X-Ray Diraction

David Sirajuddin
Nuclear Engineering & Radiological Sciences
February 8, 2007
Sirajuddin, David Lab 2 - X-Ray Diraction
Contents
1 Abstract 2
2 Introduction 2
3 Theory 3
3.1 X Rays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
3.2 Braggs Law . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
3.3 X-Ray Diractometry (XRD) . . . . . . . . . . . . . . . . . . . . . . . . . . 4
3.4 Reciprocal Space . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.5 Crystal Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.5.1 Face-Centered Cubic (FCC) . . . . . . . . . . . . . . . . . . . . . . . 9
3.5.2 Body-Centered Cubic (BCC) . . . . . . . . . . . . . . . . . . . . . . 10
3.5.3 Hexagonal Close-Packed (HCP) . . . . . . . . . . . . . . . . . . . . . 11
3.6 Diraction Pattern Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.6.1 Identifying K

and K

Peaks . . . . . . . . . . . . . . . . . . . . . . 11
3.6.2 Change of Variables and Curve Fitting . . . . . . . . . . . . . . . . . 12
3.7 Depth of Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.8 Density Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.9 Concentration of Substitutional Copper Imputurities in the Bulk Material . . 15
3.10 Error Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4 Procedure 16
5 Results and Analysis 17
5.1 Surface of Penny . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
5.1.1 Diraction Pattern Analysis . . . . . . . . . . . . . . . . . . . . . . . 17
5.1.2 Depth of Penetration . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.2 Bulk of Penny . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
6 Error Propagation 24
7 Summary and Conclusions 25
8 References 26
9 Appendix 27
9.1 Figures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
9.2 Data Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
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Sirajuddin, David Lab 2 - X-Ray Diraction
1 Abstract
The crystal structure of a United States one cent coin was investigated by X-ray Dirac-
tion. Due to the nonuniformity of the composition, two data sets were taken. Initially, the
surface of the penny was analyzed for angular values of 2 between 12 and 15 degrees. The
penny was then sanded down so as to expose the core material, and values of 2 between
10 and 60 degrees were examined. The resulting diraction patterns were used to determine
characteristic quantities of the lattice structure including the lattice type, lattice parameter,
interplanar spacing, number density, and the mass density. Additionally, these quantities
aided in labelling the crystallographic planes in regards to Miller indices on the diraction
pattern.
The data from the Copper surface indicated the material to Face-Centered Cubic (FCC).
Accuracy in the analysis of the diraction pattern was accomplished by a change of variables
from an angular dependence to a quantity s, dened to operate in reciprocal space. Each
peak was tted to a function using Kaleidagraph, and the centroid of each peak was found by
way of interpolation. Interplanar spacings for each peak were calculated from these centroid
values and used in the assignment of crystallographic plane indexing. Identifying the material
to be FCC, and discerning the appropriate {h,k,l} values allowed for a calculation of the
average lattice parameter. This value was found to be 3.622

A. Furthermore, a number
density of 8.419 10
22
atoms/cm
3
, and a mass density of 8.884 g/cm
3
was calculated. These
values were within one percent of those from literature.
The bulk material of the penny was also analyzed, and known to be composed of by
and large Zinc in a Hexagonal Close-Packed (HCP) structure. Crystallographic planes in
the diraction pattern were assigned by matching corresponding interplanar spacings with
given values of {h,k,l}. All peaks were identiable except ve. This discrepency was taken to
be due to the presence of susbtitutional Copper impurities. The number density of the bulk
material was found to be 1.9347 10
22
atoms/cm
3
, and the concentration of Copper impurity
in the material was calculated to be 3.729 atom percent. For both data sets, error was taken
into account for the centroid s of each peak, and the interplanar spacing d. The standard
deviations for both quantities calculated were found to generally be on the order of 10
4
-
10
3
. This error is minute, and it can be said that the error in the experimental procedure
did not substantially perturb the results. In all, there was a close agreement among theory,
literature, and experiment.
2 Introduction
The purpose of the experiment was to use X rays as a diagnostic tool to reveal key
parameters about the crystal structure. Motivated by the knowledge of the heterogeneity
in composition of the penny, two sets of data were conducted and analyzed: the surface of
the coin, and the core material (hereafter referred to as the bulk). In both data sets, the
penny was bombarded with X rays, and an analysis of the diraction pattern allowed for the
determination of various parameters relating to the specic crystal structure, such as the
lattice parameter, lattice type, and number density. The surface of the penny was taken to
be made of pure Copper, and was known to have a cubic type lattice. The crystallographic
2
Sirajuddin, David Lab 2 - X-Ray Diraction
planes were labelled according to the Miller indexing scheme, and the lattice parameter, and
both the mass and number densities were determined. The bulk material, presupposed to
be made of essentially Zinc and to have a hexagonal close-packed structure, was juxtaposed
to literature data for pure Zinc to aid in the labelling of the crystallographic planes in the
experimental data. Inconsistencies between the literature values and experiment were used
to pinpoint defects in the material, which were taken to be only substitutional impurities in
the form of copper atoms. The number densities of pure Zn with that of the bulk material
in the experiment were compared in order to estimate the percentage of copper impurities.
3 Theory
3.1 X Rays
X Rays are high frequency photons (30-30,000 PHz) emitted via electron transitions in
atoms. Due to their high frequency, and thusly high energy, X rays are highly penetrable
and are readily applicable to probing the microstructure of materials. Particularly of use,
is their low wavelength (10-0.01 nm), which can be utilized in tandem with Braggs Law
(Section 3.2) to construct diraction patterns that reveal key parameters of the crystalline
lattice structure of solids such as the structures lattice parameter, and its lattice type.
3.2 Braggs Law
Braggs law expresses the criterion needed for two beams to emerge after interaction
with constructive interference. The derivation is elementary, but it is instructive to present.
Without loss of generality, the expression can be formulated in two dimensions for the simple
case of two beams of common angles of incidence.
Figure 3.1 - Two X-ray beams deecting o of neighboring atomic planes. Beam travels a distance of
AB +BC farther than beam .
In order for constructive interference to occur, two waves must superimpose after their
deection to cause an increase in amplitude. This occurs only when two waves add that
are in phase with each other. It follows from Figure 3.1, that beam travels a distance of
AB + BC further than the beam . In order to stay in phase with each other, the distance
travelled by beam must be an integral multiple of the wavelength, such that:
3
Sirajuddin, David Lab 2 - X-Ray Diraction
n = AB + CD (1)
where denotes the wavelength of the beams, and n is an element of the integers. An
analysis of a triangle formed between the two atomic planes allows for the distance AB+BC
to be determined.
Figure 3.2 - A right triangle constructed involving the interplanar spacing d reveals the sidelength AB to
be equal to dsin. By inspection, AB = BC, yielding the total excess distance travelled by beam to be
simply 2AB = 2dsin.
Dening the distance between the two planes as the interplanar spacing d, the excess
distance travelled by beam can be formally recognized as simply:
AB + CD = 2dsin
Inputting this result into Eqn. (1) yields
n = 2dsin (2)
which is exactly that of Braggs Law. It is then apparent that the requisite for meeting
Braggs Law is dependent on the interplanar spacing, or equivalently, the orientation of the
planes with respect to the incident beams. For all intended purposes, the value of n can be
taken to be unity, so that Eqn. (2) takes the form
= 2dsin (3)
yielding the formulation of Braggs Law that is used throughout the analysis.
3.3 X-Ray Diractometry (XRD)
X-Ray Diractometry (XRD) involves the bombardment of a material with X rays of
a single wavelength. The wavelength is chosen so as to be on the order of the interatomic
spacing of the atoms that make up the crystal lattice in order to yield data with tractable
information. The apparatus operates on the principle of X-ray photon interactions with
4
Sirajuddin, David Lab 2 - X-Ray Diraction
the crystal lattice of the material. X rays interact with the lattice atoms and the scattered
photons are recorded by a counter situated at a certain angle with respect to the X-ray
emitter. The data gathered is used to construct a representative history of the X ray-material
interactions based upon the intensity of the counts called a diraction pattern. The resolution
of the spectrum will be highest with the incident X rays being as monochromatic as possible.
A polychromatic X-ray beam would yield too many peaks, hiding any information about the
crystal structure, and eliminate any usefulness of the experiment. These diraction patterns
reveal characteristic peaks of higher intensity at certain values of the angle of reection 2,
as per Figure 3.3. Physically, the angle 2 is the angle measured between the undiracted
path of the X ray to that of the diracted X ray being collected at receiving slit. It then
follows that, according to the setup, this angle is the angular value of 2 as described in the
discussion Braggs Law in section 3.2.
The apparatus used in the laboratory was an X-Ray Diractometer (Figure 3.3)
Figure 3.3 - Schematic of an X-ray diractometer [Ref. 3]
A powder sample is axed to the at plate in the center of the diractometer circle. X
rays are generated via an X-ray tube (Figure 3.4). A vacuum chamber containing a lament
is heated by way of passing a current through the lament which then thermionically emits
electrons. Electrons are accelerated in the vacuum tube, and are targeted at a Molybdenum
anode. The accelerated electrons contact the anode, and excite or knock o electrons from
the Molybdenum lattice sites. When these electrons decay, they emit characteristic X rays.
Most apparent are the K

