Saroj Thesis
Saroj Thesis
BACHLEOR OF TECHNOLOGY IN BIO-MEDICAL ENGINEERING By SAROJ KUMAR ROUT (Roll No- 107BM006)
Acknowledgement
I express my sincere gratitude to Prof. K. Pramanik, Professor of the Department of Biotechnology Engineering, National Institute of Technology, Rourkela, for giving me this great opportunity to work under her guidance throughout the course of this work. I am also thankful for her valuable guidance and timely suggestion without which work would not have been possible
Saroj Kumar Rout Roll no-107BM006 Bio-Medical Engineering National Institute Of Technology Rourkela
CERTIFICATE
This is to certify that the thesis entitled, DESIGN OF DIGITAL THERMOMETER AND APPLICATION IN ELECTROSPINNING submitted by SAROJ KUMAR ROUT in partial fulfilments for the requirements for the award of Bachelor of Technology Degree in Bio-Medical Engineering at National Institute of Technology, Rourkela (Deemed University) is an authentic work carried out by them under my supervision and guidance.
To the best of my knowledge, the matter embodied in the thesis has not been submitted to any other University / Institute for the award of any Degree or Diploma.
Date: 11/05/2011
Prof. KRISHNA PARMANIK Dept.Of Biotechnology and Medical Engineering NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA-769008 3
CONTENTS
Abstract Chapter 1 1.1 1.2 Chapter 2 2.1 2.2 2.3 Chapter 3 3.1 3.2 3.3 Page No. 5 6-7 7 7 8-10 8 8-9 9-10 12-16 13 13-14 15-16
INTRODUCTION Introduction outline of the project BASICS OF ELECTROSPINNING Electrospinning Structural design of an electrospinning Working principle FACTORS AFFECTING ELECTROSPINNING Parameters in electrospinning Polymer solution parameters Processing condition parameters
MATERIALS AND METHODOLOGY Materials used Block diagram Temperature sensor Analog to digital convertion calibration and signal processing Display system
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Chapter 5 5.1
Chapter 6
ABSTRACT
Electrospinning is currently available one of the best fibre forming technology with many advantages over previously available methods. But still this process requires a lot of optimization. In my project I mainly focused on design of digital thermometer which can be further used for real time temperature measurement during the run of electrospinning process. LM 35 sensor and At-mega 32 microcontroller was used. Seven segment display is used for the display of temperature. The thesis mainly covers the basics of electrospinning, factors affecting it and how to control the parameters for its optimization. But mainly the thesis focused on the design of digital thermometer. At different temperature SEM of fibre produced were taken and it was observed that at higher temperature fibre diameter decreases .So temperature control is an important aspect in electrospinning to control fibre diameter and for production of smooth fibers.
CHAPTER -
INTRODUCTION
1.1 INTRODUCTION
Traditional needle Electrospinnin available is common and versatile technique for the production of Nano fibers with diameters ranging from 10 to 1000 nm. It has wide advantage over the previously available fibre formation method because here electrostatic force is used instead of conventionally used mechanical force the production of Nano fibers. Moreover this process can produce fibers with high surface area to volume ratio and with high porosity level which has wide range of application in various fields. Still this elect spinning process needs quite a lot attention for its optimization for the production of fibers with high efficiency by optimization of various parameters. Although this electro spinning is widely used for the production of Nano fibers but still exploitation of technologies based on electro spinning is very limited due to poor understanding of the process and consequent limitation in process control, reproducibility and productivity.
2.1 ELECTROSPINNING
Electro spinning is a process for the production of fibre by the use of electrostatic force in spite of previously used mechanical force. This method is an excellent fabrication process which can be used to form Nano fibers with diameter from 10-1000 nm from fibrous polymer materials. High voltage electric field is being used in this process to generate electro spun Nano fibers.
