Vacuum Metrology for Science and Industry

Karl Jousten, PTB, Berlin

1. Applications of vacuum and leak detection

2. Traceability and primary standards for vacuum and
low flow rates (leaks)
3. Secondary and reference standards
4. New developments and future challenges

VS4, Coventry, UK, October 2013, Karl Jousten 1

 Applications of vacuum and leak detection

Nobel Prize 2013: Peter Higgs and Francoise Englert

Francois Englert (left) and Peter Higgs on July 4, Break-up of a Higgs Boson, CMS detector,
2012 at CERN LHC, CERN
Image: Maximilien Brice/CERN Image: CERN
VS4, Coventry, UK, October 2013, Karl Jousten 2
Applications of vacuum and leak detection

This was not possible without vacuum engineering:

3 huge vacuum systems,

for beam, for
superconducting magnets,
for helium distribution line:
104 km long, 15 000 m
2 times 27 km UHV < 10-8
Pa
250 000 welded joints
18 000 seals
NEG coated walls
780 ion pumps
1084 Pirani and Penning
gauges
170 BAG
LHC, 27 km, CERN
VS4, Coventry, UK, October 2013, Karl Jousten 3
 Applications of vacuum and leak detection

In the search for new energy: ITER

28.5 m

Vessel height 10.2m

Vacuum volume ~ 1330m3
29 m Plasma volume ~ 837m3
Cryostat volume: 14 000m3
Hydrogen/isotopes: < 10-5 Pa
Other impurities: < 10-7 Pa
Total leak rate Torus: < 10-7 Pa m3/s

VS4, Coventry, UK, October 2013, Karl Jousten 4

Applications of vacuum and leak detection

Microelectronic industry: no UHV/bake-out

Cluster tool MOCVD: Reactor for

ferroelectric films

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 Applications of vacuum and leak detection

Industrial applications: CD/DVD metallization

Type Cathode Pumps Cycle-time

SINGULUS V Focus Cathode 1 Turbo Molecular 2,7 s
Focus 1 Pump
SINGULUS V Focus Cathode 2 Turbo Molecular 1,5 s
Focus 2 Pumps
SINGULUS V SMART 1 Turbo Molecular 2,5 s
Smart 1 CATHODE Pump

SINGULUS V SMART 2 Turbo Molecular 1,9 s

Smart 2 CATHODE Pumps

VS4, Coventry, UK, October 2013, Karl Jousten 6

 Majority of
Introduction products

Permeation leaks Geometrical

leaks

mbar L/s Courtesy M. Bergoglio

Typical distribution of leaks in industrial products

Applications of vacuum and leak detection

Applications of partial pressure measurement:

Gas purity (Semi)

Residual gases
In-situ analysis for reagent gases
Outgassing rate measurement (EUV-Lithography)
Sputter process control
CVD monitoring, gas abatement analysis
MBE source control
End point detection (etching)
Gas chromatography

EUV Lithography

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Conclusions from applications

1. For now 150 years vacuum technology is

one of the basics for physical experiments
and progress in industrial technology, from
high-tech-industry to food packaging.
2. This will persist (microelectronic-industry)
and grow (solar cells, EUV lithography,
nanotechnology, life sciences, new
materials, optical computer, quantum
computer)!
Turnover 2008: worldwide 6 Mrd $/a.

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Conclusions from applications

3. As mature vacuum techniques are, as

reliable vacuum measurement should be.
All vacuum gauges need a calibration (at
least by the manufacturer).
4. Fast processes are required
5. Leak testing: Traceability for low flow rates
become more and more important.
6. Materials testing: Traceability and
standardization of outgassing rate
measurements become important.
7. Surface science/X-ray lasers: XHV is a
niche, but also important

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Traceability and vacuum primary standards

What is traceability (Vocabulary International Metrology)?

Property of a measurement result whereby the result can be
related to a reference through a documented unbroken chain of
calibrations, each contributing to the measurement uncertainty.
As reference serve the primary standards:
Measurement standard established using a primary reference
measurement procedure, or created as an artifact, chosen by
convention.
Primary reference measurement procedure is used to obtain a
measurement result without relation to a measurement standard
for a quantity of the same kind (in the same range).

