Hands on training on fundamentals of

Material science

For the partial fulfillment of the requirement for the degree of Master

Of science in Physics

B.JEEVITHA

PG Department of physics

Justice Basheer Ahmed Sayeed College for Women’s

Chennai-600 018

Internship done under the guidance of

Dr. D. Durgalakshmi

Assistant professor

DST-INSPIRE faculty

Department of Medical Physics

CEG campus

Anna University

Chennai-600 025.

May 2019
 CERTIFICATE

This is to certify that the internship work entitled “Hands on training on the fundamentals of
Material Science” submitted by B.Jeevitha during the academic year2019-2020 is bonafide
work done by her at Department of Medical Physics, CEG campus, Anna University, Chennai-
25 for the period of 21 days ( From 02-05-2019 to 29-05-2019) under my supervision and
guidance.

Head of the Department External Guide

 BONAFIDE CERTIFICATE

This is certify that the internship work done by B.JEEVITHA entitled “Hands on training on
the Fundamentals of Material Science” during the period from02.05.2019 to 29.05.2019, a
period of 21 days at Department of Medical Physics, CEG campus, Anna University, Chennai-25
is a bonafide work.

Dr. Maryam Usmani B.Jeevitha

Assistant professor PG Department of Physics,

PG Department of Physics, JBAS College,

JBAS College, Chennai-600018.

Chennai -600 018.

 ACKNOWLEDGEMENT
First of all, thanks to god and my parents whose blessings are there with me in every
execution of my work and helped me to complete this work successfully.

First I would like to thank Dr. P. ARUNA, Head of the Department of Medical
Physics, CEG campus, Anna University for her kind support and encouragement.

I owe my sincere gratitude to Mentor Dr. D. DURGALAKSHMI, Assistant professor,

DST-INSPIRE faculty, Department of Medical Physics, CEG campus, Anna University for
her valuable support and guidance throughout the internship.

I would like to express our sincere thanks to Research Scholar of Department of

Medical Physics, Mr. J. Mohanraj and Ms. S. Prabha for their strong and unconditional
support throughout my internship.
 INDEX

1. INTRODUCTION:

1.1. Introduction to Nanoscience and Nanotechnology

1.1.1 Definition

1.1.2 Classification of nanoparticles

1.1.3 Properties of nanoparticles

1.1.4 Synthesis of Nanoparticles

1.2. Introduction to sol-gel method

1.3. Introduction to stober method

1.4. Introduction to Bio-materials

1.5. Introduction to silicon dioxide Nanoparticles

2. CHARACTERIZATION:

2.1. FTIR spectroscopy

3. INSTRUMENTS USED:

3.1. Magnetic stirrer

3.2. Top load balance

3.3 Centrifuge

3.4. Micropipette

4. SYNTHESIS METHOD:

4.1. Cleaning procedure

4.1.1 Preparation of Aquaregia

 4.2 Preparation of 1N HcL

4.3. Preparation of silicate bio-active glass

4.3.1 By using dry gel method

4.3.2 By using stober method

4.3.3. By using microwave oven method

5. RESULT AND DISCUSSION:

5.1. FTIR spectrum of silicate bio-active glass by using dry gel method

5.2. FTIR spectrum of silicate bio-active glass by using stober method

5.3. FTIR spectrum of silicate bio-active glass by using microwave method

6. LAB VISIT:

7. REFERENCE
 INTERNSHIP REPORT

DAY 1: 02/05/2019(9:30 AM-5:00PM)

 Attended lecture on “The History of Microscope”.

 Lecture was delivered by Dr. AJAY RAKKESH (University of Madras).
 Lecture was based on “SEM & TEM” microscope.
 Learnt about the basics of crystal structure.

DAY 2: 03/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Where theoretician met experimental physics”.

 Lecture was delivered by Dr. HANNAH RUBEN (WCC College).
 Lecture was based on “Born Oppenheimer approximation, Slater determinant,
density of state, shape memory alloy”.
 Learnt about basics of nanoscience, a glance on fundamental of nanoscience and
nanotechnology.

DAY 3: 06/05/2019(9:30 AM-5:00PM)

 Attended lecture on “What physicist need to understand”.
 Lecture was delivered by Dr. Raja Lakshmi (MIT).
 Lecture was based on “Green chemistry, anticancer agents, angiogenesis effect on
embryo.
 Learnt about how to download journals and how to write reference.

DAY 4: 07/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Classical and Quantum mechanics”.
 Lecture delivered by Mr. Premkumar (Anna University).
 Lecture was based on “Newtonian mechanics, Heisenberg uncertainty principle and
Wave function”.
 Learnt about how to study journals.
DAY 5: 08/05/2019(9:30 AM-5:00PM)

 Lab visit to University of Madras (Nanoscience and Nanotechnology lab).

 Visit was based on “working of SEM &TEM”.
 Learnt about introduction of Biomaterials.

