Vacuum techniques (down to 1 K)

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Vacuum techniques (down to 1 K) For isolation (deep Knudsen regime) liquid helium dewar / inner vacuum jacket Leak testing at level 10-11 Pa m3/s (10-10 mbar l/s) liquid helium dewar & transfer syphon inner vacuum jacket helium evaporator (pot) dilution refrigerator helium sample chamber (if exists) 3He circulation (tubing, pumps, valves, storage tanks, pressure gauges, cold traps,...) Refrigeration by evaporation cooling helium evaporators dilution refrigerator ( pulse tube coolers) System design has to permit required flow rate at given vapor pressure 4He: ~ 1 10 mmol/s @ p ~ 1 mbar 3He: ~ 0.1 5 mmol/s @ p ~ 0.01 0.1 mbar 1

Cryoadsorption pumps Best possible vacuum is obtained by cryoadsorption on charcoal activated charcoal has strong binding potential on surface for gas molecules huge surface area per mass unit (~ 600 m2/g) when it is cold (< 10 K) it adsorbs anything, also He saturates, when the surface is fully covered heat to room temperature => release gases He, H2, N2, O2 (regeneration) used for securing vacuum in storage dewars used also for purifying circulating He in cryostats (kept in LN2) can be used to take care of SMALL leaks in inner vacuum jacket heat of adsorption is considerable 2

Helium leak detector Helium is used for leak detection because inert gas does not react in the system small atom, penetrates easily through the tiniest holes does not appear in natural environment (low background) light, easy to determine with a mass spectrometer Note the diffusion of He through plastics & rubber at room temperature Modern units have several modes of operation for small and big leaks direct mode counterflow mode rough mode sniffing mode 3

Helium leak detector (cont.) Mass spectrometer for leak detectors: hot cathode emits electrons, which ionize the surrounding gas ions are accelerated by electric field accelerated ions are deflected by magnetic field can be set to detect mass numbers 2 (H2), 3 (3He), or 4 (4He) calibrate by means of a standard leak: He gas diffusing through a sealed Pyrex-glass ampule 4

Leak testing 1) Huge leaks: impossible to get below 10 3 mbar or p returns above 10 mbar bubble test, soap test (if applying overpressure is possible) solvent exposure test (monitor pressure when putting alcohol on suspect spot) blue stick test (cover the hole by blue stick and see if the rest is ~ OK) 2) Big leaks: pump OK, pressure stays low, but leak detector level is high blue stick method may work sniffing technique, if test chamber can be filled with He 3) Small leaks: leak signal low (< 10 8 mbar l/s), but reacts to He exposure injection needle search; expose to He minimum area possible at a time bag test, put parts of the system (if possible) into a bag filled by He 4) Tiny leaks: leak signal low (< 10 9 mbar l/s), no response at room temperature warm systems are OK at this level cold systems must be tested at LN2 temperature and 10 K; tiny leaks show up 5) Superleaks: only appear when superfluid helium is present in the system nightmare (remake the faulty component or seam) 5

Evaporation cooling Ideal gas assumption: 1) particle diameter a << distance between particles 1/n1/3 2) no interactions between the particles 3) collisions between the particles are elastic mean free path pressure viscosity average velocity l = 1/(21/2 p a2 n) p = n kbt h = [8 m kbt/(9 p3 a4)]1/2 v = [8 kbt/(p m)]1/2 These apply well to helium gas (a ~ 0.22 nm) in all considered cases Efficiency of evaporation cooling from Clausius-Clapeyron relation: dp ΔS L = = dt ΔV T ΔV latent heat L = TDS depends weakly on temperature DV = Vg Vl Vg = NAkBT/p = R T/p 3He: L3/R ~ 2.5 K 4He: L4/R ~ 8.5 K dp/p L/R dt/t2 => p ~ e L/(RT) { 6

Sustainable mass flow depends on dimensions of the tubing; capacity of the vac pump; pp (pump) <~ pv (vapor) dn/dt = pp/kbt dv/dt (pump) pp (pump) dq/dt = dn/dt L/NA ~ e L/(RTv) (vapor) Cooling power is given by Mechanical rotary pump (10... 100 m3/h) is enough for a decent 4He evaporator Small dilution fridge can be run by a good turbo pump + mech. rotary pump Powerful dilution fridge requires heavy duty pumps: oil vapor booster + roots pump + mechanical rotary => 50 000 m3/h Viscous regime: p 2 i 1 2 i p = Molecular regime: pi 1 p i = 16 ηi l i n RT i π r 4i 3 l i n R 4 r 3i mt i 2π kb 7

4He evaporator (pot) continuous operation Tmin ~ 1 K roughly 40% of evaporating liquid is needed to cool down incoming fluid, the rest is available for cooling => dq/dt ~ 0.6 dn/dt L flow impedance (~ 1 m of 50 µm capillary) 8

9

3He evaporators Tmin ~ 0.3 K closed cycle, tight pumps, minimum volume combine with 4He pot, since Tc3 = 3.3 K impedance ~ 1012 cm 3 circulating gas must be cleaned (LN2 charcoal trap) nearly as complicated in construction as a simple dilution fridge with base-t ~ 50 mk 10

Cryocoolers Stirling cycle: Adiabatic compression => heating Adiabatic expansion => cooling TdS m = C p dt T αv V m dp 1 V m αv = ( ) V m T p T αv V m δt = δ p(s m constant) Cp Regenerator: 1. heat capacity of the matrix is larger than that of gas 2. thermal contact between gas and the matrix is perfect 3. gas behaves as ideal gas 4. the flow resistance within the matrix is negligible 5. the axial thermal conductivity is negligible Coefficient of performance: x = TL/(TH TL) 11

Pulse tube refrigerator Components: piston (or compressor + valves) heat exchangers X1, X2, X3 regenerator tube orifice buffer volume Working substance is helium gas at p ~ 20 bar Every other process is reversible except flow through the orifice Pressure in the buffer volume is practically constant Heat produced by the piston is taken out at X1 Heat absorbed at the low temperature junction X2 is taken out at X3 Coefficient of performance: x = TL/TH 12

To produce T < 4 K, two pulse tubes must work in series Ideal extracted power: dq/dt = 1/2 RT0 dn/dt Dp/p0 cos q phase q between the gas flow and pressure can be tuned by ~ 10% flow through a bypass orifice Regenerator material has to be chosen according to the operation range Low-T stage uses magnetic heat capacity of some substances 13

Real example: Cooling capacity: 1st 30 W @ 65 K 2nd 0.5 W @ 4.2 K Lowest temperature: 2.5 K Weight: 25 kg Cool down time: 100 min 14