Introduction to Dilution Refrigerators

Cryocourse 2016
School and Workshop in Cryogenics and Quantum Engineering
26
th
 September - 3
rd
 October 2016
Aalto University, Espoo, Finland
Introduction to Dilution Refrigerators
Part I-Thermodynamics
Henri GODFRIN
CNRS/IN/MCBT – Grenoble
This part of the course is based on:
Basic operation of cryocoolers and related thermal machines
A.T.A.M. de Waele
J. of Low Temp. Physics, Vol.164, pp.179-236 (2011) 
(open access)
Introduction to dilution refrigeration
A.T.A.M. de Waele
Lectures given at Cryocourse 2013 and former ones
Dilution refrigerators
H. Godfrin
Lectures given at Cryocourse 2013 and former ones
Experimental Principles and Methods Below 1 K
Lounasmaa, O.V.
Academic Press, London, p. 316 (1974).
Matter and Methods at Low Temperatures
Pobell, Frank
Springer-Verlag, Berlin, p. 461 (2007).
 
Wikipedia:
 
https://en.wikipedia.org/wiki/Dilution_refrigerator
Outline
Introduction
Schematic diagram
Thermodynamics of dilution refrigeration
Thermal properties of pure 3He
Properties of 3He-4He mixtures
The 1 K bath
Why a still heater
The mixing chamber
Osmotic enthalpy
Limiting temperature of dilution refrigerators
History
The dilution refrigerator principle was suggested by 
Heinz London in 1952
H. London, G.R. Clarke, and E. Mendoza
 
proposed a prototype of continuous refrigerator in 1962
 
It was realized in 1964 in the Kamerlingh Onnes Laboratorium at Leiden University
Das, P.; Ouboter, R. B.; Taconis, K. W. (1965). "A Realization of a London-Clarke-Mendoza Type
Refrigerator". Low Temperature Physics LT9. p. 1253. 
(Tmin~220mK)
B.S. Neganov and co-workers in 
Dubna
 and H.E. Hall and co-workers in 
Manchester 
went 
below
100 mK (1966). Dubna rapidly reached 
25 mK
.
The principles and methods of dilution refrigeration 
have been substantially developed by J. Wheatley
et al. at 
La Jolla
.
Modern « wet » refrigerators 
are based on the 
Grenoble design 
by Frossati and coworkers.
The development of sintered silver heat exchangers Tmin led to 
Tmin~2 mK
.
« Dry » refrigerators 
were developed
-
by K. Uhlig et al. 
on 
GM coolers 
(1993),
-
and 
on 
Pulse-tube coolers 
by K. Uhlig et al. (2002) and H. Godfrin (1999 to 2003, date of first
commercial unit, delivered by l’ Air Liquide)
Lancaster has the present record of low temperatures, 
1.75 mK
Phase diagram of helium mixtures
By Mets501 - Own work, CC BY-SA 3.0,
https://commons.wikimedia.org/w/index.php?curid=25250292
Phase separation upon cooling
S
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a
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.
https://en.wikipedia.org/wiki/Dilution_refrigerator
Low temperature part
https://en.wikipedia.org/wiki/Dilution_refrigerator
https://en.wikipedia.org/wiki/Dilution_refrigerator
Continuously Operating 
4
He Evaporation Refrigerator
L. E. 
DeLong
, 
O. G. Symko
 and 
J. C. Wheatley
, 
Rev
. 
Sci
. 
Inst
. 42, 147 (1971)
Enthalpy diagram of 
4
He
Enthalpy diagram of 
3
He
Incoming 
3
He at P=0.5 bar and 4.2 K has a enthalpy of 99 J/mol
3
He leaves the still at 0.7 K and P~0.  It’s enthalpy is 35 J/mol.
The deficit is huge: 64 J/mol
Solutions: 1K pot or condensation at high pressure
Global enthalpy balance of DR
(only pure 
3
He flows in and out the sub-system)
Without  1K pot: negative balance, 
External cooling needed.  
With a  1K pot at 1.2 K: positive balance, 
external 
heating
  
(usually at the still…) 
needed.  
The cooling power provided by the 1 K pot
to change the 
3
He from gas at 0.5 bar and
4.2 K to liquid at 0.5 bar and 1.2 K, is
Condensing the 
3
He  at ~3bars
J. Kraus, Cryogenics 
17
, 173 (1977)
A.T.A.M. de Waele, A.B. Reekers, H.M. Gijsman, Cryogenics 
17
, 175 (1977)
At 4.2 K the minimum enthalpy (vs.
Pressure) is 
H
m 
42 J/mol near 
3
bars
,
just above the enthalpy of the vapor
at 0.7 K (35 J/mol).
> steady state
 is possible using a
heat exchanger to precool the
incoming 3He !!!
Dilute side
The Mixing Chamber: cooling is due to expansion
Osmotic enthalpy
Osmotic enthalpy of 
3
He mixtures
- Lines of constant osmotic pressure
         
 (solid lines, values in Pa)
- Lines of constant osmotic enthalpy H3
      
(dotted lines values in J/mol);
-
and the saturation
 
concentration of the
       
dilute phase
 
xs.
 The scale on the right gives the temperature in K.
Cooling power at the MC
L
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m
i
t
i
n
g
 
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This course covers the basic operation and thermodynamics of dilution refrigerators, outlining the key components such as the mixing chamber, still heater, and thermal properties of 3He and 3He-4He mixtures. Learn about the history of dilution refrigerators, including advancements in technology that have led to record low temperatures. Explore phase diagrams and phase separation in helium mixtures, and gain insights into the principles and methods behind dilution refrigeration.

