AFM, XRD, SIMS and TEM

Training at RDC and AMC

Tran Quang Trung

Guiders: Mr Takahagi, Mr Yamazaki,Dr Tomita and Dr Takeno
 XRD
Aims
I. Introduction
II. Basic Conception
III. XRD Instrument
III.1 XRD Instrument
III.2 How to use the instrument
IV. Application
V. Experiments and Results
VI. Conclusion
Aims
1. To understand basic concept of x-ray
diffraction
2. To understand the operation of the x-ray
equipment (PANalytical's X'Pert PRO X-
ray diffraction system)
3. To understand elementary x-ray diffraction
pattern (compare experimental data with
literature data)
I Introduction
II Basic Conception
II.1 Bragg Condition – Goniometer
II.1.1 Lattice Planes and Bragg's
Law
II.1.2 Goniometer for θ - 2θ system
II.2 Safety
II.2.1 X-rays
II.2.2 High Voltage
II.2.3 Liquid Nitrogen
III X-ray Instrument

III.1 X-ray Source

III.2 Sample holder
III.3 Goniometer
III.4 Detector
III.5 Diffraction optics
IV Potential and Application

IV.1 Identification
IV.2 Polymer crystallinity
IV.3 Residual stress
IV.4 Texture analysis
IV.5 Polefigure data collection
V Experiments and Results
V.1 How to operate a diffractometter
V.1.1Detector LN
V.1.2Power status check
V.1.3Warm up
V.1.4Preparation prior to take a
diffraction pattern
V.1.5Measurement Program
V.1.6Power Down the Generator
V.2 Experiment and Results
VI Conclusion
In X-ray diffraction practice duration, with the help
of Mr. Yamazaki I basically understand:
The basic concept of X-ray diffraction
The basic operation x-ray equipment
(PANalytical's X'Pert PRO X-ray diffraction
system) and function of components
The basic X-ray potential and application.
The elementary x-ray diffraction pattern
(compare experimental data with literature data)
The basic calculation method of d values from
Bragg condition
Bibliography
[1] X-ray-diffraction
http://www.panalytical.com/index.cfm?pid=135
[2] http://www.iucr.org/iucrtop/comm/cteach/pamphlets/2/
[3] http://pubs.usgs.gov/of/of01-041/htmldocs/xrpd.htm
[4] http://rsc.anu.edu.au/~schmid/braggtheo.html
[5] http://www.mse.arizona.edu/classes/mse480/common/xr
[6] http://materials.binghamton.edu/labs/xray/xray.html
[7] http://website.lineone.net/~djtaylor/XRAY/xray1.htm
 I Introduction
• About 95% of all solid materials can be described as crystalline. When X-rays interact
with a crystalline substance (Phase), one gets a diffraction pattern.
• X-radiation ("X-rays") is the generic term used to describe electromagnetic radiation
with wavelengths between roughly 0.01 nm and 10 nm. This is shorter than ultraviolet
but longer than gamma radiation. The spacing of adjacent atoms in a crystal structure is
typically about 0.3 nm. The wavelengths of X-rays are therefore of the same order as
the atomic spacing in a crystal.
• X-ray diffraction (XRD) is a versatile, non-destructive technique that reveals detailed
information about the chemical composition and crystallographic structure of natural
and manufactured materials.
• A crystal lattice is a regular three-dimensional distribution (cubic, rhombic, etc.) of
atoms in space. These are arranged so that they form a series of parallel planes
separated from one another by a distance d, which varies according to the nature of the
material. For any crystal, planes exist in a number of different orientations - each with
its own specific d-spacing.
• When a monochromatic X-ray beam with wavelength  (lambda) is projected onto a
crystalline material at an angle θ (theta), diffraction occurs only when the distance
traveled by the rays reflected from successive planes differs by a complete number n of
wavelengths. By varying the angle θ (theta), the Bragg's Law conditions are satisfied by
different d-spacings in polycrystalline materials. Plotting the angular positions and
intensities of the resultant diffracted peaks of radiation produces a pattern, which is
characteristic of the sample. Where a mixture of different phases is present, the
resultant diffractogram is formed by addition of the individual patterns.
I Introduction
• Based on the principle of X-ray diffraction, a wealth of structural,
physical and chemical information about the material investigated can