DAY 6: 09/05/2019(9:30 AM-5:00PM)

 Attended lecture “ Harvesting the solar energy”

 Lecture delivered by Dr. Tamilselvan (IIT Madras).
 Lecture was based on “Solar energy, solar cells, basic structure of Photo voltaic
cells”.
 Learnt about physical and chemical properties of materials.

DAY 7: 10/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Maths an essay language to understand physics”.

 Lecture delivered by Dr. Sivaraman (Pi Maths association).
 Lecture was based on “Number theory, pi, Ramanujam’s formula, Fourier
transform”.
 Learnt about how to plot graph using origin software.

DAY 8: 11/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Programming of electronic devices” (Hands-on).

 Hands on given by Mr. Mani (University of Madras).
 Morning session was based on “Arduino pin configuration, evolution of Arduino
UNO, overview of C-programming”.
 Afternoon session was based on “demonstration of blink LED, automatic street light
lamp using LDR and LM35 temperature sensor”.

DAY 9: 13/05/2019(9:30 AM-5:00PM)

 Attended lecture on “The whole is more than the sum”.

 Lecture delivered by Sitabhra Sinha (IMSC).
  Lecture was based on “complex system, simple model and cardiac arrhythmia”.
 Learnt about safety measures while handling chemical compounds in laboratory.

DAY 10: 14/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Theory? Or experiment –A perspective from optics”.

 Lecture delivered by Dr. N. Yogesh (University of Madras).
 Lecture was based on “Ray optics, discovery of law of refraction, how negative index
is possible”.
 Another lecture on “Band structure: the storyteller of material properties”.
 Lecture delivered by Dr. Ashwin Kishore (Upsala University).
 Lecture was based on “Band structure, Brillouin zone, photo catalytic properties”. .

DAY 11: 15/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Radiography and imaging technique”.

 Lecture was delivered by S.Tamilselven (Mother Theresa University).
 Lecture was based on “Radiography imaging, CT scan, MRI, Gamma camera and
ultrasonic scan”.
 Learnt about how to prepare aqua regia and cleaning of beakers.

DAY 12: 16/05/2019(9:30 AM-5:00PM)

 Attended lecture on “Government job opportunities”.

 Lecture was delivered by Mr. Prasanth (Shankar IAS academy).
 Lecture was based on “what are job opportunities and how to prepare for exam”.
 Learnt about silicate bio-active glass synthesis using Sol-gel method.

DAY 13: 17/05/2019(9:30 AM-5:00PM)

 Science project demonstration was conducted.

 Projects were displayed and prize distribution happened.

DAY 14: 20/05/2019(9:30 AM-5:00PM)

  Synthesis of silicate bio-active glass by dry-gel method.

DAY 15: 21/05/2019(9:30 AM-5:00PM)

 Synthesis of silicate bio-active glass by Stober method.

DAY 16: 22/05/2019(9:30 AM-5:00PM)

 Centrifuging samples by making them neutral.

DAY 17: 23/05/2019(9:30 AM-5:00PM)

 Synthesis of silicate bio-active glass by using microwave oven.

DAY 18: 24/05/2019(9:30 AM-5:00PM)

 Studied about FTIR characterization.

DAY 19: 27/05/2019(9:30 AM-5:00PM)

 Silicate bio-active glass samples analysis using FTIR analysis.

DAY 20: 28/05/2019(9:30 AM-5:00PM)

 Plotting graph for FTIR data.

DAY 21: 29/05/2019(9:30 AM-5:00PM)

 Started report submission work

 1. INTRODUCTION:

1.1. INTRODUCTION TO NANOSCIENCE AND NANOTECHNOLOGY:

Nanoscience, Nanotechnology and Nanoparticles have become common words not only
in research but also in normal life. The concept “NANOTECHNOLOGY” was first highlighted
by Noble Laureate, Richard Feynman (1959) in his lecture “There are plenty of rooms at the
bottom”. Nanoparticles were used in several industries such as electrical, biological, chemical,
textile industries etc., Depending upon their size Nanoparticles play an important role in
electronic devices, antimicrobial expression, catalytic and electromagnetic properties

1.1.1 DEFINITION:
 NANOSCIENCE: It is the study of phenomena Nanoparticles of materials
at atomic, molecular and macromolecular scales were properties differ
significantly from those at a larger scale.
NANOTECHNOLOGY: There are design, characterization, Production
and application of structures, devices and systems by controlling shape and
size at nanometre scale.

Figure 1: Nanoscale
 The prefix ‘Nano’ derived from Greek word for dwarf.
 One nanometre = one billionth of the meter (10-9) example: a human hair is
approx.80, 000nm wide and a RBC is approx.7, 000nmwide.
1.1.2 CLASSIFICATION OF NANOPARTICLES:
Nanoparticles can be created with various modulation dimensionalities are defined by

Richard w. Siegel as:

Fig2: Classification of Nanoparticles- (a):0-D Nanoparticles, (b):1-D

nanoparticles, (c):2-D nanoparticles and (d): 3- D Nanoparticles.

