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HEAVEN OF SEMICONDUCTOR TECHNOLOGY

PROMISE FOR BANGLADESH

PROF. DR. ZAHID HASAN MAHMOOD


Department of Electrical And Electronic Engineering
University of Dhaka

21st April, 2018 Sylhet Engineering College


(Affiliated with Shahjalal University of Science and Technology)
Director of Center for Research on Semiconductor Technology
University of Dhaka

Member Laboratory Coordination Committee, Center for


Advance Research In Science, CARS, University of Dhaka

PhD Supervisor for research in Semiconductor Technology


Convener of the committee to prepare the concept paper to set up a new department named
Department of Material Science and Engineering

Member of the Technical Committee of a project on Nano Technology and Bio-Nano Technology,
Atomic Energy Center, Dhaka

Member of the Technical Committee of a project on Fabrication of Low Cost Solar Cell, IFRD,BCSIR

Member of the Technical Committee of the VLSI Fabrication Laboratory, Institute of Energy, AERE,
Savar.

Principal Investigator :
A new project based on Nano structure solar cell, Funded By Ministry of Science And Technology ,
GoB.
University of Dhaka
Center for Advanced  Research in Science
Department of Physics
Institute of Energy
Centre for Research on Semiconductor Technology

Bangladesh Atomic Energy Commission


Experimental Physics Division, Atomic Energy Centre Dhaka
Solar Cell Fabrication and Research Division, Institute of
Electronics, Atomic Energy Research Establishment
Bangladesh Council of Scientific and Industrial Research
Low cost Solar Cell Fabrication Laboratory, Institute of Fuel Research and Development

Malaysia
Solar Energy Research Institute (SERI),  University Kebangsaan Malaysia

India
Department of Electrical Engineering, Indian Institute of Technology Bombay, IITB,
Mumbai
Center of Excellence in Nano Electronics (CEN), IITB, Mumbai
National Center for Photovoltaic Research and Education (NCPRE), IITB
Tata Institute of Fundamental Research (TIFR), Mumbai
Outline
Facilities for the Fabrication of Semiconductor devices
available in our country, Glimpses of Recent Research.

Focusing Research Work done on the Fabrication Processing


and Characterization of Materials and Thin films for Solar
Cells.

Preparation of Al doped ZnO (AZO) Thin film.


Facilities for the Fabrication of
Semiconductor Devices Available in
our Country : Glimpses of Recent
Research
Essence of Thin Film
Thin film solar cell is one of the source for clean power generation. This
environment-friendly research is important for sustainable development for
the country .

The less material, lower cost and less area of installation are the main
challenges in the solar cell technology.

Thin-films are important for less material solar cell technology because of
their high absorption co-efficient and direct band gap energy.

The thin film technology shows comparatively very less area of installation.

Materials composition and hence band gap and other optoelectronic


properties can be graded in desired manner.

8
Device Structure
In Al In Al

n-doped n-doped

i-layer 800 nm i-layer

P-layer 315 nm P-layer

SiO2 Sapphire

(a) SiO2p-i-n (b) Saph-p-i-n


Al
Al
n-doped
n-doped
P
P
P+

(c) p+p-n (d) p-n

9
Subs trate prepa ra tion

i) SiO2 iii) PP+


Wet oxidation in Wet oxidation
atmospheric furnace at Spin PPR at back
950deg C for 20 min in 10 BHF dip 10 sec
sccm O2 and 10 sccm H2
Acetone dip 30 sec
flow. During heating the
furnace, N2 kept flowing to Boron diffusion furnace
(1000degC, 20 min)
keep positive pressure.
2% BHF dip 3 sec

Oxide layer thickness 413nm


measured using Refractometer
spectroscopy.
Sheet Resistivity
27ohm/square
10
Device Fabrication
HWCVD PIII
P-doped layer RF power 1000W,
Nucleation, 400 degC for Frequency 5kHz, period
200 sec at SiH4:H2:B2H6= 200s, Duty cycle 10%,
1:15:5 width 20s, substrate
Epitaxy, 540 degC for 800 bias -2kV, 20 mA,
sec at SiH4:H2:B2H6= 5:10:5
distance 9 cm*.
Intrinsic layer PH3 20 sccm for 30 sec.
Epitaxy, 540 degC for 1200
sec at SiH4:H2= 8:20