be obtained. A host of application techniques for various material
classes is available, each revealing its own specific details of the
sample studied
• Today about 50,000 inorganic and 25,000 organic single component,
crystalline phases, diffraction patterns have been collected and stored
on magnetic or optical media as standards. The main use of powder
diffraction is to identify components in a sample by a search/match
procedure. Furthermore, the areas under the peak are related to the
amount of each phase present in the sample
• Typically x-ray diffraction (XRD) can be used for:
1. Qualitative analysis
2. Quantitative analysis
3. Structure of alloys
4. Stress determination in metals
5. Determination of particle size
• Identification and raw materials evaluation
 II Basic Conception
II.1 Bragg Condition – Goniometer
If an incident X-ray beam encounters a crystal lattice, general scattering occurs. Although
most scattering interferes with itself and is eliminated (destructive interference),
diffraction occurs when scattering in a certain direction is in phase with scattered rays
from other atomic planes. Under this condition the reflections combine to form new
enhanced wave fronts that mutually reinforce each other (constructive interference). The
relation by which diffraction occurs is known as the Bragg law or equation (fig.5).
Because each crystalline material has a characteristic atomic structure, it will diffract X-
rays in a unique characteristic.
II.1.1 Lattice Planes and Bragg's Law
• X-rays primarily interact with electrons in atoms. When x-ray photons collide with
electrons, some photons from the incident beam will be deflected away from the direction
where they original travel, much like billiard balls bouncing off one anther. If the
wavelength of these scattered x-rays did not change (meaning that x-ray photons did not
lose any energy), the process is called elastic scattering (Thompson Scattering) in that
only momentum has been transferred in the scattering process. These are the x-rays that
we measure in diffraction experiments, as the scattered x-rays carry information about the
electron distribution in materials. On the other hand, In the inelastic scattering process
(Compton Scattering), x-rays transfer some of their energy to the electrons and the
scattered x-rays will have different wavelength than the incident x-rays.
• Diffracted waves from different atoms can interfere with each other and the resultant
intensity distribution is strongly modulated by this interaction. If the atoms are arranged in
a periodic fashion, as in crystals, the diffracted waves will consist of sharp interference
maxima (peaks) with the same symmetry as in the distribution of atoms. Measuring the
diffraction pattern therefore allows us to deduce the distribution of atoms in a material.
 II Basic Conception
• The peaks in a x-ray diffraction pattern are directly related to the atomic distances. Let
us consider an incident x-ray beam interacting with the atoms arranged in a periodic
manner as shown in 2 dimensions in the following illustrations. The atoms, represented
as green spheres in the graph, can be viewed as forming different sets of planes in the
crystal (colored lines in graph on left). For a given set of lattice plane with an inter-plane
distance of d, the condition for a diffraction (peak) to occur can be simply written as
2dsinθ = n λ

• which is known as the Bragg's law, after W.L. Bragg, who first proposed it. In the
equation, λ is the wavelength of the x-ray, θ the scattering angle, and n an integer
representing the order of the diffraction peak. The Bragg's Law is one of most important
laws used for interpreting x-ray diffraction data.
• It is important to point out that although we have used atoms as scattering points in this
example, Bragg's Law applies to scattering centers consisting of any periodic
distribution of electron density. In other words, the law holds true if the atoms are
replaced by molecules or collections of molecules, such as colloids, polymers, proteins
and virus particles.