TYPES OF DIMENSIONS EXAMPLES

0-D nanoparticles Atomic clusters, filaments and cluster assemblies

1-D Nanoparticles Nanotubes,nanorods and nanowires

2-D Nanoparticles Nano film, Nano layer, Nano coating

3-D Nanoparticles Nanocrystals etc.,

1.1.3.PROPERTIES OF NANOPARTICLES:

Nanoparticles often have unexpected visible properties because they are small enough to
confine their electrons and produce quantum effects. The physical and chemical properties of
matter changes at the Nano level. It has superior properties than bulk materials like,
 Magnetic properties
 Optical properties
 Mechanical strength
 Thermal stability
  Electrical conductivity etc.,

1.1.4 SYNTHESIS OF NANOPARTICLES:

All the synthesis/deposition technique of nanoparticles are divided into two categories
based on the phase of starting material .There are

 Top-down approach.
 Bottom-up approach.

BOTTOM-UP Approach:

In the BOTTOM-UP approach, molecular components arrange themselves into more

complex assemblies from the bottom using the concept of molecular self-assembly.

For example: growth of crystal

Physical& chemical processing method:

 Physical technique:
Example: Physical vapour deposition (PVD)
 Chemical technique:
Example: CVD, Self- assembled monolayer: electrolytic deposition, sol-gel method,
micro emulsion, and pyrolysis.
TOP-DOWN approach:

In the TOP-DOWN approach, nanomaterials are synthesized by breaking down of bulk

solids into Nano sizes

For example: Physical processing techniques:

 Mechanical methods:cutting,grinding,etching,ball milling etc.,

 Lithographic techniques: photo lithography, electron beam lithography etc.,
1.2. THEORY ABOUT SOL-GEL METHOD:

Sol-gel process is the spontaneous formation of a dual phase material (gel), prepared
from the solution (sol) containing inorganic precursors ad stabilizing agents with hydrolysis and
condensation reaction.(fig 3)

fig 3: sol-gel process

PROCESS:

i. The sol-gel process is a wet-chemical technique that uses either a chemical sol or
colloidal particles(sol with nanoparticles) to produce an integrated network (gel)
ii. Metal oxides and metal chlorides are typical precursors. They undergo hydrolysis and
polycondensation reactions to form colloidal system composed of nanoparticles
dispersed in a solvent. The sol evolved then towards the formation of a inorganic
continuous network containing liquid phase (gel).
iii. Formation of metal oxides involves connecting the metal centres with Oxo-(M-O-M) or
Hydroxo-(M-OH-M) bridges, therefore generating metal Oxo or metal-Hydroxo
polymers in solution.

Hydrolysis:

Si - OR + HOH Si – OH +ROH
 Condensation:

Si – OH + HO – Si Si –O - Si + H2O

Si – OR + HO -Si Si –O - Si + ROH

iv. Further, transformation of the gel phase is driven by the evaporation of the solvent and
the subsequent formation of the xerogel phase (or) if it supercritical temperature gel
phase convert in to aerogel (or) if it is directly precipitated and dried then gel becomes
uniform powder (or) if it undergoes spinning gel phase converted in to fibres.(fig 4)

fig 4: sol-gel process overview

GELATION:

The transition from a system with finite branched polymers to infinite molecules is
called “sol-gel transition” (or) “gelation” and the critical point where gel appears is called the”
gel point”(fig 5)

fig 5: gelation process

1.3. THEORY ABOUT STOBER METHOD:

 The Stober process is a chemical process used to prepare silica particles of
controllable and uniform size for application in material science.
 It is an example of a sol-gel processes where a molecular precursor is first
reacted with water in an alcoholic solution, the resulting molecules then
joining together to form larger structure.
 The reaction produces silica particles with diameter ranging from 50nm to
2000nm, depending on conditions.
 In 1999 a two stage modification was taken for controlled formation of silica
particles with small holes.
 The process is done at low pH in the presence of a surface active molecule.
  Colloidal particles are much larger than normal molecules or nanoparticles.
 But, mixing with liquid colloids appears bulky whereas nanoscience molecules
always look clear.
 The precursor for synthesizing the colloids consists of ions of metal oxides and
aloxysilanes.
 Most widely used are TMOS (tetramethoxysilane) and TEOS
(tetraethoxysilane) which forms silica gel.

The Stober process is a Sol-gel approach to prepare uniform spherical silica material.

1.4. INTRODUCTION TO BIOMATERIALS:

 Biomaterials is any substance that has been engineered to interact with biological system
for a medical purpose either a therapeutic (treatment, augment, repair or replace a tissue
function of the body) or a diagnostic one.
 The study of biomaterials is called biomaterials science or biomaterial engineering

BIO-ACTIVE GLASS:
Bioactive glass is an amorphous solid without long range order in its structure. The
oxides used to synthesis glass are classified in to three groups according to their functions

i. Network-forming oxides (SiO2,P2O5).

ii. Network-modifying oxides (CaO and Na2O).
iii. Intermediate oxides (ZnO,Al2O3).

