COMPARISON OF TRIODE AND DIODE SPUTTERION PUMPS

A comparison of triode and diode noblegas sputterion pumps was performed to determine the advantages and disadvantages of each technique. Pumping speed measurements using nitrogen and argon were obtained over the range of 5109 to 1104 Torr (6.7107 to 1.3102 Pa) and long term characteristics were obtained by pumping Ar continuously at 110 5 Torr (1.3103 Pa) until pump failure occurred. The triode has advantage at high pressure while the diode exhibits better pumping speed at low pressure. Accelerated life testing showed the diode pump to have a more stable pumping characteristic with time.

Vacuum pump
A device that reduces the pressure of a gas (usually air) in a container. When gas in a closed container is lowered from atmospheric pressure, the operation constitutes an increase in vacuum in this container. Vacuum pumps are evaluated for the degree of vacuum they can attain and for how much gas they can pump in a unit of time. In practice, where high vacuum is required, two or more different types of pumps are used in series. In the rotary oil-seal pump (see illustration), gas is sucked into chamber A through the opening intake port by the rotor. A sliding vane partitions chamber A from chamber B. The compressed gas that has been moved from position A to position B is pushed out of the exit port through the valve, which prevents the gas from flowing back. The valve and the rotor contact point are oil-sealed. Since each revolution sweeps out a fixed volume, it is called a constantdisplacement pump. Other mechanical pumps are the rotary blower pump, which operates by the propelling action of one or more rapidly rotating lobelike vanes, and the molecular drag pump, which operates at very high speeds, as much as 16,000 rpm. Pumping is accomplished by imparting a high momentum to the gas molecules by the impingement of the rapidly rotating body. The water aspirator is an ejector pump. When water is forced under pressure through the jet nozzle, it will force the gas in the inlet chamber to go through the diffuser, thus lowering the pressure in the inlet chamber. When high-pressure steam is used instead of water, it is called a steam ejector. In addition, a number of pumps have been developed which meet special pumping requirements. The ion pump operates electronically. Electrons that are generated by a high voltage applied to an anode and a cathode are spiraled into a long orbit by a high-intensity magnetic field. These electrons colliding with gas molecules ionize the molecules, imparting a positive charge to them. These are attracted to, and are collected on, the cathode. Thus a pumping action takes place. Sorption pumping is the removal of gases by adsorbing and absorbing them on a granular sorbent material such as a molecular sieve held in a metal container. Cryogenic pumping is accomplished by condensing gases on surfaces that are at extremely low temperatures.
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Vacuum pump
A pump which produces a partial vacuum in an enclosed space; may be used to remove air or steam from a chamber or a system.

Vacuum Pump
a device for removing gases and vapors from a closed space in order to create a vacuum in it. There are various types of vacuum pumps, whose operations are based on various physical phenomena: mechanical (rotary), jet, sorption, and condensate removal pumps. The principal parameters of vacuum pumps are the ultimate pressure (also residual pressure or maximum vacuum) that can be attained by the pump, the evacuation rate the volume of gas that can be pumped out at a given pressure per unit of time (m 3/sec, l/sec), and the permissible (maximum) outlet pressure in the discharge section of the pump which, if exceeded, would disrupt the normal operation of the pump. Mechanical pumps. Mechanical pumps are used to create vacuums from 1 newton per sq m (N/m2), or 10-2 mm of mercury (mm Hg), to 10-8 N/m2, or 10-10 mm Hg. The piston of the simplest vacuum pump performs a reciprocating motion that forces the gas out and, during the return stroke, creates a rarefaction in the system being pumped out. Reciprocating pumps (Figure 1) were the first mechanical pumps; they were subsequently replaced by rotary pumps. In the multiplate rotary pump (Figure 2), gas suction and ejection are accomplished by varying the volumes of the cells formed by the eccentrically mounted rotor, which has slots fitted with movable blades that press against the inner surface of the chamber and slide along it during rotation. Owing to the high rotation frequency of the rotor, these pumps have a high evacuation rate (up to 125 l/sec) considering their relatively small size. The ultimate pressure attains 2,000 N/m2 (15 mm Hg) in single-stage pumps and 10 N/m2(10-1 mm Hg) in two-stage pumps.

Figure 1. Diagram of a reciprocating pump: V is the volume to be pumped out; Vmin and Vmax represent the minimum and maximum cylinder volumes respectively. The method of pumping gas with water-ring pumps (Figure 3) is similar. Upon rotation of a radially vaned wheel eccentrically positioned in a chamber, the water filling the chamber is deflected by the vanes and thrown against the casing wall by centrifugal force, forming a water ring and a crescent-shaped chamber, into which the gas being pumped flows. When the wheel
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rotates, the cells are alternately connected to the drain, through which the pumped gas is discharged to the atmosphere. These pumps are useful for pumping out moisture-laden and contaminated gas, oxygen, and explosive gases. The ultimate vacuum is 95 percent (in singlestage pumps) and 99.5 percent (in two-stage pumps) of the theoretically possible vacuumfor example, at a water temperature of 20 C it reaches 7.1 kN/m2 (53 mm Hg) in single-stage pumps and 3.1 kN/m2 (23 mm Hg) in two-stage pumps.