and the K

emissions.
5
Sirajuddin, David Lab 2 - X-Ray Diraction
Figure 3.4 - Diagram of the X-ray tube used to generate X rays in a diractometry experiment [Ref. 3]
These X-ray photons enter the divergent slit and are incident on the target center. Upon
interacting with the material, certain diracted X rays are collected at the receiver slit,
situated at an angle 2 as identied by the graduated scale along the circumference of the
circle, and nally counted. The process is customarily automated, such that the X rays are
allowed to interact with the material at incremental angles of 2 for a xed amount of time,
both of which are speciable by the operator. The at plate is situated on a rotatable axis.
Also, the specimen and receiver slits are mechanically coupled so that for a rotation of the
counter by some angle 2x, the powder sample will rotate by an angle x. This adjustment
accounts for potential geometrical complications and any nonuniformities of interactions that
could incur from the X rays and the material. In this setup, the coupled joints allow for
the angle of reection to be equal to the angle of incidence, in accordance with Braggs Law
(Section 3.2).
The diraction pattern is constructed based upon the counts received and the respective
angle according to the diractometer. Coupling the specimen and the receiving slit provides
for the angle of incidence to be equal to the angle of reection. Only peaks that constructively
interfere, or equivalently stated, satisfy Braggs law (Eqn. 3) are counted. This idea is
illustrated in Figure 3.5.
Figure 3.5 - Two X-ray beams are depicted as interacting with the atomic planes of a crystal lattice. In
(a) the beam satises Braggs Law allowing for the outgoing beams to constructively interfere and be
counted by the detector, (b) The beam does not satisfy Braggs Law, the outgoing beams emerge out of
phase yielding destructive interference and are unable to be counted despite having the proper orientation
[adapted from Ref. 6].
Only X rays that undergo constructive interference, and those outgoing rays that are
oriented in the direction of the detector will be counted, as in Figure (3.5a). The depiction
on the right (Figure (3.5b) illustrates the idea of destructive interference not being counted
by the detector. Patterns are fashioned from the data collected, and upon analysis can
be used to discern information about the microstructure of the material.
Owing to its high penetrability, an X ray incident on a material sees a crystal lattice
consisting of regularly spaced atoms. Specically, the X ray sees planes of atoms in the mi-
crostructure of the material. The X-ray photons primarily interact with the bound electrons
of these atoms. Diraction results upon X-ray interaction with an atomic plane in a manner
6
Sirajuddin, David Lab 2 - X-Ray Diraction
that the incident X ray becomes modulated such that a redistribution of energy, and hence
intensity, of the X-ray wave occurs in a distinct manner by consequence of the interference
between X rays. The specimen used is a powder sample, a ne substrate composed of crys-
tal lattice structures oriented randomly. As the the apparatus is rotated so that the X rays
interact with dierent areas of the material, the photons necessarily interact with the atoms
of the lattice at dierent angles, and also interact with dierent atomic planes. By rotating
the components of the apparatus in this fashion, Braggs law will be periodically satised
whenever atomic planes are in the proper orientation. This variation creates more peaks so
that a diraction pattern is developed. Recalling that atoms in a lattice have essentially uni-
form spacing, the X-ray wave packets, or photons, counted by the detector are geometrically
characteristic of the structure of the material as the angle is varied.
The diraction pattern is formed as a result of X-ray photons reaching the detector. The
X rays can only reach the detector if the outgoing waves are directed towards the counter, and
also only if the wave has not been signicantly destructively interfered with. Characteristic
is the interactions between the respective outgoing waves. This interference can either reduce
or enhance the intensity peak recorded by way of destructive and constructive interference
respectively. Since the X rays primarily interact with the electrons, a higher probability of
interaction incurs in regions of higher electron densities. These regions of higher density occur
in the vicinity of the atoms in the lattice. Thus, if a material with regularly spaced atoms
in a crystal lattice is bombarded with X rays, the detector will record a characteristic X-ray
diraction pattern with sharp peaks of constructive interference that carries information
with the same symmetry as the distribution of atoms in the crystal lattice of the material.
From the diraction pattern, given that the wavelength of the emitted K