Fig.5: Illustration of Bragg Condition

 II Basic Conception
II.1.2 Goniometer for θ - 2θ system: (θ angle moving sample,
2θ angle moving detector and fixed X-ray source)
• The mechanical assembly that makes up the sample holder,
detector arm and associated gearing is referred to as goniometer.
The working principle of a Bragg-Brentano parafocusing (if the
sample was curved on the focusing circle we would have a
focusing system) reflection goniometer is shown below (fig.6).
• The distance from the X-ray focal spot to the sample is the same
as from the sample to the detector. If we drive the sample holder
and the detector in a 1:2 relationship, the reflected (diffracted)
beam will stay focused on the circle of constant radius. The
detector moves on this circle.
• For the θ: 2-θ goniometer, the X-ray tube is stationary, the
sample moves by the angle θ and the detector simultaneously
moves by the angle 2-θ. At high values of θ small or loosely
packed samples may have a tendency to fall off the sample
holder.
 II Basic Conception
II.1.2 Goniometer for θ - 2θ system (cont)
 II Basic Conception
II.2 Safety
II.2.1 X-rays.
• The X-rays we are concerned with are primarily the tube Cu K and L
characteristic lines plus continuum, but also secondary fluorescence from the
sample and holder. The highest energy X-ray possible under normal operation is
from the 40 keV continuum (Bremsstrahlung) (but there are very few of these 40
keV X-rays produced), and the highest characteristic X-ray is the Cu Kα with 8.0
keV energy (there are a lot of these) as well as Cu Lα with 0.93 keV energy (also
a lot produced, but being weaker many are absorbed by the Be window leaving
the tube).
• The potential health effects are mainly damage to cells and tissue, i.e., burns,
mutations, which under extreme conditions could lead to radiation sickness,
cataracts and cancer. The greatest danger is to rapidly growing cells, meaning
that pregnant women working in locations of potential X-ray exposure need to
pay particular attention to safety precautions.
• For the XRD lab, X-rays can only affect users if the shutter between X-ray tube
and sample is open AND the metal and leaded glass door is open, or one of the
other 5 walls of the enclosure is removed or breached. There are several fail-safe
interlocks built in to the equipment: if the HV power bulb is burned out, the HV
will not turn on. If the shutter Warning bulb is burned out, the shutter will not
open. If the door is open, the shutter cannot be opened. (It is possible to bypass
these, particularly the last one, but this is only done by experienced technical
personnel and should never be done with users in the room.)
 II Basic Conception
II.2 Safety (cont)
IV.2 High Voltage.
• There are potentially dangerous high voltages present in some of the
electronics. The users should never reach inside any of the electronics.
• In the unlikely case, someone who appeared to be accidental in contact
with a high voltage component, first quickly try to alert someone else in
the vicinity to the hazardous situation, and then switch off the main
breaker
IV.3 Liquid Nitrogen. (only for detectors need to be
cooled by liquid nitrogen)
• If the users must, handle LN with care, as can get burned (frost bite) if
any significant quantity remains in contact with the user’s skin (trapped
in clothing, gloves, shoes) for more than a couple of seconds. Normally
this is the only danger if the users have only a dewar in a moderately
large room. In an enclosed volume (overturned dewar in a van; frozen
open valve on large tank in small room) death by asphyxiation (nitrogen
displaces the air) is possible.
III X-ray Instrument
X-ray diffractometer often consists of X-ray source, , sample holder, goniometers,
detector, soller slits, divergence slit and receiver slit which are built up in a isolated
safety chamber as describing on fig.1. Beside on, there is some supported equipment
for operation such as the highly stabilized power supplies; the chiller provides a
source of clean water to cool the X-ray tube and the controller computer.