Figure 2. Diagram of a multi plate vacuum pump. Oil-sealed rotary pumps are often used to create a medium vacuum. The pumps are either immersed in an oil bath or their working chambers are filled with oil. These pumps have an evacuation rate of 0.1-750 l/sec and an ultimate pressure of 1 N/m2 (10-2 mm Hg) in singlestage pumps and 10-1 N/m2(10-3 mm Hg) in two-stage pumps. The oil effectively seals all gaps and functions as an auxiliary cooling medium, but condensed vapors contaminate the oil during prolonged operation. To prevent the condensation of vapors, which develops under compression, the chamber is filled with a specified volume of air (ballast gas), which provides a partial vapor pressure in the vapor-air mixture at the moment of discharge without exceeding the saturation pressure. In this way, the vapor is ejected from the pump without condensation. These types of pumps are called gas-ballast pumps and are used as backing pumps (to create preliminary evacuation).

Figure 3. Diagram of a water-ring vacuum pump. Two-lobe rotary pumps have two shaped, counter-rotating rotors, creating a directional movement of the gas. These pumps have a high evacuation rate and are frequently used as intermediate (auxiliary, or booster) pumps between pre-evacuation and high-vacuum pumps.
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They provide vacuums of 10-2-10-3 N/m2 (10-4-10-5 mm Hg) at an evacuation rate of 15 m3/sec (Figure 4).

Figure 4. Diagram of a two-lobe rotary pump In molecular pumps molecules pick up additional velocity in the direction of their movement during rotation of the rotor in the gas. Pumps of this type were first proposed by the German scientist W. Gaede in 1912 but were not used for a long time owing to their complexity of construction. In 1957 the German scientist W. Becker introduced the turbomolecular pump (Figure 5), with a rotor consisting of a system of disks. This type of pump attains a vacuum up to 10-8 N/m2 (10-10 mm Hg).

Figure 5. Diagram of a turbomolecular pump. Jet pumps. In jet pumps a direct stream of the working medium carries off the gas molecules entering from the volume being pumped. Liquids or vapors of liquids may be used as the working medium. Depending on the type of medium, these pumps are called water-jet, steamwater, steam-mercury, or oil-diffusion pumps. Jet pumps are of the ejector or diffusion type, according to their principle of operation. In ejector pumps (Figure 6) the pumping operation of the jet is based on an increase of the gas flow pressure under the action of a jet with higher thrust. These pumps are used to attain a vacuum of 10 N/m 2 (10-1 mm Hg). The water-jet pump, which is widely used in the chemical industry, in laboratory practice, and so on, is a simple ejector pump. The ultimate pressure of such pumps does not greatly exceed the vapor pressure of water. For example, at a water temperature of 20 C in the pump, the vacuum attained is 3,100 N/m2(23 mm Hg), but the partial pressure of the residual gases is
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approximately 670 N/m2 (5 mm Hg). The vortex pump, whose pumping action is based on the utilization of the negative pressure that develops along the axis of the vortex (Figure 7), can also be called an ejector pump. Pumps with water vapor as the working medium have a considerably higher evacuation rate and a lower ultimate pressure. An evacuation rate of 20 m3/sec with a vacuum of 0.7 N/m2 (5 x 10-3mm Hg) can be attained in multistage water-vapor pumps.

Figure 6. Diagram of a multijet ejector pump The pumping operation of diffusion pumps is based on the diffusion of the pumped gas molecules in the area of action of a jet of vapor of the working medium owing to a drop in their partial pressures. W. Gaede used mercury vapor as a working medium in 1915. Mercury provides a constant vapor saturation pressure (for a given temperature) and temperature (for a given pressure), and it remains chemically inactive and is not affected by superheating; however, the mercury vapors, even in small amounts, are dangerous to the human organism.

Figure 7. Diagram of a centrifugal vacuum pump One of the substitutes for mercury is oil. Such vacuum pumps using oil are called oil-diffusion pumps. The use of oil as a working fluid led to the widespread use of these pumps, which have evacuation rates of up to several hundred m3/sec with a vacuum of up to 10-6 N/m2 (10-8 mm Hg). In the oil-diffusion vacuum pump several pumping stages are connected in series in one

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casing (Figure 8). The operating pressure range of a three-stage oil-diffusion pump is 10-3-10-1 N/m2 (10-5-10-3 mm Hg).

Figure 8. Diagram of three-stage oil-diffusion pump Sorption pumps. Sorption pumps take advantage of the capacity of several substances (titanium, molybdenum, zirconium, and others) to absorb gas. The gas being pumped settles on the surface within the vacuum system, and one of the active absorbents is continuously sprayed on the absorption surface (evaporation pump). A porous adsorbent may also be used as the absorber. Ion pumps. The operation of ion pumps is based on the ionization of gas by a strong electric discharge and the removal of the ionized molecules by an electric field. This method is rarely used owing to complexity of construction and the large power demand, which goes mainly to create the magnetic field. At room temperature inert gases and hydrocarbons are, in practical terms, not absorbed by the sprayed-on metal films. Their removal is effected by combination getter ion (or ion-sorption) pumps, in which the sorption method of absorbing chemically active gases is combined with the ionic method of pumping out inert gases and hydrocarbons. The absorption surface is restored by the condensation of thermally vaporized titanium on the walls and also by the cathode sputtering of titanium in an electric discharge or in a magnetic field in sputter-ion or magnetic-discharge getter ion pumps (Figure 9). Getter ion vacuum pumps create vacuums up to 10-5 N/m2 (10-7 mm Hg) at a preliminary evacuation of up to 10-2 N/m2 (up to 10-4 mm Hg). The evacuation rate depends on the type of gas. For example, the evacuation rate of hydrogen is 5,000 l/sec, nitrogen 2,000 l/sec, and argon 50 l/sec. The ultimate pressure attained in highly degassed volumes with no inleakage of gas is lower than 10-8 N/m2 (10-10 mm Hg).