X ray is known,
a number of interplanar spacings can be calculated for identied values of 2 corresponding
to the observed K

peaks via Braggs law. This interplanar spacing d is xed, and can then
be used to calculate the angles of where the respective K

peaks should lie. This interplanar

spacing is presumed to be constant and a corresponding angle 2 can be found using the value
of d calculated from the preliminary analysis done using peaks granted the wavelength of
the K

emissions is used in Eqn. (3). In practice, the pattern will appear with signicant
background radiation superimposed upon the shark peaks. This background consists of
a Bremsstrahlung emission continuum resulting from the X-ray photons decelerating upon
interaction with the material. Dierent materials are composed of dierent phases and atoms
giving rise to a dierent diraction pattern due to their dierent atomic spacings, electron
densities, and lattice structures. Extracting information from the diraction patterns about
the symmetry of the distribution of atoms, identifying the lattice type, and discerning key
parameters about the lattice structure is the basis for X-ray Diractometry.
3.4 Reciprocal Space
The X rays interact with electrons in the crystal lattice structure. Thus, the diraction
pattern yielded is a reection of the symmetry of the electron density in the structure of the
material. Given the symmetry of the lattice, it follows that the electron density is periodical
in 3-dimensional space. This density depends on the electrons per atom, the binding type,
and also the lattice structure. The periodicity of the electron density function n(r) suggests
that it can be expanded in the form of a Fourier series, such that
7
Sirajuddin, David Lab 2 - X-Ray Diraction
n(r) =

G
n

G
e
i(

Gr)
(4)
where

G is a Reciprocal Lattice Vector (RLV), r is a lattice point position vector , and
n

G
are the coecients in the Fourier expansion.
The lattice is then dened in terms of reciprocal space. The electron density function of
Eqn. (4) allows for an extractable denition of a reciprocal lattice. The reciprocal lattice can
be thought of as the set of all vectors

G such that e
i

Gr
= 1. Alternatively, this corresponding
reciprocal space lattice can be envisaged as the set of imaginary points constructed so that
the direction of an arbitrary vector coincides with the direction of a normal to the real space
planes and the magnitude of that vector is equal to the reciprocal of the real interplanar
spacing d.
The vector

G is formulated as a set of volume normalized primitive vectors of real space,
such that

G can be expressed in the general form of

G = h

A + k

B + l

C, (5)
where

A,

B, and

C are the previously described primitive vectors, now operating in
reciprocal lattice. The magnitude of the reciprocal lattice vector |

G| is customarily dened
as the product of the reciprocal of the interplanar spacing d and 2, i.e. |

G| = 2/d. This
factor of 2 changes the units of

G from inverse length, to radians per unit length. This
adjustment helps to make a direct comparison among

G and the wave vector

k = 2/ of
either the incident, or outgoing X ray.
For a cubic structure, the interplanar spacing can be explicitly represented, and an ex-
pression for |

G| can be arrived at in the following fashion:

|

G| =
2
d
|

G| =
2
a

h
2
+ k
2
+ l
2
(6)
where h, k, and l denote the integral multiples of unit vectors dening the lattice. An-
other convenient quantity used to describe in analog with the reciprocal lattice vector

G is
the structure factor S

G
, which describes the manner in which radiation scatters o of the
structure.
S

G
=

j
f
j
e
i(

k r
j
)
(7)
where j represents the j
th
atom, f
j
is each atoms form factor (a property of the atom type,
and independent of its position in the lattice), r
j
is the position of the j
th
atom in the lattice,
and

k is the dierence between the wave vectors before and after interaction. That is to say,
8
Sirajuddin, David Lab 2 - X-Ray Diraction

k =

k

k, such that

k and

k

are the wave vectors of the incident and outgoing radiation

respectively. It can be shown that the condition for constructive interference demands that
this vector |

k| = |

G| =
4

sin, which is identical to the quantity s, used in the change of

variables of Section 3.6.2.
The above expression can be expressed more explicitly if a general reciprocal lattice vector
(Eqn. (5)) is considered, along with a general position vector r
j
. Under this representation,
the dot product

k r
j
in the exponential of Eqn. (7) can be expressed as

k r
j
= 2(hx
j
+ ky
j
+ lz
j
) (8)
where a factor of 2 has been factored out of the notation, and the constants have been
consolidated.
Using this explicit representation, the structure factor of Eqn. (7) can be revaluated as
S

G
=

i
f
j
e
2i(hx
j
+ky
j
+lz
j
)
(9)
Dierent lattice types will hold dierent structure factors. It is then immediately recog-
nizable that the structure factor can be used to determine the lattice type.
3.5 Crystal Structure
The atoms in material solids are arranged in a unique geometry according to its crystal
structure. A crystal structure is comprised of three dimensionally tesselated unit cells, or
lattice structures. The unit cells are comprised of one or more atoms arranged in space,
such that translational operators applied to the basis can accomplish the mathematical
tesselation. A unit cell holds a characteristic length known as the lattice parameter a. These
measurements dier depending on the type of lattice, and the lattices constituent atoms.
In this experiment, three types of lattices were of relevance: Face-Centered Cubic, Body-
Centered Cubic, and Hexagonal-Close Packed.
3.5.1 Face-Centered Cubic (FCC)
The Face-Centered Cubic lattice structure contains 4 atoms in one unit cell (Figure 3.6).
An atom is located at each of the vertices of the cube, and one is placed in the center of
each of the faces. These atoms are situated in the unit cell such that only 1/8 of an atom is
actually contained within the unit cell at each of the vertices, and only 1/2 of the atom is
contained on each of the faces.
Figure 3.6 - A diagram of the face-centered cubic unit cell. [Ref. 6]
9
Sirajuddin, David Lab 2 - X-Ray Diraction
Mathematically, an origin can be placed at the center of the cube, r
0
=