Basic components of bioactive glass and ceramics are SiO2 , P2O5 ,CaO, Na2O and also
B2O3,P2O5 ,CaO, Na2O.By varying all of these component different forms of bioactive glass can
be made. Bioactive glasses have investigated for decades and have shown good results in bone
regenerative and dentistry. The Bio compatibility of bioactive glasses generally depends on

the silicate part of the bioactive glass.

Applications of Bio-active glass:

Bio-active glasses investigated for decades and have shown good results in bone
regenerative, dentistry etc.,

 In dentistry, powdered bio-active is used as a tooth fillers

 In bone regenerative cases, the graft- bone bonding of bioactive glasses starts with
release of soluble ions after which a silica gel layer is formed on the bioactive glass
surface. After the formation of the silica gel layer amorphous calcium phosphate
precipitate on this layer where they form a natural hydroxyl apatite apatite layer due
to crystallization The hydroxyl apatite layer activities the osteoblastic cells to start the
formation of new bone

1.5.INTRODUCTION TO SILICONE DIOXIDE (SiO2) Nanoparticles:

Silicon dioxide (SiO2) is an Oxide of silicon which is in the group-14 of periodic table. It
is also called as silica with the chemical formula SiO2. It is most commonly found in nature as
quartz and in varies living organisms. When silicon is attacked by bases such as aqueous
hydroxide (example: sodium hydroxide) to form silicates.

Si(s) +4NaOH (aq) → [SiO4]-4

Properties:

Chemical formula - SiO2

Other names - Quartz, silica etc.,

Molar mass - 60.08 g/mol.

Density - 2.196
Melting point - 1,713 C
Boiling point - 2,950 C
Bond length - 148.3pm
Appearance - Transparent solid
(amorphous)
white(powder/sand)

Application:

 For protein adsorption and separation

 For nucleic acid detection and purification
 Drug and gene delivery

 Imaging contrast agents construction

 2. CHARACTERIZATION TECHNIQUES:

2.1FTIR SPECTROSCOPY:
Fourier-transform infrared spectroscopy is commonly known as FTIR
Spectroscopy is a technique used to obtain an infrared spectrum of absorption or emission of
a solid, liquid or gas. (fig 6)

FTIR spectroscopy uses Fourier transform (a mathematical process) to convert the raw data
into actual spectrum.

Infrared Spectroscopy:
 Energies of infrared radiation correspond to vibrational energies of molecules
 Like fingerprint no two unique molecular structures produce the same infrared spectrum.
 IR spectroscopy is a vibrational spectroscopy as it is based on the phenomenon of
absorption of infrared radiation by molecular vibration.
 It gives information about the molecular structure of the material.
 Both organic and inorganic materials can be analyzed.
 Commonly, the vibrational spectroscopy covers a wavenumber range from 200 to
4000cm-1

Fig 6 :Fourier-transform infrared spectroscopy

PRINCIPLE:
 FTIR works on the principle that the most molecules absorb light in the
infrared region of the electromagnetic spectrum.
 This absorption corresponds to the specified bond present in the molecule.
 Based on the bond and using wavenumber for the bond the functional
group present in the material is identified.

WORKING AND INSTRUMENTATION:

 FTIR uses a system called an interferometer to collect a spectrum.
 The interferometer consists of source, beam-splitter, moving mirror, fixed
mirror and detector.
 Infrared energy is emitted from a black body source.
 The energy goes from the source to the beam splitter which splits the beam
into two parts
 While one half is transmitted to a moving mirror, the other half is reflected to
a fixed mirror.
 The moving mirror moves back and forth at a constant velocity.
 The two beams are reflected back from the mirrors and recombined at the
beam-splitter.
 The beam from the moving mirror travels a different distance than the beam
from the fixed mirror.
 Consequently an optical path difference (δ) is introduced by change in
position of moving mirror.
 When the reflected beams are combined, some of the wavelength recombine
constructively and some destructively creating interference pattern.
 A plot of light interference periodically, with continuous change of the value
δ.
 A plot of light interference intensity as the function of optical path difference
is called an interferogram.
  This interferogram then goes from the beam splitter to the sample ,where
some energy is absorbed and some is transmitted
 The transmitted portion reaches the detector.
 The interferogram received is converted into spectrum by using algorithm
called a Fourier Transform using a computer.
∞
𝟏
𝑭(𝝎) = ∫ 𝒇(𝒕)𝒆−𝒊𝝎𝒕 𝒅𝒕
√𝟐𝝅 −∞

 Thus Fourier transformation converts an interferogram

(intensity Vs optical path difference) into infrared spectrum
(intensity VS wave number) plot.
 A reference or background single beam is also collected
without a sample and the ratio of the sample single beam to the
background single beam is expressed as a transmittance
spectrum.