Detector Sample holder x-ray source

Fig.1: X’Pert Diffraction System

 III X-ray Instrument
II.1 X-ray Source:
X-rays are electromagnetic
waves whose wavelengths
range from about 0.1 to 100 x
10-10 m. They are produced
when rapidly moving
electrons strike a cooled solid Fig.2: Shematic Cross Section of an X-Ray Tube (Source)
target and their kinetic energy
is converted into radiation

The wavelength of the emitted radiation depends on the energy of the striking
electrons. X-ray tubes with copper targets, which produce their strongest characteristic
radiation at a wavelength of about 1.5 angstroms, are commonly used. (fig.2). The actual
window through which the X-rays emerge is usually made of beryllium--which has an
atomic number of only 4 and therefore very low absorption. The windows are delicate
and should not be touched.
With several electrons bombarding the target x-rays of several different wavelengths
are created. Most experiments use monochromatic incident beams, which there is only
one wavelength of x-rays.
 III X-ray Instrument
II.1 X-ray Source (cont)
Directing the x-rays through a foil filters out the other wavelengths. Different foils filter
out (fig.3) different wavelengths so it is important to choose the correct foil for the
wavelength desired. One can also monochromize the beam with a single crystal as a
diffractor. The crystal can be set to diffract a certain wavelength by choosing different
incident angles for the x-rays.
 III X-ray Instrument
II.2 Sample holder:
The mechanical assembly that holds up the sample and associated gearing is referred
to as Sample holder (fig.1).
II.3 Goniometer:
The mechanical assembly that makes up the sample holder, detector arm and
associated gearing is referred to as goniometer (fig.1)
II.4 Detector:
Nowadays X-ray generators are available with highly stabilized power supplies,
though of course such apparatus is very expensive. It is necessary when Geiger
counters or solid-state detectors are being used to measure X-ray intensities. Some
detector in X-ray technique are listed below:
 Gas Proportional detectors
 Scintillation detectors
 Energy Dispersive Si (Li) detectors
 Position Sensitive detectors
 Area Detectors based on CCD's (Charge Coupled Device)
III X-ray Instrument
II.5 Diffraction optics:
There are many commercially available instruments for XRD work. Most are
based on the parafocussing Bragg-Brentano optics. There is a move towards
parallel beam optics led by work on thin films and its ability to cope with less
than flat and rough surfaced specimens. A schematic of typical optics is shown
below (fig.4).
 III X-ray Instrument
II.5 Diffraction optics (cont)
In most powder diffractometers systems a series of parallel plates (soller slits) arranged
parallel to the plane of the diffractometer circle and several scatter and receiving slits
(arranged perpendicular to the diffractometer circle) are used to create an incident
beam of X-rays that are (approximately) parallel. Soller slits are commonly used on
both the incident and diffracted beam, but this will vary depending on the particular
system. Soller slits control axial divergence and are typically 20mm long with 0.35mm
spacing. They are made up of thin plates of an absorbing metal (often Mo).
The scatter (or divergence) slits (on the incident beam side) may be varied to control
the width of the incident beam that impinges upon the specimen. They limit the
longitudinal spread of the beam on the specimen and are typically in the range 0.25 -
1.50 .
Receiving slits may be varied to control the width of the beam entering the detector .
They limits scattered radiation from contaminating the signal and are typically 0.05 -
0.2mm
Filters for removing Kβ may be located in the beam path on the generator or detector
side of the path; a monochromator, if present, is usually located on the detector side
between the receiving slit and the detector
 IV Potential and Application
IV.1 Identification :
• The most common use of crystal or powder (polycrystalline) diffraction are chemical
analysis. These can include phase identification (search/match), investigation of high/low
temperature phases, solid solutions and determinations of unit cell parameters of new
materials.
IV.2 Polymer crystallinity :
• A polymer can be considered partly crystalline and partly amorphous. The crystalline
domains act as a reinforcing grid, like the iron framework in concrete, and improves the
performance over a wide range of temperature. However, too much crystallinity causes
brittleness. The crystallinity parts give sharp narrow diffraction peaks and the amorphous
component gives a very broad peak (halo). The ratio between these intensities can be used
