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Chapter IV
Cryogenic Techniques:
Generation and
Measurement of
Low Temperatures
Chapt. IV - 2
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Chapter IV: Cryogenic Techniques
Contents:

IV.1 Generation of Low Temperatures
IV.1.1 Introduction
IV.1.2 Expansion Machine
IV.1.3 Regenerative Machine
IV.1.4 Joule-Thomson Cooling
IV.1.5 Summary
IV.1.6 Evaporation Cooling
IV.1.7 Dilution Cooling
IV.1.8 Pomeranchuk Cooling
IV.1.9 Adiabatic Demagnetization

IV.2 Thermometry
IV.2.1 Introduction
IV.2.2 Primary Thermometers
IV.2.3 Secondary Thermometers

Chapt. IV - 3
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Literature:

1. Tieftemperaturphysik
Enss, Hunklinger
Springer (2000)

2. Matter and Methods at Low Temperatures
F. Pobell
Springer, 2nd edition (1996)

3. Experimental Low-Temperature Physics
Anthony Kent
American Institute of Physics (1993)

4. Cryogenic Systems
Randall F. Barron
Oxford University Press, Oxford (1985)
Chapter IV: Cryogenic Techniques
Chapt. IV - 4
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IV.1.1 Introduction
background
temperature
in universe
(2.73 K)
lowest temperature
accessible in solids
(few K)
10
-7
10
-6
10
-5
10
-4
10
-3
10
-2
10
-1
10
0
10
1
10
2
10
3
10
4
10
5
10
6
10
7
10
8
10
9
t
e
m
p
e
r
a
t
u
r
e

(
K
)
center of hottest stars
center of the sun, nuclear energies
electronic energies, chemical bonding
surface of sun, highest boiling temperatures
organic life
liquid air
liquid
4
He
universe
superfluid
3
He
lowest temperatures of condensed matter
e
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u
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t
i
v
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y

Chapt. IV - 5
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experimental setup
according to Tauno Knuuttila (2000)

lowest temperature: about 100 pK
by demagnetization of Rhodium nuclei
(temperature of nuclear spins)

PhD Thesis,
Helsinki University of Technology
(Espoo, Finland)

problem:
spin temperature cannot be transferred
to lattice of solid
low temperature record
for nuclear spin system:
IV.1.1 Introduction
Chapt. IV - 6
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Generation of low temperatures by using cryo-liquids:

19
th
century: liquefaction of various gases by pressure
except for permanent gases (O
2
, H
2
, He)

1877: liquefaction of O
2
by thermal expansion
(L. Cailletet, C.R. Acad. Sci. Paris 85, 1213 (1877); R. Pictet, C.R. Acad. Sci. Paris 85, 1214 (1877))
1884: liquefaction of H
2
(precooling with liquid O
2
)
(K. Olszewski, Ann. Phys. u. Chem. 31, 58 (1887))
1898: significant amounts of lH
2
for physical experiments
(J. Dewar, Proc. R. Inst. Gt. Br. 15, 815 (1898))
1908: liquefaction of last permanent gas He by Kamerlingh Onnes
(H. Kammerlingh Onnes, Leiden Commun. 105, Proc. Roy. Acad. Sci. Amsterdam 11, 168 (1908))
1922: Kammerlingh Onnes reaches T < 1K
(H. Kammerlingh Onnes, Leiden Commun. 159, Trans. Faraday Soc. 18 (1922))
1926: adiabatic demagnetization of electron spins in
paramagnetic salts by Debye and independently
(P. Debye, Ann. Phys. 81, 1154 (1926)
1927: by Giauque
(W.F. Giauque, J. Am. Chem. Soc. 49, 1864 (1927)
since 1950th:
3
He available

3
He cryostat

3
He-
4
He dilution refrigerator
Heike Kammerlingh Onnes
(1853 1926)
Nobelpreis fr Physik: 1913
Sir James Dewar,
(1842-1923)
Peter J. Debye
1884 - 1966
IV.1.1 Introduction
Chapt. IV - 7
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Carl Paul Gottfried von Linde
* 11. Juni 1842 in Berndorf, Oberfranken
16. November 1934 in Munich
Low Temperature Technology in Germany
1868 offer of chair at the
Polytechnische Schule Mnchen (now TUM)
1873 development of cooling machine allowing
the temperature stabilization in beer
brewing
21. 6. 1879 foundation of Gesellschaft fr Lindes
Eismaschinen AG together with two
beer brewers and three other co-founders
1892 - 1910 re-establishment of professorship
12.5.1903
patent application:
Lindesches Gegenstrom-
verfahren
liquefaction of oxygen
(-182C = 90 K)
1861 study at Polytechnikum Zurich, teachers:
Rudolf Clausius, Gustav Zeuner und Franz Reuleaux
Chapt. IV - 9
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Year
l
o
w

t
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a
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u
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a
-
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o
w

t
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m
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a
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s

paramagnetic refrigeration
nuclear demagnetization
IV.1.1 Introduction
Chapt. IV - 10
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temperature
range
refrigeration technique available
since
typical
T
min
record
T
min
Kelvin universe
4
He evaporation
3
He evaporation

1908
1950

1.3 K
0.3 K
2.73 K
0.7 K
0.25 K
Millikelvin
3
He-
4
He dilution
Pomeranchuk cooling
electron spin demagnetization
1965
1965
1934
10 mK
3 mK
3 mK
2 mK
2 mK
1 mK
Microkelvin nuclear spin demagnetization 1956 50 K 100 pK
IV.1.1 Introduction
Chapt. IV - 11
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cooling techniques:
expansion of an ideal gas
expansion machine
regenerative machine
work against outside world
expansion of a real gas
Joule Thomson cooler
work against internal interactions
evaporation of a real gas:
dilution cooling (
3
He/
4
He)
adiabatic demagnetization (electronic/nuclear moments)
work against magnetic ordering
IV.1.1 Introduction
Chapt. IV - 12
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Liquefaction of gases three useful methods:

1. direct liquefaction by isothermal compression
2. letting the gas perform work against external forces at the expense of
its internal energy
cooling and eventual liquefaction
3. making the gas perform work against its own internal forces by Joule-
Kelvin or Joule-Thomson expansion
cooling and eventual liquefaction
IV.1.1 Introduction
Chapt. IV - 13
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direct liquefaction of gases by isothermal compression
starting temperature must be smaller than critical temperature T
c
ammonia (NH
3
) 406
O
2
154.5
N
2
126
H
2
33.2
4
He 5.2
3
He 3.32
critical
temperatures T
c

in K of selected
liquid cryogens
melting curve
sublimation curve
critical point
triple point
solid
liquid
gas
T
p
T
c
boiling curve
p
c
IV.1.1 Introduction
Chapt. IV - 14
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@ 1 bar
Cryogenic Liquids
T
tr
, p
tr
solid
liquid
gas
T
p
T
c
1 at

T
c
, p
c
T
m
, p
m
T
b
, p
b
IV.1.1 Introduction
Chapt. IV - 15
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cryogen boiling
point [K]
liquefaction latent heat
[kJ/I]
inversion
temp. [K]
oxygen 90.2 1877: Cailletet and Pictet 240 762
nitrogen 77.3 1883: Wroblewski and
Olszewski
160 625
hydrogen 20.4 1898: Dewar 30 203
4
Helium 4.2 1908: Onnes 2.6 43.2
3
Helium 3.2 0.5 -
liquid oxygen and hydrogen have potential hazards
liquid nitrogen and
4
He are the most widely used cryogens
liquid
3
He is very expensive
IV.1.1 Introduction
direct liquefaction of gases by expansion (Joule-Thomson-Effect)
starting temperature must be smaller than inversion temperature

Chapt. IV - 16
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gas molecules are reflected at the moving piston-surface:
incoming: laboratory system:

piston system:

outgoing: piston system:

laboratory system:
= 2

i.e.:
molecule is slower, i.e. colder

liquefaction of gases by performance of external work
average momentum transfer per time to piston = force, force distance = work
external work at the expense of internal energy cooling
IV.1.1 Introduction
Chapt. IV - 17
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efficiency:

Carnot process: technologically difficult to realize
better: gas circulation, compressor and expansion machine
are spatially separated
Carnot process:
- counterclockwise: heat pump (conversion of mechanical work into heat)
- clockwise: heat engine (conversion of heat into mechanical work)

pV diagram:
expansion cooling: adiabats
(
= , = 0
=

> 1)
heat exchange: isotherms
( = , = 0)

work per cycle:
= =
warm
T
T
Q
W A
= q
A
thermodynamic definition of temperature
IV.1.1 Introduction
V
p
Q
12
Q
34
dQ = 0 (adiabatic)
T
1
= const
(isothermic)
T
2
= const
dQ = 0
W
23
W
41
1
2
4
3
Chapt. IV - 18
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medium: He gas
Brayton method
e.g. liquefaction of air:
- condensation on cold head
- distillation in separation columns
N
2
(77.4 K) cooling
Ar (87.3 K) inert gas
O
2
(90.2 K) welding
temperature reduction:
=
(= 5/3 for He)

expansion from 100 bar to 1 bar
results in T
2
= 50 K
T
2
= 8 K can be reached in a 2 stage cycle
(should not cause
significant resistance
for flowing gas e.g.
concentric tubes)
efficiency:
Chapt. IV - 19
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heat pumps: heating and refrigerating machines
- heat pump:
heat is generated by mechanical work

- efficiency:
W
Q T T
h
A
A
=
=
=
1 1
work performed
at heat generated
- ideal efficiency for reversible Carnot process:
1
1
2 1
1
>
=
q
=
T T
T
h
C
C
(increases with decreasing temperature difference T
1
T
2
)
- refrigerating machine: removing heat (generating cold) by mechanical work
0 1
work performed
at heat removed
2 1
2 2
>
= =
=
=
T T
T
h
T T
k
C C
V
p
Q
12
Q
34
dQ = 0
T
1
= const
T
2
= const
dQ = 0
W
23
W
41
1
2
4
3
IV.1.1 Introduction
(decreases with increasing temperature difference T
1
T
2
)
Chapt. IV - 20
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Wikimedia Commons
IV.1.1 Introduction
Schematic diagram of a heat pump's vapor-compression refrigeration cycle:
1) condenser, 2) expansion valve, 3) evaporator, 4) compressor.
e.g. air conditioning e.g. heating of swimming pool
Chapt. IV - 21
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realizations of expansion machines:

piston-cylinder machine
similar to automobile engine
crankshaft, camshaft, valve
brake on turbine axis
controls rotational speed,
annihilates performed work,
use of gas bearings

cooling turbine commercially relevant
higher efficiency for larger throughput

principle:
Chapt. IV - 22
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turbine cooler
(Sulzer machine)
turbine wheel
and nozzle ring
(Source: Linde Cryogenics Ltd.)
Chapt. IV - 23
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conclusions:

expansion machines are technologically simple
multi-stage arrangements for lower temperatures
almost down to 4.2 K
but:
efficiency only acceptable for cooling turbines
no direct liquefaction of gas (mechanical problems)
liquefaction by Joule-Thomson stage
for small-scale facilities:
regenerative machines better suited
Chapt. IV - 24
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IV.1.3 Regenerative Machines
regenerator replaces heat exchanger
column with staple of fine
metal meshes (Cu, Pb)

low flow resistance
high heat capacity
low longitudinal heat conductivity
cold gained in step 2 3 has to be stored and provided in step 4 1
alternating gas flow:
cold gas upward
cooling of meshes
warm gas downward
cooling of gas

used in Stirling process
V
p
Q
12
Q
34
V = const
T
1
= const
T
2
= const
V = const
Q
23
Q
41
1
2
4
3
Stirling process (heat engine):
Chapt. IV - 25
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Stirling machine:
(heat engine)
- periodic expansion and compression of gas along
two isotherms and two isochors
- 1 2: isothermal expansion, Q
12
is added
- 2 3: isochoric cooling, Q
23
is removed
- 3 4: isothermal compression, Q
34
is removed
- 4 1: isochoric warming, Q
41
is added
- for isochoric steps there is no mechanical work

- goal: intermediate storage of Q
23
in regenerator
to be able to add it again in step 4 1
use of two pistons with phase shift
V
p
Q
12
Q
34
V = const
T
1
= const
T
2
= const
V = const
Q
23
Q
41
1
2
4
3
3 4 4 1
1 2 2 3
T
2
T
1
Chapt. IV - 26
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(beta) Stirling machine:
Power piston (dark
grey) has
compressed the
gas, the displacer
piston (light grey)
has moved so that
most of the gas is
adjacent to the hot
heat exchanger
The heated gas
increases in
pressure and
pushes the power
piston to the
farthest limit of the
power stroke.
The displacer piston
now moves,
shunting the gas to
the cold end of the
cylinder.
The cooled gas is
now compressed by
the flywheel
momentum. This
takes less energy,
since when it is
cooled its pressure
dropped.
Chapt. IV - 27
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(alpha) Stirling machine:
Chapt. IV - 30
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conclusions (Stirling machine):

advantages:
high efficiency
well-suited for small systems, especially small coolers
cryocooler
not realizable with turbines
disadvantages:
mechanically complicated
piston (compressor) at low temperature
more simple:
Gifford-McMahon machine
but: lower efficiency
Chapt. IV - 31
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)

Gifford-McMahon machine:
uses compressor with switching valve instead of piston
1. warm compression: 2 1
2. isochoric cooling: 1 4
3. expansion in cylinder: 4 3
4. isochoric regeneration: 3 2
5. warm compression: 2 1
pressure wave from valve
hot
cold
regenerator
switching valve
cycle:
V
p
Q
12
Q
34
V = const
T
1
= const
T
2
= const
V = const
Q
23
Q
41
1
2
4
3
Chapt. IV - 32
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Gifford-McMahon cycle:
Chapt. IV - 33
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the pulse tube refrigerator (PTR) or pulse tube cryocooler is based on operation
principle of Stirling cooler
PTR is made without moving parts in the low temperature part (in contrast with
other cryocoolers, e.g. Stirling cryocooler and Gifford-McMahon cooler)
compact design possible suitable for a wide variety of applications
minimum temperature about 2.5 K (with
4
He) and 1.3 K (with
3
He)
Pulse Tube Refrigerator
applications:
industrial applications such as semiconductor fabrication (e.g. cryopumps)
cooling of infrared sensors
cooling of astronomical detectors (e.g. Atacama Cosmology Telescope or the QUBIC
experiment (an interferometer for cosmology studies)
precoolers of dilution refrigerators
Kurt Uhlig (WMI), Dry dilution refrigerator with pulse-tube precooling, Cryogenics 44, (2004), pp. 5357
suggested to be used to liquefy oxygen on Mars
Chapt. IV - 34
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Stirling Cooler
regenerator
regenerator
2-1
1-4
4-3
displacer
piston
work
piston
second (displacer) piston is
replaced by pulse tube (gas piston)
3-2
motion of gas volume
element equivalent to
motion of displacer piston
90 phase shift between
motion of displacer piston
and work piston realized
by buffer volume
90 phase shift required for
finite heat transport
buffer
volume
acoustic
impedance
coldest spot between
regenerator and pulse tube
regenerator
regenerator
regenerator
regenerator
regenerator
regenerator
Q
34
Q
12
work
piston
Chapt. IV - 36
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Q
c
Q
H
Q
c
Q
H
Q
c
: removed heat, Q
H
: generated heat
Stirling Cooler
almost sinusoidal motion, phase difference of 90

Chapt. IV - 38
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principle
Pulse Tube Refrigerator (realizations)
commercially
available
pulse tube
refrigerator
with GM drive
0.5 W @ 4.2 K
T
min
= 2.3 K
(2-stage)
www.cryomech.com
Chapt. IV - 39
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pulse tube refrigerator for studies of liquefying oxygen on
Mars (580 mm total length)
Chapt. IV - 40
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conclusion (pulse tube refrigerator):

presently very active development
no moving parts at low temperatures
long endurance
mobile base stations and satellite applications
(e.g. for superconductive microwave filters)
almost no vibrations
efficiency lower than for displacer
only one simpler method:
Joule-Thomson cooling
Chapt. IV - 41
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William Thomson (Lord Kelvin)
Born: 26 June 1824, Belfast, Northern Ireland
Died: 17 December 1907, Netherhall, Largs Ayrshire, Scotland
Chapt. IV - 43
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principle:
gas performs work against its
own internal attractive forces
working medium/gas (V
1
) flows
through impedance and
expands to V
2
1 1 2 2
0
0
1 1 2 2
2
1
V p V p dV p dV p
V
V
+ =
} }
W Q U A + A = A
1 2
U U
1 1 1 2 2 2
V p U V p U + = +
1
st
law of thermodynamics:
= 0 (adiabatic)
this means: process with constant enthapy: . const pV U H = +
- for ideal gas: p
1
V
1
= p
2
V
2
and hence U
1
= U
2
resp. T
1
= T
2
no cooling !!
Chapt. IV - 44
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weak long-range attraction:
tends to keep molecules closer together, same effect
as additional compression of the gas.

