Metrology of high vacuum and ultra high vacuum, Primary / Secoundary Gauges; Leak detection

Lise-Marie Lacroix, LPCNO, Toulouse

Motivations / Objectives

Vacuum used in : - chemical industry / pharmaceutics - microelectronics - material science - aeronautics / aerospace

Important to measure the vacuum, its quality, the gas composition : avoid pollutants, contaminations, test under severe conditions

Motivations / Objectives
Nanoparticles synthesis under inert atmosphere

Co Au

Fe Fe

Co Co

Fe

Fe

biomedical applications, magnetic data storage

Motivations / Objectives
Surface modification by plasma etching on nanoparticles

Hydrophobicity

Buoyancy

Self cleaning properties

biomedical applications, textile, windows, car manufacturers.

Motivations / Objectives
Organic thin film grown for a new generation of transistor

Motivations / Objectives

http://www.ams02.org/2010/04/welcome/ http://www.ams02.org/vr_cern/20.html Simulation of spatial environment : test of the Alpha Magnetic Spectrometer
Measurement of the gamma-ray emitted by the implosion of supernova Answer to the question : is there also antimatter in space?

h = 400km, P = 10-4mbar = 7.5 * 10-5 torr, T= [-40 , +50] C System : turbomolecular pump, ionisation gauge, He leak detection

Motivations / Objectives

New ion pump : based on Xenon ion ejected and accelerated by an EM field

P = 10-6mbar = 7.6 * 10-7 torr, T= 20K = -256 C Cryogenic pumps, ionisation gauge, leak detection

Overview

I. II.

General introduction Absolute measurements

III. Industrial Gauge IV. Partial pressure measurements V. Leak detection

I. General Introduction
Welcome to the vacuum world Rough Vacuum 50 Primary Vacuum 10-3 Secondary Vacuum (HV) Ultra High Vacuum (HV)

10-7

760 380

75

7,5. 10-4

Pressure (torr)

th Ca

nt Mo nc Bl a

T St-

b ffee Co

ez rop

o di cT

Need for different measurement apparatus to cover this 12 decade of pressure !

s ean

ub e( ) TV

I. General Introduction
How to measure vacuum?

Use adequate gauges which can be sorted by :

-Physics behind -Vacuum range -Selectivity vs. Gas -Hysteresis phenomena -Fragility against environement

I. General Introduction
How to measure vacuum? Gas pressure : Molecule collision against the system wall. Physics behind

Use this collision process ! Mechanic gauge

Use other properties of gas : - electric conductivity - thermic conductivity - ionisation Relative measurement : Need a calibration -Pirani, Thermocouple -Bayard-Alpert, Mass Spectrometry

Absolute measurement -Torricelli, Mc Leod -Bourdon -Capacitive, Piezoelectric

I. General Introduction
How to measure vacuum? Rough Vacuum 50 Primary Vacuum 10-3 Secondary Vacuum (HV) Vacuum Range Ultra High Vacuum (HV)

10-7

Pressure (torr)

Bourdon Mc Leod Piezoelectric Capacitive Pirani Thermocouple Penning Bayard-Alpert

I. General Introduction
How to measure vacuum? A . Absolute measurement B. Relative measurement : Need a calibration

Gas nature depency Calibrated for N2 usually Keep in mind Daltons law : Ptotal = xP1+yP2+ Measurement might change with time due to pollution Dont trust measurement below 10-3 Torr; 50-100% of error is common! Below 10-3 Torr the measurement is dependent of the design of the gauge The calibration is a tricky procedure.

I. General Introduction
How to choose the right gauge? a. Range of pressure b. Condition of use : - pressure gradient (due to air entry) - corrosif gas / contaminating vapours - mechanical vibrations - temperature range c. Positionment in the system : - for high pressure (viscous flow regime) - for low pressure (molecular flow regime)

Have an idea of the pressure, not really measure it precisely!

I. General Introduction
Features / Specifications : Sensitivity (sensibilit) Accuracy / Resolution (prcision) Fidelity Linearity Vacuum range Over pressure Operating temperature range

I. General Introduction
Features :

Overview

I. II.

General introduction Absolute measurements

III. Industrial Gauge IV. Partial pressure measurements V. Leak detection

II. Absolute measurements

A. Torricelli Barometer (1643) Evangelista Torricelli (italian mathematician), studied with Galileo suggested that air has a weight.