2.2
Traditionally available needle electrospinning apparatus mainly consists of following parts Syringe High voltage power supply Metallic needle with an orifice at the tip Polymer or composite solution Collector electrode
The whole electro spinning setup is paced in a Plexiglas box that helps in limited exposure of the whole system to the exterior. This box helps in isolating the electro spinning process from unpredictable air current and from various ambient parameters such as humidity and pressure that can alter the fibre production process. The inside of the Plexiglas box also contains acetone bath used to saturate the electro spinning environment with acetone. A computer controlled device controls the electrode separation distance. Syringe location can also be adjusted. The syringe is driven by a syringe pump which is used to control the flow rate and volume of the polymer being ejected. The syringe being used is having a capacity of 1-mL. syringe is attached to a thin tube that leads to a thin needle that ejects the polymer solution. The electrode plate was placed on a stand made of acrylic acid. The electrode is generally grounded and is used for the collection of both random and aligned fibre.
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2.3.2 Formation of the cone-Jet:The polarity of the fluid depends upon the voltage generator. Now in the polymer solution repulsion between the similar charges at the free electrical double layer work against the surface tension and fluid elasticity to deform the droplet into a conical shaped structure known as Taylor-cone. Beyond a critical charge density Taylor-cone becomes unstable and jet of fluid id emitted from the tip of the cone. 2.3.3 Thinning of the jet This jet then seeks a path to the ground. This fluid jet then forms a slender continuous liquid filament. The charged fluid is accelerated in the presence of electrical field. This region of fluid is generally linear and thin. 2.3.4 Instability of the jet:These Fluid elements are accelerated and thus stretched and succumbs to one or more fluid instabilities which distort as they grow following many spiral and distort path before
collected at the collector electrode. This region of instability is also known as whipping region. 2.3.5 Fibre collection:Charged electro spun fibers travel downfield until impact with a lower potential(grounded) collector plate. Orientation of the collector affects the alignment of the fibers. Different type of collector used are- Rotating drum collector, moving belt collector, rotating wheel with bevelled edge, multifilament thread, parallel bars, simple mesh collector etc.
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3.1 PARAMETERS IN ELECTROSPINNING PROCESS Electro spinning is a method is affected by various parameters. Broadly these parameters can be classified into two categories
a) Polymer solution parameters b) Process parameters
Solution parameters Molecular weight and solution viscosity Surface tension Solution conductivity Dielectric effect of solvent
B) Processing parameters Voltage Feed rate Temperature Effect of collector Diameter of the orifice of needle
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3.2.2 SURFACE TENSION At lower viscosity Surface tension leads to the formation of bead formation along the fibre length because it leads to the decrease of the surface area. But at higher viscosity effect of surface tension is nullified because of the uniform distribution of the polymer solution over the entangled polymer molecules .Lower surface tension leads to the smooth fibre formation. Lower surface tension can be achieved by addition of surfactant to the polymer solution 3.2.3 SOLUTION CONDUCTIVITY Increased conductivity of the solution lead to the distribution of higher charge on the electro spinning jet which leads to the increased stretching of the solution during fibre formation leading to the yield of smaller diameter smooth fibre. Increased conductivity of the polymer solution also lowers the critical voltage for the electro spinning. Increased charge leads to the higher bending instability leading to the higher deposition area of the fibre being formed; as a result jet path is increased lading to formation of finer fibre. Solution conductivity can be increased by the addition of a salt or polyelectrolyte. It can also be increased by the addition of drugs and proteins which dissociate into ions when dissolved increasing the conductivity of the solution. When polymers of smaller diameter is dissolved then due to its greater mobility under external electrostatic field, there is greater elongation force leading to formation of smaller diameter fibre 3.2.4 Dielectric effect of solvent Higher the dielectric property of the solution lesser is the chance of bead formation and smaller is the diameter of electro spun fibre. With increase in dielectric property there is increase in the bending instability of the jet leading the increased deposition area of fibre. As a result jet path length is increased leading to the formation of finer fibers
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3.3.3 TEMPERATURE: Higher temperature leads to lower viscosity and higher evaporation rate. At higher temperature the fibre being produced are of uniform diameter due to lower viscosity and higher solubility which allows greater stretching of the solution. At higher temperature due to low viscosity columbic force exert a greater stretching. Increased polymer mobility due to higher temperature just helps this stretching. But due care should be taken while dealing with biological substances such as enzymes and proteins because it may be the reason for loosing functionality 3.3.4 EFFECT OF COLLECTOR In electro spinning collector material is made of conductive material being electrically grounded to create stable potential difference between needle and collector. Had a nonconducting material been used then the charges on the electro spinning jet would have been developed an opposite charge on the collector reducing the amount of fibre being deposited with lower packing density. But in case of conducting collector there is accumulation of closely packed fibers with higher packing density. Porus collector yields fibers with lower packing density as compared to non-porus collector plate. In porus collector plate the surface area is increased so residual solvent molecules gets evaporated fast as compared to non-porus collector where there occurs accumulation of residual solvent around fibers leading to a dense packed structure. In porus surface the residual charges remain on the fibre repelling each fibre leading to lower packing density but in case of uniform surface residual charges conducts away to collector leading to less repulsion so more packing density. Rotating collector is useful in getting dry fibers as it provides more time to the solvents to evaporate. It also increase fibre morphology 3.3.5 DIAMETER OF PIPETTE ORIFICE Orifice of smaller internal diameter reduces the clogging effect due to less exposure of solution to the atmosphere. Small orifice leads to the formation of smaller diameter fibers . However very small orifice has the disadvantage that it creates problem in extruding od droplet of solution at the tip of the orifice
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Number of items
1 1 3 1 1 1
4.2 BLOCK DIAGARM:The following flow chart provides the general principle of operation of a digital thermometer. Each section is described in details in the following sections
The building blocks such as temperature sensor, ADC conversion and display system is explained one by one .