11
Device Fabrication
RTP Annealing Laser (CW-1070nm)
Annealing
600 degC for 600 sec at Power 0.8 W
N2 & O2 ambient Scan speed 20mm/sec
Pulse duration 9s
Fluences 10 J/cm2
Frequency 10kHz

950 degC for 5 sec at N2 Pulse duration 10s


ambient Fluences 11 J/cm2

12
Impurity concentration

TOF-SIMS profile of boron doped


intrinsic poly silicon film using *TOF-SIMS profile of phosphorous
HWCVD doped silicon film using PIII

13
Electrical Measurements

* Activation energy E = ln R1  ln R2  8.6 105


1 1 
  
 T1 T2 

[*] H. Fritzsche, Journal of Non-Crystalline Solids, 49(1971) 62.

14
Electrical Measurements
Intrinsic Activation Energy
Resistance in Resistivity
poly From 1/T Vs
ohm ohm-cm
Silicon Resistivity graph
SiO2-Si 1108 2105 0.55 eV
Saph-Si 2.9108 5105 0.42 eV

· Intrinsic poly silicon film on sapphire is more resistive than the


film on SiO2
· Activation energy of poly silicon film on sapphire shows
substrate effect.
· This effect may be due to broken and dangling Si-H bond. This
can be reduced using further H2 dilution.

15
I-V measurement
 Dark and illuminated I-V
measurement were taken
using AAA class one sun
simulator by ABET
Technology
 In forward bias it shows
diode characteristics
 In reverse bias it shows
leakage current.
 Photo response is very low
on one sun illumination
 Series resistance may
effect the forward current
Figure: Dark and illuminated I-V on
sample (c) p+p-n

16
Improvement of photoconductivity
Hydrogen passivation

 An atomic hydrogen soaking step while cooling the


sample ( after deposition of the film at 540oC)* ,
 A thin deposition (~100A) of a-SiH4:H2 at about
200oC , before cooling the substrate to room
temperature.

*40th Photovoltaic Specialists Conference, June 7 ‐13, 2014, Denver, Colorado, USA.
http://ieeexplore.ieee.org/xpl/articleDetails.jsp?arnumber=6925162
25 November 2016 ... ... ... FENI UNIVERSITY 17
Photoconductivity

Photo current spectral response

 The decrease in photoconductivity at shorter wavelengths (λ <


400 nm) indicates surface recombination and may be improved by
better passivation

 The decrease in photoconductivity at longer wavelengths (λ >


800 nm) is related to low value of α (absorption coefficient).
18
Photoluminescence (PL)

 Multiple peaks are from interference from glass substrate


 Emission spectrum is very broad from 0.9 eV to 1.1 eV.
 The decrease in intensity at 1.4 eV is due to cut-off wavelength of the InGaAs
detector.
 Noise around 1.2eV is due to water vapor absorption in the air.
 There are two radiative transitions providing : i) emission from near band edge and ii)
emission from deep level defects[*,**]

19
Conclusion
 p-n junction diode fabricated on SiO2 and
sapphire substrates
 On white light illumination diode shows little
photocurrent.
 Improvement of film was done using hydrogen
passivation
 Passivated film showed an increase in photocurrent
in visible spectrum range.
 PL emission observed in room temperature which
shows that the film was well passivated.

20
Substrate selection
Oxidised Silicon Wafer at 950 degC for 20 min in wet
oxidation furnace. (180 nm)
*TiO2 deposited on ITO coated glass
Sapphire (Al2O3) hexagonal c-plane oriented
Nickel 5% Tungsten (EVICO Germany)

* Tandeep S. Chadha, School of Engg & Appl. Sci. Washington Univ. St. Louis

21
Approaches to the intrinsic film growth
 Nucleation at 400 degC for 120
sec using 20 H2 : 1 SiH4 (4.7%)
 Thick film growth at 540 degC for
29 minuets at maximum 20 H2 : 8 SiH4
(29%)
 Six Step Ramp Run
 Film thickness 2200 nm
22
Approaches to the p-doped film growth
 Nucleation at 400 degC for 120 sec
using 15 H2 : 1 SiH4: 5 B2H6
 Thick film growth at 540 degC for 18
minuets at maximum
10 H2 : 5 SiH4 : 5 B2H6
 Six Step Ramp Run
 Film thickness 1085 nm
23
Electrical Measurements
Intrinsic Activation Energy
Resistance Resistivity
poly From 1/T Vs
in ohm ohm-cm
Silicon Resistivity graph
SiO2-Si 1108 2.105 0.55 eV
Saph-Si 2.9108 5105 0.42 eV
TiO2-Si 3105 5107 0.24 eV

 No photoconductivity observed.