0, with atoms
placed at r
1
= (a/2)( x + y), r
2
= (a/2)( y + z), r
3
= (a/2)( x + z), where a is the lattice
parameter of the cell. Noting that the form factor f
j
is only dependent on the type of atom,
it follows that for a monatomic lattice, all of the form factors f
j
are identical (f
j
= f for
all j). Inputting this into the structure factor formulation of Eqn. (9), yields the following
result:
S

G
= f
_
e
i

0
+ e
i

G(a/2)( x+ y)
+ e
i

G(a/2)( y+ z)
+ e
i

G(a/2)( x+ z)
_
= f
_
1 + (1)
h+k
+ (1)
k+l
+ (1)
h+l
_
it follows from elementary number theory that any two even or odd integers will yield an
even sum, and any mixed parity will yield an odd number, giving way to the general result:
S

G
=
_
4f if h, k, l are all even or odd
0 if h, k, l are of mixed parity
Thus, if the values of a set of indices h, k, l are known, whether or not these correspond to
FCC can be ascertained from a simple crosscheck between the indices and the above result.
3.5.2 Body-Centered Cubic (BCC)
The body centered cubic has 2 atoms in the unit cell, one located at the unit cells center,
and an atom is located at each of the vertices. The entirety of the atom is located at the
center, and 1/8 of the atoms on the vertices are contained within the cell giving way to a
total of 2 atoms per unit cell in a BCC structure.
Figure 3.7 - A diagram of the body-centered cubic unit cell [Ref. 6]
Mathematically, if the origin is located at the center, r
0
=

0, then this describes the
location of the center atom, and r
1
= (a/2)( x + y + z), where a is the lattice parameter of
the unit cell. A similar treatment, as per the FCC analysis, of the structure factor yields
the result:
S

G
=
_
2f if h + k + l is even
0 if h + k + l is odd
The dierences between the conditions for the integral multiples h, k, and l in regards to
the structure factor S

G
in both cubic structures allow for lattice structure to be characterized
based upon whichever set of indices is consistent. That is the say, both cubic lattices have a
10
Sirajuddin, David Lab 2 - X-Ray Diraction
constant lattice parameter a, which is related to the interplanar spacing d and the indices h,
k, and l via Eqn. (9). Deducing the structure of the material by analysis of the diraction
pattern can be accomplished by selecting the appropriate values of h, k, ad l that allow for
the lattice parameter to remain constant. Upon nding the proper set of values of h, k, l,
the structure can be discerned from a juxtaposition of the indices with each lattices criteria
for the structure factor.
3.5.3 Hexagonal Close-Packed (HCP)
The Hexagonal Close-Packed (HCP) unit cell contains 6 atoms situated as shown in
Figure 3.8.
Figure 3.8 - A diagram of the hexagonal closely packed unit cell [Ref. 6]
The structure consists of six triangular prisms conjoined so as to form a hexagonal prism.
The characteristic lengths associated with the HCP structure include its height c, and the
side length of the basal triangles is the its lattice parameter a. The triangles that compose
the bases of the hexagonal prism are equilateral of length a. Thus, all that need be known to
calculate the volume of the cell is the height c, and the side length a. Deriving an expression
for the volume V
HCP
of the HCP unit cell is elementary, and thusly not shown in this report;
however, the equation that results is simply:
V
HCP
= 6

3
4
a
2
c (10)
3.6 Diraction Pattern Analysis
The general methods described above are now explicitly represented.
3.6.1 Identifying K

and K

Peaks
It is apparent that whether the analysis of the pattern is done with exclusively the K

or
the K

peaks is completely arbitrary (as both will yield the same information of the crystal
structure). However, an observation of the diraction pattern reveals that the K

peaks
are much more visible due to their higher amplitudes. Thus, it is more reliable to analyze
the pattern based upon these peaks rather than the lower amplitude K

peaks (which can

often be hidden amidst the background noise of the spectrum). It is important to analyze
11
Sirajuddin, David Lab 2 - X-Ray Diraction
either only the , or only the peaks. Examining both would be redundant, and analyzing
a mix of the two would give untrue information about the symmetry of the lattice. It is
then necessary to distinguish these K

peaks from the K

peaks on the spectrum from one

another for a consistent analysis of only the K

peaks. This is done in a two step process.

As a rst step, the K

peaks can be identied by inspection of the diraction pattern.

The angle 2 is denoted, and the interplanar spacing d is calculated via Braggs Law (Eqn.
(4)):
d =

K
2sin
(11)
Where
K
is the characteristic wavelength the K

The interplanar spacing is a constant,

and should remain the same whether the or peaks are used. Thus, after arriving at a
value for d, the angle 2
K

can be calculated for the emission, if

K

is used in Eqn. (4):

2
K

= 2sin
1
_

2d
_
(12)
The second step involves a cross-checking of peaks. Since the identication of the K

peaks was done by inspection, it is necessary to see if any of the K

peaks previously
identied are in fact K

peaks. Should this be the case for any peak, it should be

removed from further analysis to ensure consistent calculations throughout. Once the K

peaks have been assigned, the K

peaks can then be discarded as the remainder of the

analysis will be conducted on the K

peaks.
3.6.2 Change of Variables and Curve Fitting
In order to ease the analysis, a change of variables is introduced. The quantity s is used
instead of the angular dependence, where
s = |

k| = (4/)sin (13)
and has units of inverse length. The quantity s is dened to operate in reciprocal space.
As noted in Section 3.4, the condition for constructive interference yields an equivalence
between a corresponding s value to the reciprocal lattice vector

G. Thus, given an angular
value 2 that corresponds to the centroid of a K

1
peak on the diraction pattern, Eqn. (11)
can be rewritten in terms of the quantity s, such that
d =
2
s
(14)
In order to locate this centroid, a function I(s) is tted to each peak. This function is
plotted atop of the data points, and a centroid value can be interpolated from the function.
The function I(s) used for the tting is of the form:
12
Sirajuddin, David Lab 2 - X-Ray Diraction
I(s) = As + B + c(2f
s
1
,s
(s) + f
s
2
,s
(s)) (15)
where
f
s
i
,s
(s) = exp
_

1
2
_
s s
i
s
_
2
_
and A, B, c, s
i
, s are constants. The former part of Eqn. (5) is a linear approximation
of the background noise, c is a constant that modulates the height Gaussian peak, s is
the Full Width at Half Maximum (FWHM) of the peak, s
i
is the moment center of the ith
peak, where i can either be K

1
or K

2
. The factor of two is introduced as a multiplicative
factor appended to the Gaussian approximation of the peak corresponding to the K

