Thin Film Deposition & Gas Sensor Design
Thin Film Deposition & Gas Sensor Design
On
EVAPORATION
&
Undertaken at
DRDO, JODHPUR
CONTENTS
1. INTRODUCTION
1.1 Gas Sensor
1.2 Vacuum Coating Unit
1.3 Physical Vapor Deposition
1.3.1 Vacuum Thermal Evaporation
1.3.2 Sputtering
1.3.3 Thin Film Deposition Of Alloys
1.3.4 Uniformity and Deposition Rate
1.3.5 Step Coverage
1.3.6 Quartz Monitor
1.3.7 Vacuum Pumps
2. EXPERIMENTAL WORK
2.1 Thin Film Deposition
2.2 Designs for Circuit
Gas sensor has recently attracted much attention due to increasing demand of
environmental monitoring and other gas detecting applications. Among different types of gas
sensor, thin film gas sensor has been much of interest because of microelectronic batch-
fabricated compatibility, reproducibility, and ability to form multilayer device structures. In
this work, thin film based gas sensing circuit is designed for immediate applications of CO
detection for environmental monitoring. Ion assisted deposition (IAD) process offers several
advantages for gas sensor fabrication, including reactive deposition for gas-sensitive metal-
oxide material optimization and improved thin film adhesion for better device reliability. The
metal oxide layer was deposited on alumina or glass substrates. The sensors were tested with
reducing gases, in the temperature range between 200oC and 350 oC and the electrical change
in gas sensor is detected.
Gas sensors interact with a gas to initiate the measurement of its concentration. The
gas sensor then provides output to a gas instrument to display the measurements. Common
gases measured by gas sensors include ammonia, aerosols, arsine, bromine, carbon dioxide,
carbon monoxide, chlorine, chlorine dioxide, Diborane, dust, fluorine, germane, halocarbons
or refrigerants, hydrocarbons, hydrogen, hydrogen chloride, hydrogen cyanide, hydrogen
fluoride, hydrogen selenide, hydrogen sulfide, mercury vapor, nitrogen dioxide, nitrogen
oxides, nitric oxide, organic solvents, oxygen, ozone, phosphine, silane, sulfur dioxide, and
water vapor. Important measurement specifications to consider when looking for gas sensors
include the response time, the distance, and the flow rate.
The response time is the amount of time required from the initial contact with the gas
to the sensors processing of the signal. Distance is the maximum distance from the leak or
gas source that the sensor can detect gases. The flow rate is the necessary flow rate of air or
gas across the gas sensor to produce signal. Gas sensors can output a measurement of the
gases detected in a number of ways. These include percent LEL, percent volume, trace,
leakage, consumption, density, and signature or spectra. The lower explosive limit (LEL) or
lower flammable limit (LFL) of a combustible gas is defined as the smallest amount of the
gas that will support a self-propagating flame when mixed with air (or oxygen) and ignited.
In gas-detection systems, the amount of gas present is specified in terms of % LEL: 0% LEL
being a combustible gas-free atmosphere and 100% LEL being an atmosphere in which the
gas is at its lower flammable limit. The relationship between % LEL and % by volume differs
from gas to gas. Also called volume percent or percent by volume, percent volume is
typically only used for mixtures of liquids. Percent by volume is simply the volume of the
solute divided by the sum of the volumes of the other components multiplied by 100%.
Trace gas sensors given in units of concentration: ppm. Leakage is given as a flow rate like
ml/min. Consumption may also be called respiration given in units of ml/L/hr. Density
measurements are given in units of density: mg/m^3. A signature or spectra measurement is
a spectral signature of the gases present; the output is often a chromatogram. Common
outputs from gas sensors include analog voltage, pulse signals, analog currents and switch or
relays. Operating parameters to consider for gas sensors include operating temperature and
operating humidity.