a is a measure of the long-range attraction
strong short-range repulsion:
molecules are rigid: p
as soon as the molecules touch each other.

b ( 4
3
/3): excluded volume per particle
Van der Waals equation:
E
pot
(r)
short-distance
repulsion
long-distance
attraction
-3
-2
-1
0
1
2
3
4
1.5 2.0 2.5 3.0 3.5 4.0
distance
E
n
e
r
g
y
r
real gas:
transformation of gas into liquid on decreasing T and (or)
increasing p due to
work against attractive interaction between the
molecules
2
V
a
p p
eff
+ =
b V V
eff
=
expansion (decrease of pressure):
low pressure:
attraction costs work
cooling of gas
high pressure:
repulsion provides work
heating of gas
( ) RT b V
V
a
p
m
m
=
|
|
.
|
\
|
+
2
Chapt. IV - 45
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interaction potential:
E
pot
r

repulsive attractive
p

repulsive attractive
AU (p,T)
T = const.
minimum
with
Chapt. IV - 46
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0 = A
|
|
.
|
\
|
c
c
+ A
|
.
|
\
|
c
c
= A p
p
H
T
T
H
H
T
p
more detailed analysis of Joule-Thomson process (isenthalpic expansion):
p
p
H
T C C
T
H
T
p p
p
A
|
|
.
|
\
|
c
c
= A =
|
.
|
\
|
c
c

JT
H T
p
p
T
p
H
C

A
A

|
|
.
|
\
|
=
|
|
.
|
\
|
c
c
1
V
p
S
T
p
H
p V S T H
T T
+
|
|
.
|
\
|
c
c
=
|
|
.
|
\
|
c
c
A + A = A
p
T
T
V
p
S
|
.
|
\
|
c
c
=
|
|
.
|
\
|
c
c
|
|
.
|
\
|
|
.
|
\
|
c
c
=
|
|
.
|
\
|
c
c
=
|
|
.
|
\
|
= V
T
V
T
C p
H
C p
T
p p
T
p
H
JT
1 1
A
A
Joule-Thomson coefficient
with
with
> 0: cooling on expansion
< 0: heating on expansion

Chapt. IV - 47
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)

ideal gas:
0 = = =
|
.
|
\
|
c
c
=
JT
p
T
V
p
R
T
V
RT pV
0 .
2
5
2
3
) , ( =
|
|
.
|
\
|
c
c
= = + = + =
T
JT B B B
p
H
const T Nk T Nk T Nk pV U p T H
equipartition theorem
for monoatomic gas
ideal gas law
areas of
H = const.
lines of intersection with
H = const.
@ T = const
Chapt. IV - 48
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3
)

real gas: ( ) RT b V
V
a
p
m
m
=
|
|
.
|
\
|
+
2
at low densities: we use approximation and obtain b V
V
a
p >> >> ,
2
( )
p
T
RT pb
V
a
pV ... ,
c
c
= +
2
2
,
V
a
p
R
T
V
R
T
V
V
a
T
V
p
p p p

=
|
.
|
\
|
c
c
=
|
.
|
\
|
c
c
|
.
|
\
|
c
c
|
.
|
\
|
~
|
|
.
|
\
|
= b
RT
a
C p
T
P
H
JT
2
1
A
A
JT
> 0 for T < 2a/bR cooling on expansion
JT
< 0 for T > 2a/bR heating on expansion
inversion temperature:
bR
a
T
inv
2
=
. ) , (
2
5
) , ( const T p U T Nk pV U p T H
B
= A + = + =
|
|
.
|
\
|
|
.
|
\
|
c
c
=
|
|
.
|
\
|
c
c
=
|
|
.
|
\
|
= V
T
V
T
C p
H
C p
T
p p
T
p
H
JT
1 1
A
A
insert into
Chapt. IV - 49
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areas of
H = const.
lines of intersection with
H = const.
inversion curve
Chapt. IV - 50
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3
)

Joule-Thomson coefficient (without approx.):
( )( ) | |
2
2
1 2 1
) 1 )( 2 (
V b VRT a C
b V b RT a
p
JT

=
large volume (p >> a/V
2
, V >> b) :
|
.
|
\
|
~ b
RT
a
C
P
JT
2
1
inversion curve: points where
JT
= 0
vdW gas: (2a/RT)(1-b/V)
2
= b
inversion temperature T
inv
:
2
1
2
|
.
|
\
|
=
V
b
bR
a
T
inv
equation of state gives T
inv
(p,T)
maximum inversion temperature:
bR
a
T
inv
2
=
maximum
inversion
temperature
Chapt. IV - 51
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experimental data for N
2
:
H
JT
p
T
|
|
.
|
\
|
c
c

slope of
isenthalps
repulsion
attraction
Chapt. IV - 52
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gas maximum inversion temperature [K]
Helium-3 (23)
Helium-4 45
Hydrogen 205
Neon 250
Nitrogen 621
Air 603
Carbon monoxide 652
Argon 794
Oxygen 761
Methane 939
Carbon dioxide 1500
Ammonia 1994
vdW gas can be liquefied only for T < T
inv
!!!
Chapt. IV - 53
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closed cycle cooling:
gas is cooled by JT-expansion until liquid drops
out the impedance
Carl von Linde
(1842 1934)
Linde-process
(Source: PTB Braunschweig)
patent application by Carl von Linde on May 12, 1903
(liquefaction of oxygen)
Chapt. IV - 54
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Lindesche
Gasverflssigungsanlage (1895)
Chapt. IV - 55
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Professor Dr. Carl Paul Gottfried von Linde (* 11. Juni 1842 in Berndorf, Oberfranken; 16. November 1934 in Mnchen) war ein deutscher Ingenieur, Erfinder
und Grnder eines heute internationalen Konzerns, der Linde AG.

Linde begann 1861 ein Studium am Polytechnikum Zrich, wo Rudolf Clausius, Gustav Zeuner und Franz Reuleaux seine Lehrer waren. 1864 beendete er sein
Studium. Reuleaux vermittelte ihm eine Lehrstelle in der Baumwollfabrik Kottern in Berlin, die er im selben Jahr antrat. Es war aber nur kurze Zeit, bevor er nach
Mnchen zog, um als Konstrukteur bei der Lokomotivenfabrik Krauss zu arbeiten. 1866 heiratete er Helen Grimm: aus der 53-jhrigen Ehe folgten sechs Kinder.
1868 folgte er einem Ruf der Polytechnischen Schule Mnchen, wo er zunchst - mit erst 26 Jahren - auerordentlicher Professor, 1872 dann ordentlicher
Professor fr Maschinenbau wurde. Am Polytechnikum richtete Linde ein Maschinenlabor ein, an dem unter anderem Rudolf Diesel ausgebildet wurde. 1871
verffentlichte Linde einen Aufsatz ber verbesserte Kltetechnikverfahren. Viele Brauereien interessierten sich dafr, und bald versorgte Linde sie mit den neuen
Maschinen, an denen er stndig arbeitete.

Linde schuf wesentliche Grundlagen der modernen Kltetechnik. 1871 konzipierte er eine mit Methylether arbeitende Kltemaschine, die er in der
Maschinenfabrik Augsburg (heute MAN AG) herstellen lie. Die zweite, 1876 folgende Generation von Khlmaschinen arbeitete mit Ammoniak. Das Prinzip der
Abkhlung von Gas, das vorher mechanische Arbeit geleistet hatte, war beiden gemeinsam. Ein Preisausschreiben fr eine Khlanlage zum Auskristallisieren von
Paraffin war 1873 fr den Hochschullehrer der Anreiz zum Bau einer Khlmaschine, die beim Bierbrauen die Grung bei konstanter Temperatur zulie. Brauereien
in ganz Europa (so Dreher in Triest, die Mainzer Actien-Bierbrauerei, Spaten in Mnchen, Heineken in den Niederlanden, Carlsberg in Dnemark) interessierten
sich prompt fr die neue Kltetechnik.
Am 21. Juni 1879 gab der Erfinder sein Lehramt auf und rief mit zwei Brauern und drei anderen Grndern die "Gesellschaft fr Lindes Eismaschinen AG" ins Leben
(heute Linde AG). Nach relativ kurzer Zeit war das Unternehmen in Europa fhrend auf kltetechnischem Gebiet, auch begnstigt durch einen milden Winter
1883/1884. Es kam deshalb zu einer Knappheit bei Natureis, das zum Khlen des Gerstensaftes in Bierkellern eingesetzt wurde. Bisherige Vorbehalte der Brauer
gegen das Kunsteis schmolzen dahin, Khlmaschinen waren pltzlich gefragt und Linde lieferte umgehend.
Khlhuser fr Lebensmittel und mehrere Eiswerke lie Linde nach und nach sogar selbst bauen. Doch auch auf Eislaufbahnen, in Molkereien und bei der
Verflssigung von Chlor und Kohlensure war sein Verfahren gefragt. Die Firma florierte, 1890 zog sich Linde aus dem operativen Geschft in den Aufsichtsrat
seiner Aktiengesellschaft zurck. In den Jahren 1892 bis 1910 nahm er seine Professur wieder auf.

