EP2406811B1 - Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant - Google Patents

Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant Download PDF

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Publication number
EP2406811B1
EP2406811B1 EP10714937.9A EP10714937A EP2406811B1 EP 2406811 B1 EP2406811 B1 EP 2406811B1 EP 10714937 A EP10714937 A EP 10714937A EP 2406811 B1 EP2406811 B1 EP 2406811B1
Authority
EP
European Patent Office
Prior art keywords
filament
ionization
entrance
cage
ionization cell
Prior art date
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Active
Application number
EP10714937.9A
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German (de)
English (en)
French (fr)
Other versions
EP2406811A1 (fr
Inventor
Laurent Ducimetiere
Cyrille Nomine
Jean-Eric Larcher
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pfeiffer Vacuum SAS
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Pfeiffer Vacuum SAS
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Publication of EP2406811A1 publication Critical patent/EP2406811A1/fr
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/147—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment

Definitions

  • the present invention relates to an ionization cell for a mass spectrometer.
  • the invention applies to mass spectrometers in which an electric heating filament emits electrons.
  • the invention also relates to a leak detector comprising the ionization cell.
  • a gas sample is analyzed by bombarding the sample with a stream of electrons and then moving the ionized particles thus obtained to differentiate them, for example, according to their trajectory.
  • the mass spectrometers of the leak detectors measure and quantify a tracer gas, such as helium.
  • Mass spectrometers comprise, for example, an ionization cell comprising an ionization cage and a heating electric filament emitting electrons.
  • the molecules of the gas to be analyzed are bombarded by the electron beam and a large part of the molecules of the gas to be analyzed is converted into ionized particles. These ionized particles are then accelerated by an electric field. They then arrive in an area subject to a magnetic field, which has the property of deflecting the trajectories of the ionized particles according to their mass.
  • the stream of ionized particles of the tracer gas is proportional to the partial pressure of the gas in the installation, and its measurement makes it possible to know the value of the flow rate of the leak detected.
  • certain ionization cells comprise two filaments.
  • a first working filament is powered to produce the electron beam and a second backup filament is to be powered in case of failure of the first working filament.
  • the waiting time after which the second emergency filament is made operational so as to allow a stable and reproducible measurement, representative of the amount of tracer gas, can prove to be excessively long (up to two hours wait may be necessary).
  • the object of the invention is therefore to reduce the waiting time required for the ionization cell to be operational again during the passage of the first faulty working filament to the second emergency filament.
  • the inventors have found with surprise that with this arrangement of the ionisation cell, the second emergency filament is not altered by the first working filament in operation.
  • the invention also relates to a mass spectrometer leak detector comprising an ionization cell as described above.
  • the figure 1 represents a leak detector 1 with mass spectrometer 2, tracer gas, such as helium (He 3 or He 4 ) or hydrogen (H 2 ).
  • tracer gas such as helium (He 3 or He 4 ) or hydrogen (H 2 ).
  • the mass spectrometer 2 is connected to the suction of a secondary pump 3 whose discharge is connected to the suction of a primary pump 4, via a first isolation valve 5.
  • the gases to be analyzed 6 possibly containing the tracer gas revealing a leak, are sucked into the intake of the secondary pump 3, via a second isolation valve 7.
  • Part of the gases to be analyzed 6 is then sampled by the mass spectrometer 2
  • the detector 1 may also comprise a pressure sensor 8 for determining the gas pressure at the connection pipe with the secondary pump 3, upstream of the second isolation valve 7.
  • the magnetic deflection mass spectrometer 2 comprises an ionization cell 9 and means for deflecting and selecting the ionized particles 14a, 14b, 14c.
  • the ionization cell 9 comprises an ionisation cage 10, in the form of a parallelepiped box, having a first entrance slot 11 for the passage of the electron beam 12.
  • the ionization cell 9 also comprises a first filament of 13 to form the electron beam 12 when powered.
