UNIVERSITY OF DELHI,

NEW DELHI, 110009

LAB REPORT

PHYSICS AT NANOSCALE -I LAB - SEM III

Instructors: Submitted by:

Dr. YANA BAGBI Avichal Yadav (23222762029)
Dr. DEBABRATA MISHRA

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Contents
Contents Page no.

1.1 Aim …………………. …………………………………………………………...3

1.2 Apparatus Required ……………………………………………………………....3
1.3 Principle ………………………………………………………………………….3
1.4 Formula Used …………………………………………………………………….3
1.5 Diagram ……………………………………………………………………………4
2. Experimental setup and Theory …………………………………………………….5
2.1 Experimental Setup ……………………………………………………………….5
2.2 Theory ………………………………………………………………………………7
2.2.1 DC Sputtering Mechanism …………………………………………………….7
2.2.2 XRD ……………………………………………………………………………8
3. Experiment Procedure ………………………………………………………………11
4. Observations and Calculations…………………………………………………………11
5. Result and discussion ………………………………………………………………...14
6. Precautions……………………….……………………………………………………14
7. References ………………………………………………………………………………15

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1.1 Aim: DC Sputtering deposition of thin copper film on a glass slide and its structural characterization
using XRD.

1.2 Apparatus Requirement: DC Sputtering system, Argon gas, glass slide, Target material (Copper
metal), High voltage (0-300 V), XRD (XtaLAB Synergy-S)

1.3 Principle: It is based on the energy and momentum conservation of particles. The incident particle
experiences a difficult scattering process in the target, collides with an atom there, and transfers some of its
momentum to the atom. The atom then collides with further atoms in the target, creating a cascade process.
Some target atoms near the surface obtain enough momentum during this cascade to move away from the
target and are sputtered out of it.

Fig. 1.1 - Schematic for deposition of thin films by DC Sputtering

1.4 Formula used:

1. Braggs’ law:

2dsin (θ)=n λ

Where, d= interplanar spacing

θ = angle between the incident x-ray beam and the Bragg plane

λ = X-ray wavelength

n = an integer that represents the order of diffraction.

2. Debye Scherrer Formula:

D = kλ/ β cosθ

Where, D= The size of the crystallite or nanoparticle

K= The Scherrer constant, which is usually taken as 0.89 but can range from 0.62–2.08

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 λ = wavelength of x-ray

β = Full width at half maxima (FWHM)

θ = Bragg angle

Diagram:

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 Fig 1.2 – Diagrams of the DC Sputtering system

2. Experimental Setup and Theory:

2.1 Experimental Setup:

When the Hi Vac valve is ON, then there will be potential difference. High
ionization will create and AR+ and e − will be there. Plasma will be created using potential difference and
AR+ hits to cathode and create sputtering to target material.
Schematic diagram is given in Figure 1.3, at the bottom of the chamber
we have to keep the target material for heating. At the top of the chamber substrate is fixed where we have
to deposit the thin film.

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 Fig 1.3 – Animated Diagrams of the DC Sputtering system

Pirani gauge: A Pirani gauge is a type of vacuum pressure gauge used to measure low pressures,
typically in the range of 10^-4 to 1,000 millitorr. It operates based on the thermal conductivity of gases and
consists of the following key components:

Key Components:

1. Sensor Element: Typically, a thin wire or filament that is heated electrically.

2. Thermal Conductivity Principle: The gauge measures the cooling effect of the gas on the heated
filament. As gas pressure decreases, fewer gas molecules collide with the filament, leading to less
heat loss.
3. Temperature Measurement: The filament’s temperature is related to the pressure of the gas; the
lower the pressure, the higher the temperature of the filament for a constant input power.
4. Electronic Circuit: Converts the temperature change into a pressure reading, often displayed on a
digital readout.