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Traceability and vacuum primary standards

VS4, Coventry, UK, October 2013, Karl Jousten 12

Traceability and vacuum primary standards

Calibration chain and uncertainties

primary
u prim usec,cert u 2prim ucal
2
standard

secondary standard usec usec,

2
cert ulst usec,cal
2 2
uwork ,cert usec
2
uwork
2
,cal

working standard uwork uwork

2
,cert ulst u work ,cal
2 2 uord ,cert uwork
2
uord
2
,cal

ordinary vacuum gauge uord uord

2
,cert ulst uord ,cal
2 2

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 Traceability and vacuum primary standards

Relative uncertainties of pressures in primary standards

1E+00
Relative Uncertainties (k =2)

1E-01
2E-02
1E-02
5E-03
1E-02 4E-03
2E-03
Mercury Manometer
1E-03 3E-04
Continuous expansion Series expansion
5E-05
1E-04
2E-05
p
6E-06 5E-06 atm
1E-05

1E-06
1E-10 1E-08 1E-06 1E-04 1E-02 1E+00 1E+02 1E+04 1E+06

p in Pa

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Traceability and vacuum primary standards

Mexiko

Singapore

Fully developed primary standards down to high vacuum

National standards down to high vacuum

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Secondary laboratories

Secondary labs
Use secondary standards as reference (calibration by
comparison)
Are accredited by a National Body (technical
accreditation of their calibration procedure)
Work according to ISO 17025 and in vacuum in
addition according to ISO 3567 and 27893
Distribute the scale more economically to the end user

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Secondary and reference standards

Reference gauges

Quartz Bourdon gauge

High
accuracy
Resonance silicon gauge
Good long
term stability
Good
Ionization gauge
transport
Capacitance diaphragm gauge
stability
Spinning rotor gauge

Ultra high
vacuum high vacuum Fine vacuum Rough vacuum

-7 -5 -1 2 5
10 10 10 10 10
p in Pa

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 Secondary and reference standards
1E+00 1

0,2 Ionisation gauge Membrane

Relative Uncertainties (k =2)

1E-01 0,1 0,1

(mechanical)
0,05 0,05
0,02 0,02 Pirani 0,02
1E-02 0,01 SRG 0,01 0,01
0,005 0,004 CDG
0,003
0,002
1E-03 0,001
Continuous expansion Series expansion QBS
RSG
1E-04
Piston
p atm
1E-05
Mercury Manometer
1E-06
1E-10 1E-08 1E-06 1E-04 1E-02 1E+00 1E+02 1E+04 1E+06

p in Pa

Lowest relative uncertainties for vacuum gauges and primary standards

.

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Traceability and vacuum primary standards

Leak rate threshold

Written standards
Choose appropriate leak EN 1518, 1779, 13184, 13185,13192
ISO 3530, 27895
test method
AVS practice (1992)

Leak test
(quantitative)
Hood filled with
known
concentration of
Geometrical standard leak tracer Standard leak
Test piece gas
(capillaries) Vacuum (Validates your leak test)
pressurized
Vacuum
withTest piece
tracer
Permeation standardpressure
leak gas communicating
with leak
detector
Leak
detector
Leak detector
sensitive
to sensitive
tracer to
gastracer gas
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Traceability and vacuum primary standards

The standard leak enables the user

To validate the applied method

To verify and calibrate the reading of a leak detector
Perform accurate measurements in-situ

Written standards require that

The standard leak is calibrated (traceability to a primary standard)

There is an uncertainty associated with the specified leak rate

Calibration/Traceability:

Primary flow Secondary Reference leak

meter standard leak for leak detector

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Traceability and vacuum primary standards

Several types of gas flow measurement in vacuum metrology:

pV V p
q pV p V
t t t

pressure rise technique

defined volume change, fixed pressure

flowmeter (constant pressure, variable volume)

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 Traceability and vacuum primary standards
PTB primary flowmeter (1E-8 Pa L/s1E-2 Pa L/s)
V2
V

CDG Gas Flow

V3
p=const
C
"Leak"
V1 p

Gas Inlet V q pV
q pV p q
t RT
Temperature
stability !