1
X-ray
interaction due to its tendency to be approximately twice the amplitude of the K

2
peak.
Another reason for the change of variables is that the quantities s
1
and s
2
have a xed
relationship, and an expression can therefore be formulated to constrain the t even further.
By invoking Braggs law and recognizing that the interplanar spacing d is the same for a
given pair of K

1
and K

2
peaks, relation between the two s values can be arrived at (Ref.
2):
s
2
= s
1
(
K
1
/
K
2
) (16)
The above relation reduces the number of tting parameters in the function I(s) of Eqn.
(15).
3.7 Depth of Material
In order to nd the estimated depth of the material being probed, it is necessary to
discern how penetrating the X ray is with respect to the interacting medium. The surface of
the penny is considered for this calculation, and is presumed to be made of pure Cu-29. The
X rays are taken to be targeted at the material as a collimated beam with a nite diameter.
A one-dimensional treatment of the scenario is both a good approximation, and does not
cause a loss of generality in the result. The intensity I of the beam through the material
can be modeled as a dierential equation to nd an expression for the mass attenuation
coecient . Specically,
dI
dx
= I
where x is a spatial coordinate along the path of the X-ray beam. The negative sign
follows from the derivative on the LHS of the equation
dI
dx
< 0. The equation is routinely
solved to yield:
I(x) = I
0
e
x
(17)
13
Sirajuddin, David Lab 2 - X-Ray Diraction
where I
0
is the intensity before interaction with the material. Thus, the attenuation
with increasing distance x along the path of the X-ray beam is explicitly represented in
Eqn. (17). The above equation provides the mass attenuation coecient , which provides
all the information needed to estimate the depth of the material. Since the distribution is
exponential, the mean of the distribution is simply the reciprocal of the mass attenuation
coecient, which is physically recognized as the mean free path of an X ray in the material.
Mass attenuation coecients are tabulated in literature with respect to incident photon
energy, and the medium of interaction. The energy of the incident X-ray photon can be
found by the usual idea of quantized energies:
E = h
E =
hc

(18)
where and are the linear frequency and wavelength of the photon respectively. The
incident energy can thusly be extracted from this formulation, and the mass attenuation
coecient can thereafter be found from literature.
After acquiring the mass attenuation coecient, there is still a matter to decipher how
the incident depth of the material varies as a function of the incident angle. Figure 3.9
provides an illustration of the process.
Figure 3.9 - An X ray is incident on a copper medium at an arbitrary angle . The average distance the
X ray is expected to travel is equal to the mean free path = 1/. The depth D is a function of angle with a
magnitude of D = (1/)sin()
If an X-ray photon of a given energy is incident on a material at an arbitrary angle, it
can be expected to travel approximately its mean free path (i.e. 1/). Thus, the relationship
between the depth D and the angle is quickly deduced as simply:
d() = (1/)sin()
As per the laboratory instructions, in order to plot the depth D as a function of 2, all
that need be done is to multiply the argument by a form of one (i.e. 2/2):
14
Sirajuddin, David Lab 2 - X-Ray Diraction
d(2) = (1/)sin(
2
2
) (19)
Thus, the depth of penetration is proportional to the sine of the angle of incidence.
3.8 Density Calculations
The number density N has units of atoms per unit volume. Since this quantity is nor-
malized by the volume, any arbitrary volume can be used. It is convenient to consider a unit
cell. The density can then be expressed mathematically as:
N =
_

V
_
cell
(20)
where and V are the number of atoms and volume of the unit cell respectively. The
volume of the FCC and BCC is simply the lattice parameter cubed (V
FCC
= V
BCC
= a
3
),
and the volume of the HCP was given in Eqn. (16).
The mass density has units of mass per unit volume, and is given by the following
expression:
=
NA
N
A
(21)
Here, A is the molecular mass in units of grams per mol, and N
A
is Avogadros number.
3.9 Concentration of Substitutional Copper Imputurities in the
Bulk Material
An X-ray diraction analysis of the bulk material necessarily incurs indicative character-
istics of the bulk being composed of not entirely Zn. The dierence manifests itself in slightly
dierent density values, and unidentiable peaks in the diraction pattern. It is presumed
in this experiment, that any dierence can be attributed to substitutional impurities in the
form of Copper in the HCP lattice of the bulk material. Assuming that the Cu atoms are
only substitutionally arranged in the lattice, an impurity concentration can be calculated
if the assumption is also enforced that the measured atomic volume is a weighted average
of the atomic volumes of Cu and Zn in pure elements. Because the atomic volume is a
quantity involving the densities of the material, and the bulk materials actual density is
unknown, it is approximated that the atomic volume is directly proportional to the number
densities computed. This assumption is only valid so long as this is true, and also that the
number density of Cu (found in pure element form as only a cubic lattice) does not change
signicantly when incorporating its eect on an HCP lattice. The impurity concentration
can be formulated as follows:
15
Sirajuddin, David Lab 2 - X-Ray Diraction
N
b
= (1 )N
Zn
+ N
Cu
=
N
b
N
Zn
N
Cu
N
Zn
(22)
where N
b
, N
Zn
, and N
Cu
are the number densities of the bulk material, Zinc, and Copper
respectively.
3.10 Error Analysis
The error attributed to the experiment came only from the value of the centroid s.
This error,
s
was indicated among the tting parameters outputted by Kaleidagraph when
each peak was analyzed. Subsequent error was propagated in only the calculation of the
interplanar spacing d, where
d =
2
s
A simple quadrature can be performed to account for the error in d,
d
, such that
_

d
d
_
2
=
_

2
2
_
2
+
_

s
s
_
2
(23)
Noting that the variance of a constant is zero, the factor of 2 can be removed from Eqn.
(24) to yield the following:
_