Working Principle:

• When the filament is heated, it loses heat to the surrounding gas. The amount of heat loss depends on
the thermal conductivity of the gas, which varies with pressure.
• At higher pressures, more gas molecules collide with the filament, leading to greater heat loss.
Conversely, at lower pressures, fewer collisions result in less heat loss, allowing the filament to
maintain a higher temperature.
• The gauge is calibrated to convert temperature readings into pressure values.

Applications:

• Commonly used in vacuum systems, such as in semiconductor manufacturing, research laboratories,

and other applications where low pressures need to be monitored.

Rotatory Pumps:rotary pumps are crucial for creating and maintaining the necessary vacuum conditions
within the sputtering chamber. Here’s an overview of the types of rotary pumps commonly used and their
roles:

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Types of Rotary Pumps:

1. Rotary Vane Pump

o Description: A positive displacement pump that uses vanes mounted on a rotating rotor to
compress and transport gas.
o Function: Efficiently removes air and other gases from the chamber, achieving vacuum
levels typically down to about 10^-3 torr. It’s often used as a primary pump.
2. Scroll Pump
o Description: Consists of two interleaved spiral scrolls; one is fixed, and the other orbits
around it.
o Function: Provides high pumping speed and low ultimate pressure (down to about 10^-6
torr), making it suitable for rough to medium vacuum applications.

Roles in DC Sputtering:

• Initial Pumping: Rotary pumps are used to quickly lower the pressure in the sputtering chamber
from atmospheric levels to the desired vacuum level.
• Maintenance of Vacuum: Once the desired vacuum is achieved, rotary pumps help maintain that
environment by continuously removing any gas that may leak into the chamber during operation.
• Compatibility: They can handle various gases, making them versatile for different sputtering
applications.

2.2 Theory:
2.2.1 DC Sputtering Mechanism:
DC sputtering is a specific type of sputtering process used in thin
film deposition, characterized by the use of direct current (DC) to create and maintain a plasma. Here’s a more
detailed breakdown of the DC Sputtering Mechanism:

1. Vacuum Chamber: The process occurs in a vacuum chamber to minimize contamination and ensure
that the sputtered particles can travel freely from the target to the substrate.

2. Gas Introduction and Plasma Creation: Argon gas is introduced into the chamber and ionized by
applying a high DC voltage between the target and anode, creating a plasma of positive ions and electrons.

3. sputtering Process: Positive argon ions are accelerated towards the target, dislodging atoms from its
surface. These ejected atoms travel through the chamber in vapor form.

4. Deposition on Substrate: Ejected atoms condense on the substrate, forming a thin film or coating as
they adhere to the surface.

5. Process Control Parameters: Key parameters include gas pressure, voltage, target-to-substrate
distance, and target material, all of which influence the sputtering rate, film uniformity, and properties.

2.2.2 Advantages and Disadvantages

• It is the most standard sputter equipment with a simple structure.
• The deposition rate is almost constant for various types of metals.

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 • It is easy to control because the current amount and thickness of the thin film are almost in direct
proportion.
• The deposition rate is higher compared to RF sputtering. v. High uniformity in thin films.
• Ensures high adhesion since it requires high energy.
➢ Target material is limited to metals.
➢ High Air pressure is required. (10 to 15 mTorr).
➢ The substrate is prone to overheating.

2.2.2 X-Ray Diffraction

X-Ray Production:
X-rays are produced through the interaction of high-energy electrons with a target
material in an X-ray tube. The process begins with the generation of electrons in a heated filament (cathode)
which are then accelerated towards the anode (target) by applying a high voltage between the cathode and
anode.
When these high-energy electrons strike the target material, typically made of a high atomic
number element like tungsten, they interact with the atoms in the target. This interaction causes the ejection
of inner-shell electrons from the target atoms, and the subsequent filling of these vacancies by outer-shell

electrons results in the emission of X-rays. These X-rays are then directed through a window in the tube and
out towards the sample or detector.
Fig 1.4 - X- ray production diagram

Bragg’s law:

Bragg’s Law was introduced by Sir W.H. Bragg and his son Sir W.L. Bragg. The law states that when the x-
ray is incident onto a crystal surface, its angle of incidence, θ, will reflect back with a same angle of
scattering, θ. And, when the path difference, dd is equal to a whole number, n, of wavelength, a constructive
interference will occur.