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Figure 9. Diagram of a magnetic-discharge getter ion pump: N and S are the north and south poles of a magnet, A is the anode, and C is the cathode. Condensate removal (cryogenic) pumps. The operation of condensate removal (cryogenic) pumps is based on the absorption of gas by a surface that has been cooled to a low temperature (Figure 10). The hydrogen-condensation pump proposed by B. G. Lazarev and his colleagues at the Physicotechnical Institute of the Academy of Sciences of the Ukrainian SSR has a constant evacuation rate over a wide range of pressures. The cooling liquid hydrogen is produced by a liquefier located in the unit. The noncondensable gases (hydrogen and helium) are evacuated by a pump connected in parallel with, for example, a diffusion pump. A preliminary vacuum is required to engage this type of pump.

Figure 10. Diagram of a cryogenic pump

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TRIODE SPUTTER ION PUMPS FOR CREATING UHV

These pumps are used to create UHV in charged particle accelerators, surface analytical spectrometers, mass spectrometers etc.Technology for 35, 70, 140 & 270 LPS capacity pumps. Easy maintenance - Dismantle type body feature except for 35 LPS design INTRODUCTION The triode sputter ion pumps are employed to create hydrocarbon-free ultra high vacuum. They utilise the high intensity cold cathode discharge produced in a magnetic field to sputter a highly reactive metal. The reactive metal layer called getter film combined with the active gas molecules such as hydrogen, nitrogen, oxygen, water vapour etc to form low vapour pressure stable compounds, thus reducing the number of gas molecules and hence gas pressure in the system volume. These pumps operate in the pressure range 10 -3 to 10-10 Torr. They do not require the services of a backing pump continuously but only need initial forepressure of 10 -3 Torr. The discharge current being proportional to the background pressure, the pumps also serve as pressure measuring gauges. These pumps have higher pumping capacity for inert gases compared to its predecessor diode sputter ion pump. These pumps can be mounted on a system in any orientation. APPLICATIONS The triode sputter ion pumps are used to create ultra high vacuum in charged particle accelerators, surface analytical spectrometers, mass spectrometers etc. R&D institutes, universities may require such types of pumps. SPECIFICATIONS Pump Type Pumping For N2 Speed (1/s) For Ar Starting Pressure (Torr) Ultimate Pressure (Torr) TSIP-35 35 8 < 5x10-3 5x10-10 TSIP-70 70 16 < 5x10-3 5x10-10 TSIP-140 140 32 < 5x10-3 5x10-10 TSIP-270 270 60 < 5x10-3 5x10-10
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Baking Temp.With magnets (C) 250 Connecting flange NB 63 CF Magnetic Field (Gauss) 1200 Stray magnetic field at Flange <2 (Gauss) No. of sputtering Assemblies 1 Max. Operating Voltage (kv) 6.2 Short Circuit Current (mA) 100 Weight (kg.) 20

250 100 CF 1200 <2 2 6.2 200 33

250 150 CF 1200 <2 4 6.2 500 52

250 150 CF 1200 <2 4 6.2 750 82

For details contact : Head, Technology Transfer & Collaboration Division, BHABHA ATOMIC RESEARCH CENTRE, TROMBAY, MUMBAI - 400085 Tel : 091-022-5505337/5593897 Fax : 091-022-5505151 Email : headttcd@barc.gov.in

VACUUM TUTORIAL #1
OUTGASSING OF STAINLESS STEEL AND PUMPING FOR UHV SYSTEMS

UNITS: SI including Pascal, 1 Pa = 0.01mbar. (1 Torr = 133.322 Pa)

1. Introduction UHV has long been an important tool in research and development laboratories for the physical sciences particularly those concerned with the preparation and analysis of materials often in the form of thin films. The need for rapidly and reliably obtained UHV is also a developing need in certain production industries and perhaps particularly those concerned with semiconductor manufacture. Stainless steel has been traditionally used for such systems and remains the most popular material for ease of fabrication and economic reasons, although in recent years there has been some move towards the use of aluminium (Ishimaru et al., 1992). UHV nowadays is standard technology and can be achieved rapidly and reliably providing cost is no object. In this tutorial we will consider the practical realities of the research laboratory which often involve working with existing systems, complex internal fittings for experimental purposes and sometimes the enforced use of non-UHV compatible materials. The aim is to be able to make estimates of what can be expected in less than ideal situations where a compromise may have to be reached using the available equipment. 2. Basic principles UHV may be roughly defined as vacuum pressures below E-8 mbar. For fusion or outer-space simulation applications, pressures below E-10 mbar with low hydrogen content would probably be required, whereas some high rate deposition processes for example, although sensitive to impurities, would tolerate E-8 to E-9 mbar and hydrogen may or may not be a problem. Hydrogen is highlighted for good reason; once surface adsorbed water, carbon oxides and
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hydrocarbons are removed by baking and assuming no leaks or build-up of poorly pumped gases, then hydrogen diffusing from the walls of stainless steel chambers and from internal fittings is the main source of residual gas and will be directly related to the wall thickness of the vacuum vessel. It can be shown experimentally and theoretically from Fick's Law (Jost, 1960), that long-term high-temperature bakeouts are necessary for thick-walled vessels if these are to be used at elevated (300C) operating temperatures (Santeler, 1991). Before examining the significant factors in the attainment of UHV it is worthwhile to take as a simple example a typical vacuum chamber of say 450 mm diameter and 750 mm length, an area,A, of about E+4 cm2. The pressure,p, achieved in the chamber is given by the relation,

p = QA/S mbar

....