Auf der Grundlage der Arbeiten von James Prescott Joule, Sir William Thomson (Lord Kelvin of Largs) und der Einfhrung des Gegenstromverfahrens konnte Linde
1895 erstmals grere Mengen Luft verflssigen (Linde-Verfahren). Damit schuf er die Mglichkeiten fr physikalische Tieftemperaturuntersuchungen und zur
Trennung der Luftbestandteile durch fraktionierte Destillation. 1901 folgte die Errichtung einer Anlage zur Gewinnung von Sauerstoff und (ab 1903) Stickstoff.

Linde war Mitglied wissenschaftlicher und Ingenieurvereinigungen, unter anderem gehrte er dem Kuratorium der Physikalisch-Technischen Reichsanstalt und der
Bayerischen Akademie der Wissenschaften an. Er wurde vom bayerischen Knig Ludwig II in den nicht erblichen Adelsstand erhoben. Linde war 1916 der erste
Preistrger des Siemens-Rings.

Ab 1910 zog sich Linde als Direktor seiner inzwischen ungeheuer erfolgreichen Aktiengesellschaft zurck und reichte sie an seinen Shne Friedrich und Richard
weiter. Die Weltwirtschaftskrise von 1929 versetzte der Linde AG einen starken Schlag; das Unternehmen erholte sich aber, und die Gewinne fingen schon wieder
an zu steigen, bevor Linde 1934 im Alter von 92 Jahren starb.
Chapt. IV - 56
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schematics of a Helium liquefier
Chapt. IV - 57
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IV.1.5 Summary
Chapt. IV - 58
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IV.1.5 Summary
Chapt. IV - 59
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specification for cryocooler:
1 Watt of cooling @ 80 K, rejecting heat at 300 K
10 year life
230 K to 340 K survival temperature
survival of launch vibration (non-operating)
low exported vibration
high efficiency
no maintenance possible oil-free
Northrop Grumman's HEC cryocooler
IV.1.5 Summary
Stirling cycle miniature cryocooler:
- lightweight cooler, ideal for cooling of
sensors and other electronics when low
power consumption is important
- mean time before failure of 24,000 hours
- cooling capacity of 1 W @ 80 K
- power consumption of only 55 W.
Sumitomo Heavy Industries
Chapt. IV - 60
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Chapt. IV - 61
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everyday experience: sweating, wind direction, cooling of coffee,
moisten finger, evaporation cooling
microscopically:
evaporation: work required to overcome binding forces
only the fastest molecules will do it
high-energy particles are lost
liquid cools down
Chapt. IV - 62
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limit of evaporation cooling: k
B
T becomes too small compared to AH
vap

(heat of evaporation)

AH
vap
should be small to reach large cooling power at low temperatures
numbers: about 1 K can be reached with
4
He, about 0.3 K with
3
He
boiling point can be calculated by using the Clausius-Clapeyron equation, if
heat of vaporization and the vapor pressure of the liquid at a certain
temperature is known
Chapt. IV - 63
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Clausius-Clapeyron equation:
AH
vap
: molar latent
heat [J/mole]
approximate expression using pV = RT (ideal gas):
integration yields (assuming that AH
vap
is constant over the considered T range):
90 J/mole
for
4
He
normal boiling temperature:
pressure above liquid

boiling temperature at p
0
(boiling point corresponds to
the temperature at which the
vapor pressure of the liquid
equals the surrounding
environmental pressure)
Chapt. IV - 64
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Chapt. IV - 65
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www.mallister.com/graphics/vapor3.jpg
Chapt. IV - 67
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liquid
4
He (c.f. chapter II)

boson
liquid down to 0 K (@ 1 atm)
superfluid
4
Helium at 2.17 K
Bose condensation: macroscopic number
of atoms in ground state
very low viscosity
very high heat conduction
strange thermomechanical effects
creeping on vertical surfaces
vortex core with radius 0.8 @ 0.6K
explained by a two-fluid model
density 125 kg/m
3

Chapt. IV - 68
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Liquid Helium cryostats:

LHe has small latent heat
good thermal insulation by vacuum
LHe container of poor thermal conductivity, glass or
stainless steel
thermal radiation shield at liquid Nitrogen temperature
to reduce black-body radiation
bath cryostat - sample is immersed in the LHe
gas flow cryostat - sample is located in cold He gas
Chapt. IV - 69
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LHe
Liquid Helium container
vacuum
radiation shields
narrow neck to minimize

- heating by radiation
- heating by thermal conduction
typical losses
- 1 l of LHe / day
Chapt. IV - 70
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He-bath cryostat
Chapt. IV - 71
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He-gas flow cryostat
Chapt. IV - 72
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no liquid Nitrogen required
radiation shield cooled by cold helium return gas
He-gas flow cryostat (II)
Chapt. IV - 73
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reducing the vapour pressure over
bath of
4
Helium
temperature down to 1.2 K
at pumping speed of 10 m
3
/h
AH
vap
: molar latent heat [J/mole]
N
A
E
binding
: 90 J/mole for
4
He
Liquid
4
He temperature < 4.2 K
cooling power:
|
.
|
\
|
=
RT
H
p H n Q
vap
vap
gas
A
A exp
rate of atoms going to gas phase

up to 10 mW cooling power @ 1.2K
Chapt. IV - 75
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Liquid
3
Helium (c.f. chapter II):

fermion
superfluid at 2.5mK
formation of weakly bound fermions: Cooper pairs
density 59 kg/m
3
higher vapour pressure than
4
He due to smaller latent heat:
AH
vap
= 40 J/mole cooling power 80mW @ 1.2K and 10 m
3
/h pumping
speed
0.3 K by pumping
3
He vapour
some cm
3
0.1mW cooling power @ 0.3K

3
He obtained by nuclear reactions
extremely expensive
1 liter of
3
He gas costs about US $5.000 (2012)
Chapt. IV - 76
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Liquid
3
He cryostat
4
He
3
He 0.3 K
4
He
pump
3
He
pump
3
He
backflow
4
He impedance 4
He
bath
4.2 K
vacuum
condensation of backflowing
3
He gas
latent heat of
3
He: AH
vap
= 40 J/mole
as compared to 90 J/mole for
4
He
larger cooling power

80mW @ 1.2 K for
3
He as compared to
10mW @ 1.2 K for
4
He
minimum temperature: 300 mK
(cooling power 0.1 mW)
1.2K
flow restriction for condensed
3
He
|
.
|
\
|
=
RT
H
p H n Q
vap
vap
gas
A
A exp
Chapt. IV - 77
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makes use of miscibility gap of
3
He/
4
He mixtures (compare section I.6)
revision of some facts on
3
He/
4
He mixtures
cf. chapter I.6
Chapt. IV - 79
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bonding:

>
1
2

+

complete miscibility (e.g. water and alcohol)

1
2

>

phase separation (e.g. water and petrol)
A A A B B B
V
AA
V
AB
V
BB
critical point
miscibility gap
increasing mixing with increasing T:
F = U TS min
binding
energy
thermal
motion
optimization of binding energy
complete phase separation @ T = 0
minimization of free energy
IV.1.7 Dilution Cooling revision of I.6
Chapt. IV - 80
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binding energy of
3
He in
3
He (V
33
) and
4
He (V
34
):

(i)
3
He in
3
He: binding energy is given by the latent heat of evaporation L
3
:
binding energy for single
3
He atom:
3,
=

3
=

3,
3,
= chemical potential of pure (concentrated)
liquid

(ii) single
3
He atom in liquid
4
He:
binding energy for single
3
He atom:
3,
(
3
0) =

3,

3
0

3,
= chemical potential of dilute phase

3,
0 >
3,
or vice versa ?

