APPARATUS AND EXPERIMENTAL TECHNIQUE

2.1 INTRODUCTION
In recent years thin film science has grown in to a major research area. Athough,the study of thin film phenomenon dates back well over a century ,it is only over a century,it is only over the last two decades that they have been used to a significant level in practical application.The major exploitation is still in the the field of microelectronics. However ,there are growing application in other areas like thin film for optical and sensor device.The development of deposition technique for the preparation of thin filmwith controlled ,reproducible and defined properties plays and important role in technological application.Although,there is a widw range of thin films deposiion techniques,thermal evaporation technique has many advantage.Transparent conductor thin films can be used as a gas sensors,transparent electrodes for solar cells,transistors ,protective coating and resistors.To study the proreties of these materials ,it is possible to prepare stable and homogeneous thin films of these materials .Indium oxide,Tin oxide and Indium Tin oxide thin films are prepared for investigating their electrical ,optical and structural properties .Properties of these thin film strongly depend on the method of deposition ,the substract materials,the substrate temperature,the rate of deposition and background pressure.It is known that growth condition and the nature of the substrate materials affect the structure and crystallinity of the films. Different machines have been used in our project .In this chapter .we will study some of the technique that we have adopted.Also ,we have study some of the machines like the ultrasonic cleaner ,spin coating machine ,vacuum coating unit ,vacuum pumps such as rotary pump and diffusion pump and digital source meter .We have used Keithley 2400 manufactured by Keithley Instrument,US.

2.2 ULTRASONIC CLEANER

An ultrasonic cleaner as shown above in the fig,is a cleaning device that used ultrasound(usually from 20-400kHz) and an appropriate cleaning solvent (sometimes ordinary water) to clean dedicate items.The ultrasound can be used with only water but used of a solvent appropriate for items to be cleaned and the soiling enhance the effect,Cleaning normally last between three and six minutes.Ultrasonic cleaners are used many different types of objects,including jewellery ,lenses and other optical parts,watches dental and surgical instruments,tools,coins,fountain pens,golf clubs,window blind,firearms,industrial parts and electronic equipment.They are used in many jewellery workshops,watchmakers esablishments,and electronics repair workshops.

Ultrasonic cleaning uses high frequency sound waves to agitate in a liquid .Cavitaion bubbles induced by the agitation act on contiminants adhering to substractes like metals,plastic,glass,rubber,and ceramics.This action also penetrates blind holes,crackes,and recesses.The intension is to thoroughly remove all traces of contamination tightly adhering or embedded onto solid surfaces.Water or other solvents can be used,depending on the type of contamination and workpiece.Contaminants can include dust ,dirt,oil,pigments,rust,grease,algae,fungus,bacteria,lime scale,polishing compounds,flux agents,fingerprints,soot wax and mold release agents,biological soil like blood,and so on.Ultrasonic cleaning can be used for a wide rang of work piece shapes,sizes and materials, and may not requirethe part to be disassembled prior to cleaning.Object must not be allowed to rest on bottom of the device during the cleaning process,because that will prevent cavitation from taking place on the part of the object not in contact with water.

2.3 SPIN COATING MACHINE

Spin coaing (refer figure) is a procedure used to apply uniform thin films to flate substrate .In short ,an excess amount of a solution is placed on substrate ,which is then rotated a high speed in order to spread the fluid by centrifugal force.A machine used to spin coater,or simply spinner. Rotation is continued while the fluid spin off the edges of the substrate,untill the desired thickness of the film is achieved.The applied solvent is usually volatile,and simultaneously evaporates.So ,the higher the angular speed of spinning,the thinner the film.The thickness of the film also depends on the concentration of the solution and the solvent. Spin coating is widely used in micro fabrication,where it can be used to create thin films with thickness below 10 nm.It is used intensively in photolithography,to deposite layers of photoresist about 1 micrometer thick.Photoresist is typicallyspun at 20 to 80 revolution per second for 30 to 60 seconds.

