Vacuum technology Chambers and pumps Vacuum (Latin vacuo): nothingness, empty space, lack of gas lack of gas is measured by pressure SI unit: Pa widely used in engineering: mbar common sense as scientist: atm Pressure units 2 Vacuum range mbar Pa Particle density Mean free path Kn Rough vacuum 1000 - 1 105 - 100 1025 - 1022 m-3 l << d << 1 1 - 10-3 100 - 0.1 1022 - 1019 m-3 l≈d ≈1 10-3 - 10-7 10-1 - 10-5 1019 - 1015 m-3 l>d >1 < 10-7 < 10-5 < 1015 m-3 l >> d >> 1 < 10-11 < 10-9 < 1011 m-3 l >>> d >>> 1 RV Medium vacuum MV High vacuum HV Ultra-high vacuum UHV Extremely-high vacuum (XHV) vacuum chamber: recipient of dimension d suitable for holding a low pressure for long periods of time - implosion proofed! typical materials: steel (304, 316), glass (only HV) Vacuum chambers 3 Vacuum chambers 4 vacuum chambers are interconnected using flanges and valves available in various systems: ISO-KF (kleinflansch): 10 - 50 mm KF10, KF16, KF25, KF40, KF50 ISO-F: 63 - 630 mm F63, F80, F100, F160(150), F200, F250, F320, F400, F500, F630 ISO-K: 63 - 630 mm K63, K80, K100, K160(150), K200, K250, K320, K400, K500, K630 HV vacuum flange systems http://eu.trinos.com 5 components: blank flanges full or half nipples flex hoses centering rings clamps various connectors are available for standardized constructions sealing material for rings: Neoprene, Silicone, Teflon, Viton, metal (aluminum) suitable for multiple use except for metal sealings suitable pressure range: RV to HV metal sealing must be used for pressures below 10-6 mbar (10-4 Pa) HV vacuum flange systems http://eu.trinos.com 6 vacuum valves are critical points in a vacuum system since are most prone to leakages diaphragm valves angle valves in-line valves gate valves control valves (butterfly) Vacuum valves http://www.vatvalve.com 7 a proper selection of vacuum pumps is critical for vacuum applications gas transfer pumps positive displacement pumps - this pumps suck! oil sealed pumps: rotary vanes, rotary piston trapped volumes of gas are isolated using oil dry pumps: roots, scroll, piston/diaphragm trapped volumes of gas are isolated using close clearances between moving parts or O-rings - oil free pumps kinetic (momentum transfer) vacuum pumps diffusion pumps, turbomolecular pumps gas binding pumps - molecules are removed through adsorption or condensation on surfaces inside the pump cryo-pumps, getter pumps, sublimation pumps, sputtering pumps Vacuum pumps 8 a) rotary vanes pump b) rotary piston pump a volume of gas is trapped inside the pump due to mechanical movement of a rotor from inlet, the gas is compressed and forced out through outlet the rotor is partially submerged in an oil bath for a better sealing or isolation between zones with various partial pressures pumping speeds: 1 - 1500 m3 h-1 working temperature: 20 - 90°C ultimate pressure: single stage: 1 Pa (10-2 mbar) dual stage: 10-2 Pa (10-4 mbar) Oil sealed pumps 9 pump oil selection must be done accordingly with the application and its special requirements for commonly used oils (mineral) the oil viscosity specified by the pump manufacturer must always be respected - too low viscosity leads to leakage and noise, too high viscosity leads to difficulty of starting at room temperature and occasionally seizures oil types: Hydrocarbon oils - highly refined mineral oil - the most usual oil used - may contain additives for minimizing the corrosion effects of vapors being pumped Synthetic organic-type oils - used for heavy-duty applications at high temperatures - have improved oxidation resistance Fluorinated (perfluoropolyether) fluids - higher grade oils used for an increased operation time between pump maintenance periods. Advantages: chemical inertness - ideal for pumping aggressive materials (semiconductor industry) noninflamable - no fire risk high thermal resistance - no residual “tar” is formed by overheating oxygen-compatible - allows safe pumping of oxygen Oil sealed pumps 10 momentum p mv m1 elastic collision - momentum conservation massive target m1<<m2 ' v1 v1 m2 p 0 m1v1 m2 v2 v momentum transfer pumps momentum is transferred to gas molecules so that a continuous flow is ensured between inlet and outlet moving surface v positive displacement pumps are trapping volumes of gas between inlet and outlet - fundamental difference momentum can be transported by: high speed vapor streams - diffusion pumps continuously moving parts - turbomolecular pumps Kinetic vacuum pumps 11 concept: vapors from liquids (e.g. Hg or petroleum) are produced in a boiler (D) when inserted in an evacuated chamber through a small opening (nozzle), the vapors will expand acquiring a high forward mass velocity - vapor jet (P) expansion of the vapor jet is limited by the