24
Surface Topography (Nucleation)

(a) SiO2 (b) TiO2

(c) Sapphire (d) Nickel

25
Surface Topography (Epitaxial Growth)

TiO2 Sapphire

26
Surface Topography (Epitaxial Growth)

SiO2 Nickel

27
Surface Topography (Epitaxial Growth)
 Grain size and shape of film on SiO2, TiO2 and
Sapphire are same (length 300 nm & width 100
nm)
 For Nickel grain sizes are 2 microns, Column
length is 12 micron
 These films are of 2200nm and films do not have
any substrate effects but Nickel

28
Optical Measurements

Sapphire TiO2

29
Optical Measurements

Sapphire
30
Optical Measurements
 Optical band gap of Thick film on Sapphire is 1.32 eV
and for TiO2 is 1.5 eV.
 These film contain both amorphous and crystalline
phase
 For Sapphire, TiO2 and Nickel, reflectance is below
20 % and for SiO2, reflectance is below 30 % in visible
range.

31
P-doped films Surface topography

SiO2-PSi TiO2-PSi

32
P-doped films Surface topography

Nickel-PSi Sapphire-
PSi
33
P-doped film Optical Measurements

Sapphire Nickel

SiO2 TiO2

34
P-doped film Optical Measurements
 For SiO2 reflection is 40 % in visible range
 For TiO2 reflection is below 20 % in visible range
 For Sapphire, reflection is below 30 % in visible range
 Reflection from nickel substrate is below 20 % in
visible range.

35
P-doped film Optical Measurements

Sapphire TiO2
 In visible range transmission of p-doped sapphire
is very low, nearly 15 % max, and for TiO2 its below
3%

36
Conclusion
 We have explored the viability for the growth of (220)
oriented crystalline poly silicon films on SiO 2, Sapphire,
TiO2 and Nickel substrates.
 Grain size was as large as 700 nm reported for 43 % SiH 4
concentration and 400 nm with 29 % SiH 4.
 At 29% SiH4 the film got highly sticky to all substrate.
The thicknesses of thick film were 2.2 micron with 29 %
SiH4 at 540 degC.
 These films are suitable for photovoltaic application as
Reflection as well as transmission in visible range is 20
to 40 %
37
Characterization of Silicon Nanowires
Synthesized by Electroless Metal Deposition

In this work silicon nanowires (SiNWs) are


grown on p-type Si wafer surface following a
top-down approach. It is simple electroless
metal deposition and wet etching process.

It is a simple, low cost and effective method to


synthesize SiNWs with unique optical
characteristics

38
SEM images of hexagonal SiNWs for the 60 sec
Ag deposition duration and
30 min etching duration

Published in the Proceedings of IWPSD 2015, India

39
EDX is also carried out to see the
composition of our samples. It reveals the
total count for Si and Ag, which are found
~97% and ~3%, respectively.
40
Surface Texturing
One of the essential process in solar cell manufacturing of
crystalline silicon is surface texturing. Before texturing wafer
are cleaned by saw damage removal method.
Well textured surface enhances the internal quantum
efficiency by enhancing the effectiveness of light absorption.
The average etch rate of silicon wafer surface using KOH/IPA
solution in our experiment was 1.19 µm /min whereas the
standard single side etch rate is about 2.1 µm/min.
Normally percentage reflectance of textured wafer is in
between 12 to 18%. For all the etching method satisfactory
reflection reduction found.
41
Different Etching Methods
 Etching Method 1
No. Solution Time Temperature
01 Acetone (C3H6O) 2
minutes
02 Methanol(CH4O) 2
minutes
03 Dehydration bake 15 80°C
in hot plate minutes

This is a acidic solution. Weight loss and brightness change


were negligible. Here Etching rate is slow. This etching
method is introduced in BAEC solar cell laboratory.
42
Texuring Method
No. Solution Ratio Time Temperatur
e
01 KOH : IPA : H2O 10 70°C
(DI) minute
1 gm : 5 ml : 125 ml s

02 DI Water 1
minute
03 HF:H2O (DI) 3
1 gm : 50 ml minute
s
04 DI Water 1
minute

43
Percentage Reflectance
 (%) Reflectance graph of textured sample etched by methods 1.2
and 3 with respect to mirror image
45