What information can FTIR can provide?

 It can determine the quality or consistency of a material.
 It can determine the amount of components in a mixture.
 It will take few seconds to record.

ADVANTAGE:

 Non-destructive technique.
 Provides a precise measurement (accurate)
 It can increase speed, sensitivity.
 Optical output is much higher resulting on in lower noise
level.
 The instruments employs He-Ne laser as an internal
wavelength the calibration standard.
 These instruments are self-calibrating and no need to be
calibrated by the user.
 3. INSTRUMENTS USED:

3.1Magnetic stirrer:
 A magnetic stirrer is a device widely used in laboratories and consists of rotating
magnet and stationary electromagnet that creates a rotating magnetic field. It is
shown in figure 7
 This device is used to make stir bar immerse in a liquid for quick spin or stirring
to mix a solution uniformly

fig 7: magnetic stirrer

 A magnetic stirrer generally includes a couple heating system for heating
 A stir bar size varies from a few millimetres to few centimetres. It is shown in
figure 8
 fig 8: stir bar

3.2. Topload balance:

Top load balance also called as an analytic balance, are highly sensitive lab instrument
designed to measure the mass accurately. It has readability range between 0.1mg to 0.01mg.(fig
9)

Preparing the balance before use:

 Before weighing anything on the analytic balance you must make sure that it is levelled
and zeroed
 To check levelling on the balance, use levelling bubble on the floor of the weighing
chamber. If it not centred, centre it by turning the levelling screws on the bottom toward
the back of the balance.
 Close all the chamber doors and press the control bar to make it zero

Weighing a substance:
 Place a butter sheet (for solid) or a weighing container (for liquid)on the balance pan and
close the doors
 Tare the container/butter sheet by briefly pressing the control bar. The readout will read
zero with the container sitting on the pan. This allows the mass of your sample to be read
directly
  Add the substances to be weighed without spill it on the balance pan
 With the sample and container/butter sheet, close the chamber doors and read the display
to find the mass your sample.

Cleaning up and shutting down the balance:

 When you done, properly cleaned up with chemicals (acetone) that may have spilled on
it.
 Then, the balance can be turned off by lifting up gently on the control bar.

fig 9 : Top load balance

3.3. Centrifuge:
A Centrifuge is a type of research equipment that spins the liquid suspension at high
rotation rates to separate it into distinct layers based on density.(fig 10)

fig 10: centrifuge device

Load the sample into centrifuge:

 Place a centrifuge tubes on a firm, level surface (fig 11)
 Choose the proper rotor to use at the speed you need
 Place the tube directly opposite to each other in the Centrifuge
 Enter the centrifuge speed by RPM and set time as you need but it do not exceed
15minutes
 Turn off the Centrifuge if it is wobbling
 fig 11: inner view of centrifuge
 Open the lid only after the rotor completely stopped
 Remove the tubes carefully after the centrifuge as completely stopped spinning
 At last wipe down rotor and after each use leave the lid open so it can air out and remain
dry

3.4.Micropipette:
 The micropipette is used to transfer small amount (<1ml) of liquids.
 The scale on micropipettes are in microliters (1000μl = 1ml).
 They are used in conjunction with disposable sterile plastic tips.(fig 12)

Load the sample:

 The plunger will stop at two different positions when it is depressed.
 Push the plunger down slowly to the point of first resistance: this is load volume.
 Because this first stopping point is dependent on the volume that is being transferred, the
distance you have to push the plunger to reach the point of initial resistance will change
depending on the volume being pipette.
 Fig 12. Parts of Micropipette.
 While holding the plunger at the load volume set point, put the tip into the solution so
that it is immersed just enough to cover the end (3-4mm), not as deep as possible.
 Slowly release the plunger to draw up the liquid making sure to keep the tip immersed.
 Visually inspect the load to make sure it is correct – there should be no air space in the
distal end tip.

Deliver the sample:

 Place the tip into the receiving vessel.(fig 13)
 Depress the plunger to the point of initial resistance.
 Wait 1 second.

Fig 13. Proper way of delivering sample.

 Continue to press the plunger all the way to the bottom – this expels all the liquid.
  Then, without releasing the plunger, withdraw the tip.
 While holding the tip over an appropriate waste receptacle, press the discharge slider on
the back of the grip.
4.SYNTHESIS METHOD:
4.1.CLEANING PROCEDURE:

PREPARATION OF AQUAREGIA:
 Aquaregia is a corrosive acid mixture made by combining nitric acid and
hydrochloric acid.
 It is used to dissolve gold, platinum and Palladium.

fig 14:aquaregia

Preparation:

 Usual ratio of acids is 3 parts of hydrochloric acid and 1 part of nitric acid.