II. Absolute measurements

A. Torricelli Barometer (~1640)

P = PA-PB = g ha
Exemple : advantage of using Hg ( =13.56 g.cm-3) versus H2O?

II. Absolute measurements

B. Liquid manometer

PA = PB + g h

Cathetometer

II. Absolute measurements

B. Liquid manometer Choice of liquid : - Hg low saturated vapour pressure (10-3 torr @RT) high density low wetting of glass Toxic Can be oxidized - mineral oil low saturated vapour pressure high wetting of glass sensible to gas pollution

Accuracy : for P > 10 mm Hg = 10 Torr : 1% for low P : ~10% ; pb of saturated vapour pressure of the liquid Vacuum range : 760 - 10 Torr

II. Absolute measurements

C. Mechanic gauge

P1V1

P2V2

Calcul to make : Finally

S p=h V + S (h0 h)
2

II. Absolute measurements

C. Mechanic gauge

S p=h V + S (h0 h)
2

Quadratic : Kammerer gauge Scale

V >> S (h0 h)

Find the new relation

Linear : Mc Leod gauge Different way of measurement : Vc is kept constant !

II. Absolute measurements

C.1. MacLeod gauge

Go back to Mariottes law, This time Vc is constant

V >> Sh0 V >> Sh = VC

Find the new relation

II. Absolute measurements

C.1. MacLeod gauge Gauge design : - displacement of Hg : - capillarity phenomena : through the position of the reservoir via 2 valves connected to air or vacuum (cf TP) use of tube with exact same diameter

II. Absolute measurements

C.2. Gauge Mc-Leod/Dunoyer Increasing the sensitivity and the vacuum range Linear scale : fixed reference corresponding to various compression factor Cf use in TP

II. Absolute measurements

C.3. Limitation Kammerer Mc Leod

S p=h V
2

VC p=h V

p small if .. S : below a diameter of 0.8mm : Hg attached to the glass. V : above 250cc : weight too much! Whats the lower pressure measured (h=0,5mm; l=1mm)?

II. Absolute measurements

C.4. Conclusion Mc Leod gauge Absolute gauge Sensitivity : up to 10-6 in McLeod/Dunoyer configuration Pressure range : 10 torr 10-5 torr Measurement : length of displacement (mm) Drawbacks : - fragile - expensive - use of Hg - repetitive / long measurements

II. Absolute measurements

D. Capacitive gauge. Symetric configuration

C=

S d

Difference between C1 and C2 measured with an electronic bridge

II. Absolute measurements

D. Capacitive gauge. Asymetric configuration Limited corrosion related only to the diaphragm.

Electronique

Vide rf. Electrode de rfrence Membrane de mesure

Capa. rfrence

Capa. mesure

Vide mesurer

Rq : the piezoelectric gauge has a similar architecture

II. Absolute measurements

D. Conclusion Capacitive gauge (Baratron) Absolute gauge Sensitivity : very high. 0.25 to 0.5% of reading Pressure range : 750 torr 7*10-6 torr (depending on the diaphragm thickness) high pressure for thick diaphragm Excellent linearity; good stability especially vs TC Measurement : voltage. The signal is demodulated and processed to finally indicate a pressure.

Drawbacks :

- corrosion of the active element - expensive

III. Industrial measurements

A. Mechanic gauge. Bourdon manometer Material used : brass (Cu-Zn : laiton)

III. Industrial measurements

A. Mechanic gauge. Bourdon manometer Pressure range : >760 torr 1 torr (according to the nature of the material used) Independant of the nature of the gas Do not reach a plastic deformation of the tube : keep a relatively low pressure

Other use : - pneumatic pressure

III. Industrial measurements

B. Gauge based on gas conductibility

If you heat a filament in a gaz atmosphear : - the temperature reached is dependent of the heat exchange

Rappel : Heat exchange 3 mechanisms : - conduction, convection, rayonnement

Gaz conductibility decreases when P < 50 torr Applications :