2.4 VACUUM COATING UNIT

The type of vacuum equipment needed depends on the desired purity of the film.Detailed review on various types of the vacuum systems and their ultimate pressures are given by Holland ,Caswell,Dushman and Roth.The vacuum system employed to deposite and characterize thin film in the present work contain in assortment of pumps,tubings,valves and gauges to establish and measure the required pressure as shown in the figure(). Basically the vacuum system ,Hind Hivac coating unit(Model No.12 A4) consist of 0.4m diffusion pump in conjuction with an oil sealed rotary pump.The ultimate pressure achieved in a 0.3m diameter stainless steel bell jar is a of the order of 6*10-6 Torr.It has set-ups for electron beam evaporation and flash evaporation and flash evaporation.Subsstrates can be cleaned by ion bombardment.A low tension transformer of 10V-100Ais used for filament heating .Most of the

evaporation obtained by rotatory pump is measured by means of a Pirani Gauge and a diffusion vacuum is measured by a Penning gauge.The figure 2.3 below shows the schematic diagram ovacuum coating unit. Following are the component of the vacuum coating unit:1.Bell jar 4.source shutter 7.Penning gauge 10.Diffusion pump 13.Fore line trap 2.Substrate 5.Electrone beam gun 8.Roughing valve 11.High vacuum valve 14.Isolation valve 3.Thickness monitor 6.Current feed through 9.Baffle valve 12.Pirani gauge 15.Rotary pump

The pirani gauge (A6STM) as shown in the figure ,has two gauge heads,which facilitate the measurements of the fore vacuum and roughing vacuum.Change of the pressure in the system bring above a rise or fall in the number of the gas molecules present and hence a rise or fall in the thermal conductivity of the gas.Thus he heat loss of the constant voltage electrically heated filament has high temperature coefficient of resistance.So a slight change in the system pressure brings about useful change in the filament resistance resulting in an out of the balance current in a wheatstones bridge which can be read as pressure on a meter shown in the figure .The filament is often reconditioned if the gauge behave erratically when it is filled with contaminates .The gauge head is flushed with acetone and throughly dried.10V DC is applied across the filament to volatilize the deposite on the filament. The penning gauge(STP4M-1) as shown in the figure is used to measure the vacuum in the range 0.7510^-3 to 0.7610^-6 Torr in two ranges with instant range chaning provided by a toggle switch .This is a cold cathode as given in the Figure().A potencial difference of about 2.3kV ia applied between anode and cathode through current limiting resistor .A magnetic field is introduced at right angles to the plane of the electrodes by an permanet magnet having nearly 800 Gauss,which will increase the ionisation current .The electrone emitted from the cathode of the gauge head are defelected by the means of the magnetic field and are made to take helical path before reaching he anode loop. Thus following very long path ,the chance of the collision with gas molecule is high even a low pressure .The secondary electrons produced by ionisation and the rate of ion increases rapidly.Eventually the electrone produced by ionization increases rapidly .Eventually the electrone are caputured by the anode and equllibrium is reached when the number of electrones produced per second is the sum of positive ion current to the cathode and the electrone current to the anode and is used to measure the pressure of the gas.If the gauge shown unstable pressure reading due to the contaminationof the gauge head by forming a thin layer of deposition of the anode loop and cathode liner ,it is cleaned chemically by heating at 333k for 20 minues in a

solution of 20-30% HNO3 and 2-3 %HF acids.Figure shows the photograph of the coating unit along the with the accessories. 1.High Vacuum 3.Sensing Wire 1.Magnetic Field 3.Cathode(-) 2.Reference wire 4.Vacuum System 2.Anode (+) 4.Ballast Resistor

2.5 OIL SEALED ROTARY PUMP

Mechanically pumps are seldom operated below 100m Torr,and for this reason they are often referred to as roughing pumps.This is the most widely used mechanically pump to establish necessary force vacuum for high vacuum pumps. A cross section of the pump used (Hind hivac ED12) is shown in the figure.The gas transport is affected as the keyed shaft rotates the eccentric rotor .The gas is isolated from the inlet after one cycle and then compressed and exhausted during the next cycle.As shown in the figure the pump consist of an eccentrically mounted rotor placed inside a stator.Two spring loaded varies sliding in diametrically opposite slots in the rotor press against he inner surface of the stator .Friction the wear and tear are minimized by an oil film,which lubricated all parts of the pump and also seals the minute gap at the seat.The exhausted end is closed by a pressure valve leading into an oil reservoir.During the operation ,vanes slide in and out enabling the rotor to draw air through the inlet side into the pump.The crescend-shaped air volume is then compressed to a pressurejust above one atmosphere which causes the outlet valve to open and dishcharge the air through the oil seal into the atmosphere. A vented outlet valve admitting a small airflow into the compression section ,which is called gas ballsting, reduces condensation of water vapour by lowering the compression ratio.The fluid in the rotary pump can be either mineral oil or diphenylethers , as the high vapour pressure oils decompose during operation.The problem of back sreaming of oil vapour is solved by the installing fore- line traps.These operate by condensation on liquid nitrogen traps or by adsorption on surface-active materials.Adsorption traps containing activated alumina is used which is superior to charged zeolite and activated charcoal.The most important characterstics of rotary pump is speed at which it remove the gases from the system.The pressure ,which can be achieved using a rotary pump ,is approximately 10^-3 Torr. 1.Outlet Valve 3.Rotor 5.Vanes 2.Seal 4.Inlet 6.Stator