to calculate the amount of crystallinity in the material.
IV.3 Residual stress :
• Residual stress is the stress that remains in the material after the external force that caused
the stress have been removed. Stress is defined as force per unit area. Positive values
indicate tensile (expansion) stress, negative values indicate a compressive state.
• The deformation per unit length is called strain. The residual stress can be introduced by
any mechanical, chemical or thermal process. E.g. machining, plating and welding.
• The principals of stress analysis by the X-ray diffraction is based on measuring angular
lattice strain distributions. That is, we choose a reflection at high 2-θ and measure the
change in the d-spacing with different orientations of the sample. Using Hooke’s law the
stress can be calculated from the strain distribution.
 IV Potential and Application
IV.4 Texture analysis :
• The determination of the preferred orientation of the crystallites in polycrystalline aggregates is
referred to as texture analysis, and the term texture is used as a broad synonym for preferred
crystallographic orientation in the polycrystalline material, normally a single phase. The preferred
orientation is usually described in terms of polefigures.
• A polefigure is scanned be measuring the diffraction intensity of a given reflection (2-θ is constant)
at a large number of different angular orientations of the sample. A contour map of the intensity is
then plotted as a function of angular orientation of the specimen. The most common representation
of the polefigures are sterographic or equal area projections. The intensity of a given reflection (h, k
, l) is proportional to the number of h, k , l planes in reflecting condition (Bragg’s law). Hence, the
polefigure gives the probability of finding a given crystal-plane-normal as function of the specimen
orientation. If the crystallites in the sample have a random orientation the recorded intensity will be
uniform.
• We can use the orientation of the unit cell to describe crystallite directions. The inverse polefigure
gives the probability of finding a given specimen direction parallel to crystal (unit cell) directions.
• By collecting data for several reflections and combining several polefigures we can arrive at the
complete orientation distribution function (ODF) of the crystallites within a single polycrystalline
phase that makes up the material.
• Considering a coordinate system defined in relation to the specimen, any orientation of the crystal
lattice (unit cell) with respect to the specimen coordinate system may be defined by Euler rotation
(three angular values) necessary to rotate the crystal coordinate system from a position coincident
with the specimen coordinate system to a given position.
• The ODF is a function of three independent angular variables and gives the probability of finding
the corresponding unit cell (lattice) orientation.
IV.5 Polefigure data collection :
• The systematic change in angular orientation of the sample is normally achieved by utilizing a four-
circle diffractometer. We collect the intensity data for various settings of CHI and Phi. Normally we
measure all PHI values for a given setting of CHI, we then change CHI and repeat the process.
 V Experiments and Results
V.1 How to operate a diffractometter
V.1.1 Detector LN:
• Normally, check the red LED on the front of the detector; if illuminated, the detector is
warm and will need to be refilled and then there will be a 30-45 minute wait before
experiment can be proceed.
• For example: Germanium (Ge) solid state detector. The detector should be at or near 90°
to be filled; move it to that position with software controls, then must be filled the LN
dewar. Normally, a programmed DataScan automatically return to that position after the
end of each run.
V.1.2 Power status check:
• Check the power supply for the X-ray tube: normal operating procedure is to keep some
power ON to the tube, unless the machine is to be unused for an extended length of time
(i.e. >5 days). Therefore, for example:
• See the ‘X-ray On’ lit red and the ‘Intlk Closed’ indicator lit (this refers to the cooling
water interlock being closed because water is flowing). If these are NOT the conditions,
then begin “Cold Start up” for checking a cooling water is now flowing into a X-ray tube.
V.1.3 Warm up:
• The user should go from the standby settings of 10 kV and 2 mA, to 40 kV and 35 mA,
gradually, over a minute or so: 1) turn HV to 15 kV and current to 4 mA, then wait a few
seconds; 2) then 20 kV and 6 mA, wait; 3) then 25 kV and 8 mA, wait; 4) then 30 kV and
10 mA, wait; 5) 35 kV and 12 mA, wait; 6) 40 kV and 14 mA, wait; and 7) now turn up