Eqn. 1

where Q is the outgassing rate from the walls of the chamber in mbar l/ s cm2, and S is the pumping speed in l/s. Outgassing rates from cleaned and /or low temperature-baked, (<150C) stainless steel have been quoted in the literature over a wide range from E-8 to E-11 mbar l/s cm2, but using a commonly quoted (but fairly conservative), value of E-10, (Young, 1969; Sullivan, 1992; Dylla et al.,1993) gives a pressure,p, of E-8 mbar for a pumping speed of 100 l/s (a small ion-pump or turbo); or E-9 mbar for a speed of 1000 l/s (a much more expensive pump). Hence to achieve low pressures in systems containing fittings and fixtures which may involve a considerable amount of metal area and gas traps (if for example mechanical parts or manipulators are involved), it is necessary to reduce the outgassing rate by orders of magnitude if reasonable size pumps are to used. If costs are no object, pump size may be increased with advantage but not without limit, since the pump itself adds a considerable area of metal in its connecting tubulation; the outgassing from this area must be reduced to the same level as the rest of the system if advantage is to be taken from the increased pumping capacity. One should note also that in a laboratory where old equipment may have been pressed into service, the outgassing rate may well be considerable higher than in the above example even with rigorous cleaning techniques.

The principal method of reducing outgassing is baking at elevated temperature although other factors as discussed below can also be significant. 3. Factors involved in the achievement of UHV 3.1 Materials for construction and hardware

Stainless steel is the most frequently used material for fabricating vacuum chambers and for internal hardware but significant variations of outgassing rate have been found between different grades as reviewed for example by Adams (1983). Early systems and components were often made with 304 and later with 316 but considerations of outgassing, fabrication and quality control have led to the almost standardized use of 316L. Considerable variations in outgassing performance have been reported even for this one material leading to the conclusion that the quantity of gas held trapped in the metal is in many cases uncontrolled in the manufacturing process. Thus for the highest performance as required for example in fusion devices, space hardware and particle accelerators, or experiments involving the elimination of monolayers on surfaces, vacuum-melted 316L is the material of choice. The outgassing rate for
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cleaned but unbaked 316L is quoted as E-9 to E-10 mbar l/s cm2, whereas vacuum induction melted/vacuum arc remelted (a double vacuum-melting process) has an unbaked outgassing rate of E-11 mbar l/s cm2, (Sullivan et al., 1992). The use of such a material is a major advantage and can yield outgassing rates a further two or three orders of magnitude lower when surface passivation and baking techniques are subsequently used. 3.2 Surface condition Desorption of surface gas is a major component of outgassing load and it is therefore to be expected that the condition and chemistry of internal surface layers would be of importance in determining achievable vacuum. Significant factors include: chemical composition, structure and thickness of oxide layers since these affect adsorption and desorption from the surface as well as diffusion from underlying metal (Ishikawa, 1995); surface passivation to produce Cr oxide or fluoride rich or boron nitride layers (Tomari, 1991; Yoshimura et al., 1991; Tohyama et al., 1991); effect of metal forming and subsequent machining or surface finishing techniques employed (Young, 1969); polishing, which may be chemical, electro-chemical or mechanical; and cleaning where a wide range of possible techniques is available. 3.2.1 Surface chemistry Early work (Huffine and Williams, 1960), suggested that oxidation of the surface of stainless steel could reduce hydrogen outgassing by a factor of ten or more. Other workers have since found that outgassing can be reduced by oxidation. More recently Ishikawa (1995), examined the effect of a surface oxide layer on outgassing from stainless steel and found that oxidation in air produced a surface layer of iron oxide whose effect was to form a diffusion barrier for hydrogen diffusing from the bulk metal. The improvement is rather less than an order of magnitude but evidence is given that carbon contaminants also are reduced and hence carbon containing outgassing species. Young (1969), found evidence that oxidation of 304 stainless steel in air at 450C reduced outgassing by depleting hydrogen from the steel rather than any diffusion barrier effect. According to Sullivan (1992), the important chemical processes that cause the formation of volatile gases, occur in the near surface layer which extends through the native oxide and to some extent into the bulk. These authors conclude that a thin dense and chemically clean surface oxide layer reduces the probability of chemical surface processes contributing to outgassing rates. 3.2.2 Surface structure Some early workers tended to assume that outgassing would be higher from rough rather than smooth surfaces on the assumption that a rougher surface would contain more gas traps and have greater surface area. This view was questioned by Young (1969), who produced evidence with 304 stainless steel to show that outgassing from smooth electropolished surfaces was no different from glass bead shot-blasted surfaces, both surfaces having subsequently been baked at 250C. His results interestingly, agreed quantitatively with Calder and Lewin (1967) who used U15C material and who did not state any particular surface treatment. Dylla et al. (1993), examined the effect of surface roughness on outgassing performance and showed that there was no effect when the surface roughness was varied by over two orders of magnitude. It may be stated that there is little if any real evidence to show that electropolishing together with other forms of fine surface machining reduces outgassing and while such processes are
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commonly used as finishing techniques by manufacturers, their main function would seem to be cosmetic. 3.2.3 Surface Cleaning It is obvious that rigorous cleaning should be undertaken before exposing surfaces to vacuum and bakeout. ESCA studies (Sullivan et al., 1992), have shown that electropolishing alone or in combination with abrasive polishing does not result in noticeably lower surface carbon content than just trichloroethane vapor degreasing, and this conclusion applies to most other impurities examined. The authors criticise the use of electropolishing in manufacturing practice for quality control reasons, since commercial electropolish suppliers may not change solutions frequently enough to remove impurities which can lead to outgassing products as well as particles and corrosion centers. They conclude that for vacuum component manufacture, an environmentally safe cleaning process using an alkaline-based detergent, hot deionized water rinse and drying is an effective technique resulting in surfaces that desorb water efficiently and also have extremely low particulate generation. A form of cleaning which has been used successfully in the fusion energy field is glow discharge cleaning (Santeler, 1991). In this process the higher energies (compared to thermal motions), of the plasma particles removes tightly bound carbon oxides and and hydrocarbons which are removed by the pumps. This is of vital importance when a low surface contamination is necessary (for example when surfaces are to be subsequently bombarded during a processing schedule). Plasma cleaning may be combined with simultaneous baking for maximum effectiveness. 3.3 Baking Early workers baked systems only to about 200C which was effective in removing weakly bound surface water and hydrocarbon molecules. It was not long before it was discovered that baking to higher temperatures was required to remove more tightly bound species and the hydrogen diffusing from the bulk, both of which had the effect of limiting the ultimate system vacuum. The effectiveness of high temperature bakes is amply demonstrated for example by Calder and Lewin (1967), who showed that outgassing could be reduced to about E-16 mbar l/s cm2 by baking for 11 days at 300C or 1 hr only at 635C. Barton and Govier (1968), showed that baking new 18/18/1 stainless steel components at 450C in vacuo, with the exception of traces of hydrogen, successfully removes all gases resulting from the previous history . Interestingly these workers found that gas adsorbed at the surface of stainless steel on re-exposure to atmosphere could be remove by baking at this temperature for 2 to 3 hrs. If pressures only of the order of E-9 mbar were required then sufficient gas could be removed by a 12 hr bake at 200 to 300C; for some applications it is thus worthwhile to use a separate vacuum oven for baking new components at 450C thus avoiding the need for the main system to withstand high temperatures. Santeler (1991), quotes early work by Aero Vac Corporation which gives valuable data on the effect of baking to different temperatures which is reproduced here below: Outgassing rates in Torr l/s cm2