 When mixing the acid is important to add the nitric acid to the
hydrochloric acid not the other way around.

Safety measures:

 Make and use Aquaregia solution inside fume hood.

 Prepare the minimum value needed for your application.
  Make sure glassware is cleaned.
 Wear safety goggles.
 Wear a lab coat and gloves
 If you spill acid on your skin, wipe them off immediately and rinse with
lots of water.
 In case of inhalation, move immediately to fresh air.
 In case of ingestion, rinse mouth with water.

4.2.PREPARATION OF 1N HCl:

Calculation:
1N HCL:

Density = 1.2.

Assay = 37%.

Molecular weight = 36.46.

Density x Assay xtotal litre

Molarity = Molecular weight

1.2 𝑋 0.37 𝑋 1000

= 36.46

= 12.177ml.

1000
1N HCL = 12.177

= 82.12203.

V1N1 = V2N2

15
V1 =82.12203

= 0.18266ml for15ml (HCL)

= 182.66μl.
 = 15- 0.18266.

= 14.81743 ml (of water).

Preparation:
 By using the calculation of normalisation, add 0.12177ml of Hcl and 9.878223ml of
distilled water into the cleaned and dried glass beaker.
 Let it for 10 minutes until it gets dissolved completely.

4.3. EXPERIMENTAL PROCEDURE:

MOL% Precursors Molecular formula Moles needed

SiO2–60% Tetraethoxy silane C6H2O4Si 0.60*1=0.60

( TEOS )

CaO -36% Calcium nitrate tetra Ca(No3)2 4H2O 0.36*1=0.36

hydrate

P2O5 – 4% Triethyl phosphate (TEP) OP(OC2H5)3 0.04*2=0.08

General procedure:

SILICATE BIO-ACTIVE GLASS

Tetraethoxy silane (TEOS)

Triethyl phosphate (TEP)

Calcium nitrate tetra hydrate

4.3.1. PREPARATION OF SILICATE BIO-ACTIVE GLASS BY USING

DRYGEL METHOD:

Calculation:
1. Tetraethoxy silane(TEOS)

Moles needed = 1.2.

Molecular weight = 61.83.
Assay = 0.99%.
1.2 𝑋 100 𝑋 61.83
= 1000

moles needed x molecular weight x volume of solvent needed

Molarity=
1000

1.2 𝑋 100 𝑋 61.83

= 1000

Molarity = 7.4196 gm/100ml

2. Triethyl phosphate(TEP)
 Moles needed = 0.08.
Molecular weight = 182.16.
Assay = 0.98.
Density = 1.068 g/ml.

Density x Assay x volume needed

Molarity = .
Molecular weight

1.068 x 0.98 x 1000

= 182.16

Molarity = 5.7457.

Volume needed:

Cs Vs = Cf V

0.08 x 100
= = 13.9234 ml
5.7457

Volume needed = 1.39ml for 100ml.

3. Calcium nitrate tetra hydrate:

Moles needed = 0.36.
Molecular weight = 236.15.

moles needed x molecular weight x volume of solvent needed

Molarity =
1000

0.36 x 236.15 x 1000

=
1000

Molarity = 8.5014 gm/100ml.

Materials needed:
 1N Hcl –15ml
 TEOS-13.65ml
 TEP-1.39ml
 Calcium nitrate tetra hydrate-8.504mg

Preparation:
 At first, prepare 1N Hcl for 15ml using normalisation calculation
 Step 1: Add 95 ml of distilled water, 5ml of 1N Hcl in cleaned and dried 250ml Teflon
beaker. Let it stirring for approximately 30minutes.
 Step 2: By using the calculation, now add 13.65 ml of Tetraethoxy silane (TEOS) in the
stirring mixture. Let it stirring for approx.60 minutes until it gets dissolved completely.
 Step 3: After that, Add 1.39ml of triethyl phosphate in the mixture slowly using
measuring jar and micropipette. Then, keep it stirring for approx.30 minutes until it gets
dissolved thoroughly.
 Step 4: Then, weigh and add 8.504 ml calcium nitrate tetra hydrate slowly into the
mixture. Let it stirring for about 60 minutes approximately until it gets dissolved.
(NOTE: Before adding the component each time check and note down the PH value and
time)

Aging:

 Displace the stirring mixture into the 6- well petridish

 Keep it aging for above 55hours at 60C
 After 55 hours, liquid phase of mixture converted into gel phase. Collect it in sample
tubes for future purpose(fig 15)
 fig 15: dry gel silicate bio-active glass
Sintering:

 Clean the sintering boat using Aquaregia method and dry it completely.
 Take the pinch of dried sample silicate into the boat.
 Then, sintered it for 24 hours at 600C for high purity using furnace

4.3.2. PREPARATION OF SILICATE BIO-ACTIVE GLASS BY USING

STOBER METHOD:

Calculation:

1. Tetraethoxy silane(TEOS):
Moles needed = 1.2.
Molecular weight = 61.83.
Assay = 0.99%.
 moles needed x molecular weight x volume of solvent needed
Molarity=
1000

1.2 X 25X 61.83

= 1000

Molarity = 1.8549 gm/25ml

2. Triethyl phosphate(TEP):
Moles needed = 0.08.
Molecular weight = 182.16.
Assay = 0.98.
Density = 1.068 g/ml.

Density x Assay x volume needed

Molarity = .
Molecular weight

1.068 x 0.98 x 1000

= 182.16

Molarity = 5.7457.
Volume needed:

Cs Vs = Cf Vf
0.08 x 25
= 5.7457

= 0.3475 ml
Volume needed = 0.3475for 25ml.