current to 35 mA. At the present, in some modern XRD system (for example: X’Pert
diffractometer system), this process is controlled automatically.
V Experiments and Results
V.1 How to operate a diffractometter (cont)
V.1.4 Preparation prior to take a diffraction pattern.
User Setup
1. Open the X’Pert Data Collector program.
2. Enter your user name and password.
3. Select the Thin Film as the Configuration for thin films analysis. Then press
the OK button.
Optics Setup
4. Select the Instrument Settings tab. Double click an item related to the
generator settings, select the X-ray tab, and set the Generator to 45 kV and
40 mA. Then, press OK.
Sample Mounting
5. Double click an item related to the sample stage positions. Select the position
tab.
6. Open the enclosure doors and mount the sample as flat as possible on the
stage.
7. Optimize the Z position of the sample using either the dial gauge method, or
the beam bisection method as explained below.
*In our experiments, we select the dial gauge method.
 V Experiments and Results
V.1 How to operate a diffractometter (cont)
V.1.4 Preparation prior to take a diffraction pattern.
(cont)
Dial Gauge Method for Sample Z position optimization
a. Mount the dial gauge on the stage and close the enclosure doors.
b. Return the stage to its upright position by setting psi to 0 degrees
and pressing the Apply button.
c. Move the z position of the sample stage until the dial gauge reads
1.0. (The small inner dial will read 1 and the large outer dial should
point to the 0 at the top of the dial gauge.) Press the OK button to close
this window.
d. Remove the dial gauge (Z position = 5.0) and close the doors.
e. Click OK to close the instrument settings window
8. Select Measure/Manual Scan from the main menu.
9. Select Omega for the Scan Axis (Scan mode: Continuous) 2 degrees for
theRange, 0.01 degrees for the Step Size, 0.20 sec for the Time Per Step,
Scanspeed 0.05 and press Start.
10. After finished scan, use the Peak mode to select the maximum intensity,
and Move to.
 V Experiments and Results
V.1 How to operate a diffractometter (cont)
V.1.4 Preparation prior to take a diffraction pattern.
(cont)
11. Back in the Manual Scan window, enter the follow parameters: Psi in
the Scan Axis field, enter 0.05 in the Step Size field, 8 in the Range field,
and 0.1 in the Time Per Step field.
12. Then, press the Start button. (This is in the case of a symmetric
reflection. If an asymmetric reflection is being studied enter phi for the
Scan Axis and leave all the other scan parameters as suggested here.)
13. After the measurement is completed press the right mouse button and
select Peak mode/Move mode.
14. Back in the Manual Scan window, enter the following parameters:
omega in the Scan Axis field, enter 0.002 in the Step Size field, 1 in the
Range field, and 0.1 in the Time Per Step field. Press the Start button.
15. If the omega peak position has changed, return to step 8.
16. Once you are satisfied with the alignment, close the manual scan
windows.
17. Select User setting/Sample offset. 2 Theater = 69.1290, Omega = 34.56
 V Experiments and Results
V.1 How to operate a diffractometter (cont)
V.1.5 Measurement Program
1. Select File/New Program/Absolute Scan.
2. Enter the following information: omega-2theta or 2theta-omega for the Scan
Axis depending if you want your graph plotted with omega or 2theta (note a 2
degree scan in omega-2theta is the same as a 4 degree scan in 2theta-omega),
set the start angle to whatever you determined appropriate, set the end angle,
enter the Step Size, enter the Time Per Step.
3. Select File/Save as and enter a name for the program and then press the OK
button. Close this window.
------------------------------- later -------------------------
V1..6 Power Down the Generator: when experiments are finished for the
day (X’ Pert PRO X-ray diffraction system is automatically performed)
a. Dial current down to 2 mA – slowly
b. Dial down to 10 kV – slowly
c. DO NOT turn off the Power
d. Leaving it on to reduce stress on the tube.
V Experiments and Results
V.2 Experiment and Results
V.2.1 Experiment
Sample:
• The sample used in this experiment was oxygen implanted Si wafers.
• Implanted conditions: 100 keV, 5e14 cm-2.
X-ray Generator:
• X-ray source selected CuKa1 λ=1.5405981
• X-ray Generator set to 45 kV and 40 mA
θ - 2θ goniometer Configuration:
• 2θ angle : 10 – 50o
• Omega in the Scan Axis field (or θ): 0.002 in the Step Size field, 1
degrees in the Range field, 0.1 in the Time Per Step field, and Scan
speed 0.05 (it take about 2 hours for measurement)
Detector:
• Solid state detector
V Experiments and Results
V.2.2 Result
Diffraction Pattern