BAKING TIME
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BAKING TEMP 150C 250C 400C 500C

20 hrs 6.3E-11 6.3E-12 4.0E-13 8.0E-15

40 hrs 5.3E-11 5.3E-12 1.7E-13 8.0E-16

100 hrs 2.8E-11 2.8E-12 1.0E-13 4.0E-17

200hrs 2.0E-11 2.0E-12 1.0E-13 8.0E-19

The data above bring home clearly the benefits of high baking temperatures and the diminishing returns from increasing baking time much beyond 20 hrs for baking temperatures up to 400C; at 500C the table shows that it is worthwhile to bake for as long as 200 hrs although one might legitimately question the unusually low value of 8.0E-19 torr l/s cm2 that is quoted. Recent work (Ishikawa, 1995; Ishikawa et al 1991; and Ishikawa and Odaka1990), confirms the values above for lower temperatures but indicates that surface treatments and raw material quality can improve these figures substantially, (section 3.2 above). 3.4 Pumping systems The selection of pumps, whether for research or production, is not always straightforward and invariably involves cost considerations. All four main types of high vacuum pump: turbo, cryo, diffusion and ion, are capable of producing pressures in the UHV region, often with the addition of a titanium sublimation pump (TSP), to achieve the lowest pressures. The choice of pump will often be determined by the application. However, there are characteristics of pumps which limit their ultimate UHV performance and capability of removing products of outgassing and these are now considered. 3.4.1 Turbomolecular pumps (TMPs) These are compressors and are limited inherently by the low compression ratio for hydrogen which is the main residual gas in a UHV system. To achieve pressures approaching E-10 mbar or less it is advisable to combine this type of pump with a titanium sublimation pump for the above reason. TMPs can usually be baked to a maximum of about 120C and for some models less, hence some thought is necessary when designing connecting manifolds to avoid overheating the pump and at the same time minimising the area of metal that is heated only to low temperature during bakeout. Lower cost TMPs have hydrocarbon oil or greased bearings which is a potential source of contamination but providing the pump is operated correctly hydrocarbon molecules will not migrate into the vacuum vessel. Correct venting is particularly important and the pump must not be stopped under vacuum. Higher cost TMPs are available with air or magnetic bearings which avoid these possible problems. 3.4.2 Cryopumps(CPs) These pumps are limited by their capacity to cryosorb hydrogen onto cold charcoal. An ultimate system pressure somewhat below E-9 mbar is typical which can be extended to below 5E-10 mbar with a TSP. The capacity to adsorb hydrogen will decrease with time once the hydrogen cryosites are used up and this can result in an increase in system pressure. CRPs cannot be baked and moreover must be shielded from radiated or conducted heat caused by baking or processing schedules of the main system. The area of unbaked shields and tubulation must be minimal if UHV pressures are to be achieved. Some manufacturers have incorporated
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additional radiation cold shields and baffles into their pump designs to reduce the scale of this problem. Cryopumps have very high pumping speeds for water-vapour, but in a UHV system water-vapour is removed by baking so that this may not be such a great advantage. CRPs require periodic regeneration and a high vacuum isolation valve; for the lowest pressures an all metal bakeable design is necessary, but many UHV systems operate satisfactorily with a viton plate seal and copper gasket or wire seals for flanges with a bellows sealed drive. The viton seal can be baked safely to 120C closed and 150C in the open position. As stated above the area of metal not heated to the full baking temperature must be minimised. 3.4.3 Diffusion pumps (DPs) DPs will pump to about 5E-10 mbar which can be extended to well below E-10 mbar with a TSP. Current practice is to use low vapour pressure hydrocarbon based fluids with a liquid nitrogen and/or water or cryo-cooled baffle. Thorough tests have shown, (for example, Gay et al., 1994; Dennis et al., 1982) have shown that even with only a water-cooled baffle hydrocarbon contamination from the pump is at the limits of measurement and effectively close to zero for all practical purposes. The work by Gay et al., is particularly illustrative; the experiments were made to confirm contamination free conditions for a GaAs source which could not tolerate hydrocarbons or CO and revealed the importance of correct operation not only of the diffusion pump, but the foreline where trapping and purging procedures were found to be essential to ensure isolation from rotary pump backstreaming. Dennis et al., showed that integral diffusion pump/baffle/valve systems could be cleaner than hydrocarbon lubricated turbopumps. DPs do carry the risk of gross contamination from the consequences of accidental air-dumping or partial contamination from faulty operation. Diffusion pumps, like turbopumps, act by compression and hence their pumping action in a UHV system is also finally limited by the compression ratio for hydrogen, but the problem is less severe with a DP compared to a TMP. A high vacuum valve is normally used to isolate the pump when the system is vented, but some designs of UHV system would eliminate this to achieve higher pumping speeds and remove a source of outgassing. 