(i) Gas Leak Protection: - These are areas of industry where the possibility of flammable
gas build-up is small, but the consequences of a gas escape could be catastrophic. These tend
to be industries which by their nature have large volumes of gases piped around the works:
• Engineering companies
• Metal working plants
• Research laboratories
The most prominent application for portable gas detection instruments. The instrument is
used to check the atmosphere of sewers, tanks and other vessels prior to entry for
maintenance purposes. These instruments invariably are 'multi-gas'. They have 3 or even 4
sensors included in the package. Large volumes of these instruments are purchased by:
(iii) Hazardous Area: Working Areas of industry where the build-up of flammable gas or
vapour is an ever present danger. These instruments are very often the same multi-gas
instruments used for confined space entry, but there are areas where single gas monitors
('explosimeters') are used. Typical industrial sectors here are:
Pellistors are miniature calorimeters used to measure the energy liberated by the
burning of a combustible (flammable) gas or vapour. A pellistor consists of a coil of small-
diameter platinum wire supported in a refractory bead on which is deposited a layer of
catalytic material, on which the gas is burnt. The coil serves two purposes. Firstly, it is used
to heat the bead electrically to its operating temperature, about 500°C, and secondly it is used
to detect changes in temperature produced by the oxidation of the flammable gas. The earliest
forms of catalytic gas sensors consisted solely of bare coils of platinum wire, operating at
800-1000°C. At such temperatures, platinum wire evaporates extremely quickly causing
signal drifts resulting from a reduction in the wire diameter. The specification for such a
sensor, which is still produced commercially, requires that the sensor has a life of 100 hours.
The majority of present day devices, as stated earlier, have the coil cloaked in a porous
ceramic onto which is deposited the precious metal catalyst. The enhanced catalytic activity
resulting from the much larger surface area of catalyst available permits much lower
operating temperatures of around 500°C, resulting in lower power drain and longer device
lifetime.
Fig 1.2 Pellistor gas sensor
The concept of the pellistor is based on the fact that the most foolproof way to determine
whether a flammable gas is present in air is to test a sample by trying to burn it! A pellistor
consists of a very fine coil of wire suspended between two posts. The coil is embedded in a
pellet of a ceramic material, and on the surface of the pellet (or 'bead') there is a special
catalyst layer.
In operation, a current is passed through the coil, which heats up the bead to a high
temperature. When a flammable gas molecule comes into contact with the catalyst layer, the
gas 'burns'. The reaction occurs without a flame since the level is below the Lower Explosive
Limit (or LEL) of the gas. However, just as in a burning reaction, heat is released which
increases the temperature of the bead. This rise in temperature causes the electrical resistance
of the coil to rise. There is another bead in the circuit which is identical to the detector bead,
but does not contain any catalyst.
(ii) Thermal Conductivity Gas Sensors: Pellistors measure the flammability of a gas; they
cannot be used to measure levels of gas above the Lower Explosive Limit (LEL), since the
reducing level of oxygen will result in a fall-off of signal. However, a similar device can be
used to monitor these high levels of gas. We have a range of thermal conductivity sensors,
which are designed to complement the pellistor range in terms of electrical characteristics, so
that they can be used in the same Wheatstone Bridge circuits. They are supplied with a
compensator bead which is in a sealed enclosure of air. This enclosure acts as the thermal
conductivity reference in exactly the same way as it acts as the reference for a pellistor.
Thermal conductivity measurements do not rely on the flammability of the gas, the technique
can be used to analyze a whole range of gas mixtures, provided that there are only two gases
present and that the two gases have significantly different thermal conductivities. Examples
includes
Thermal conductivity cannot be used for gas mixtures where the thermal conductivities of the
two gases are similar. The best example of this is oxygen levels in air, as the thermal
conductivities of oxygen and nitrogen are too close to give a meaningful signal.Our pellistors
and thermal conductivity sensors can be obtained already packaged as complete, flameproof
gas detection heads for use in fixed gas detection systems.
Infrared Gas Sensors exploit the property that many gases absorb radiation in the 2-14
micron, infrared region of the spectrum. These spectral absorbance show features which may
be regarded as 'fingerprints' to identify the gases and enable their concentrations to be
deduced. The sensor bodies contain an infrared source and infrared detectors inside a
compact and combined gas cavity/ optical cell. The detectors have infrared band pass filters
placed in front, which tune them to the specific gases to be sensed. When the specific gas
enters the cavity it is registered as a change in detector signal. The magnitude of this change
is related to the concentration of that gas via a simple exponential formula.By utilizing
different infrared filters a range of gases can be sensed and discriminated with these devices.
In cases where spectral lines overlap, then an individual sensor may show cross sensitivities
to a gas range. Infrared gas sensors are very robust devices not affected by contact with a
harsh chemical environment. Any changes in ambient conditions such as temperature are
compensated for in software. Their dimensions and power requirements are compatible with
and complementary to pellistor gas sensors. After over thirty years of successful manufacture
of pellistor-based flammable gas sensors, the range of Non-Dispersive Infra-red (NDIR) gas
sensors represents the first of many diversifications into other areas of gas sensor technology.