3
He has smaller mass larger zero point fluctuations occupies larger volume
binding of
3
He is larger in
4
He than in
3
He due to larger density of
4
He

|
3,
0 | > |
3,
|

corresponds to case
>
1
2

complete miscibility expected,

why miscibility only up to 6.5% ??
Chapt. IV - 81
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Questions:
why cant we dissolve more than 6.5% of
3
He in
4
He at T = 0 ?

two effects:

(i)
3
He forms degenerate Fermi liquid

increases with
3

for
3
> 6.5%, the Fermi energy exceeds the gain in binding energy

(ii)
3,

3
>
3,
(
3
= 0)
effective attraction between two He atoms (magnetic and volume effect)

why dont we have a complete phase separation into
3
He and
4
He at T = 0 ?

results in finite disorder, violation of 3. law of thermodynamic ?
no: we have degenerate Fermi gas, ordering in k-space
Chapt. IV - 82
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x
3
0.065
3,
(0)
3,

0 gaseous He
pure liquid He
He diluted in
4
He
= +
=
for
3
> 6.5%:
>
,
=
= +
=

separation of pure He
energy

Chapt. IV - 83
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for Fermi liquid:
C
concentrated
< C
diluted
(x
3
= 0.065) (

2/3
)

with we therefore obtain:

U
concentrated
(T) < U
diluted
(T)

on transition across phase boundary:
F U = const

increase of U results in decrease
of temperature !

He/
4
He dilution refrigerator
operation principle:
remove He atoms from the dilute phase below T
k
= 0.87 K
transport of He atoms across phase boundary
to maintain equilibrium concentration
corresponds to evaporation of He from concentrated phase
cools as the latent heat of evaporation is removed
concentrated
(lighter)
diluted,6.5%
(heavier)
He
U
T
U
concentrated
U
diluted
He
Chapt. IV - 84
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assumption: one mole of He crosses boundary

removed heat depends on enthalpy difference between concentrated and dilute phase

cooling power

since there is no volume change

with and

we obtain the entropy
(standard expressions for Fermi liquid)
Chapt. IV - 85
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3
He, concentrated
3
He, diluted
Fermi
sphere
large
3
He density
large Fermi sphere
high T
F

small
3
He density
small Fermi sphere
low T
F
fraction of thermally
excited
3
He atoms
increases ( T/T
F
)

entropy increases going
from concentrated to
diluted phase

removed heat: dQ = TdS
thermally
excited
3
He atoms
plausibility consideration
k
B
T
k
B
T
Fermi
sphere
Chapt. IV - 86
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large cooling power requires large throuphput
2
3
84 T n Q

=
> 90%
3
He
3
He
pump
from 1.2 K
3
He condenser
heat exchangers
< 1%
3
He
still
( 0.7 K)
flow impedance
concentrated
phase
dilute
phase
6.5%
3
He
100%
3
He
heater to allow for
effective pumping of
3
He
mixing
chamber
( 0.01 K)
dilute phase
concentrated phase
pumping of
3
He generates
osmotic pressure

3
He flows from mixing chamber
to still
only possible if
3
He atoms cross
phase boundary
cooling
minimum temperature:
1.5 mK
Chapt. IV - 87
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1
3
)

numbers: vapor pressure of
3
He at 0.7 K: 0.0828 mbar = 8.28 Pa
@ 300 K we obtain:

large
3
He pump is required

what is the required pumping speed ??

we assume that
3
He is an ideal gas (R = 8.31 J / mole K)

example: desired cooling power: 10
-5
W
still temperature: 0.7 K
mixing chamber temperature: 10 mK
s / mole 0012 . 0
) 10 ( 84
10
2 2
5
3
= =

p RT n V /
3
=
l /s 360 s / m 0.363 28 . 8 / 300 31 . 8 0012 . 0
3
~ = = V
2
3
84 T n Q

=
= 8.31 J/mole K
Chapt. IV - 88
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mixing
chamber
heat
exchangers
still
Chapt. IV - 89
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JANIS Model JDR-500 Dilution Refrigerator
Chapt. IV - 90
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3
He shows minimum in melting
curve at T = 0.32 K (compare I.5.2)

can be used for cooling of He
Pomeranchuk effect
Isaak Jakowlewitsch Pomeranschuk
( ;
born: 20. Mai 1913 at Warschau;
died: 14. Juli 1966 at Moscow)
Russian physicist.
0.1 1 10
10
1
10
2
10
3
10
4

p

(
b
a
r
)
T (K)
phase diagram of
4
He and
3
He
3
He
4
He
hcp
bcc
liquid
hcp
liquid
bcc
fcc
Chapt. IV - 91
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|
|
.
|
\
|
~ =
F
liquid solid
T
T
TR S S T n Q
2
- l n2 ) - (
2
3
t
explanation:
solid phase: atoms are ordered,
spins are disordered and determine entropy: S
solid
= R ln2
at low T: antiparallel ordering of spins, S decreases towards zero

liquid phase: atoms are spatially disordered, but ordering in k-space (Fermi liquid)
entropy of Fermi liquid:

always: V
sol
< V
liq

for T < 0.32 K:
disorder larger in
solid than in liquid
phase !!
S

lnT

R ln2

0
liquid
solid
320 mK
cooling power:
Chapt. IV - 92
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1
3
)

stamp
stainless steel
bellow
liquid
solid pressure cell
precooling to T < T
min

adiabatic compression
solidification and cooling

lowest T: 1.5 mK
limitation due to antiparallel
spin ordering in solid
3
He
10
-3
10
-2
10
-1
10
0
2.8
2.9
3.0
3.1
3.2
3.3
3.4

p

(
M
P
a
)
10
-3
10
-2
10
-1
10
0
0.0
0.2
0.4
0.6
0.8

S

/

R
T (K)
liquid
solid
liquid
solid
T
min
ln 2
Chapt. IV - 93
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IV.1.9 Adiabatic demagnetization
magnetic refrigeration: based on the magnetocaloric effect
magnetocaloric effect:

- magneto-thermodynamic phenomenon

- reversible change in temperature is
caused by exposing a material to a
changing magnetic field

- also known as
adiabatic demagnetization
Chapt. IV - 94
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)

Adiabatic magnetization:
- substance is placed in an insulated environment
- increasing external magnetic field (+H) causes magnetic
ordering reduction of magnetic entropy and heat capacity
- overall energy is not lost and therefore total entropy is not
reduced (T + T
ad
).

Isomagnetic enthalpic transfer:
- added heat is removed by coupling to heat sink (-Q)
- magnetic field is held constant
- after heat removal, magnetocaloric material and the coolant
are separated (H = 0).

Adiabatic demagnetization:
- the substance is decoupled from heat sink no heat
exchange with environment entropy stays constant
- magnetic field is decreased, the thermal energy causes the
magnetic moments to overcome the field, and thus the sample
cools energy (and entropy) transfers from thermal entropy
to magnetic entropy (disorder of the magnetic dipoles).

Isomagnetic entropic transfer:
- the magnetic field is held constant to prevent the material
from heating up
- the material is brought in thermal contact with the
environment being refrigerated cooling effect
- magnetic materials heats up (+Q)
thermodynamic cycle:
Chapt. IV - 95
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adiabatic

experiment:
use of copper: B
i
= 3 T, B
f
= 0.3 mT, T
i
= 10 mK T
f
1K
generation of temperatures below 1 mK
dQ = TdS = dU dW = dU + pdV B dM dU B dM (for solid: pdV small)
adiabatic cooling: dQ = 0 dU = B dM
step1: magnetize sample with field B, work must be done on sample and
heat is released to thermal bath at T
i
step2: thermally isolated sample and remove magnetic field B, sample
uses internal energy to demagnetize and temperature falls to T
f
< T
i

Chapt. IV - 96
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)

more detailed discussion:

which amount of heat AQ
spin
can be absorbed by the spin systems ?
} } |
|
.
|
\
|
c
c
= = = A
i
f
i
f
T
T
B
spin
T
T
spin spin
dT
T
S
T dT C B Q ) 0 (
)
`
+ +
+ =
2
2
int
2
2
2 2