2.6 DIFFUSION PUMP

The idea of evacuating a vassel by a molecular momentum transfer from streaming to diffusion molecule was first described by Gaede.Diffusion pumps use oil for pumping out gas molecules.The performance can be improved by using traps and baffles in conjuction with the pumps to eliminate the problem of back streaming of vapour. A schematic diagram of diffusion pump used is shown in Figure .The heater vapuorizes the work fluid and hot vapour rises in achimney .The direction of flow of vapoures the work-fluid and hot vapour is reversed at the jet cap so that it issues out through an annular nozzle with supersonic speed.This is due to the pressure difference between the inner the outer side of the chimney.The high speed jet of the molecules imparts momentum to the random moving gas molecules.Thus the gas molecule move towards the outlet where it is removed by a backing pump.The vapour jet condenses on the cooled pump walls and to the boiler .The gas molecules diffuse to the vapour molecules ,hence the name diffusion pump. The working fluid should have high molecular weight ,low vapour pressure ,necessary thermal stablity and be the least reactive.Commonly used fluids are hydrocarbons,silicon fluids,polyphenyl ehter and perfluropolyether.We have used silicon oil,DC704(Tetraphenyl tertamethyl siloxane) as working fluid.This oil is superior to other fluids because of its low vapour pressure and high resistance to oxidation at high working temperature. 1.High vacuum intake 3.Throat 5.Fore-vacuum 7.Boiler 9.Nozzle 2.Jet cap 4.Vaapour jet 6.Heater 8.Oil 10.Water cooled casing

To prevent back diffusion of the gas from dense to the raze zone vapour jet should retain as much of its density as possible.To reconsile this requirement with wide throat area for maximum gas intake,the cross section of lower zone is narrowed through aerodynamically shaped tapering stacks.The outer walls are water cooled to recover the work fluid back and to produce a denser boundary layer by removing vapour molecules,which travel laterally without contributing to the jet action.To enhance the directionality ans the speed of the vapour the pumps employ multistage stacks,with three jets working in series.The working range of pressure for diffusion pump is 10^2 Torr to 10^-6 Torr.The diffusion pumo is coating unit used has an evacuating speed of 500 Litters/s.

2.7 KEITHLEY 2400

To characterize the fabricated organic solar cell,we make use of a digital source meter.Hence,we have used Keithely Digital Source 2400,as shown in the figure ,for the

characterizaion of the solar cell.The instrument gives the track of voltage and/or current when one of them is varied.The result is expressed in the graphical form and the required data is calculated from it .There is a pre-installed Keithley software in the system.The hardware kit is connected to the system(computer).The solar cell fabricated is characterrized before it gets deteriorated.Prior to our characterization of the cells,we keep them in the vacuum chamber so that the cells do not deteriorate.The fabricated samples are tranferred to the destination,where he samples will be studied,using forceps. An oraganic solar cell in our research is studied for two types of charactertics-dark and light characteristics.For both types of characterstics,we have used the same instrument-Keithley 2400(refer figure). To study the dark characterstics.For both types of characterstics,we keep the solar cell away from a light of moderate intensity.The probes from Keithley 2400 are connected to the two electrodes of the oraniic cell.The result of the simulation is obtained on the computer screen.The graph if accurate ,is saved or else repeat the simulation till the time a desired shape of the graph is obtained. With 3 instruments tightly integrated inti a single chassis,Keithley Sources Meter instruments offer a powerfull solution for the lab bench,and a flexible,low cost solution for device characterization.s