Intensity (a. u.)

15 20 25 30 35 40 45
2 θ (degrees)
 V Experiments and Results
V.2.2 Result (cont)
Reference Data:Literature(#27-1402)
• Si sample, this sample is NBS Standard Reference Material No. 640.
• X-ray=CuKa1, λ=1.5405981 Ref.Natl. Bur. Stand. (U.S.) Monogr. 25, 13 35 (1976)
• Fd3m (227) Z=8
• a = 5.4309
• Calculated density = 2.329 measured density = 2.33A
• Strong peak ： 3.14/X 1.92/6 1.64/3 1.11/1 1.25/1 0.86/1 0.92/1 1.36/1 1.05/1 0.96/1
• Reflections calculated from precision measurement of a 0. a0 uncorrected for
refraction.
• To replace 5-565 and 26-1481.
 V Experiments and Results
V.2.2 Result (cont)
Reference Data:Literature(#27-1402)
d(nm) I(f) I(v) h k l 2θ θ 1/(2d) 2π/d
• 0.3135 100.0 100.0 1 1 1 28.442 14.221 0.01595 0.20039
• 0.1920 55.0 90.0 2 2 0 47.302 23.651 0.02604
0.32723
• 0.1637 30.0 57.0 3 1 1 56.121 28.060 0.03053 0.38371
• 0.1357 6.0 14.0 4 0 0 69.130 34.565 0.03683 0.46278
• 0.1245 11.0 28.0 3 3 1 76.377 38.189 0.04013 0.50431
• 0.1108 12.0 34.0 4 2 2 88.026 44.013 0.04510 0.56677
• 0.1045 6.0 18.0 5 1 1 94.948 47.474 0.04784 0.60115
• 0.0960 3.0 10.0 4 4 0 106.715 53.357 0.05208 0.65450
• 0.0918 7.0 24.0 5 3 1 114.087 57.044 0.05447 0.68444
• 0.0858 8.0 29.0 6 2 0 127.541 63.770 0.05823 0.73171
• 0.0828 3.0 11.0 5 3 3 136.890 68.445 0.06037 0.75866
 V Experiments and Results
V.2.2 Result (cont)
Caluculated d-values from Bragg Condition was shown below:
Si
Measured Literature (#27-1402)
2θ d(A) Intensity(au) 2θ d(A) Intensity (au) hkl Δd/d
16.87 5.25 2747
18.39 4.82 1020
23.91 3.72 393 No DATA
25.49 2.49 600
25.57 3.48 576
29.35 3.04 3913 28.442 3.135 100 111 -3.1%
47.302 1.920 55 220
56.121 1.637 30 311
V Experiments and Results
V.2.2 Result (cont)
Remarks
• We should have measured at wider 2 theater range.
• Peak at near 2 θ = 33 degree is maybe scattered x-ray
from slit or second order diffraction.
• The measurement of peak position shows larger shift in
direction of a larger angular position in comparison to
that of the literature value.
• The sample used in this experiment was oxygen
implanted Si wafers. Implanted conditions: 100 keV,
5e14 cm-2. We think that sample itself or incompletely
alignment may be cause the disagreement between
experimental data and literature data.
• We need further experiment to clear this agreement.