Consider a single crystal with aligned planes of lattice points separated by a distance d. Monochromatic X-
rays A, B, and C are incident upon the crystal at an angle θ. They reflect off atoms X, Y, or Z.

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The path difference between the ray reflected at atom X and the ray reflected at atom Y can be seen to be
2YX. From the Law of Sines, we can express this distance YX in terms of the lattice distance and the X-ray
incident angle.

If the path difference is equal to an integer multiple of the wavelength, then X-rays A and B (and by extension
C) will arrive at atom X in the same phase. In other words, given the following conditions:

then the scattered radiation will undergo constructive interference and thus the crystal will appear to have
reflected the X-radiation. If, however, this condition is not satisfied, then destructive interference will occur.

Bragg’s law: nλ=2dsinθ

where:

• λ is the wavelength of the x-ray,

• d is the spacing of the crystal layers (path difference),
• θ is the incident angle (the angle between incident ray and the scatter plane), and
• n is an integer

Principle and working of XRD

It is based on the principle of Diffraction of X-rays. XRD relies on the diffraction of X-rays
by the atoms in a crystalline material. When X-rays interact with the crystal, they are scattered in various
directions. The pattern of scattered X-rays, or diffraction pattern, reveals information about the crystal
structure.

Max von Laue and Co., in 1912, discovered that crystalline substances act as three-dimensional diffraction
gratings for X-ray wavelengths similar to the spacing of planes in a crystal lattice (Friedrich et al., 1912). X-
ray diffraction is now a common technique for the study of crystal structures and atomic spacing. X-ray
diffraction is based on constructive interference of monochromatic X-rays and a crystalline sample. These X-
rays are generated by a cathode ray tube, filtered to produce monochromatic radiation, collimated to
concentrate, and directed toward the sample. The interaction of the incident rays with the sample produces
constructive interference (and a diffracted ray) when conditions satisfy Bragg’s law: nλ=2dsinθ where n is an
integer, λ is the wavelength of the X-rays, d is the interplanar spacing generating the diffraction, and u is the
diffraction angle. This law relates the wavelength of electromagnetic radiation to the diffraction angle and the
lattice spacing in a crystalline sample. These diffracted X-rays are then detected, processed, and counted. By
scanning the sample through a range of 2θ angles, all possible diffraction directions of the lattice should be
attained due to the random orientation of the powdered material. Conversion of the diffraction peaks to d-
spacings allows identification of the compound because each compound has a set of unique d-spacings.

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Typically, this is achieved by comparison of d-spacings with standard reference patterns. X-ray
diffractometers consist of three basic elements: an X-ray tube, a sample holder, and an X-ray detector
(Connolly, 2007). X-rays are generated in a cathode ray tube by heating a filament to produce electrons,
accelerating the electrons toward a target by applying a voltage, and bombarding the target material with
electrons. When electrons have sufficient energy to dislodge inner shell electrons of the target material,
characteristic X-ray spectra are produced. These spectra consist of several components, the most common
being Ka and Kb. Ka consists, in part, of Ka1 and Ka2. Ka1 has a slightly shorter wavelength and twice the
intensity of Ka2. The specific wavelengths are characteristic of the target material (Cu, Fe, Mo, Cr). Filtering,
by foils or crystal monochrometers, is required to produce monochromatic X-rays needed for diffraction. Ka1
and Ka2 are sufficiently close in wavelength such that a weighted average of the two is used. Copper is the
most common target material for single-crystal diffraction, with CuKa radiation D 1.5418 A. These X-rays
are collimated and directed onto the sample. As the sample and detector are rotated, the intensity of the
reflected X-rays is recorded. When the geometry of the incident X-rays impinging the sample satisfies Bragg’s
law, constructive interference occurs and a peak in intensity appears. A detector records and processes this X-