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Traceability and vacuum primary standards

PTB measurement standard for vacuum standard test leaks

(1E-8 Pa L/s1E-2 Pa L/s)

QMS

Valve 2
Flowmeter

Valve 3
Valve 1

Testleak

Enclosure T=const.
(necessary for permeation leaks)

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Traceability and vacuum primary standards
PTB measurement standard for sniffer test leaks against atmosphere

Testleak

CDG 133 kPa FS T1 Needle

V1
V2 T2

V = 5.1 cm

T3 CDG 133 Pa FS

V3 T4

Thermal insulation V = 6.1 cm

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Traceability and vacuum primary standards

Metre Convention (1875) Diplomatic Treaty

General Conference on Weights and Measures (CGPM) Governments of

member states
every 4 years

International Committee for Weights and Measures (CIPM) International

Organizations
18 individuals elected by CGPM

10 Consultative Committees (CCs) CIPM MRA (1999) National

Metrological
each chaired by a member of CIPM
Institutes (NMI)

Working Groups (WG)

International Bureau of Weights and
Measures (BIPM, Sevres, France)

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Traceability and vacuum primary standards

The Mutual Recognition Arrangement

(MRA) of the CIPM
to provide for the mutual recognition of calibration and
measurement certificates issued by NMIs
by
international comparisons of measurements, to be known as
key comparisons, and as well supplementary international
comparisons (http://www.bipm.org/kcdb)
demonstration of competence by NMIs by publishing their
calibration measurement capabilities
establish an internationally accepted quality system in each
NMI.

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Traceability and vacuum primary standards
CCM.P-K12 (key comparison for leak rate measurement, 2012):
Transfer standards

Reservoir cannot
be refilled

Two helium permeation leaks:

410-11 mol/s (110-4 Pa L/s, 23C) and 810-14 mol/s (210-7 Pa L/s),
no clogging, long-term stable, but decreasing rate
Temperature coefficient about 4%/K
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Traceability and vacuum primary standards
Results of CCM.P-K12 (key comparison for leak rate measurement, 2012)

q,1 (4.3746 0.0249) 10 11 mol/s .

Dj
En
2u Dj

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New developments
Dynamic vacuum standard for rough vacuum at PTB

High
Fast pressure
opening volume
valve

Low pressure
volume

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New developments : dynamic vacuum standard

Pressure step

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 Future developments

On its way: Vacuum metrology for production environments (EMRP

IND12, 2011-2014)
Work package 2 Leak measurement and testing
Task 1: Leak elements with defined geometry
Task 2: Improvement of the theory of flow in narrow ducts
Task 3: Leak elements performance (environmental conditions)
Task 4: Development of a practical guide on metrological performance of
leak detectors
Task 5: Feasibility study on alternative methods than mass spectrometer
leak detector to detect leaks within few seconds

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 Future developments

On its way: EMRP IND12

Work package 3 Partial pressure and outgassing
rate measurement
Triggered by EUV-Lithography
Written standards for vacuum gauge calibrations and
perhaps design for ionization gauges
Written standards for QMS calibration and outgassing
rate measurements
Furter developments of optical methods for vacuum
measurement, also for leak testing
Developments for harsh environments like Fusion
(tritium, magnetic fields,)
XHV (but niche)
EUV-Lithography

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 Conclusion
Traceable calibrations are more important than 20 years ago.
Primary standards are available world wide.
An international validation scheme ensures equivalence of vacuum gauge
and leak rate calibrations world wide.
Reasonable secondary gauges for full vacuum range except for low HV
and UHV.
Written standards are in progress and shall transform our present
knowledge into long-lasting practical solutions. Need to be extended for
partial pressure and outgassing rate measurement.
Dome of the Reichstag in Berlin