d
d
_
2
=
_

s
s
_
2
_

d
d
_
=
_

s
s
_

d
=
d
s

s
(24)
where
s
is supplied by Kaleidagraph. These errors are listed among the tting parame-
ters in the Appendix. The ratio d/s is approximately equal to unity in the majority of the
tabulated values, thus, this factor does not change the error signicantly. The errors of the
quantities s and d are both small.
4 Procedure
Material properties of a penny were investigated by performing XRD analysis on the
pennys surface and bulk material. A powder specimen was placed on the xed plate in
the X-ray diractometer as per Figure 3.3, and an automated diraction experiment was
conducted.
16
Sirajuddin, David Lab 2 - X-Ray Diraction
The penny surface examined angular values of 2[12, 55] degrees in increments of 0.05
degrees. Diraction was analyzed at each angle for 10 seconds, yielding a total experiment
time of 8600 s, or approximately 2.38 hours.
The penny was then sanded down to the core in order to probe the bulk material, and
placed in the apparatus. Values of 2[10, 60] degrees were sampled in 0.05 degrees increments
at a sampling time of 30 seconds per increment for a total duration of experiment at 30000 s,
or approximately 8.33 hours. The above listed parameters for the experiment are summarized
in Table 4.1, and the detection circuitry involved is included in the generic block diagram of
Figure 4.1.
Specimen Initial Angle Final Angle Step Size Time/Sample Total Duration
Center 10 60 0.05 30 2.38
Surface 12 55 0.05 30 8.33
Table 4.1 - Experimental parameters for the XRD of the surface and center of the penny are summarized.
Figure 4.1 - Block diagram of signal chain for pulse counting of X rays.
Subsequent analysis of the diraction patterns was conducted, in accordance with the
Theory section.
5 Results and Analysis
5.1 Surface of Penny
5.1.1 Diraction Pattern Analysis
The diraction experiment produced a data set that recorded the intensity at respective
values of the angle 2. The raw data was plotted as intensity versus the angle 2 (attached
in the Appendix), and also with respect to the quantity s. The K

peaks were isolated from

the K

peaks for later analysis by the procedure prescribed in Section 3.6.1. Kaleidagraph
was then used to t the K

peaks to function I(s) as per Eqn. (15) in Section 3.6.2. Two

representative plots along with the tted function is shown in Figure 5.1.
17
Sirajuddin, David Lab 2 - X-Ray Diraction
Figure 5.1 - Representative plots with corresponding ts to the rst two peaks in the X-ray diraction
pattern of the surface of the penny. (a) corresponds to a centroid value of s = 2.993

A
1
, and (b)
corresponds to s = 3.4593

A
1
The tting parameters for all peaks tted in Kaleidagraph can be found in the Appendix.
The centroid values were found from the tted function of each of the peaks, and a corre-
sponding interplanar spacing d was calculated using Eqn. (14). These parameters are given
in Table 5.1. From these interplanar spacings, the lattice type was deduced from two sets
of given candidate values of the indices h,k,l corresponding to either FCC or BCC lattices.
Recognizing that the reciprocal lattice vector |

G| s = (4/)sin for the case of construc-

tive interference, the use of the indices {h,k,l} can be used in accordance with Eqn. (6) to
yield the general result for a cubic lattice:
a = d

h
2
+ k
2
+ l
2
(25)
The above equation was then used to nd the corresponding lattice parameter a for each
peak given the candidate values {h,k,l}. Upon subsequent calculations, the results indicated
an approximately constant value of the lattice parameter for the candidate values of {h,k,l}
for the FCC lattice, indicating that the surface was indeed an FCC structure. A table
summarizing calculated values of the interplanar spacing, lattice parameter is shown in Table
5.1 along with their Miller indexing assignments. The comparison to the values found for
the corresponding BCC values for {h,k,l} are attached in the Appendix. Only the rst ve
candidate indices of {h,k,l} of Table 5.1 were given; however, using the criteria prescribed
the Theory Section 3.4 relating to the structure factor, the remainder of the {h,k,l} values
were able to be deduced based whether the determined indices yielded a constant lattice
parameter. All calculated values are displayed in Table 5.1.
18
Sirajuddin, David Lab 2 - X-Ray Diraction
K

peak centroid (

A
1
) Interplanar spacing d (

A) Lattice parameter a (

A) (hkl)
2.9923 2.0998 3.6367 111
3.4593 1.8163 3.6326 200
4.9053 1.2809 3.6229 220
5.7538 1.0920 3.6218 311
6.0114 1.0452 3.6207 222
6.9406 0.9053 3.6212 400
7.7649 0.8092 3.6189 331
7.8058 0.8049 3.5990 420
Table 5.1 - K

peaks identied by their centroid s, and the corresponding calculated values of the
interplanar spacings, lattice parameter and Miller index assignments. The values of {h,k,l} imply an FCC
crystal structure for the surface of the penny.
With the peaks assigned, the diraction pattern was labeled, and is shown in Figure 5.2.
Figure 5.2 - Labelled diraction pattern for the surface of the penny plotted with respect to s.
All of the K

peaks were identiable. Approximately half of the calculated K

peaks
were not resolvable above the background noise of the spectrum. This information is given
in Table 9.1.
From the lattice parameters of Table 5.2, an arithmetic mean of the lattice parameter was
computed to arrive at an average lattice parameter a. A unit cell volume was computed, and
the number and mass densities were calculated as per Eqns. (20)-(22), using the atomic mass
A = 63.546 g mol
1
[Ref. 5]. The results are given in Table 5.2, along with a comparison
to literature values for pure Cu.
19
Sirajuddin, David Lab 2 - X-Ray Diraction
Average lattice parameter a Number density N (cm
3
) Density (g cm
3
)
Surface 3.622 8.419 10
22
8.884
Pure Cu 3.610 8.502 10
22
8.900
Percent Dierence 0.3269 0.9762 0.1798
Table 5.2 - Experimental values for the lattice parameter, and the number and mass densities are
compared to literature values at STP. [Ref. x, lennentech, webelements, nrl]
All the experimental values all hold less than 1% error in regards to the literature values.
These dierences are minute, and could be a reection on an inherent innaccuracy of the
X-ray Diractometer; however, more likely is just the presence of defects within the material.
Since the coin used in lab has necessarily aged and been weathered, also due to the coin being
made not entirely of pure copper reects the possibility of vacancies, voids, susbtitutional
impurities, etc. within the material that could alter the densities. The defects can create
localized regions of stress giving rise to a small change in the lattice parameter.
5.1.2 Depth of Penetration
The depth of penetration was plotted as per Theory Section 3.7. The CRC Handbook of
Chemistry and Physics was consulted for the mass attenuation coecient values (given in
terms of mass attenuation coecient per density of incident material). The energy calcula-
tion using Eqn. (9) yielded an incident photon energy of 17.516 keV. The values listed in
the CRC Handbook of Chemistry and Physics did not list a value for this specic energy.
Four values were taken in the vicinity of the this energy, and tted to a power function.
The function was used to nd the mass attenuation coecient corresponding to the incident
X-ray photon energy. The tted plot is given in Figure 5.3.
Figure 5.3 - Mass attenuation coecient per density of incident material is plotted versus photon energy,
and t to a function in order to interpolate for the proper coecient corresponding to an energy of 17.516
keV.
20
Sirajuddin, David Lab 2 - X-Ray Diraction
Using the density of copper (Ref. x), a mass attenuation coecient was found, and a
corresponding mean free path to be 2.071 10
3
cm. Using this value, a plot was made of
the depth of penetration into the material versus the angle 2.
Figure 5.4 - Mass attenuation coecient per density of incident material is plotted versus photon energy,
and t to a function in order to interpolate for the proper coecient corresponding to an energy of 17.516
keV.
The plot intuitively exhibits sinusoidal character. The lesser degree to which this is
present is due to the limited range of angles in the plot. The depth of penetration is shown
to increase with increasing angle, and can be expected to reach a maximum when the photon
is normally indicident on a material.
5.2 Bulk of Penny
The penny was sanded down so as to expose the bulk material in the X-ray diratometry
experiment. The procedure was essentially the same as for the surface of the penny. The
K