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4.3.2 OPERTING PRINCIPLE OF LM35 In LM35 temperature sensor as the temperature increases the voltage across a diode increases at a constant rate because of the voltage drop between the base and the emitter. This voltage change is directly related to the temperature change. THE OUTPUT VOLATGE IS 10 MILLIVOLT PER DEREE CENTIGRADE So temperature in C= (Vout in millivolt) /10
The analog output of the LM35 temperature sensor is converted into corresponding digital values using the ADC port of ATMEGA 32 microcontroller
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4.6 DISPLAY SYSTEM (SEVEN SEGMENT DISPLAY) Seven segment display is used to display numerical output in many electronics devices. Seven segment display is divided into 7 different segment which can be switched on or off independently according to a user defined program. Different combinations of segments switched on produces different numbers. 7 segment displays also contain a decimal point. Basically the seven segment display contains 7 segments (a,b,c,d,e,f.g) and a decimal point( DP).
The one common end of all the LEDs are connected while the rest are available. Depending upon whether anode or cathode of all the LEDs are connected these are of 2 types, a) Common cathode seven segment display b) Common anode seven segment display
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4.6.2 PIN CONFIGURATION OF SEVEN SEGMENT DIPALY Seven segment display contain 10 pins. The middle two pins are internally connected and rest ach pin is the free end of each LED. Three common anode seven segment displays are connected in parallel. But first the first cell is powered and the other two remain unpowered. Then the second one is powered on keeping the other two off and same for the third seven segment display.
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5.1 RESULT
After soldering all the components and powering on by 9V power supply the temperature sensor reads the atmosphere temperature converts it into analog form and then send it to the microcontroller where it is converted into its corresponding digital values. Then according to the calibration and formula provided in the chapter 4 we can measure the temperature in degree Celsius. The temperature values so detected are shown in three seven segment display as described above. The main aim to design thermometer for measuring atmosphere temperature is that it can give visual and easily understandable atmosphere temperature. So that we can maintain the inside temperature of the Electrospinnin box to the optimal value so that fibre morphology can be used. In future prospect The whole electro spinning box can be surrounded with the pipes which can flow hot or cold water according to our need to either increase and decrease the inside temperature of the Electrospinnin box to get optimal temperature value.,. And thermometers becomes handy in measuring the inside atmospheric temperature. EFFECT OF TEMPERATURE ON FIBRE MORPHOLOGY Higher temperature leads to lower viscosity and higher evaporation rate. At higher temperature the fibre being produced are of uniform diameter due to lower viscosity and higher solubility which allows greater stretching of the solution. At higher temperature due to low viscosity columbic force exert a greater stretching. Increased polymer mobility due to higher temperature just helps this stretching. But due care should be taken while dealing with biological substances such as enzymes and proteins because it may be the reason for loosing functionality
Different temperature affects fibre morphology. Here I have provided 3 different SEM images of the fibre being produced at different temperature (T1, T2, and T3) and the different fibre morphology is clearly visible in the pictures. T1>T2>T3. Frome the SEM images it is clearly understood that with increasing temperature fibre diameter is reducing because of lowering of viscosity. But temperature should not be kept very high because it may lead to the melting of the electro spun fibers being produced
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Fig 5.3 SEM OF ELECTRO SPUN FIBER AT TEMP T3 Below are the two snapshots of my thermometer with two different temperatures -