ray signal and converts the signal to a count rate, which is then output to a device such as a printer or computer
monitor. The geometry of an X-ray diffractometer is such that the sample rotates in the path of the collimated
X-ray beam at an angle u while the X-ray detector is mounted on an arm to collect the diffracted X-rays and
rotates at an angle of 2u. The instrument used to maintain the angle and rotate the sample is termed a
goniometer. For typical powder patterns, data are collected at 2θ from 5 to 70 and for thin films it’s from 10
to 80, angles that are preset in the X-ray scan. X-ray powder diffraction is most widely used for the
identification of unknown crystalline materials (e.g., minerals, inorganic compounds). Determination of
unknown solids is critical to studies in geology, environmental science, material science, engineering, and
biology. Other applications include characterization of crystalline materials, identification of fine-grained
minerals such as clays and mixed
Fig 1.5– Schematic diagram of Diffractometer system.

layer clays that are difficult to determine optically, determination of unit cell dimensions, and measurement
of sample purity. With specialized techniques, X-ray diffraction (XRD) can be used to determine crystal
structures by using Rietveld refinement, determine modal amounts of minerals (quantitative analysis),
characterize thin film samples, and make textural measurements, such as the orientation of grains, in a
polycrystalline sample (Brindley and Brown,

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3. Experiment Procedure:
• Switch on the mains circuit breaker.
• Switch on the rotatory pump by using the circuit breaker.
• Switch on the pirani Gauge and select the GH-1 for its satisfactory operation of rotatory pump.
• Open the isolation valve and select GH-2 to read the chamber vacuum.
• Close the isolation valve, and vent the chamber
• Open the base plate and load the required substrate on the substrate holder, and fix the target.
• Close the top base.
• Open the isolation valve to read the chamber vacuum.
• Admit the Argon gas by using gas admittance needle valve for required vacuum level.
• Switch on the 'HT' circuit breaker, make sure all the interlocks are closed (Door switch and vacuum
switch) Know increases the 'HT' controller rider for required level of power and read 'HT' current in
'HT' meter observe the plasma generated.
• Reduce the 'HT' to zero, and switch off the 'HT' circuit breaker.
• Close gas admittance needle valve.
• Close the isolation valve
• Vent the chamber by using air admittance valve.
• Take the substrate outside.
• The operator is advised to leave the chamber under vacuum at all the times when unit is not in use in
order to prevent exposure of chamber interiors to atmosphere.
• Evacuate the chamber down to 1x102 mbar then close the isolation valve.
• Switch off the pirani Gauge.
• Switch off the Rotary pump circuit breaker on the control panel.
• Switch of the mains circuit breaker.

4. Observations and Calculations:

Sputtering presets: Sample-1
Voltage -150V
Current-14mA
Time-8min
Target Material-Copper

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 Graph 2.1: Graph obtained for copper nanocrystal (8min sputtering)
Calculation:
For Time= 8 min
Wavelength of x-ray= 0.154 nm, Scherrer Constant = 0.9

[Link]. Voltage Current 2θ(degree) θ FWHM Cos(θ) D=Crystallite

size
(volts) (mA) (degree) (radian)
(nm)
1. 150 14 44.60 22.30 0.00424 0.952 34.35

K=0.9
λ=0.154nm
β=0.004238rad
cosθ=0.952
D = kλ/ β cosθ
0.9×0.154
D = 0.004238×0.952
D = 34.35nm

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Sputtering presets: Sample-2
Voltage -150V
Current-14mA
Time-6min
Target material-Copper

Graph2.2: Graph obtained for Copper nanocrystal (6min sputtering)

Calculation:
For Time=6min
Wavelength of x-ray= 0.154 nm, Scherrer Constant = 0.9

[Link]. Voltage Current 2θ(degree) θ FWHM Cos(θ) D=Crystalline

size
(volts) (mA) (degree) (radian)
(nm)
1. 150 14 44.66 22.33 0.00497 0.925 30.14

