Vacuum gauges for the fine and high vacuum

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1 Vacuum gauges for the fine and high vacuum Karl Jousten, PTB, Berlin 1. Measurement of vacuum pressures and the calibration chain 2. Overview of measurement principles and gauge types 3. Direct gauges, indirectly measuring gauges 4. Accuracy of vacuum gauges CAS_2006

2 Measurement of vacuum pressure The definition of pressure p: F Mass Time p = A Length It follows one of the measurement principles. 2

3 Measurement of vacuum pressure Gas pressure p p = F A p 0 A F Balance as force meter This is a traceable instrument usable as primary standard 3

4 Errors and uncertainties Error: A wrong reading of a gauge. A deviation from a true value defined by the SI units. True value Error/deviation Indicated value Uncertainty: The possible range by which a reading may not reflect the true value defined by the SI units. Possible true value Uncertainty Indicated value 4

5 Measurement of vacuum pressure Gas pressure p p = F A p 0 A F Balance as force meter 5

6 Errors and uncertainties The calibration chain Reliability increases Uncertainty increases secondary standard primary standard working standard ordinary vacuum gauge 6

7 Traceability and primary standards Fully developed primary standards partly developed standards 7

8 Best accuracy available Relative uncertainties of pressures in primary standards 1E+00 Relative Uncertainties (k =2) 1E-01 1E-02 1E-03 1E-04 1E-05 1E-06 2E-02 1E-02 4E-03 2E-03 Continuous expansion Series expansion Mercury Manometer 3E-04 1E-04 3E-05 7E-06 p atm 3E-06 1E-10 1E-08 1E-06 1E-04 1E-02 1E+00 1E+02 1E+04 1E+06 p in Pa Traceability and primary standards 8

9 Measurement uncertainty 1E+00 1E-01 1E-02 1E-03 Ionisation and Suppression of X-ray and ESD Ionisation Gas dependent-difficult to interpret 1E-04 1E-12 1E-10 1E-08 1E-06 1E-04 1E-02 1E+00 1E+02 1E+04 pressure in Pa Viscosity p = Heat conductivity Gas independent F A Total pressure Piezo Piezoresistive Membrane Mechanical Resonance Capacitance Piston/Cyl U-tube 9

10 10

11 11

12 Gas inlet p F = = ρgδh A The mercury U-tube exists since Torricelli (1644). It is still the most accurate vacuum gauge > 100 Pa (1 mbar)! 12

13 The rotating piston gauge p = F A Gas Gap: 0.2µm 13

14 Mechanical gauges M R A Z Ra um 1 Ra um 2 P 1 P 2 3 Groups: 1. Ref.side p atm and contains meas.dev. 2. Ref.side p=0, meas.dev. on test side (1) 3. Ref.side p=0 and contain meas.dev. 14

15 Mechanical gauges: Bourdon gauges 15

16 Mechanical gauges: Bourdon gauges Light source 2 Photo cells Mirror Amplifier Coils Quartz spiral Precise Resistor 16

17 Mechanical gauges: Bourdon gauges 17

18 Piezoeffect used by membrane 18

19 Piezoresistive effect Material: Silicon (MEMS) 19

20 Capacitance diaphragm gauge Sensitivity of deflection: 0.4 nm! Membrane (INVAR, Ceramic): as low as 25 µm. Two improve zero stability: 2 capacitors plus thermostated housing 20

21 Electrical block diagram of capacitance diaphragm gauge 21

22 Thermal transpiration effect Cross section n 2 = n p 2 = p 1 1 T T T T

23 Thermal transpiration effect 318 =

24 Resonance Silicon Gauges Designed by MEMS 24

25 25

26 Heat conductivity through a gas 26

27 Uncertainties due to the physical principle of measurement Example: Pirani gauge convection Heat transport by gas Radiation and conduction 27

28 Electrical circuit for Pirani gauge Constant temperature Constant heating voltage, current, or power 28

29 Mikro Pirani (MEMS manufactured) by MKS Heated sheet 60 C MEMS: higher Knudsen number, no convection 29

30 Correction factor for helium for 4 different Pirani gauges Correction factor CF He/N2 1,40 1,20 1,00 0,80 0,60 0,40 VM1 (Pfeiffer) VM2 (Thyracont) VM3 (MKS) VM4 (Leybold) Mean Helium MEMS Pirani 0,20 0,00 1E-03 1E-02 1E-01 1E+00 1E+01 1E+02 p in mbar 30

31 Experimental standard deviations of repeat calibrations for 4 different Pirani gauges at various pressures # Gauge s in % 0,05 mbar 3 mbar 30 mbar 1 Pfeiffer TPR 280 0,19 0,13 0,09 2 Thyracont VSP52 0,06 0,35 3,30 3 MKS 925C 0,10 0,12 0,19 4 Leybold TTR91 0,03 0,09 0,12 31