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5.2.1 TO INCREASE THE FIBER DIAMETER Viscosity of the solution should be increased Surface tension of the solution should be decreased by the addition of various surfactant Conductivity of the polymer solution should be increased either by the addition of polyelectrolyte or by the addition of drugs and proteins Voltage supply should be decreased to reduce the stretching AC supply should not be used as it always results thicker fibers Feed rate of the solution should be increased Operating temperature should be low Diameter of needle orifice should be high but shouldnt be very high enough
5.2.2 DECRESE IN BEAD FORMATION Viscosity of the polymer solution should be low Solution conductivity should be increased by addition of polyelectrolyte or by addition of drugs and proteins Voltage supply should be high enough Feed rate should be increased Operating Temperature should be high Rotating or moving collector can be used to increase the flight time to decrease bead size Diameter of the needle orifice should be low Distance between the needle tip and collector should be decreased
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5.2.3 SMALLR DEPOSITION AREA Smaller deposition area is always desirable in Electro spinning process. Because if the deposition area is larger then fibers may not be collected at the electrode completely leading to the wastage of fibre and also the fibre diameter also decreases due to increased flight time. Smaller deposition area can be achieved by Viscosity of the solution should be increased Conductivity of the polymer solution should be decreased No addition of surfactant should be there so that surface tension should be kept minimal High voltage which leads to higher field strength
5.3 OUTLOOK
Further different modification of the existing electro spinning machine can be achieved by various methods. Here is the brief overview of what can be done further
A) Use of heat exchanger system around the box of the electro spinning to regulate the temperature of the electro spinning process and thereby regulating fibre morphology B) Use of rack pinion mechanism to control the distance between the TIP and collector so that fibre morphology can be adjusted according to parameters and our need C) Use of rack pinion mechanism to move the collector to control the fibre alignment thereby reducing fibre wastage by reducing the deposition are D) Use of High electric field sidewise on the fibre jet so as to compress it decrease the width of the jet thereby reducing the deposition are which ultimately reduce fibre wastage
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CHAPTER 6 CONCLUSION
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6.1 CONCLUSION
The study reports the various parameters that need to be modified according to the need of the process for the production of Nano fibers with high yield and optimum quality according to the use. Also successfully digital thermometer is designed for the design of environment temperature. This can be further used for the real time temperature measurement during electro spinning process so that by temperature feedback method electro spinning temperature can be set to optimum value.
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REFERENCES A) journals
[1] Reneker DH, Chun I. Nanometre diameter fibresof polymer produced by electrospinning. 1996;7:216 23. [2] Bognitzki M, Wendorff JH, Greiner A. Submicrometer shaped polylactide fibers by electro spinning. Polymer Prep (ACS, PMSE) 2000;82:115 6. [3] Warner SB, Buer A, Ugbolue SC, Ruteldge GC, Shin MY. M98-D01 A fundamental investigation of the formation and properties of electrospun fibers. Department of Textile Sciences, University of Massachusetts Dartmouth; Department of Chemical Engineering and Material Sciences, Massachusetts Institute of Technology Cambridge, 2000. [4] Reneker DH, Yarin AL, Fong H, Koombhonge S. Bending instability of electrically charged liquid jets of polymer solutions in electrospinning. J Appl Phys 2000;87:4531 47.
B) WEB REFERENCES
[5] http://www.facstaff.bucknell.edu/mastascu/elessonshtml/Sensors/TempLM35.html
[6] http://www.national.com/mpf/LM/LM35.html#Overview
[7] http://www.ladyada.net/learn/sensors/tmp36.html
[8] http://en.wikipedia.org/wiki/Seven-segment_display
[9] http://en.wikipedia.org/wiki/Seven-segment_display_character_representations
[10] http://www.thelearningpit.com/lp/doc/7seg/7seg.html
[11] http://extremeelectronics.co.in/avr-tutorials/interfacing-seven-segment-displays/
[12] http://www.ikalogic.com/proj_dig_thermo.php
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