3. Calcium nitrate tetra hydrate :

Moles needed = 0.36.
Molecular weight = 236.15.
moles needed x molecular weight x volume of solvent needed
Molarity =
1000

0.36 x 236.15 x 25
=
1000
 Molarity = 2.125 gm/25ml.

Materials needed:
 1N Hcl – 10ml
 TEOS-3.4125 ml
 TEP-0.3475ml
 Calcium nitrate tetra hydrate-2.125mg

Preparation:

 At first, prepare 1N Hcl for 10ml by using the calculation of normalisation

 Step 1: Add 23.75 ml of distilled water, 1.25ml of 1N Hcl in cleaned and dried 250ml
Teflon beaker. Let it stirring for approximately 15minutes.
 Step 2: By using the calculation, now add 3.4125 ml of Tetraethoxy silane (TEOS) in the
stirring mixture. Let it stirring for approx.30 minutes until it gets dissolved completely.
 Step 3: After that, Add 0.3475 ml of triethyl phosphate in the mixture slowly using
measuring jar and micropipette. Then, keep it stirring for approx.15 minutes until it gets
dissolved thoroughly.
 Step 4: Then, weigh and add 2.15mg calcium nitrate tetra hydrate slowly into the
mixture. Let it stirring for about 30 minutes approximately until it gets dissolved.
(NOTE: Before adding the component each time check and note down the PH value and
time)

The above solution is known as source solution

 Step5: Add 75 ml of ethanol and 25 ml of distilled water in a separate cleaned and dried
beaker. Then the beaker is placed in a stirrer until it gets dissolved completely
 Step6:Then Add 3.75ml of ammonia in to the above mixture and keep it for stirring
 Step7: Finally add 5ml of source solution into the above mixture. A white precipitate is
formed and place it for stirring approx. about 10 minutes
 Step8:pour final solution into the centrifuge tubes in equal density and keep it centrifuge
for about 15 minutes
  Step9:wash and centrifuge it until PH value becomes neutral using 1N Hcl
 Step10: finally keep the neutral solution into the oven at 80C for 2days

After 2 days, liquid phase of mixture converted into powder. Collect it in sample tubes for future
purpose

Sintering:

 Clean the sintering boat using Aquaregia method and dry it completely.
 Take the pinch of dried sample silicate into the boat.
 Then, sintered it for 24 hours at 600C for high purity in furnace

2.6.1. PREPARATION OF SILICATE BIO-ACTIVE GLASS BY USING

STOBER METHOD:

Calculation:
1. Tetraethoxy silane(TEOS):
Moles needed = 1.2.
Molecular weight = 61.83.
Assay = 0.99%.

moles needed x molecular weight x volume of solvent needed

Molarity=
1000

1.2 X 25X 61.83

= 1000

Molarity = 1.8549 gm/25ml

2. Triethyl phosphate(TEP):
Moles needed = 0.08.
Molecular weight = 182.16.
Assay = 0.98.
Density = 1.068 g/ml.

Density x Assay x volume needed

Molarity = .
Molecular weight
 1.068 x 0.98 x 1000
= 182.16

Molarity = 5.7457.

Volume needed:

Cs Vs = Cf Vf
0.08 x 25
= 5.7457

= 0.3475 ml
Volume needed = 0.3475for 25 ml.

3. Calcium nitrate tetra hydrate :

Moles needed = 0.36.
Molecular weight = 236.15.

moles needed x molecular weight x volume of solvent needed

Molarity =
1000

0.36 x 236.15 x 25
=
1000

Molarity = 2.125 gm/25ml.