gas present in the pump - at low pressures a diffuse layer of vapor mixed with penetrating gas molecules is formed gas diffused into vapors is moved in the jet direction separation of vapors and gas is done through condensation on cold surfaces (walls of the pump) (F) gas molecules are trapped by vapor barriers special design of the nozzles (e.g. umbrella-type) diffusion pumps require backing (forevacuum) pumps (N) Diffusion vacuum pumps Langmuir’s diffusion pump 12 multistage pumps - more efficient in trapping gas under several jet barriers the narrowing neck in front of the vapor jet - diffuser (Venturi tube) diffusion not necessarily happen - jet speed is high enough so that the barrier is very efficient diffusion pumps - historical name from Venturi small molecules can diffuse back - not efficient for H, He, etc used for achieving HV in “dirty” processing chambers special diffusion oil chemically inert (resistant to oxidation) operating pressure: 10-1 - 10-6 mbar pumping speeds: up to 1000 l s-1 (3600 m3 h-1) Q gas throughput (load) Q SP S pumping speed P desired pressure Diffusion vacuum pumps Edward’s diffusion pump 13 momentum transfer from a fast rotating surface (turbine blade) to the gas molecules - molecular drag rotors and stators alternating lead to a controlled direction of the moving gas molecules successive collisions/deflections produce a net molecular flow from the inlet to the outlet progressive inclinations of the blades minimize the back-deflection extremely high-speed motors (up to 1.25 kHz - 75000 RPM) Boeing turbo jet engine - 36500 RPM huge compression factors: N2 up to 1011 (1:10 for Boeing) if mean free path of the gas molecules higher than the distance between rotor and stator blades: molecules interact mainly with the blades backing is needed pumping speeds: up to 3200 l s-1 operating pressure: 10-2 - 10-10 mbar Turbomolecular vacuum pumps 14 various designs available - single rotation axis - most common critical point: mechanic support of the rotors mechanical rotor suspension (ceramic ball bearings - zirconia) magnetic rotor suspension - for low vibration, hydrocarbon free vacuum service intervals: bearing exchange 10000 - 15000 h (14 - 21 months) rotor axis exchange 45000 - 100000 h (5 - 12 years) magnetic suspension are service-free pumps frequency converters are necessary to be used with turbo pumps extra caution should be used when mounting a turbo pump to a vacuum chamber!!! always use steel screw/bolts (as many as possible, at least M8) v never start a turbopump if is not properly connected to the chamber (big mass) r = 0.05 m, f = 1.25 kHz - circumference L = π/10 m - radial speed v = Lf = 395 m/s m = 0.001 kg rotor imbalance - dropping a peanut E 1 2 mv 80 J 80 N m 2 distance to the chamber d = 0.01 m, F = 8 kN - similar with a cannonball energy r Turbomolecular vacuum pumps http://www.oerlikon.com 15 Vacuum technology Vacuum measurement gauge = pressure sensor (transducer) - various phenomena can be exploited: displacement of a liquid column, diaphragm, or other deformable element by force due to a pressure differential (RV) viscous drag acting upon a moving element (MV - HV) thermal conductivity (HV) ionization by electrons, nuclear radiation, or laser photons, and sensing either ion current or emitted light (UHV) Capacitance diaphragm gauge Piston pressure gauge U-tube manometer P1 P2 gh P1 P2 mg / A Vacuum gauges a2 C Y P 4T T = membrane radial tension 17 a hot filament loses heat by: radiation, conduction to supports, transfer to the surrounding gas total energy WT WR WC WG Thermocouple gauge: temperature is measured from the potential drop arising at the junction between two dissimilar metals Pirani gauge: temperature of the filament is measured from its resistance energy loss due to gas pressure - temperature loss electrical resistance change the filament resistance is measured in a Wheatstone bridge the gauge measures the pressure correctly in the linear regime Thermal conductivity gauges 18 Bayard-Alpert gauge hot cathode electron emission triode design the collector current iC is proportional with the pressure iC Ki P ir K depends on cell geometry i- - incident electron current ir - residual current due to photoelectrons ejected from grid and collector positioning the BA gauge inside vacuum is critical the entire volume of the triode must be inside the bulk vacuum the flanges containing the gauge cannot be placed inside tubes - more X-rays can be generated pressure range: 10-3 - 10-12 mbar Ionization gauges 19 Thermal evaporation a conductor having a potential difference between two planes will accelerate electrons in a field E E Fe the electric force Fe will be opposite to a material specific resistance