6
) 1 (
) 1 2 ln(
T
B B
k
J J g
J Nk S
B
B
B
|
|
.
|
\
|
+
+
=
2
int
2
2
int
2
B B
B B
T T
i
f
i f
remaining internal field due to finite magnetic interactions
(should be as small as possible)
(cooling capacity)

entropy of spin system with spin quantum number J for g
B
B << k
B
T:

final temperature
Chapt. IV - 97
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T
i
T
f
B
f
= 0 B
i
= 5T
e
n
t
r
o
p
y

S

1
2
1 switch on magnetic field at constant T
i
(coupling to heat sink)
2 switch off magnetic field for thermally isolated sample cooling to T
f
} } |
|
.
|
\
|
c
c
= = = A
i
f
i
f
T
T
B
spin
T
T
spin spin
dT
T
S
T dT C B Q ) 0 (
) 1 2 ln( + J Nk
B
0
0
medium
heat sink
heat
switch
T

Chapt. IV - 98
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paramagnetic salts:
e.g MAS = MnSO
4
(NH
4
)
2
SO
4
6H
2
O
cooling of electron spins
material with large entropy S/R but large B
int

lowest temperatures T
f
100 mK
large cooling capacity

e.g CMN = 2Ce(NO
3
)
3
2Mg(NO
3
)
2
24H
2
O
cooling of electron spins
material with small entropy S/R but small B
int

lowest temperatures T
f
2 mK
small cooling capacity

nuclear demagnetization:
e.g
63
Cu (L = 3/2) or
65
Cu (L = 3/2) (B
int
0.3 mT, T
i
10 mK, B
i
3 T)
cooling of nuclear spins
T
f
(B
f
= 0) 1 K
problem: transfer of spin temperature to lattice
long spin-lattice relaxation time

other materials:
141
PrNi
5
(L=5/2),
195
Pt (L=1/2)
Chapt. IV - 99
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1
3
)

spin-lattice coupling cools the lattice

metals: 1000 s (hyperfine interaction: t = C
Korringa
/T
e
, Korringa relation)

non-metals: hours to several days

spin-lattice coupling: spin temperature increases and lattice temperature decreases

in thermal equilibrium

calculation of equilibrium temperature for copper:
(B
int
0.3 mT, T
i
10 mK, B
i
3 T)

T
eq
= 1.03 K

lowest reported experimental temperature

demagnetization of Pt: T
eq
= 2 K (F. Pobell et al., (1996))

0 = +
} }
n
T
T
nuclear e
T
T
electron
dT c dT c
eq
f
eq
i
Chapt. IV - 100
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R. Gloss et al.,
J . Low Temp. Phys. 73, 101 (1988)
Cu demagnetization stage
(length: 525 mm, diameter: 78 mm)
Chapt. IV - 101
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1
3
)

K facility of PTB Berlin:

Lattice temperatures measured on the
105-mol-copper stage of the Berlin
microkelvin facility with Pt-NMR. The
achieved minimal temperature was
23.3 K. The red line depicts the
calculated course of temperature for
the thermodynamically optimized
demagnetization function.

heat leak: below 1.5 nW.

Chapt. IV - 102
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Cryogen-free Two Stage Adiabatic
Demagnetization Refrigerator from Janis
A cryogen-free two stage adiabatic demagnetization refrigerator using a 4 K pulse tube cryocooler.
Gallium Gadolinium Garnet (GGG) and Ferric Ammonium Alum (FAA) paramagnetic pills were used
for the first and second stage of the ADR, with Kevlar string supports for each stage. The FAA stage
reaches a base temperature below 50 mK, and remains below 100 mK for more than two days.
Chapt. IV - 104
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Continuous Adiabatic Demagnetization
Refrigerator (CADR) under development at
NASAs Goddard Space Flight Center

- CADR to cool from below 5K to 35 mK
- advantage: no stored cryogens
maximizing the lifetime/mass
ratio for the instrument
Chapt. IV - 105
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Contents:

IV.1.1 Introduction
IV.1.5 Summary

IV.2 Thermometry
IV.2.1 Introduction

Chapt. IV - 106
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IV.2 Thermometry
IV.2.1 Introduction
temperature and temperature scales
temperature of a system in thermodynamic equilibrium:
defined as the relation between the amount of heat Q incident on the system during
an infinitesimal quasi-static transformation, and the variation S of its entropy during
this transformation:

for reversible Carnot process (dS = 0):
S
Q
T
o
o
=
}
o
=
T
Q
0
Kelvin scale
Celsius scale (1742)
see http://www.its-90.com

Lord Kelvin (1854): there is an absolute zero of temperature scale

T
0
= 0 K = - 273.15C 1 K = 1C
Chapt. IV - 107
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William Thomson (Lord Kelvin)
http://br.geocities.com/saladefisica3/fotos/kelvin.gif
Lord Kelvin by Hubert von Herkomer

Born
26 June 1824(1824-06-26)
Belfast, Co. Antrim, Ireland
Died
17 December 1907 (aged 83)
[1]

Largs, Ayrshire, Scotland
[1]

Residence
Cambridge, England
Glasgow, Scotland
Nationality
United Kingdom of Great Britain
and Ireland
Institutions University of Glasgow
Alma mater
Glasgow University
Peterhouse, Cambridge
A variety of physical phenomena and concepts with
which Thomson is associated are named Kelvin:
Kelvin material
Kelvin water dropper
Kelvin wave
Kelvin-Helmholtz instability
Kelvin-Helmholtz mechanism
Kelvin-Helmholtz luminosity
The SI unit of temperature, kelvin
Kelvin transform in potential theory
Kelvin's circulation theorem
Kelvin-bridge (also known as Thomson-bridge)
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 108
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SI temperature scale
- the SI temperature scale is the Kelvin scale. It defines the triple point of water as the
numerical value of 273.16, i.e., 273.16 K. The unit of temperature in this scale is the
Kelvin (K).
Celsius scale:
the Celsius scale has units of C (degrees Celsius) with the size of the unit equal to
1 Kelvin.
T(C) = T(K) 273.15
agreement of bureaus of standards:

ITS-90 temperature scale for T > 0.65 K
(Comit International des Poids et Messures 1990)
- the ITS-90 is defined by 17 fixed points and 4 defining instruments. It spans a
temperature range from 0.65 K to 10 000 K. For cryogenic purposes the three defining
instruments are helium vapor pressure thermometry, gas thermometry, and platinum
resistance thermometry.

PLTS-2000 for lower T
(Provisonal Low Temperature Scale, melting curve of
3
He )
- the PLTS-2000 is defined by a polynomial, relating the melting pressure of
3
He to
temperature from the range 0.9 mK to 1 K. The pressure to temperature relationship
is based on primary thermometers such as Johnson noise and nuclear orientation.
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 109
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The Water Triple Point

The triple point of water is the most important defining
thermometric fixed point used in the calibration of
thermometers to the International Temperature Scale of
1990 (ITS-90).
It is the sole realizable defining fixed point common to
the Kelvin Thermodynamic Temperature Scale (KTTS)
and the ITS-90; the assigned value on these scales is
273.16 K (0.01C)
solid
liquid
gaseous
critical
point
triple
point
(0.01C, 603 Pa)
273.15 K
(374C, 21800 kPa)
273.16 K
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 110
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Defining Fixed Points of the ITS-90
Number Temperature Substance
a
State
b
Wr (T
90
)
T
90
/K t
90
/C
1 3 to 5 -270.15 to -268.15 He V
2 13.8033 -259.3467 e-H
2
T 0.001 190 07
3 ~17 ~-256.15 e-H
2
(or He) V (or G)
4 ~20.3 -252.85 e-H
2
(or He) V (or G)
5 24.5561 -248.5939 Ne T 0.008 449 74
6 54.3584 -218.7916 O
2
T 0.091 718 04
7 83.8058 -189.3442 Ar T 0.215 859 75
8 234.3156 -38.8344 Hg T 0.844 142 11
9 273.16 0.01 H
2
0 T 1.000 000 00
10 302.9146 29.7646 Ga M 1.118 138 89
11 429.7485 156.5985 In F 1.609 801 85
12 505.078 231.928 Sn F 1.892 797 68
13 692.677 419.527 Zn F 2.568 917 30
14 933.473 660.323 Al F 3.376 008 60
15 1234.93 961.78 Ag F 4.286 420 53
16 1337.33 1064.18 Au F
17 1357.77 1084.62 Cu F
a
All substances except
3
He are of natural isotopic composition, e-H
2
is hydrogen at the equilibrium concentration of the ortho- and para-molecular forms.
b
V: vapour pressure point; T: Triple Point (temperature at which the solid, liquid and vapour phases are in equilibrium); G: gas thermometer point; M,F melting point, freezing point
(temperature, at a pressure of 101 325 Pa, at which the solid and liquid phases are in equilibrium)
see http://www.its-90.com
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 111
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temperature measurement
definition of temperature via reversible Carnot process is not well suited for
establishing useful measuring methods