It is a versatile laboratory model coating unit for thin film application with facilities
for evaporation, Optional accessories like Substrate Heating, Rotary Drive, Flash
Evaporation, EB Gun evaporation etc. It is an ideal unit for thin film coatings in Research,
Educational institutions, semiconductor, optics the Vacuum coating unit & chamber
gadgetries are manufactured using high vacuum compatible materials.
Salient Features
Optional Accessories:
Rotary Drive, Radiant Heaters, Cold Fingers, Thickness Monitor, Flash
Evaporations, Multi Filament Turrets, Liquid Nitrogen Trap(LNT), substrate heater,
Electron Beam Gun 3KW Single Source/4 Source.
Technical Specification
1. Vacuum Chamber ……………………….Beljar Type
2. Chamber Size ……………………………300 mm Dia x 350 mm height (nominal)
3. Material …………………………………Stainless Steel - SS 304.
4. Base Plate ………………………………SS304, 330mm dia, with 11 Nos. ports for
Various feed through
5. Chamber Lifting…………………………Manual lifting with spring & ball cage assembly
6. CHAMBER GADGETORIES: (STD.)
a. Work holder Size …………… 225 mm Dia.
b. LT Evaporation ……………… 10 V A.C(Sequential)
c. Ion Bombardment …………… 1 set, 3.5 KV, 50 MA D.C
d. Source Shutter (manual)……… 1 set
7. VACUUM PUMPING SYSTEM
a. Diffusion pump type & speed…… ………………OD-114D, 280 Lit/Sec
b. Rotary Vacuum Pump type & speed……………… ED-15, 250 Lit/Min
c. High Vacuum Valve……………………………….100mm Butterfly Valve
d. Roughing, Backing Valve…………………………25mm size(CV-25)
e. Vacuum Gauges……………………………………Analog, Pirani, Penning Gauge
with sensors to measure
Vacuum in the range of
0.5 mbar to 1 x 10-3 mbar
and 10-3 to 10-6 mbar)
8. Ultimate Vacuum with DC-704 oil……………………… 6.5 x 10-6 mbar. without LN2 &
1 x 10-6 m.bar. With LNT
9. Utilities Required
a. Power…………………………………………… 230V AC, 50Hz, Single Phase, -
15 Amps.
b. Water at 25 C ………………………………… .. 2 Lit/min at a pressure of
1.5 - 2 Kg/cm2
1.3 Physical Vapor Deposition:-
Vapor deposited physically on the glass/metal substrate with the help of Vacuum
Coating Unit .In this Unit we have several methods to Evaporate the metal .These methods
are as follows:
1.3.1 Vacuum Thermal Evaporation
The vacuum thermal evaporation deposition technique consists in heating until evaporation
of the material to be deposited. The material vapor finally condenses in form of thin film on
the cold substrate surface and on the vacuum chamber walls. Usually low pressures are used,
about 10-6 or 10-5 Torr, to avoid reaction between the vapor and atmosphere. At these low
pressures, the mean free path of vapor atoms is the same order as the vacuum chamber
dimensions, so these particles travel in straight lines from the evaporation source towards the
substrate. This originates 'shadowing' phenomena with 3D objects, especially in those regions
not directly accessible from the evaporation source (crucible). Besides, in thermal
evaporation techniques the average energy of vapor atoms reaching the substrate surface is
generally low (order of kT, i.e. tenths of eV). This affects seriously the morpholgy of the
films, often resulting in a porous and little adherent material.
In thermal evaporation techniques, different methods can be applied to heat the material. The
equipments available in the laboratory use either resistance heating (Joule effect) or
bombardment with a high energy electron beam, usually several KeV, from an electron beam
gun (electron beam heating)
1.3.2. Sputtering
Multiple layers of metals can easily be deposited using either filament or e-beam
evaporation.
Because alloys contain materials with different vapor pressures, it is difficult to
deposit an alloy by evaporation.
One method of evaporating alloys is to melt two sources simultaneously in separate
crucibles, and control each evaporation rate separately. This can be difficult a
second possibility is to sputter the material.