III. Industrial measurements

B. Gauge based on gas conductibility

Pirani Gauge
V = constant Pressure Temperature Resistivity

Thermocouple Gauge
I = constant Pressure Temperature

DZ e 2 C = k BT
Nernst-Einstein law

R=

III. Industrial measurements

B. Gauge based on gas conductibility

Too few molecules : Heat transfer only rayonnement

Too many molecules (viscous regime): Heat transfer constant

III. Industrial measurements

B. Gauge based on gas conductibility 1. Pirani gauge

Theoretical configuration

2 filaments (platine or tungstene, 20m) used as resistance in a wheastone bridge. Difference of resistance due to the temperature, i.e. to the pressure : The bridge is not equilibrated : a current is measured!

III. Industrial measurements

B. Gauge based on gas conductibility 1. Pirani gauge

Commercial configuration R

mA R1 100 R2 100

Equilibrium of the bridge at Patm. When P decreases : RPirani increases, a current is driven through the amperemeter Application : W : 10cm long, 0,8 mm in diameter, Patm : R0 ~20

III. Industrial measurements

B. Gauge based on gas conductibility 1. Pirani gauge Not linear Current measured. (old style)
/ new style : measurment of the power used to keep T constant

Pressure range : 50 torr 10-3 torr Gas dependant (conductivity dependent of the gaz) Sensitive to corrosion. Platinum would be the best choice but too expensive (Ni) The wire material is crucial : - high modification of the resistance with the temperature :

(T ) = 20 (1 + 20T )
- high melting point - no oxidation

III. Industrial measurements

B. Gauge based on gas conductibility 1. Pirani gauge

Calibration curves

III. Industrial measurements

B. Gauge based on gas conductibility 2. Thermocouple gauge

At low pressure , T ~ 200C

III. Industrial measurements

B. Gauge based on gas conductibility 2. Thermocouple gauge : building your own thermocouple !

http://www.belljar.net/tcgauge.htm

III. Industrial measurements

B. Gauge based on gas conductibility 2. Thermocouple gauge : conclusion Not linear Tension measured. (old style)
/ new style : measurment of the power used to keep T constant

Pressure range : 50 torr 10-3 torr Gas dependant (conductivity dependent of the gaz) Very robust. Cheeper but slower than a Pirani gauge. The accuracy is not as good Use : Primary vaccuum, on independant pump or a complex pumping unit

III. Industrial measurements

B. Gauge based on gas conductibility Calibration curves

Gaz K

Air 1

H2 0.7

He 0.9

Ne 1.2

A 1.6

Kr 2.2

Xe 4

CO2 1.05

III. Industrial measurements

C. Gauge based on ionisation 1. Introduction to the ionisation phenomena

III. Industrial measurements

C. Gauge based on ionisation 1. Introduction to the ionisation phenomena
H.T 1-3kV

Pompage

ions electrons

III. Industrial measurements

C. Gauge based on ionisation 1. Introduction to the ionisation phenomena

Discharge tube (here Hg pressure)

III. Industrial measurements

C. Gauge based on ionisation 2. Discharge tube

High pressure : no current (the tension is too low) Intermediate : electrons generate ions Low pressure : too low probability of ionisation (mean free path of electron too long)

III. Industrial measurements

C. Gauge based on ionisation 2. Discharge tube Indication of the pressure Indication of the gaz

III. Industrial measurements

C. Gauge based on ionisation 3. Penning Gauge : cold cathod discharge 2.106 B N S
H.T 1-3kV

Pompage

III. Industrial measurements

C. Gauge based on ionisation 3. Penning Gauge : cold cathod discharge

10-3 Torr 10-4 Torr 10-5 Torr 5 10-6 Torr-

1.8 mA 120 A 8 A 1 A

Current measured in Penning gauge according to the pressure

Advantages :

-robust, good accuracy - easy to clean - large vacuum range : 10-3 to 10-6 torr (up to 10-10) - Adsoprtion of the ions on the cathode - Work as a pump : can indicate a pressure below the real one.