32 Thermocouple gauge 32

33 Measurement principles Viscosity p 8kT πdρ & ω = RD( ω ) πm 20σ ω 33

34 Sprinning rotor gauge 34

35 Sprinning rotor gauge 2,15E-07 s -1 2,10E-07 Residual drag vs. frequency of rotor 2,05E-07 DCR-Signal 2,00E-07 1,95E-07 1,90E-07 1,85E Rotor frequency f s -1 35

36 Sprinning rotor gauge No gas consumption (e.g. by ionization) No dissociation (hot cathode) Low outgassing rate Predictable reading High accuracy High long-term stability 36

37 Measurement principles Ionisation 37

38 Measurement principles Ionization gauges for different vacuum ranges Fine vacuum IG 38

39 Measurement principles Ionisation gauges for fine vacuum 39

40 Measurement principles I ( 1) ( 1) S ΦnL λ = I λ e 0 p = kt S( T ) Φ( λ 1 λ 1 0 ln ) L 1 I 0( λ ) 1 I( λ ) Previous investigations showed that TDLAS is applicable for vacuum measurement: CO, mid-infrared (5 µm), resolution down to 10-5 Pa, high accuracy. Intensity (a.u.) Partial Absorpion, Reference Predicted from ch time (ms) 40

41 How accurate are vacuum gauges? Reasons for inaccuracies of vacuum gauges General Uncertainties due to calibration chain Uncertainties due to installation Uncertainties due to operation Inaccuracies caused by the physical principle of measurement Uncertainties caused by the device itself Example Has the vacuum gauge been ever calibrated? Against what standard? Pressure at gauge position may not reflect the pressure where the experiment takes place. Outgassing of an ion gauge may falsify an outgassing rate measurement. Thermal conductivity or ion gauge is used, but gas mixture is not (accurately) known. See Table 2. 41

42 How accurate are vacuum gauges? Gas species dependence: Reasons for inaccuracies Real total pressure only for force/area measuring gauges and > 100 Pa (1 mbar)! Below 100 Pa consider the thermal transpiration effect. Spinning rotor gauges: Use a weighted mean mass, if approximate relative composition is known. 2 = n n meff ai mi a i = 1 i= 1 Thermal conductivity gauges and ionisation gauges : Scaling factors are available, but do have high uncertainties. i= 1 CF eff = n a CF i= 1 i i 42

43 How accurate are vacuum gauges? Offset measurement Offset instability (drift) Resolution Uncertainties due to the vacuum gauge itself General Influences of environment (mainly temperature) Non-Linearity Integration time (scatter of data), repeatibility Reproducibility (stability of calibration constant) Hysteresis Prior usage, cleanliness Examples residual drag in SRG, zeroing of Pirani gauge, X-ray- and ESD-effect for ion gauges Offset drifts with environmental temperature (Piroutte effect in SRG), bridge is no more balanced with time Number of digits shown Enclosure temperature of Pirani changes varies, thermal transpiration effect changes in CDG, amplifier changes amplification Ion gauge (sensitivity changes with pressure) Same signal at repeat measurements? Integration time in SRG, in picoammeter with ion gauge. Calibration constants change with time. Mechanical gauges (up, down measurement) Surfaces change, accommodation coefficients change, secondary yield changes 43

44 How accurate are vacuum gauges? Table: Relative measurement uncertainty of commercially available vacuum gauges. Gauge type Measurement Normal Optimum range Lowest range in Pa uncertainty in Pa uncertainty Piston gauges Quartz-Bourdon-manometer x x10-4 Resonance silicon gauges x x10-5 Mechanical vacuum gauge Membrane vacuum gauge Piezo Thermocouple gauge Pirani gauges Capacitance diaphragm gauges Spinning rotor gauges Penning gauges Magnetron gauges Ionisation gauges (Emission cathodes)

45 How accurate are vacuum gauges? 1E+00 1 Relative Uncertainties (k =2) 1E-01 1E-02 1E-03 1E-04 1E-05 1E-06 0,2 Ionisation gauge Continuous expansion 0,05 0,05 0,006 SRG Series expansion 0,02 0,004 Pirani 0,003 0,01 0,1 CDG 1E-10 1E-08 1E-06 1E-04 1E-02 1E+00 1E+02 1E+04 1E+06 0,002 Mercury Manometer Mechanical 0,02 QBS Piston 0,01 0,001 p atm p in Pa Lowest relative uncertainties for vacuum gauges and primary standards Errors > 100 % (error factor > 1) are possible. 45

46 Todays commercial gauges Pirani gauge Old classical gauges: Gauge head + controller Today: Active gauges or transmitter (all in one) or Digital gauges (digital output via interface) 46

47 Todays commercial gauges Transmitter gauge plus Profibus Converter 47

48 Todays commercial gauges Commercial active Line vacuum gauges 48

49 We have discussed: Metrological system - primary standards- calibration chain Measurement principles and gauges Direct, indirect measuring gauges Sources of uncertainties with values from 0.001% up to 100% or factor CAS_2006

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