2

Equation 2: Relationship between planar spacing (d), lattice constant (a) and miller indices (h,k,l)

Method

Identification of unknown metals

There were two unknown metals placed in the x-ray diffraction machine, one at a time. The machine run

its course, as explained above, and the results were plotted electronically. The two possibilities for the

metals were Aluminum (FCC unit cell structure) and Iron (BCC unit cell structure). In order to

differentiate between the experimental data, it is necessary to know the positions of expected peaks for

each metal structure. This may be achieved using the structure factor (F). F can be thought of as a

formula which provides the different (hkl) peaks that Bragg’s Law is satisfied. For FCC, there will be

peaks if (hkl) are unmixed (numbers are either all even or all odd) only. Therefore the first 3 peaks will

show on (111), (200) and (220). For BCC there will be a peak only if (h+k+l) = even number. Therefore

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the first 3 peaks will be (110), (200) and (211). In order for a metal to be an FCC metal the ratio of planar

spacing for its 1st and 2nd peaks (d2/d1) should equal 0.866. For BCC (d2/d1) = 0.707.

The planar distances can be found using equation 1 since the wavelength of radiation (1.54 Angstroms)

is known and the angles are determined experimentally. The ratio for each metal was calculated and this

was used to identify the metals. Rearranging equation 2 in order to make a (lattice constant) the subject

was used to calculate the lattice constant values.

Orientation of Si wafer

The orientation of the silicon wafer was determined based on the theoretical fact that the diffraction

peak obtained from the wafer’s experiment with have a value parallel to the orientation of the wafer.

Comparing the peak to data for poly-crystaline Si x-ray diffraction, the (hkl) indices where determined

and its orientation was found.

Results

Graphs

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Figure 1: Copper Kα radiation diffracted intensity against angle (2θ) for unknown metal 1

Figure 2: Copper Kα radiation diffracted intensity against angle (2θ) for unknown metal 2

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Figure 3: Copper Kα radiation diffracted intensity against angle (2θ) for Silicon wafer

Figure 4: Copper Kα radiation diffracted intensity against angle (2θ) for Silicon powder

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Figure 5: Unfiltered Copper radiation diffracted intensity against angle (2θ) for silicon wafer

Calculation Results

Metal 1

d2/d1 = 0.698 ~ 0.7

Theoretically: BCC d2/d1 = 0.707 ~ 0.7

Therefore metal 1 is Iron (BCC)

First 3 peaks = (110), (200) and (211)

Lattice constant (a) = 2.903 Angstroms

Metal 2

d2/d1 = 0.871 ~ 0.87

Theoretically: FCC d2/d1 = 0.866 ~ 0.87

Therefore metal 2 is Aluminum (FCC)

First 3 peaks = (111), (200) and (220)

Lattice constant (a) = 4.041 Angstroms

Si wafer orientation

Diffraction data matches Si (400) plane. The (400) plane is parallel to the (100) direction since these two

vectors are scalar multiples. Therefore, the orientation is (100).

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Si wafer Kα and K-beta radiation

Since the filter was removed in Figure 5 there is no longer monochromatic. From theory, the larger the

wavelength of x-ray the larger the diffraction angle. Therefore the larger angle in Figure 5 corresponds

to Kα radiation.

Kα wavelength = 1.54 Angstroms and K-beta wavelength = 1.39 Angstroms

From Equation 1 d = λ(Kα) / 2*sinθ(Kα) = 1.54 / 2*sin(34.5) = 1.35 Angstroms

d = λ(K-beta) / 2*sinθ(K-beta) = 1.39 / 2*sin(31) = 1.35 Angstroms

Discussion

Using experimental data in conjunction with theoretical information about the planar spacing in both

FCC and BCC metals, the metal structures for both samples were determined. Calculation of structure

factors for FCC and BCC metals will allow determination of the (hkl) incides where peaks are expected to

occur. The orientation of the silicon wafer was determined by finding a parallel direction to the (hkl)

observed from experimental data since the plane is parallel to the orientation. Figure 3 and Figure 4

have very different graphs although the material in which the x-rays were passed through was silicon in

both cases. This is because silicon wafers (figure 3) are made from single crystal silicon and are therefore

aligned in one specific direction. The one peak present corresponds with that one specific direction.

Poly-crystalline silicon (figure 4) does not contain only one orientation. It shows the complete diffraction

pattern for silicon. In Figure 5, there are two diffraction peaks. This occurs because the filter initially

used for the x-rays was removed, allowing another characteristic radiation (K-beta) apart from Kα to be

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sent. The difference in wavelength of the two characteristic radiations causes the difference in angle of

the two peaks. However, as shown in the results, both peaks refer to the same plane.

Sample Calculations

Example with metal 1

Bragg’s Law example calculation (using 2θ = 44):

2dsinθ = nλ (where n=1)

d = λ / sinθ = 1.54 / 2*0.375 = 2.053 Angstroms

2θ (from graphs) Θ (2θ/2) sinθ d (using bragg’s law)

(Angstroms)
44 22 0.375 2.053
65 32.5 0.537 1.434
d2/d1 = 0.707 ~ 0.7

Lattice constant calculation (from Equation 2):

From structure factor 1st BCC peak is (110). Therefore d = 2.053 corresponds with (hkl) = (110)

a = sqrt(h2+k2+l2) * d = sqrt(2) * 2.053 = 2.903 Angstroms

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