1.3.4. Uniformity and Deposition Rate
Step coverage describes the conformity of a thin film grown over a feature. Step
coverage can be improved by
Sputtering will in general have superior step coverage (for aspect ratios < .5) as
sputtered atoms have random velocities. Evaporated substances tend to be
Quartz crystals are used to monitor deposition rates. The quartz oscillates at a
resonance frequency that is dependant on the thickness and atomic mass of the
film deposited onto it. When a voltage is applied across the faces of a properly
shaped piezoelectric crystal, the crystal is distorted and changes shape in
proportion to the applied voltage. At certain discrete frequencies of applied
voltage, a condition of very sharp and repeatable electro-mechanical resonance is
seen. Quartz monitors are capable of measuring thickness of less than a single
atomic layer with 0.5% accuracy.
The rotary pump is a device which is for creating vacuum in chamber upto 10-3 Torr.
In this two dumbbell shape rotary fans are creating the vacuum by sucking the air the
chamber and the air is forwarded toward the outlet valve.
(ii) Diffusion Pump - High vacuum pump operating in the ranges from 10-5 Torr to10-6 Torr
featuring relatively high pumping speed; Diffusion pumps operate by boiling a fluid, often
silicon oil, and forcing the dense vapor stream through central jets angled downward to give a
conical curtain of vapor. Gas molecules from the chamber that randomly enter the curtain are
pushed toward the boiler by momentum transfer from the more massive fluid molecules
removed from high-end applications because of the oil vapor back streaming into the vacuum
system and contaminating the chamber. Pressure 10-6 Torr or better is referred to as high
vacuum (HV). They tolerate operating conditions (e.g. excess particulates or reactive gases)
that would destroy other pumps; they have often very high pumping speeds relatively low
cost, and are vibration- and noise-free. Fig 1.3.2 shows this schematic diagram of diffusion
pump.
Salient Features:
• Compact solid state electronics
• Two gauge head capability
• Factory calibrated
• Reliable and repeatable
Pressure indications
• Excellent Zero stability
2. EXPERIMENTAL WORK
2.1 Thin Film deposition:-
The Thin Film have been deposited by using thermal evaporating Vacuum Coating.
Thin film of Al and Fe was deposited on glass substrate. The fabrication process is explained
here in following steps.
First of all thermal evaporator unit was installed in vacuum chamber the chamber
should be cleaned to avoid contamination the required material to be deposited was kept in
filament or boat with stand assembly
1. Close the chamber. We can use the Vacuum grease to tightly attach the bell jar with
chamber.
2. Now, turn on power supply and Water flow. Start the rotary pump by using puss
button switch.
3. Open back pump and turn on pirani gauge power. Wait until pressure drops to 0. 5
torr. Open the chamber in the backing mode.
4. When pirani gauge shows pressure drops above 0.05 torr. Initiate the roughing pump
and start the heater of the diffusion pump. Keep the chamber in this mode until the
pressure drops to more than 0.05 torr .It will take approx. 30 min.
Evaporation of material
In the evaporation deposition technique, the material is heated until fusion by means
of an electrical current passing through a filament or metal plate where the material is
deposited (Joule effect). The evaporated material is then condensed on the substrate. Other
ways of heating are used, such as a RF coil surrounding a graphite or BN crucible, where the
material to be evaporated is fused. The assembly of the technique is simple and results
appropriate for depositing metals and some compounds with low fusion temperature (Al, Ag,
Au, SiO, etc.).
Typical metals used as heating resistance are tantalum (Ta), molybdenum (Mo) and wolfram
(W), with vapor pressure practically zero at the evaporation temperature (Tevap = 1000-2000
°C). When a helical filament surrounds the material it is convenient that the evaporant
material wets the metal. A scheme of the deposition equipment used in the laboratory is
showed in the Fig 2.1 The thermal evaporator uses resistive energy to evaporate thin films
onto a given substrate. The thickness is controlled by the use of a quartz crystal monitor
The block diagram of thin film gas sensor is based on the fact that when sensor
sense the gas there is a change in the internal resistance, so we use a versatile continuity tester
attached with thin film .As there is a change in the internal resistance of the film the
continuity tester will check the resistance and start the Buzzer. And we can find the leakage
of the gas.
O/p Port
Comparator
2.2.3Continuity Tester:-
The continuity tester is a widely used in the electronic circuits for the purpose of
checking and testing of continuity of various electronic components. The versatile continuity
tester works according to the indication of LED to different resistances ranges. When a
component is placed between test lead A and B, one of the four LEDs will glow depending
upon of resistance of given component. The simple continuity tester has four resistance
ranges for quick and reliable fault finding in electronics equipment.