in practice: use of fixpoints and interpolation polynoms
primary thermometers:
measured quantity is related directly to temperature
(in a theoretically predictably way)
no calibration is required
secondary thermometers:
measured quantity varies with temperature in a reproducible way
must be calibrated using a primary thermometer
requirements for temperature measurement:
good thermal contact between thermometer and sample
low self-heating
fast response to temperature changes
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 112
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T(K)
typical temperature range of some thermometers
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 113
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most common thermometers for 1K < T < 300K

gas thermometer: p = p(T)
Helium gas ideal gas down to 10K:

vapour pressure thermometer: T
liquid
= f(p
vapor
)
pressure of 10 Pa corresponds to 0.4K for
3
He

thermocouples: V
th
= V
th
(T)

resistance thermometry: R = R(T)
1K - 300K
semiconductors (e.g. Ge doped with Arsenic has 100-500 /K @ 4.2K,
self-heating around 10A)
p-n junction diode (problem with high bias current self heating)

capacitance thermometry: C = C(T)
based on temperature change of dielectric properties
virtually no magnetic field-induced errors

noise thermometer: S = S(T)
Johnson noise in resistor: S
V
= 4k
B
TR
like gas thermometer, but with electrons
with SQUID measurements: 0.1% @ 1K
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 114
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1mK T 1K:

magnetic suceptibility thermometer
T
C
B
M
= =
0
_ Curies law:
Cerium magnesium nitrate (CMN) useful from 1K - 10mK
low temperature limit set by magnetic ordering at 1mK
_
0
f m m=
mutual inductance between two coils:
most common thermometers for T < 1K
T < 1mK:

Nuclear Magnetic Resonance (NMR) thermometer

temperature dependence of spin relaxation
platinum ideal choice for NMR thermometry
M: magnetization
B: applied magnetic field
C: Curie constant
resistance thermometers
IV.2 Thermometry
IV.2.1 Introduction
Chapt. IV - 115
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Contents:

IV.1.1 Introduction
IV.1.5 Summary

IV.2 Thermometry
IV.2.1 Introduction

Chapt. IV - 116
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IV.2 Thermometry
gas thermometers
ideal gas would be a perfect thermometer:
nRT pV =
measure pressure at constant volume
{ } + + + + =
3 2
) ( ) ( ) ( T T d T T c p T b RT n pV
virial coefficients (tabulated ITS-90 values)
systematic errors:
dead volumes
thermal expansion of cell, elastic deformation of cell
adsorption and desorption from walls

mainly used in calibration laboratories !
for real gases life is more complicated deviations from ideal behavior
Chapt. IV - 117
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in practice, a set of secondary vapour pressure scales is used:

ITS-90:

with
3
He and
4
He: ITS defined down to 0.65 K
vapour pressure thermometry

for ideal gas (pV = RT):

if AH
vap
(T) is known determine T of liquid (e.g. He) via measurement of He pressure
above liquid
T V
T H
T V V
T L
dT
dp
gas
vap
liquid gas
) (
) (
) ( A
~
=
}
= + dT
T
T H
const p R
vap
2
) (
. l n
A
i
i
i
C
B p
A T
)
`
+
=
) (ln
(in principle no primary
thermometer !!)
limited
T range
IV.2 Thermometry
Chapt. IV - 118
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values of the constants for the helium vapour-pressure, and the temperature range for which each equation,
identified by its set of constants, is valid (see http://www.its-90.com).

3
He
0.65K to 3.2K
4
He
1.25K to 2.1768K
4
He
2.1768K to 5.0K
A
0
1.053 447 1.392 408 3.146 631
A
1
0.980 106 0.527 153 1.357 655
A
2
0.676 380 0.166 756 0.413 923
A
3
0.372 692 0.050 988 0.091 159
A
4
0.151 656 0.026 514 0.016 349
A
5
-0.002 263 0.001 975 0.001 826
A
6
0.006 596 -0.017 976 -0.004 325
A
7
0.088 966 0.005 409 -0.004 973
A
8
-0.004 770 0.013 259 0
A
9
-0.054 943 0 0
B 7.3 5.6 10.3
C 4.3 2.9 1.9
IV.2 Thermometry
Chapt. IV - 119
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4
He
3
He
4
He
IV.2 Thermometry
Chapt. IV - 120
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www.mallister.com/graphics/vapor3.jpg
IV.2 Thermometry
Chapt. IV - 121
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www.bm-industries.com
IV.2 Thermometry
Chapt. IV - 122
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3
He melting curve thermometry
use of melting curve of
3
He to define PLTS-2000 temperature scale down to 0.9 mK

polynom for melting curve:

coefficients given by PLTS-2000
also use of 4 fix points (minimum of melting curve, transition temperatures
to A and B phase and afm order of nuclear spins in solid
3
He)
=
=
9
3 i
i
i
T p o
IV.2 Thermometry
Chapt. IV - 123
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3
He melting curve thermometry
melting curve of
3
He
Source:
R.L. Rusby et al. (2001)
IV.2 Thermometry
Chapt. IV - 124
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noise thermometry
Nyquist theorem:

valid only in the low frequency limit f << k
B
T / h ( 20 GHz @ 1K)

temperature determined by measurement of S
V
and R
TR k S
B V
4 =
voltage noise
power spectral density
(V/Hz)
resistance
temperature

example: R = 10 kO, T = 1K, band width Af = 10
5
Hz

(S
V
Af)
1/2
210
-7
V sensitive amplifier required SQUID preamplifier

P 10
-18
W
IV.2 Thermometry
Chapt. IV - 125
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superconducting fix point thermometers
based on the precise measurement of the transition temperatures of superconductors

available from NIST at Boulder
ITS-90
NIST fixpoint device
IV.2 Thermometry
Chapt. IV - 126
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Contents:

IV.1.1 Introduction
IV.1.5 Summary

IV.2 Thermometry
IV.2.1 Introduction

Chapt. IV - 127
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IV.2 Thermometry
Chapt. IV - 128
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resistance thermometers
required: well established relation between resistance and temperature,
sufficiently large dR/dT

advantage: resistance easy to measure resistance thermometry very popular

fact: temperature variation of resistance may have very different physical origin

commonly used:

Pt resistors (PT-100, PT-1000)
RhFe resistors
carbon resistors (Speer, Allen-Bradley)
carbon glass resistors
Ge resistors
RuO
2
resistors
IV.2 Thermometry
Chapt. IV - 129
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Platinum resistors
Source: Lake Shore Cryotronics, Inc.
The platinum resistance thermometer (PRT) is very widely used below 500 C as a thermometric sensor. There is a wide
range of quality of PRT available, from the standard instrument (SPRT) of the ITS-90 to some industrial types (IPRT) that
are accurate only to within a few tenths of a kelvin or, perhaps, even a kelvin or more. The major difference of the
industrial type of fabrication from the standard type is not just the purity of platinum, but also the less strain-free
mounting of the film or wire which is embedded (partially or totally) in a cement (glass or refractory). Furthermore, in
most cases, the thermometer body is not hermetically sealed.
IV.2 Thermometry
Chapt. IV - 130
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W(29.7646 C) 1.118 07
W(-38.8344 C) 0.844 235
Platinum resistors
ITS-90 requirement for Pt resistance thermometer (PRT)
W(T
90
) = R(T
90
)/R(0.01 C)
industrial PRT
IV.2 Thermometry
for 0 < T < 100C
R = R
0
(1 + a T)
a = 3.85 10
-3
/ K

allowed errors in C:
classA: dT = (0.15 C + 0,002 T)
class B: dT = (0.30 C + 0,005 T)
1/3 class B: dT = 1/3 (0.30 C + 0.005 T)
temperatures are determined in terms of the ratio of the resistance R (T
90
) at a
temperature T
90
and the resistance R(273.16 K) at the triple point of water:
Chapt. IV - 131
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for the range 13.8033 K to 273.16 K the following reference function is defined:
IV.2 Thermometry
Chapt. IV - 132
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Rhodium with
0.5% Fe
RhFe resistor thermometer
IV.2 Thermometry
Chapt. IV - 133
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commercial carbon-composition resistors manufactured by Allen-Bradley were introduced as
temperature sensors by Clement and Quinnell in 1952. The carbon composition resistor is a small
cylinder consisting of graphite with a binder encased in an outer phenolic shell.