40 Reflectance (%) Vs wavelength


35

30
Reflectance (%)

25
Etching method 1
20 Etching method 2
Etching method 3
15

10

0
400 500 600 700 800 900 1000 1100 1200 1300
Wavelength (nm)

only 14%, 21% and 17% light is reflected from the textured wafer surface
etched by method 1, 2 and 3 respectively as these are the lowest values.
44
Scanning Electron Microscope Images
SEM images of wafer surfaces etched by method 1,2 and 3 respectively: [5]

For Si wafer etched by method 1 bigger pyramids were Etched


Etched by found. by For Sample
Etched by
Si wafer etched
method 1by method 2 smaller pyramids
method 2 were found and
method 3 they were
densely distributed. For Si wafer etched by method 3 the SEM image was
not clear to describe.

45
NANOPHYSICS LAB
SCANNING TUNNELING MICROSCOPE

The scanning tunneling


microscope (STM) is an
instrument for imaging
surfaces at the atomic
level. It is a type of
electron microscope that
shows three-dimensional
images of a sample
surface. It is based on the
concept of quantum
tunneling.
ATOMIC FORCE MICROSCOPE

Atomic force microscopy


(AFM) is a type of scanning
probe microscopy, widely used
in topographic imaging at high
resolution on the nanometer
scale.
SOURCE MEASUREMENT UNIT
Model: KEITHLEY
2401 SourceMeter

• Source voltage
from 5μV to 21V;
measure voltage
from 1μV to 21V
• Source current
from 50pA to
1.05A; measure
current from
10pA to 1.055A
• Maximum
source power
22W
The SMU is a special kind of instrument that can work as a
constant current source or as a constant voltage source. It
simultaneously sources to a pair of terminals at the same time
measuring the current or voltage across those terminals.
(A) KEITHLEY 2200-30-5
programable power supply
30V, 5A
(B) KEITHLEY 2110 5 1/2 DIGIT
MULTIMETER
(C) KEITHLEY 2100 6 1/2 DIGIT
MULTIMETER
OVEN VACUUM OVEN

Type: ED 53 Model: Shel Lab 1407 economy vacuum


BINDER ED series heating oven: oven-Analog temperature control
routine drying and sterilization The general purpose Is the preparation
applications up to 300 °C (572 °F). or testing of materials is done at
approximately atmospheric pressure.
MUFFLE FURNACE

Thermo Scientific Thermolyne


Furnace
Type FB 1400
Temperature: Operating range
(continuous): 982˚C;
(Intermittent): 1100˚C

The furnace is ideal for most


types of organic and inorganic
samples, heat treating small steel
parts, performing ignition tests,
conducting gravimetric analysis
and for the determination of
volatile and suspended solids.
SPIN COATER

Laurell Technonogies
Corporation
WS-650 Spin processor

Spin Coating is a procedure used


to apply uniform thin films to flat
substrates. An excess amount of
a solution is placed on the
substrate, which is rotated at
high speed in order to spread the
fluid by centrifugal force.
Rotation is continued while the
fluid spins off the edges of the
substrate, until the desired
thickness of the film is achieved.
LAUDA VISCOCOOL

LAUDA VISCOCOOL 6
Viscothermostat with Peltier
cooling and ECO SILVER control
head
This device is a Viscothermostat
with Peltier cooling and
transparent bath and is specially
designed for applications of
capillary viscometry close to room
temperature. In this respect it
involves a cooling, heating bath
thermostat, also designated as a
cooling thermostat in the
following. It is used for cooling/
heating liquids. The device is
constructed as a double-chamber
system.
ULTRASONIC BATH, DIGITAL BALANCE AND HOTPLATE STIRRER
James Products Limited
Sonic series 4500M Ultrasonic Cleaner.

Ultrasonic cleaning is a process that uses


ultrasound (usually from 20–400 kHz) and an
appropriate cleaning solvent (sometimes
ordinary tap water) to clean items. These
ultrasonic baths or cleaners have large
transducer areas and tanks that produce a high-
powered ultrasonic intensity throughout the
entire oscillating tank.

Sartorius
Analytical
Balance

Thomas Scientific
Hot Plate
SHIMADZU CORPORATION Lab Tech
Electronic Analytical Balance Hotplate Stirrer
Model: AW, AX and AY series
SOLDERING STATION & OSCILLOSCOPE
THANK YOU
VERY MUCH

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