The four resistance ranges indicated by LEDs button:
¾ VLO: - Very Low resistance= resistance between test clips is smaller than
5Ω.Buzzer sound.
¾ LO: - Low resistance= resistance ranges between test clips is 5Ω and 100K Ω.
¾ HO: - High resistance= resistance ranges between test clips is 100K Ω and 15M Ω.
¾ VHO: - Very High Resistance= resistance ranges between test clips is higher than
15M Ω.
Explanation to Circuit:-
The circuit shows that three Operation Amplifiers compares the drop across the test
lead to a fixed voltage and indicate which of the two is highest by switching their output to
the positively supply level or ground- see the accompanying table.
VLO LO HO VHO
A1 0 1 1 1
A2 0 0 1 1
A3 0 0 0 1
LED D4 D3 D2 D1
The fourth OP-AMP output, (A4), function as a rectangular wave generator for
driving the buzzer. The generator is switched on by diode D7, because it is allowed to operate
when the output of A1 is low and D1 lights (VLO).After completion of the continuity tester
on the PCB shown, ranges VLO and LO are adjusted with P1 and P2. Clip the test lead to a
5Ω resistor, and adjust for adjusting P2 until D2 and D3 go out and light respectively.
Current consumption of the tester is less than 20mA. The tester can, of course, also be
powered from mains adaptor. It is recommended to a decouple R8 with a 22uF electrolyte
capacitor when the supply voltage is relatively low. To boost the sound output of the buzzer,
R16 can be replaced with a preset-adjust this until the buzzer resonates.
D1
DIODE U1
Node1 78L08 Node3
T1 IN OUT
220V C2
COM 10uF
50Hz D2 C1
DIODE 2200uF Node2
D6
R3 R5 R7 1N4148
1k R1
1k 1k 1k
R13
100k R15
100k
R9
470
U4
U3 D1VHO D5 LM339
LM339 LED1 1N4148
sensor1
R10 R16
P1 470
2k 40% 47k
U1
C1 P2 LM339 D2HO
10uF 2k 40% LED1
R11
470
U2 D3LO
LM339 LED1
+
D7 C2
1N4148 10nF BZ1
R14
100k
-
R12
470
R2 R4 R8
2.2k 40% 2.2k 40% 1.8M
R6
2.2k 40% D4VLO
LED1
OP-AMP as a Comparator
A comparator compares a signal voltage on one input terminal of the OP-AMP with a
reference voltage applied to other input terminal. The comparator circuit has only two
possible output voltages, which indicate whether the applied input voltage is greater than or
less than the reference voltage. The simplest type of comparator is the basic non inverting
comparator as shown in fig. given below.
U1A
LM324
+
Vo
+
Vin
-
+Vsat
+Vin
0
-
Vin
-Vsat
The switching of Vo from +Vsat to –Vsat or vice-versa occurs when the input voltage Vin
crosses the zero level. The circuit is therefore also known as zero crossing detectors.
The various applications of comparators arte zero crossing detectors, level detector and
window detectors.
a. IC
7809
b. CAPACITOR
C1=0.1uF
C2=2200uF
c. TRANSEFORMER
909 One
d. DIODE
IN4007 Two
4.0
V-ICHERECTRISTICS OF Al THIN FILM
3.5
3.0
Voltege(mV)
2.5
2.0
1.5
1.0
40
V-I charectristics of iron-oxide
35
30
Voltage(mA)
25
20
15
10
0.006 0.008 0.010 0.012 0.014 0.016 0.018
Current(mA)
5 CONCLUSIONS
* Thin film of Aluminum of thickness 145 kA was deposited with thermal evaporation
technique .
V-I characteristics of film was studied with four probe technique.
* The conductivity of Al thin film was found 55.17241 siemens per c.m.
* Thin film of Iron Oxide of thickness 1.623 kA was deposited with thermal evaporation
technique .
V-I characteristics of film was studied with four probe technique.
* The conductivity of Iron Oxide thin film was found 6.4548 siemens per c.m.
* The resistivity of Al and Iron Oxide was measure with the help of the formula
ρ=RA/L
WHERE
R=Resistance of the film
A=Cross sectional area of film
L=Length of the film
* The oxide thin films are best materials for gas sensing applications.
* The circuit for gas sensing device was successfully design.
* With passage of gas through the thin film the resistance of the thin film changes &
corresponding LED is glow