The carbon resistors used as thermometers are generally characterized by their room temperature
resistance and their wattage [see Rubin (1980)], and have come largely from the following
manufacturers:

Allen-Bradley
Airco Speer (usually referred to simply as Speer)
Ohmite
Matsushita,
CryoCal
carbon resistors
A: thermistor,
B: 68 Allen-Bradley,
C: 220 Speer (grade 1002),
D: 51 Speer (grade 1002),
E: 10 Speer (grade 1002)
IV.2 Thermometry
Chapt. IV - 134
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carbon glass resistors
A porous glass is prepared by removing the boron-rich phase from a borosilicate
alkaline glass to leave a material having the appearance of silicate spheres of about 30
nm diameter, randomly distributed and separated by 3 to 4 nm pores. The spaces are
then partially filled with high-purity carbon to form amorphous fibres better
stability than carbon resistors.
IV.2 Thermometry
Chapt. IV - 135
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Cernox resistors
Patents:
#5,363,084, Nov. 1994, Film Resistors Having Trimmable Electrodes

#5,367,285, Nov. 1994, Cernox, Metal Oxy-nitride Resistance Films and
Methods of Making the Same,

small magnetic field coefficient: AT/T typically smaller than 0.5% @ 19 T
IV.2 Thermometry
Chapt. IV - 136
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Cernox resistors
IV.2 Thermometry
Low temperature thermometry in high magnetic fields VII. Cernox sensors to 32 T, B.L. Brandt et al,
Rev. Sci. Instrum., vol 70, No 1, 1999, pp 104-110.
Chapt. IV - 137
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Germanium resistors
IV.2 Thermometry
Chapt. IV - 138
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Germanium resistors
IV.2 Thermometry
Chapt. IV - 139
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Thermocouples
based on Seebeck effect:

measurement of difference of thermovoltages of two different materials
T S V A = A S = thermopower
AV
B
AV
A
Cu
Cu
T
1
T
2
well-known reference temperature
Thermocouples are pairs of dissimilar metal wires joined at least at one end, which
generate a net thermoelectric voltage between the the open pair according to the size of
the temperature difference between the ends, the relative Seebeck coefficient of the wire
pair and the uniformity of the wire-pair relative Seebeck coefficient.
IV.2 Thermometry
Chapt. IV - 140
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Thermocouples
Chromel-Gold/Iron (0.07%)
consists of a Gold (Au)-0.07 at % Iron (Fe) as the negative thermoelement and a
Ni-Cr alloy (Chromel) as the positive thermoelement. This thermocouple is more
widely used because of ist relatively high thermoelectric sensitivity (>15 V/K
above 10 K).

Type E (Chromel (Ni-Cr-alloy) / Constantan (Cu-Ni-alloy) )
has the highest sensitivity among the three standard thermocouple types
typically used at low temperatures (types E, K, and T). The best choice
for temperatures down to 40 K.

Type K (Chromel (Ni-Cr-alloy) / Alumel (Ni-Al-alloy) )
recommended for continuous use in inert atmospheres. Has a sensitivity
of 4.1 mV/K at 20 K (about of Type E).

Type T (Copper / Constantan)

many more !!
IV.2 Thermometry
Chapt. IV - 141
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Thermocouple Type Names of Materials Useful Application Range
B
Platinum30% Rhodium (+)
Platinum 6% Rhodium (-)
2500 -3100F
1370-1700C
C
W5Re Tungsten 5% Rhenium (+)
W26Re Tungsten 26% Rhenium (-)
3000-4200F
1650-2315C
E
Chromel (+)
Constantan (-)
200-1650F
95-900C
J
Iron (+)
Constantan (-)
200-1400F
95-760C
K
Chromel (+)
Alumel (-)
200-2300F
95-1260C
N
Nicrosil (+)
Nisil (-)
1200-2300F
650-1260C
R
Platinum 13% Rhodium (+)
Platinum (-)
1600-2640F
870-1450C
S
Platinum 10% Rhodium (+)
Platinum (-)
1800-2640F
980-1450C
T
Copper (+)
Constantan (-)
-330-660F
-200-350C
Thermocouples
IV.2 Thermometry
Chapt. IV - 142
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Thermocouples
IV.2 Thermometry
Chapt. IV - 143
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Diode Thermometers
The temperature-indicating parameter is the forward-biased junction voltage,
which decreases approximately linearly with increasing temperature when
the current is kept constant, since I exp(eV /k
B
T)
The typical I-V characteristic is such as to make the internal impedance
of the device very high (easily greater than 100 k) at small currents; or else - using a larger current -
one encounters unacceptably high power dissipation at low temperatures.
There is a transition region in the conduction mechanism around 20 K that makes fitting a V-T
characteristic over the whole temperature range difficult for GaAs and impossible for Si

Si Si
IV.2 Thermometry
Chapt. IV - 144
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Capacitive Thermometers
based on the well defined relation between the dielectric constant and temperature

temperature is determined via a capacitance measurement

advantage: virtually no magnetic field dependence
IV.2 Thermometry
Chapt. IV - 145
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Capacitive Thermometers
IV.2 Thermometry
Chapt. IV - 146
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magnetic field effects
IV.2 Thermometry
Chapt. IV - 147
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magnetic field effects
IV.2 Thermometry
Chapt. IV - 148
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IV.2 Thermometry
Chapt. IV - 149
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IV.2 Thermometry
Chapt. IV - 150
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Magnetic Susceptibility Thermometers
C T T
C
= _ Curie-Weiss law:

measure _ as a function of T, calibaration requires determination of C and T
C
experimental techniques:

inductance bridge: compare inductance of coil containing the magnetic
material to empty reference coil
resolution:
AT/T 10
-10
@ 1K
increases 1/T
T.C.P. Chui et al., Phys. Rev. Lett. 69, 3005 (1992)
I
c
I
c

u
first order
gradiometer
L
i

L
p

L
M
i
V
out

sample
reference coil
B
ext
I
SQUID magnetometer:
IV.2 Thermometry
Chapt. IV - 151
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materials (use of electronic magnetic susceptibility):

paramagnetic salts: e.g. Ce-Mg-nitrate (CMN)
++ very low ordering temperature: T
C
~ 2 mK
++ large Curie constant
- - long time constant at low T (~ 100 s)
- - cannot be used in vacuum (instable)

nonmagnetic metals: e.g. PdFe or AuEr
M. Jutzler, B. Schrder, K. Gloos, F. Pobell,
Z. Phys. B64, 115 (1986)
- usable down to about 0.3 mK
- response time: 1 s @ 10 mK
IV.2 Thermometry
Chapt. IV - 152
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materials (use of nuclear susceptibility):

use of nonmagnetic metals: e.g. Cu
- - nuclear moments much smaller sensitive SQUID magnetometer
- - perturbing magnetic impurities very pure materials
(e.g. 1 ppm Fe in Cu gives similar signal as all Cu nuclear spins)
++ can be used below 1 mK
IV.2 Thermometry
Chapt. IV - 153
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Nuclear Magnetic Resonance Thermometers
are not based on static orientation of nuclear moments as in susceptibility
thermometers

have selectivity to specific nuclear moments (less sensitive to magnetic impurities)

usable at temperatures below 1 mK

materials: predominantly
195
Pt

experimental techniques: stationary and pulsed NMR
measures resonance absorption
of high frequency signal
allows to determine induced
M
y
M
0
(T) 1/T
N
at resonance
requires small B
y
1T to avoid
saturation effects
B
z
B
y
cos et
measures decay of induced
M
y
(t) after 90 pulse
amplitude dM
y
(t = 0) or integral of
decay curve M
0
(T) 1/T
N

general problem: one measures temperature T
N
of nuclear spins
are they in thermal equilibrium with lattice ??
IV.2 Thermometry
Chapt. IV - 154
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Nuclear Magnetic Resonance Thermometers
comparison of the Curie and Korringa
temperatures of a Pt sample:

the inverse nuclear susceptibility 1/_
N

(arb. units) is plotted against the
electron temperature
T
e
= (1/t
1
) 29.9 x 10
-3
K sec.
A.I. Ahonen et al.,
J. Low Temp. Phys. 25, 421 (1976)
IV.2 Thermometry

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Chapter IV

molecule is slower, i.e. colder

(= 5/3 for He)

> 0: cooling on expansion

< 0: heating on expansion

rate of atoms going to gas phase

complete miscibility expected,

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