peaks were identied, and tted to an equation of the form of Eqn. (x). This t was
used to determine the centroid, which was then used to calculate interplanar spacings. Two
represenatitive peaks are shown in Figure 5.5.
21
Sirajuddin, David Lab 2 - X-Ray Diraction
Figure 5.5 - The rst two peaks in the X-ray diraction pattern of the bulk material along with their
corresponding tted functions are shown.
Fitting parameters are attached in the Appendix. Because of the more complex structure,
a direct methodology for determining the indices {h,k,l} was not utilized. Instead, a data
set consisting of labeled peaks with corresponding interplanar spacings d
lit
from literature
was compared to the experimental calculations for the interplanar spacings d
exp
. In this
fashion, the indices were assigned to the experimental peaks. All peaks that were unable
to be assigned were presumed to be due to substitutional impurities in the form of Copper.
The analysis is summated in Table 5.3.
22
Sirajuddin, David Lab 2 - X-Ray Diraction
Centroid s (

A
1
) d
exp
(

A) d
lit
(

A) (hkl)
2.5474 2.467 2.473 002
2.7171 2.313 2.307 100
3.0027 2.093
3.7283 1.685 1.687 102
4.204 1.347 1.332 110
5.0384 1.247 1.236 004
5.3585 1.173 1.173 112
5.4421 1.154 1.153 200
5.5897 1.124
5.6242 1.117
5.7806 1.087 1.090 104
6.0172 1.0442 1.045 202
6.6517 0.9446
6.9408 0.9053 0.906 114
7.3112 0.8594 0.872 210
8.1545 0.7705
Table 5.3 - Experimental values of the interplanar spacing were compared with pre-indexed K

peaks
with corresponding interplanar spacings. The Miller indexing was done for all peaks that matched the
data, all other peaks are taken to be due to substitutional impurities.
A plot of the Intensity as a function of the quantity s was labeled, and shown in Figure
5.6.
Figure 5.6 - A plot is shown of the X-ray diraction pattern of the bulk material in a penny with Miller
indexing assignments.
23
Sirajuddin, David Lab 2 - X-Ray Diraction
It is evident that the structure in the pennys bulk material is dierent than that of pure
Zn. To quantify this, the Cu concentration was assessed under the assumption that the
experimental atomic volume is a weighted average of the atomic volumes of Cu and Zn as
pure elements. For the experimental data, the volume of the HCP lattice is computed via
Eqn. (10). The height c is identied as 2d(002)
exp
, and the lattice parameter can be extracted
from the length d(110)
exp
, which is realized as the altitude of each of the basal triangles in
the structure. Simple trigonometric analysis yields the lattice parameter a = 2dtan

6
. Thus,
inputting these results into Eqn. (x), the volume of the HCP lattice was found. Because
the actual density of the bulk material was not known, an approximation was enforced such
that the number densities of the materials were directly proportional to the atomic volumes.
Furthermore, it is noted that Copper is found as a pure element in a cubic lattice, and
thus the approximation is only valid if the number density does not dier signifantly. The
experiment indicated a bulk number density of 1.9347 10
23
atoms/cm
3
. The number density
of copper was found from the previous section to be 8.419 10
22
atoms/cm
3
, and literature
values indicated that the number density of Zn is 9.16 10
22
atoms/cm
3
. Using these values,
in accordance with Eqn. (x), it was found that there is approximately 3.729 atom percent
copper in the Bulk material.
6 Error Propagation
The standard deviation in the centroid s is listed in Table 9.4, and Table 9.5. The
error the calculation of the interplanar spacing d was found via Eqn. (24), and yielded the
following standard deviations.
K

peak centroid (

A
1
) Interplanar spacing d (

A) Standard deviation in d (

A) x 10
3
2.9923 2.0998 39.28
3.4593 1.8163 37.45
4.9053 1.2809 6.210
5.7538 1.0920 1.206
6.0114 1.0452 1.952
6.9406 0.9053 86.82
7.7649 0.8092 9.206
Table 6.1 - Error values for the calculations of the surface values for the interplanar spacing d.
24
Sirajuddin, David Lab 2 - X-Ray Diraction
Centroid s (

A
1
) d
exp
(

A) Standard deviation in d
exp
(

A) x 10
4
2.5474 2.467 3.934e-4
2.7171 2.313 5.746e-4
3.0027 2.093 2.238e-4
3.7283 1.685 6.317e-5
4.204 1.347 1.029e-4
5.3585 1.173 4.549e-5
5.4421 1.154 6.613e-5
5.5897 1.124 4.836e-5
5.6242 1.117 1.249e-4
5.7806 1.087 6.445e-5
6.0172 1.0442 3.099e-4
6.6517 0.9446 4.432e-5
6.9408 0.9053 5.800e-5
7.3112 0.8594 4.461e-5
8.1545 0.7705 6.136e-5
Table 6.2 - Error values for the calculations of the bulk values for the interplanar spacing d.
In both the bulk material and the surface, the error was found to be small.
7 Summary and Conclusions
X-ray Diraction was used to probe the crystal structure of a penny. The analysis
allowed for an identication of the lattice type, assignment of Miller indices to the peaks in
the diraction patternf, and calculation of the lattice parameter, and both the number and
mass densities. An analysis of the surface revealed a Copper Face-Centered Cubic lattice
structure with an average lattice parameter of 3.622