Materials needed:
 1N Hcl – 10ml
 TEOS-3.4125 ml
 TEP-0.3475ml
 Calcium nitrate tetra hydrate-2.125mg

Preparation:
 Step 1: Add 23.75 ml of distilled water, 1.25ml of 1N Hcl in cleaned and dried 250ml
Teflon beaker. Let it stirring for approximately 15minutes.
  Step 2: By using the calculation, now add 3.4125 ml of Tetraethoxy silane (TEOS) in the
stirring mixture. Let it stirring for approx.30 minutes until it gets dissolved completely.
 Step 3: After that, Add 0.3475 ml of triethyl phosphate in the mixture slowly using
measuring jar and micropipette. Then, keep it stirring for approx.15 minutes until it gets
dissolved thoroughly.
 Step 4: Then, weigh and add 2.15 mg calcium nitrate tetra hydrate slowly into the
mixture. Let it stirring for about 30 minutes approximately until it gets dissolved.
(NOTE: Before adding the component each time check and note down the PH value and
time)

Aging:
 Keep it drying for above 15 minutes at 60C in microwave oven
 After15 minutes, liquid phase of mixture converted into powder phase. Collect it in
sample tubes for future purpose

Sintering:
 Clean the sintering boat using Aquaregia method and dry it completely.
 Take the pinch of dried sample silicate into the boat .
 Then, sintered it for 24 hours at 600C for high purity using furnace
 5. RESULT AND DISCUSSION:

5.1 FTIR SPECTRUM OF SILICATE BIOACTIVE GLASS BY DRYGEL

METHOD:

Wavenumber (Cm-1) Functional group

438 Si-O-Si bending
568 Binding vibration of PO4-3
803 stretching vibration of Si-O-Si
948 stretching vibration of Si-O-Si
1044 C-OH+C-O-C Stretching
1437 O-H bend
1630 C=C Stretch
 3387 O-H Stretchig

 Thus, silicate glass was prepared by dry-gel method and FTIR characterization was taken.
 The functional group present in the sample confirms the formation of silicate.

5.2 FTIR SPECTRUM OF SILICATE BIOACTIVE GLASS BY STOBER

METHOD:

Graph 2. FTIR spectrum of Stober borate.

Wavenumber (Cm-1) Functional group

439 Si-O-Si bending
813 stretching vibration of Si-O-Si

1048 C-OH+C-O-C Stretching

1430 O-H bend

 1637 C=C Stretch

 Thus, silicate glass was prepared by Stober method and FTIR characterization was taken.
 The functional group present in the sample confirms the formation of silicate.

5.3 FTIR SPECTRUM OF SILICATE BIOACTIVE GLASS USING

MICROWAVE OVEN:

Graph 3. FTIR spectrum of borate using microwave.

Wave number (Cm-1) Functional group

695 C-H bend (mono)

924 stretching vibration of Si-O-Si

 Thus, silicate glass was prepared by keeping the sample in microwave oven and FTIR
characterization was taken.
 The functional group present in the sample confirms the formation of silicate.
6. LAB VISIT:

6.1 SCANNING ELECTRON MICROSCOPE (SEM):

Fig16. Scanning Electron Microscope.

PRINCIPLE:

 SEM produces the image of a sample by scanning the surface with focused beam of the
electron.(Fig 16)
 Electron are produced at the top of the column, accelerated down and passed through a
combination of lenses and aperture to produce a focused beam of the electrons which hits
the surface of the sample.
 The electrons interact with atoms in the sample, producing various signals that contain
information about the surface topography and composition of the sample.
6.2 TRANSMISSION ELECTRON MICROSCOPE (TEM):
Transmission electron microscope (TEM), which is a microscopy technique in
which a beam of electrons is transmitted through a specimen to form an image (fig 17).

Fig 17. Transmission Electron Microscopy

PRINCIPLE:

 When an electron beam passes through a thin section specimen of a material,

electrons are scattered.
 A sophisticated system of electromagnetic lenses focuses the scattered electron into
an image or a diffraction pattern or a Nano-analytic spectrum, depending on the
mode of operation.
REFERENCE:

1. Tadasi kokubo,”bioactive glass ceramics: properties and applications”, biomaterials, 12(2)

(1991)155-163

2. Julian R. Jones, “Review of bioactive glass: from Hench to hybrids”, Acta Biomaterialia,
9(1) (2013)4457-4486

3. Oscar peitl,” highly bioactive P2O5-Na2O-CaO-SiO2 glass ceramics”, journal of Non-

crystalline solids, 292(1-3) (2001)115-126

4. I.D.Xynos et al,”Bio glass ® 45s5 stimulates osteoblast turnover and enhances bone
formation invitro: implications and applications for bone tissue engineering “, calcified
tissue, 67(4)(2000)321-329

5. Ibrahim Khan et al, “Nanoparticles: properties, application and toxicities”, (2017).

6. Freddy C. Adams et al, “Nanoscience, nanotechnology and spectrometry”, (2013), 584-854.

7. M. M. Pereira et al, “Calcium Phosphate formation on Sol-gel derived bioactive glasses in

vitro”, 28(1994), 693-698.

8. Jipin Zong etal, “Processing and properties of Sol-gel bioactive glass”, 53(2000), 694-701.

9.https//www.researchgate.net/publication/326956531_3D_printing_of_SiC_ceramics_direct_in
k_writing_with_a_solution_of_preceramic_polymers

10. https//www.thermofisher.com

11. www.sciencedaily.com

12. www.slideshare.com