  • Dilution Refrigerators
  • Cryogenics
  • Quantum Engineering
  • Thermodynamics
  • Low Temperatures

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  1. Cryocourse 2016 School and Workshop in Cryogenics and Quantum Engineering 26th September - 3rd October 2016 Aalto University, Espoo, Finland Introduction to Dilution Refrigerators Part I-Thermodynamics Henri GODFRIN CNRS/IN/MCBT Grenoble

  2. This part of the course is based on: Basic operation of cryocoolers and related thermal machines A.T.A.M. de Waele J. of Low Temp. Physics, Vol.164, pp.179-236 (2011) (open access) Introduction to dilution refrigeration A.T.A.M. de Waele Lectures given at Cryocourse 2013 and former ones Dilution refrigerators H. Godfrin Lectures given at Cryocourse 2013 and former ones Experimental Principles and Methods Below 1 K Lounasmaa, O.V. Academic Press, London, p. 316 (1974). Matter and Methods at Low Temperatures Pobell, Frank Springer-Verlag, Berlin, p. 461 (2007). Wikipedia: https://en.wikipedia.org/wiki/Dilution_refrigerator

  3. Outline Introduction Schematic diagram Thermodynamics of dilution refrigeration Thermal properties of pure 3He Properties of 3He-4He mixtures The 1 K bath Why a still heater The mixing chamber Osmotic enthalpy Limiting temperature of dilution refrigerators

  4. History The dilution refrigerator principle was suggested by Heinz London in 1952 H. London, G.R. Clarke, and E. Mendoza proposed a prototype of continuous refrigerator in 1962 It was realized in 1964 in the Kamerlingh Onnes Laboratorium at Leiden University Das, P.; Ouboter, R. B.; Taconis, K. W. (1965). "A Realization of a London-Clarke-Mendoza Type Refrigerator". Low Temperature Physics LT9. p. 1253. (Tmin~220mK) B.S. Neganov and co-workers in Dubna and H.E. Hall and co-workers in Manchester went below 100 mK (1966). Dubna rapidly reached 25 mK. The principles and methods of dilution refrigeration have been substantially developed by J. Wheatley et al. at La Jolla. Modern wet refrigerators are based on the Grenoble design by Frossati and coworkers. The development of sintered silver heat exchangers Tmin led to Tmin~2 mK. Dry refrigerators were developed - by K. Uhlig et al. on GM coolers (1993), - and on Pulse-tube coolers by K. Uhlig et al. (2002) and H. Godfrin (1999 to 2003, date of first commercial unit, delivered by l Air Liquide) Lancaster has the present record of low temperatures, 1.75 mK

  5. Phase diagram of helium mixtures By Mets501 - Own work, CC BY-SA 3.0, https://commons.wikimedia.org/w/index.php?curid=25250292

  6. Phase separation upon cooling

  7. Schematic diagram of a Schematic diagram of a standard ( wet ) standard ( wet ) dilution refrigerator. dilution refrigerator. https://en.wikipedia.org/wiki/Dilution_refrigerator

  8. Low temperature part https://en.wikipedia.org/wiki/Dilution_refrigerator

  9. https://en.wikipedia.org/wiki/Dilution_refrigerator

  10. Continuously Operating 4He Evaporation Refrigerator L. E. DeLong, O. G. Symko and J. C. Wheatley, Rev. Sci. Inst. 42, 147 (1971)

  11. Enthalpy diagram of 4He

  12. Enthalpy diagram of 3He Incoming3He at P=0.5 bar and 4.2 K has a enthalpy of 99 J/mol 3He leaves the still at 0.7 K and P~0. It s enthalpy is 35 J/mol. The deficit is huge: 64 J/mol Solutions: 1K pot or condensation at high pressure

  13. Global enthalpy balance of DR (only pure 3He flows in and out the sub-system) Without 1K pot: negative balance, External cooling needed. With a 1K pot at 1.2 K: positive balance, external heating (usually at the still ) needed. The cooling power provided by the 1 K pot to change the 3He from gas at 0.5 bar and 4.2 K to liquid at 0.5 bar and 1.2 K, is

  14. Condensing the 3He at ~3bars At 4.2 K the minimum enthalpy (vs. Pressure) is Hm 42 J/mol near 3 bars, just above the enthalpy of the vapor at 0.7 K (35 J/mol). > steady state is possible using a heat exchanger to precool the incoming 3He !!! J. Kraus, Cryogenics 17, 173 (1977) A.T.A.M. de Waele, A.B. Reekers, H.M. Gijsman, Cryogenics 17, 175 (1977)

  15. Dilute side

  16. The Mixing Chamber: cooling is due to expansion

  17. Osmotic enthalpy

  18. Osmotic enthalpy of 3He mixtures - Lines of constant osmotic pressure (solid lines, values in Pa) - Lines of constant osmotic enthalpy H3 (dotted lines values in J/mol); - and the saturation concentration of the dilute phase xs. The scale on the right gives the temperature in K.

  19. Cooling power at the MC

  20. Limiting Limitingtemperature temperature of DR of DR

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