Drawbacks :

III. Industrial measurements

C. Gauge based on ionisation 4. Thermoionic gauge P
Pompage

G mA UG UP Qq V + 170V - 30V A

(Bayard Alpert configuration)

III. Industrial measurements

C. Gauge based on ionisation 4. Thermoionic gauge : Bayard Alpert Vacuum range : 10-3 to 10-10 torr
10-3 torr : above electric discharge may happen between the filament and the grid 10-10 torr : below that the cathode generates Xray (Roentgen effect). The ion current is no more proportionnal to the pressure

Vacuum range : 10-3 to 10-10 torr

10-3 torr : above electric discharge may happen between the filament and the grid 10-10 torr : below that the cathode generates Xray. The ion current is no more proportionnal to the pressure

III. Industrial measurements

C. Gauge based on ionisation 4. Thermoionic gauge : Bayard Alpert Disadvantage : less robust than Penning gauge Lots of sorption on the collector : need to clean it often The bulb and the metallic part are degazing (high TC used) : P > real P The filament might be broken if oxygen is present Huge difference of sensitivity according to the gaz used (related to the ionization coefficient)
Gaz Hlium Hydrogne Oxygne Azote Air sec Monoxyde carbone Dioxyde carbone Argon Sensibilit 14 16 85 110 100(rfrence) de112 de120 162

Annexes : thermoionic emission : gun for electronic microscopy

Annexes : thermoionic emission : gun for electronic microscopy

Dans lil du microscope lectronique. Florian Houdellier http://www.cemes.fr/microscopie/

Annexes : thermoionic emission : Xray lamp

Coolidge tube

III. Partial pressure measurements

A. Mass spectrometer magnetic sector 1. Ionisation of the gas 2. Separation of the fragments 3. Collection of the spectra (filtered in specific mass)

III. Partial pressure measurements

A. Mass spectrometer magnetic sector 1. Ionisation of the gas

Generation of a plasma : The molecule are ionized by a flow of electrons

The molecule can be ionized once or twice leading to Ar+ or Ar2+ Their specific weight will be different : m/q Ar : m = 40; m : molecular weight q : number of electron lost Ar+ : m/q=40; Ar2+ : m/q=20

III. Partial pressure measurements

A. Mass spectrometer magnetic sector 2. Separation of the fragments The ions are placed in strong fields: - magnetic B - electric E According to the specific weight, the ions will be deflected

R=

m K 2 E q B2

We can collect the information for each specific mass by tuning the electric field

III. Partial pressure measurements

A. Mass spectrometer magnetic sector 3. Collection of the data set

III. Partial pressure measurements

B. Mass spectrometer quadripole filter Similar idea but instead of using a magnetic field we use an AC electric field For one high frequency, only one type of ion Will reach the end of the tube

Limit partial pressure reached : 10-15 torr thanks to a detector which is also a electron multiplicator Advantage : more accurate than the first design presented

The green and red dots show that La and Mn occupy different columns in the La0.7Sr0.3MnO3layers. The red dots near the left interface indicate that Ti in the SrTiO3 layers occupies columns that are equivalent to those occupied by Mn in the La0.7Sr0.3MnO3 layers. Interestingly, in the composite image purple dots are visible at the interface between the two layers. This is evidence that, at this particular interface, there was a mixing of Ti and Mn within individual atomic columns.

IV. Leak detection

If the pumping system does not reach the optimum vaccuum : You may hace some leaks. - real leaks : leak from the atmosphear towards the system - virtual leaks : impregnated gaz are released - degazing due to material inside the system What leak can we tolerate? Depends on the pressure wanted, on the pumping rate ex : P = 10-8 torr; S = 5 l/s P = 10-4 torr; S= 10 000 l/s

3 different units : Torr.l/s lusec (mTorr.l/s) atmosphere. cm3/s

IV. Leak detection

What type of leak do we have?

Saturation pressure

IV. Leak detection

How to detect leaks? 1. Vaccuum detection Check the different pieces Use the discharge tube to check the nature of the leak (air, gas, moisture)

2. Vaccuum detection with a tracor gas

IV. Leak detection

How to detect leaks? 3. Pressured gaz

If the pieces tested are too fragile to be kept under vaccuum, or the chamber to big to reach a good vaccuum

IV. Leak detection

How to detect leaks? 4. Ressuage technic