3.4.4 Ion pumps (IPs) IPs will pump to 5E-10 mbar or less with extension to below E-10 mbar with a TSP. In many respects the ion pump which has no moving parts or working fluids is ideal for UHV in cases where there is no subsequent process gas load. The IP does have certain characteristics which the user needs to be aware of and may cause problems in some circumstances: (i) Selective pumping. Pumping is by gettering for chemically active gases and burial for inert gases, which occurs at a much lower pumping speed. Inert gases will therefore tend to build up as a residual gas background, the lighter inerts (He and Ne), are particularly prone since these may diffuse out again from beneath the surface. Hydrogen readily diffuses into titanium as a solid solution, but will be released again on heating. The presence of argon in the residual enhances sputtering and hence the chemical removal of hydrogen as titanium hydride. Methane is normally present in the residual since this is generated at titanium surfaces although also removed by dissociation in the pump discharge. (ii) Memory effects. These are characteristic of IPs and will affect the residual gas composition, gas ions buried in the cathodes earlier in the life-cycle are released by subsequent sputtering. The effect can be particularly bad for inert gases and leads to the phenomenon of argon instability where significant amounts of released argon lead to periodic increases of pressure. This has been designed out of some models of pump by slotted cathodes, triode structures or Ti/Ta cathodes. (iii) No tolerance to gas load. IPs
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are not suitable for even small loads and particularly inert or hydrocarbon gases; once the pressure inside the pump rises above E-6 to E-5 mbar, the pumping speed falls and pumping may become unstable. This can eventually lead to heating inside the pump and the additional release of hydrogen, helium and neon. Undetected leaks during starting can be a particular problem. (iv) IPs have magnetic fields which can interfere with processes unless screened which is not always possible. The ion pump may be operated with sorption pumps (some workers use a turbopump) for starting, to produce a completely contamination free system. The whole system including the pump can be baked, the baking temperature depending on whether the ion-pump magnets are removed. A high vacuum valve, which increases outgassing load and reduces pumping speed, is not necessary although this can be useful for isolation for faster starting during pump-down. 4. Example from a silicon processing research laboratory A small stainless steel chamber 30 cm diameter by 50 cm long and used for SIMS analysis is attached through a Viton-sealed gate-valve to the central distribution chamber of a cluster-tool which processes 8 inch diameter silicon wafers. The gate-valve is of 'letter-box' design allowing the wafer to pass back and forth through a slot between the two chambers. The SIMS chamber is pumped directly by a 150 l/s ion pump with no high vacuum valve, the chamber and ionpump being initially roughed from atmosphere through a small Viton-sealed valve connected via a foreline to a turbopump. A titanium sublimation pump is available and an additional 50 l/s turbopump is used to evacuate the SIMS ion-gun, but this pump is ineffective in pumping the chamber because of the constriction to gas-flow by the ion-optics. After loading the wafer and closing the gate-valve the system is required to be pumped to less than E-9 mbar and pressures approaching E-10 mbar would be preferred. A fast cycle time is important to prevent a bottle-neck as processed wafers are passed from the other process chambers. The budget on this project is exhausted and only minor purchases can be considered. What baking times and temperatures are required and are they consistent with all the requirements? Would the titanium sublimation pump overcome any limitations of the baking schedules? The total area of the chamber with flanges and tubulation is about 6000 cm2. It is difficult to calculate the area of the internal parts which contain many gas traps in the form of bearings and screw threads of manipulators, several sets of bellows and in addition the ion optics and detector components of the surface analysis system. For the sake of the example we will assume a total area of three times the above, that is 18000 cm2. For a preliminary estimate, assume a 20 hr bake at 150C which creates no problems for the Viton seals provided the valves are open (this assumes the distribution chamber is open during the bake which may not be desirable). Using Equation 1, and Santeler's values above for Q, then:

p = 6.3 * E-11 * 18000/150 Torr = E-8 mbar

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This is clearly inadequate for the application and too high to make worthwhile use of the titanium sublimation pump. To achieve a pressure just an order of magnitude lower would require baking for 20 hrs at 250C, so that for the required lower pressures, baking at 300C would probably suffice. The difficulty is protecting the Viton seals. The options available are: (i) Cool the seals. This is difficult and may be impossible to engineer with the geometries and existing construction of the gate-valve although the small roughing valve could cooled without difficulty. (ii) Replace the valves with metal sealed versions. In this example the budget does not allow new capital purchases, moreover, a metal sealed UHV gate-valve which would pass an 8 inch diameter wafer would be of high cost although the small roughing valve could possibly be replaced with a small conflat sealed valve. (iii) Use larger pumps. The example shows that a pump of considerable more than 1500 l/s would be required and again this is beyond budget. (iv) Bake for longer times. This is not acceptable, even 20 hrs is too long for process turn-round requirements. The table above shows that in any case the gains from longer bakes are only minimal. One is left with a compromise situation; unless residual vacuum requirements are relaxed, one must try and bake the chamber at the highest temperature possible while relying on the large mass of the distribution chamber to keep the gate-valve at an acceptable temperature to protect the seals. It is worthwhile to estimate the permitted fraction,x, of the area of the chamber metal baked at lower temperature in order to achieve required pressures. The final pressure will then be the sum of two components from metal outgassed at lower and at higher temperature. For the estimate we will ignore the temperature gradient and assume average values. If x not too large then the contribution from baking the main chamber at 300C for 20 hrs assuming an outgassing rate of E-12 mbar l/s cm2, is given to an approximation by: p(300) = E-12 *(18000)/150 mbar .... Equ. 2

The contribution from baking a smaller area, 6000x cm2, at 150C for 20 hrs with an outgassing rate of 8*E-11 mbar l/s cm2 is given by: p(150) = 8*E-11 * 6000x/150 mbar .... Equ. 3

Adding Equs. 2 and 3 yields: p(300) + p(150) = 1.2 E-10 + 3.2 E-9x .... Equ. 4

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The second term in Equ. 4 equals the first when x is about 4%, yielding a pressure of 2.4E-10 mbar, if x is allowed to increased to 10%, the total pressure increases only to 4.4E-10 mbar, which is perfectly acceptable for the application. This approach looks feasible, the example illustrates the initially assumed fact that outgassing is dominated by the internal parts and it is clearly important to ensure thorough degassing of the internal mechanisms when the gatevalve is maintained at lower temperature. Once the pressure is below E-9 mbar it is worthwhile to use a titanium sublimation pump for attaining lowest pressures.

Titanium Sublimation Pumps

Titanium Sublimation Pumps (TSP) are often used in combination with ion getter pumps, because they have an especially high pumping speed for some gases. In a TSP, filaments of a titanium alloy are heated electrically until titanium sublimates from the surface of the filaments into the vacuum. The titanium sublimates to the nearby areas and forms a thin layer. This layer has a high pumping speed for reactive gases, which either form a chemical compound or are adsorbed. But with increasing covering by these gases the pumping speed decreases. By cooling the surfaces with water or liquid nitrogen it is possible to increase the pumping speed considerably. TSP are especially useful for gases such as H2O, CO, CO2 and O2. Using nitrogen cooling, H2 and N2 can be effectively pumped as well

WHAT IS SPUTTERING?
A technique used to deposit thin films of a material onto a surface (a.k.a. "substrate"). By first creating a gaseous plasma and then accelerating the ions from this plasma into some source material (a.k.a. "target"), the source material is eroded by the arriving ions via energy transfer and is ejected in the form of neutral particles - either individual atoms, clusters of atoms or molecules. As these neutral particles are ejected they will travel in a straight line unless they come into contact with something - other particles or a nearby surface. If a "substrate" such as a Si wafer is placed in the path of these ejected particles it will be coated by a thin film of the source material. Although SPUTTERING as described above seems relatively intuitive, familiarization with the following terms / concepts will give a more comprehensive understanding of this process: Sometimes described as the "fourth state of matter" (the first three being solid, liquid, gas), a gaseous plasma is actually a "dynamic condition" where neutral gas atoms, ions, electrons and photons exist in a near balanced state simultaneously. An energy source (eg. RF, DC, MW) is required to "feed" and thus maintain the plasma state while the plasma is losing energy into its surroundings. One can create this dynamic condition by metering a gas (e.g. Ar) into a pre-pumped vacuum chamber and allowing the chamber pressure to reach a specific level (eg. 0.1 Torr) and introducing a live electrode into this low pressure gas environment using a vacuum feedthrough.

POWERING THE ELECTRODE WITH DCV WILL RESULT IN:

1. Ever present "free electrons" will immediately be accelerated away from the negatively charged electrode (cathode). These accelerated electrons will approach the outer shell electrons of neutral gas atoms in their path and, being of a like charge, will drive these electrons off the gas atoms. This leaves the gas atom electrically unbalanced since it will have more positively charged protons than negatively charged electrons - thus it is no longer a neutral gas atom but a positively charged "ion" (e.g. Ar +).

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2. At this point the positively charged ions are accelerated into the negatively charged electrode (a.k.a. "cathode") striking the surface and "blasting" loose electrode material (diode sputtering) and more free electrons by energy transfer. The additional free electrons feed the formation of ions and the continuation of the plasma.