A, a number density of 8.419 10
22
, and
a mass density of 8.884 g cm
3
. All of these values were within 1% of literature values.
The bulk material of the penny was also analyzed. The K

peaks in the diraction

pattern were assigned according to the Miller indexing scheme by matching corresponding
interplanar spacings with given values of {h,k,l}. Five of the peaks were unidentiable in
the lattice, and this taken to be due to the presence of substitutional impurities in the form
of Cu. The number density of the bulk material was found to be 1.9347 10
22
atoms/cm
3
,
and the concentration of Copper impurity in the material was calculated to be 3.729 atom
percent.
25
Sirajuddin, David Lab 2 - X-Ray Diraction
8 References
1. Atzmon, M. X-Ray Diraction Lecture Notes, January 2007
2. Atzmon, M. Transparencies, January 2007
3. CRC. CRC Handbook of Chemistry and Physics, 87th Edition. 2003.
4. Hirose, Akira. Lonngren, Karl. Wave Phenomena. Kreiger Publishing Company.
Malabar, Florida. 2003.
5. USGS Coastal and Marine Geology Program, http://pubs.usgs.gov/of/2001/of01-
041/htmldocs/xrpd.htm, Accessed - February 16, 2007.
6. Wikipedia, X-ray Crystallography, http://en.wikipedia.org/wiki/X-raycrystallography,
Accessed - February 16, 2007.
7. Web Elements. Zinc,Copper, http://www.webelements.com, Accessed - February 16,
2007.
26
Sirajuddin, David Lab 2 - X-Ray Diraction
9 Appendix
9.1 Figures
Figure 9.1 - A plot of the raw data for the surface of the penny acquired from the XRD experiment. The
intensity is plotted versus the angle 2.
Figure 9.1 - A plot of the raw data for the bulk material of the penny acquired from the XRD
experiment. The intensity is plotted versus the angle 2.
27
Sirajuddin, David Lab 2 - X-Ray Diraction
9.2 Data Tables
K

peak, s (

A
1
) K

peak, 2 (

) K

peak, 2 (

)
2.9923 19.5 17.36
3.4593 22.55 20.07
4.6914 30.75 27.34
4.9053 32.15 28.50
5.7538 37.95 33.69
6.0114 39.65 35.19
6.9406 46.20 40.94
7.5685 50.60 44.79
7.7649 52.00 46.00
Table 9.1 - Surface values for the K

peaks with their corresponding calcuated K

peaks.
K

peak, s (

A
1
) K

peak, 2 (

) K

peak, 2 (

)
2.5474 16.55 14.74
2.7171 17.65 15.72
3.0027 19.50 17.37
3.7283 24.30 21.63
4.204 30.85 27.43
5.3585 35.20 31.28
5.4421 35.80 31.803
5.5897 36.80 32.69
5.6242 37.00 32.861
5.7806 38.1 33.83
6.0172 39.65 35.19
6.6517 44.10 39.19
6.9408 46.15 49.89
7.3112 48.75 43.17
8.1545 54.80 48.44
Table 9.2 - Bulk values for the K

peaks with their corresponding calcuated K

peaks.
Energy (MeV) Mass attenuation coecient

(cm
2
/g)
0.01 216
0.02 33.8
0.05 2.61
0.1 0.458
Table 9.3 - Mass attenuation coecient listed with respect to incident photon energy in Copper. The data
was tted to a power function, and the proper mass attenuation coecient was interpolated at the photon
energy used in experiment.
28
Sirajuddin, David Lab 2 - X-Ray Diraction
Centroid s
i
(

A
1
) A B c s
2
R
2.5474 4.0619 10
4
1672.8 572.26 14403 .0078031 3.734710
7
.99069
2.7171 6.7494 10
4
-5185.5 18892 4148.2 .0070848 1.374610
7
0.96084
3.0027 3.211 10
4
-1117.2 8181 25960 .0068209 1.66810
8
0.98505
3.7283 1.3978 10
4
-959.09 6977.7 6357.1 0.0060571 3.97210
6
0.99298
4.204 3.211 10
4
-1117.2 8181 25960 0.0068209 1.66810
8
0.98505
5.3585 2.0783 10
4
863.16 -1329.4 5259 0.0055909 3.020710
6
0.99057
5.4421 3.1188 10
4
-1222.3 9794.9 463.57 0.0048169 11650 0.99169
5.5897 2.4051 10
4
-508.79 6139.3 2148.3 0.0051995 66304 0.99778
5.6242 6.2899 10
4
-20815 1.203210
5
1074.6 0.0042943 1.07110
5
0.98722
5.7806 3.4272 10
4
-1599.9 12089 641.62 0.010186 15839 0.99608
6.0172 1.7861 10
3
-0.3278 2740.5 97.941 0.011606 1.93810
6
0.77624
6.6517 3.1211 10
4
387.97 50.867 985.31 0.0062698 1.770810
5
0.9857
6.9408 4.4472 10
4
-588.47 6741.9 1204.2 0.012487 1.83210
5
0.99295
7.3112 3.7953 10
4
-1458.6 13387 1599.8 0.0059565 5.445110
5
0.98149
8.1545 6.4937 10
4
365.85 -517.82 623.47 0.0085668 1.472510
5
0.97295
Table 9.4 - Fitting parameters with associated error in the interplanar spacing d for the bulk material of
the penny.
Centroid s
i
(

A
1
) A B c s
2
R
2.9923 2.7561 10
4
389.47 73.077 6823.2 0.015172 7.031910
6
0.99674
3.4593 1.9662 10
4
-365.41 2443.1 3706.9 0.014853 5.903210
5
0.0.9989
4.6914 1.3825 10
3
269.98 -657.73 149.46 0.011866 20873 0.95809
4.9053 3.6584 10
4
14.86 578.86 770.48 0.012472 1.023910
5
0.99490
5.7538 2.2895 10
4
177.49 -332.43 1358.4 0.014487 5.645910
5
0.99571
6.0114 3.3934 10
4
-135.62 1461.3 551.51 0.011659 38809 0.99436
6.9406 1.1324 10
4
-138.51 1531 207.34 0.015678 34138 0.9708
7.5685 8.9627 10
4
221.62 -1103.7 201.12 0.014212 21702 0.97725
7.7649 9.5937 10
4
-103.57 1357.5 178.4 0.015274 21996 0.97645
Table 9.5 - Fitting parameters with associated error in the interplanar spacing d for the surface material
of the penny.
29