K=0.9
λ=0.154nm
β=0.00497rad
cosθ=0.925
D = kλ/ β cosθ
0.9×0.154
D = 0.00497×0.925
D = 30.14nm

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5. Result:
We have successfully obtained the crystallite size for the copper using the Debye Scherrer formula
–
D = kλ/ β cosθ
Wavelength of x-ray= 0.154 nm, Scherrer Constant = 0.9
[Link]. Voltage Current 2θ(degree) Sputtering FWHM Cos(θ) D=Crystalline
Time size
(volts) (mA) (radian)
(nm)
1 150 14 44.66 6(min) 0.00497 0.925 30.14
2 150 14 44.60 8(min) 0.00424 0.952 34.35

Discussion:
• The standard values for the copper nanocrystal are - 43.4, 50.5, and 74.2 correspond to the (1 1 1), (2 0
0), and (2 2 0) peaks of copper (JCPDS, file no. 04-0836).
• As we can see from the graphs, the values we got from the XRD of the copper sample are –
(44.60,44.66),(50.01,50.38),73.75 (degrees) corresponds to the (111), (200) and (220). So, our data
matched from the JCPD file.
• From the graph 2.2, the values we got from the XRD of the copper sample are – 44.66,50.38,73.76
(degrees) corresponds to the (111), (200) and (220). So, our data matched from the JCPD file.
• From the observed (h k l) values, the structure of the copper nano crystal is found to be FCC. This is
because for the FCC structure our (h k l) values should be in the form of (h + k=even), (k + l=even) and
(h + l) = even. So, in our case this condition is satisfied. Hence it is FCC structure.
• The peak has been obtained for the copper nano crystal due to the highly nanocrystalline properties of
the metal.
• From XRD pattern, it was found that crystallite size of copper deposited on glass slide increases as we
increase the sputtering time. For 8 minutes deposition time , the obtained crystallite size is 34.35 nm and
for 6 minutes sputtering time, crystallite size is 30.14 nm. This is because when the sputtering time
increased , deposition of copper is more on the glass slide. Hence, crystallite size is increased when we
increase the sputtering time.

• When the geometry of the incident x-rays impinging the sample satisfies the Bragg’s Law, Constructive
interference occur and a peak in the intensity appears.

• As we can see from the Graphs, we have peaks at angles other than 44.62,50.38,73.75 (degrees) are due
to the impurities and the oxides formation of copper.

• The peak in the Graph2.2 at angle 2θ =37.02 degree is the peak for copper oxide.

6. Precautions:
• Surfaces of the sputtering unit may be very hot or very cold. Do not touch hot or cold surfaces such as
the source, substrate holder, diffusion pump, cryopump or liquid nitrogen pump.
• Wear clean lint – free gloves when you handle components in the chamber to prevent the contamination
of the source and its accessories.

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 • Do not operate the source in the area where there is equipment subject to magnet interference.
• After depositing thin film of copper on the glass substrate leave it for 2-3 min then take out it from the
chamber and cover it with the tissue. (Do not cover it until it cools down.)
• Place all the thin films in the air tight chamber to avoid contacts with moisture and air to prevent it
from the oxides and sulphides in air.

7. References:
• Lab manual copy provided by lab staff
• [Link]
• X-ray diffraction: instrumentation and applications research paper by Andrei A Bunaciu 1, Elena
Gabriela Udriştioiu, Hassan Y Aboul-Enein
• 10.1080/10408347.2014.949616
• [Link]
• [Link]
physics-notes%2Fx-ray-imaging%2Fproduction-of-x-
rays%2F&psig=AOvVaw3HVmTrdipTmV_o75jlU3lQ&ust=1726130110222000&source=images&
cd=vfe&opi=89978449&ved=0CBEQjRxqFwoTCND_0fS9uogDFQAAAAAdAAAAABAE
• [Link]

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