3. All the while free electrons find their way back into the outer electron shells of the ions thereby changing them back into neutral gas atoms. Due to the laws of conservation of energy, when these electrons return to a ground state, the resultant neutral gas atom gas gained energy and must release that same energy in the form of a photon. The release of these photons is the reason the plasma appears to be glowing.

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MAGNETRON SPUTTERING
The "diode sputtering" example given above has proven to be a useful technique in the deposition of thin films when the cathode is covered with source material ("sputtering target"). Diode sputtering however has two major problems - the deposition rate is slow and the electron bombardment of the substrate is extensive and can cause overheating and structural damage. The development of magnetron sputtering deals with both of these issues simultaneously. By using magnets behind the cathode to trap the free electrons in a magnetic field directly above the target surface, these electrons are not free to bombard the substrate to the same extent as with diode sputtering. At the same time the extensive, circuitous path carved by these same electrons when trapped in the magnetic field, enhances their probability of ionizing a neutral gas molecule by several orders of magnitude. This increase in available ions significantly increases the rate at which target material is eroded and subsequently deposited onto the subtrate.

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WHAT IS A MAGNETRON SPUTTERING SOURCE?

A tool to deposit thin film that mounts to a vacuum chamber by means of either flanges or feedthroughs and consists of a water cooled cathode/target holder with an imbedded magnet array and appropriate grounded shielding. Numerous designs and magnet configurations are employeed to address particular requirements.

MODULAR MAGNET ARRAY - MAGNETRON SPUTTER SRC.

A special magnetron sputtering source feature developed by AJA International, Inc. in 1991 to allow the end user to convert the specific magnetic field of the source to a variety of configurations. For example, each source can be configured to operate in the:
"Balanced mode" to minimize substrate ion / electron bombardment "Unbalanced mode" to utilizing simultaneous ion bombardment to enhance film properties "Magnetic material mode" to help the magnetic field saturate and overcome the shunting effect of magnetic target materials allowing the magnetron sputter deposition of high permeability targets such as Fe.

CONFOCAL SPUTTERING

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A sputtering system configuration where multiple magnetron sputtering sources are arranged in a specific circular pattern and are aimed at a common focal point. When a substrate is placed in the vicinity of this focal point and rotated on its own axis, it is possible to deposit highly uniform single layers, multi-layers and co-deposited alloy films. It is an extremely popular technique for the following reasons:
Exceptional deposition uniformity on substrates twice the diameter of the source targets. Ability to easily control the growth of successive layers ranging in thicknesses from less thanone atomic monolayer to thousands of Angstroms. Minimizes time delay between subsequent layers since the substrate does not have to be re-positioned for each layer. In a con-focal multi-layer deposition, every source shutter opens about one second after the previous shutter has closed thereby keeping the deposited film surface on the substrate "in the plasma". This keeps the interface surface free from contamination by residual gas and prevents nucleation of the next layer material. Complete freedom to easily grow alloys of any number of materials in any ratio with precise control. This is ideal for combinatorial chemistry applications and for optimization of compound material target stoichiometries for production applications. The con-focal sputtering configuration is compact and maintains the substrate holder in an axial orientation. This allows for much more freedom and sophistication in substrate holder design and keeps overall costs down. For low deposition rate materials it is possible to boost the rate by running 2-3 targets of this material simultaneously from a single power supply.

IN-SITU TILT SOURCES IN A CONFOCAL SPUTTERING SYSTEM

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In powerful R&D sputtering systems with the maximum level of flexibility, end users like to have the ability to operate at different "working distances" (distance between target and substrate). In order maintain high deposition uniformity, the focal point of the magnetron sputtering sources must be variable by adjusting the source head angle. Also, the deposition profile of materials deposited with DC, with RF and with magnetic materials are all different, so the optimal angle for each material is not identical even if the working distance remains unchanged. In 1991 AJA International, Inc. invented the world's first UHV and HV magnetron sputter sources with INSITU TILT. Without breaking vacuum, each source head angle could be individually set with a precision micrometer to a specific angle. If removed for service or cleaning, it could be returned to the system and set to precisely the same angle - this is much more difficult to accomplish with manually adjustable, source head tilt assemblies. IN-SITU TILT combined with a load-lock on the sputtering system also saves a significant amount of time in performing quick test runs in succession to zero in on the optimal source angles. What can be done in a few hours on a system with load-lock and IN-SITU TILT can take weeks on a system with manual source head tilt since adjustment requires venting the chamber each time to reset the angle. Finally, IN-SITU TILT permits the user to tilt the source away from the substrate and grow "gradient" or "wedge" films which are popular in combinatorial chemistry applications.

DIRECT SPUTTERING

A sputtering system configuration where the substrate is positioned or moving directly in front of and parallel to the magnetron sputtering source targets. As a rule, target diameters (or "lengths" as in the case of rectangular magnetron sputtering sources) should be about 20% to 30% larger than the substrate to achieve reasonable uniformity. For example a 100 mm wafer would require a 150 mm sputter target to

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achieve +/- 5% deposition uniformity. Although this configuration is much less flexible and generally more expensive than con-focal sputtering, it has its place in production applications which require maximum deposition rates (semiconductor wafer metallization), applications which utilize large substrates (e.g. flat panel displays) and a few techniques that demand "line-of-sight deposition" (e.g. "lift-off"). Utilizing a direct sputtering configuration for R&D is justified in certain instances, but often is chosen because it is what the researcher has "seen before". Like diode sputtering, this was the original sputter system configuration and "old habits die hard". It is important to clearly evaluate your needs before choosing between direct and con-focal deposition orientation.

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