Calibration for ultra high

vacuum
(Establishing a primary standard
for the range down to 10-10 Pa)

Ladislav Peksa
Common Metrological Vacuum Laboratory
Faculty Math&Phys Charles University in Prague
and Czech Metrological Institute
Czech Republic
ladislav.peksa@mff.cuni.cz
ORIFICE FLOW STANDARD
 VACUUM
Low vacuum
E 5 > p ≥ E 2 Pa
(rough vacuum)
Medium vacuum
E 2 > p ≥ E -1 Pa
(fine vacuum)

High vacuum (HV) E -1 > p ≥ E -6 Pa

Very (ultra-) high

E -6 > p ≥ E -10 Pa
vacuum (UHV)
Extremely high
E -10 > p Pa
vacuum (XHV)
This way in Europe; the borderline between HV and UHV is E-7 in the USA.
 The primary standard is (according the definition) a standard that is
having the highest metrological qualities and whose value is accepted
without reference to other standards of the same quantity.

Principle of the vacuum primary standard

Vacuum ↔ gas pressure

Standards of gas pressure can be generally classified into two groups:

A. Measuring instruments whose scales can be established only based on

measurement of basic quantities, i.e. length, mass, time, temperature
and so on.

B. Apparatuses in which can be by means of thermodynamic processes

adjusted such conditions that the (?)pressure(?) can be theoretically
determined (computed).
Word or two about the first group:
Conclusion concerning the standards from the first group:
Gauges based on transfer of momentum can hardly achieve the lower range limit 10-9 Pa
or 10-10 Pa in near future. Some of them are very precise instruments after calibration (for
example the SRG) but none of them became ever a primary standard, because better
metrological qualities can be achieved with the apparatuses from the second group.
Published results obtained with the apparatuses using optical methods are as far as
metrological qualities even worse.

Main problem of the second group concerning very low pressures:

Main problem of the secong group is that apart from the desirable controlled processes
with the gas admitted on purpose undesirable spontaneous processes occur with gas
appearing in the apparatus unwillingly. In order to obtain a standard of high
metrological quality the amount of undesirable gas has to be negligible in comparison
with the amount of the working gas.

To meet this condition is the more difficult the lower pressure are of interest because less
and less amount of gas is used. Idea enabling to design primary standards for
pressures from the ranges of high and ultrahigh vacuum is to exchange the working
gas during the process of calibration, to admit new pure working gas and
simultaneously to pump it out together with the undesired gas. This way the ratio of
the desired and undesired gas amounts is much better, influence of the undesired gas
can be neglected.
Gas must not be pumped out from the calibration chamber during the
calibration! (?)
Gas pressure as a physical quantity which can be expressed in one
instant as one reading (the same for any point of the vessel) is defined
only for gas in equilibrium state with Maxwellian velocity distribution.

The apparatuses used as vacuum primary standard can be classified into

3 groups:

1. With zero pumping speed and thus with entirely undisturbed in the
calibration chamber;
2. With so small pumping speed that the disturbance of Maxwellian
distribution is negligible;
3. With so high pumping speed in the calibration chamber that the
Maxwellian distribution there is significantly disturbed.
 Static expansion system

Probably the lowest lower pressure range limit ever reported:

5E-7 Pa (NPL GB)
(in Jousten et al.: Comparison of the standards for HV and UHV at three national standard laboratories. J. Vac. Sci.
Technol. A 15(4), 1997, 2395)
Usually much higher.
Orifice (continuous) flow standard

Q
p
S EFF

(
Molecular beam/enclose gauge principle is
comparable with the OFS.
Grosse G Messer G. Calibration of vacuum gauges at
pressures below 10-9 mbar with a molecular beam mehtod.
Vakumm Technik 1981; 30: 226-331
)
 Pressure ratio technique
(pressure division, dynamic reduction)
 Question:
Can be a primary UHV standard down to 10-10 Pa based on the orifice
flow principle (at present state of vacuum science and technology)?

To achieve 10 % uncertainty at adjusting p = 10-10 Pa the pressure of the residual

gas (mainly hydrogen) has to be less than 10-11 Pa. The basic equation
Q
p
S EFF
is valid also for the residual gas. Q is the gas released from the surfaces:

Q q SURFACE
q is the outgassing rate. SEFF is surely higher than single conductance C of the
opening in the calibration chamber, most advantageous shape with smallest possible
surface is a sphere, thus
11 q SURFACE
1 10 Pa p
438 SURFACE / 1000
Material with achievable outgassing rate in the order of magnitude
10-12 Pa·m/s - 10-13 Pa·m/s has to be used.
BRIEF EXCURSION INTO MATERIALS FOR VACUUM CHAMBER DESIGN

1.7×10-9 Pa m/s [Calder&Lewin]

2 ×10-10 Pa m/s [VAT]
VACUUM COMPONENTS MADE FROM BeCu ALLOY
TITANIUM SUBLIMATION PUMP - TSP
NONEVAPORABLE GETTERS - NEG
SPUTTER ION - NEG
TURBOMOLECULAR PUMP
DIFFUSION PUMP (VACUUM JET PUMP, VAPOR-JET PUMP
Fluctuations of pressure in UHV systems pumped with
diffusion pumps
 CRYOPUMP

REFRIGERATOR-COOLED

BOILING POOL-CRYOPUMP
(BATH)
BAKE-ABLE REFRIGERATOR CRYOPUMP
LEYBOLD 2007
Special solution suitable to reach XHV:
cryopump with additional LN2-cooling
during baking allows baking of chamber
and pump housing to >180 C
during bakeout
Pult1 x 10-9... 1 x 10-10 mbar
􀂄after bakeout
Pult< 1 x 10-12 mbar
Cryopump is used during bakeout
much more effective to pump water
vapour

Disassembling the refrigerator before baking

+ BAKE-ABLE ANTIREFLEXIVE LAYER !

Hydrogen must be pumped in the regime of cryosorption
SUFFICIENTLY LARGE CRYOSURFACE (4.8 K)
 CRYOPUMP PRESSURIZED
5E-8
Pressure [Pa]

4E-8

3E-8

2E-8

1E-8

434000 435000 436000

Time [s]
Helmer gauge = deflector 90°
Deflector 180° / ion spectroscopy gauge -
Watanabe
Bent-beam = Deflector 256,4°
Extractor gauge
Axial tranmission – Bessel Box
Hot-cathode magnetron gauge
POSSIBLE TRANSFER STANDARD - BBB Gauge (F. WATANABE)
Conclusion:
To establish a vacuum primary standard for the
UHV range down to 10-10 Pa is at present state of
vacuum science and technology possible,
nevertheless it is always difficult, not routine task.

Thank you for your attention.