force Fr Newton law: Fe Fr ma eE kv ma eE V1 V2 when the movement is uniform, a=0 V1 > V2 v e and the speed of the electrons is: k the current density through the conductor ca be j V ve expressed as a function of the volume charge density: Fr Ohm’s law can be directly derived eE j V j E k where is the electrical conductivity the resistance force Fr is the classical description of the interactions (collisions) between moving carriers (electrons) and the phonons of the crystalline structure of the conductor kinetic energy is transferred to the material Ohm’s law for electric conductivity 21 Joule effect: electrons passing through a conductor will generate heat due interactions with the crystalline structure of the conductor - kinetic energy transfer must depend on material’s electrical resistivity (resistance) r - characterizes the intensity with which the material opposes the current flow 1 l V Fe must depend on the current intensity must depend on the time V the electrostatic force Fe produces work: W Fe l qEve t V V Eve t j EVt work is transformed into heat: W Q j2 Vt I2 Sn 2 Vt I 2 l t S n where the electric current depends on the current density j and normal surface Sn: Joule-Lenz law expresses the heat produced in any portion of resistive and homogeneous solid: Q I Rt 2 R j I Sn l l r S n Sn Joule effect 22 Joule effect is used for heat generation in furnaces - evaporation sources in vacuum evaporation sources (thermal elements) high melting point metals (W, Ta, Mo, and their alloys) direct evaporation the material to be evaporated comes in direct contact with the thermal element risk of alloying between the thermal element and the material - short lifetime indirect evaporation - the thermal element is used for heating a crucible (e.g. Al2O3) Thermal filaments point source loop source small amounts of material for wire materials coils baskets serpentines spirals low deposition temperatures average amounts of material (mg) for small flakes, pellets higher deposition temperatures possible Evaporation sources www.lesker.com 23 Thermal boats dimple notched Thermal boxes top hat long through canoe single or multiple reservoirs for plane source simulation Rod sources (Cr on W) high amounts of material high deposition rates Evaporation sources high temperatures www.lesker.com 24 Coated thermal elements (alumina) inverted hat basket interaction with the thermal element is minimized alloying is avoided lifetime is extended Crucibles - heated by coils or baskets alumina quartz C Ta, Mo, W boron nitride used when indirect deposition sources are necessary evaporated material should not alloy (or diffuse into) with the crucible e.g. Al suitable for deposition from alumina or W, but not from C Evaporation sources www.lesker.com 25 designs of single or multiple sources are possible two highly conductive electrodes (pure Cu) are used for transporting high currents (300A DC or AC) to the thermal element cooling of the current feedthroughs is necessary liquid (the inner part of the rods is hollow) or air (outside the chamber ventilators are used for cooling the entire rod) Thermal evaporator design 26 most of the time, thermal / evaporation shielding has to be used for protecting the chamber 1) pumping unit 2) pressure measurement 3) power source 4) vacuum chamber with implosion protection Thermal evaporator design 27 Thin film uniformity Thickness distribution point source evaporation equal amounts of material go in all directions Ms total evaporated mass Me dAs total deposited (condensed) mass Ms dAs r r0 substrate plane at distance r0 from source elementary substrate surface dAs dAc d Me arbitrary condensation surface on the sphere dAc cut by a solid angle d arbitrary elementary surface projected through the solid angle d distance to dAs is r evaporation angle Thin films thickness 29 condensation surface depends on dAs dAc dAs cos Ms dAs dAs r r0 the fraction of material accumulated on substrate must be proportional to the surface fraction through each the evaporand escapes the sphere dM s : M e dAc : 4r dAc d Me 2 simple mathematics: dM s Me dM s Me cos 2 2 dAc 4r dAs 4r if Ms0 is the amount deposited at zero angle, then: 3 M s r0 r0 3 cos cos 0 2 Ms r r 2 cos law for point source Thin films thickness 30 plane source (Knudsen cell) - similar to Lambert law: 2 dM s M e M s r0 2 cos cos 0 2 cos cos dAs r Ms r general case: dM s M e n 1 n cos cos 2 dAs 2r d 2 M s r0 n n0 cos cos 0 2 Ms r If the evaporation angle and the deposition angle are the same: 3 M s r0 4 cos cos 0 Ms r plane 3 M s r0 n n 3 cos cos 0 Ms r Thin films thickness general 31 32 33 34 35 material: Al; evaporation distance: 65 mm Experimental data 36
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