  • the first working filament 13 is arranged facing the first electron entry slot 11 of the ionization cage 10, so that a maximum of electrons enter the ionization cage 10.
  • the ionization cell 9 thus makes it possible to ionize the gases to be analyzed 6 by bombarding them with the electron beam 12, obtaining a beam of ionized particles 14.
  • the ionization cage 10 also has an outlet slot 15 on one side 16, for the passage of the ionized particles 14a, 14b, 14c formed in the cage Ionization 10.
  • the side 16 containing the exit slot 15 corresponds to the upper face of the ionization cage 10.
  • the deflection and selection means comprise, for example, means for generating an electric field (not shown) for accelerating the ionized particles 14a, 14b, 14c and means for generating a magnetic field (not shown) oriented substantially according to the arrow B , such as permanent magnets, to deflect the trajectory of the ionized particles 14a, 14b, 14c, according to radii of curvature Ra, Rb, Rc, depending on the mass of the ionized particles.
  • the beam of ionized particles 14, which contained ionized particles of different masses, is divided into several beams 14a, 14b, 14c, each beam containing only ionized particles of the same ratio m / e (ratio of the atomic mass of the particle on the number of electrons lost at the moment of ionization).
  • the ionized particles of helium 14c are separated from the lighter ionized particles of hydrogen 14b whose radius of curvature Rb is smaller or ionized particles heavier with nitrogen or oxygen 14c whose radius of curvature Rc is bigger.
  • the total pressure in the chamber of the mass spectrometer 2 must be kept below 10 -1 Pascal so that the trajectories of the electrons and the ionized particles are not disturbed by the residual molecules.
  • the deflection and selection means may also comprise a triode electrode 17 for collecting the ionized particles 14a whose mass is higher than that of the tracer gas, as well as a diaphragm 18, for selecting the ionized particles of tracer gas 14c, and a braking electrode 19 for removing noise from other ionized species.
  • the leak detector 2 also has an acquisition chain comprising in particular a DC amplifier 20 downstream of a target 21 receiving the stream of incident ionized particles of tracer gas 14c originating from the braking electrode 19, to transform it in electronic current.
  • the ionization cell 9 further comprises a second emergency filament 22, intended to be powered in the event of failure of the first working filament 13 to produce an electron beam instead of the first working filament 13.
  • the filament 22 is arranged facing a second electron entry slot disposed on one face of the ionization cage 10 (not visible on the figure 2 ).
  • the ionisation cell includes means for switching the supply, enabling selectively supplying one of the two filaments to ensure continuity of work by allowing switching of the supply of the first working filament 13 to the second filament emergency 22 if the working filament 13 has a failure.
  • the first working filament 13 is fed and produces the electron beam 12, directed by the magnetic field B to the corresponding first input slot 11 of the ionization cage 10.
  • the power supply the first working filament 13 is cut off and the second emergency beam 22, which produces a beam to the second corresponding input slot of the ionization cage 10, is powered alone.
  • the supply of the filaments 13, 22 is carried on the one hand by an electric current to carry the filament filament.
  • the filaments 13, 22 are connected to a power supply 23a with a power of 14W at 3A.
  • the filaments 13, 22 are supplied with voltage by a voltage supply 23b between 100V and 300V, connected to the filaments 13, 22 so that the potential of the ionization cage 10 is greater by at least 100V at the potential of each filament 13, 22 (see figure 2 ).
  • the filaments 13, 22 may be in iridium wire covered with an oxide deposit.
  • the oxide deposit is for example a layer of yttrium oxide (Y 2 O 3 ) or thorium oxide (ThO 2 ).
  • tungsten filaments 13, 22 are provided.
  • the tungsten filaments have a very low service life at low pressure of the order of 10 -1 Pascal, compared to yttriated iridium filaments.
  • yttria iridium filaments have better resistance to air entrances.
  • the filaments 13, 22 are for example fixed at their ends 24 in a respective support 25 ceramic.
  • Each ceramic support 25 is mounted in the ionisation cell 9 of the spectrometer 2, so that the filaments 13, 22 are arranged opposite their respective inlet slot of the ionization cage. 10.
  • the second inlet slot 26 is disposed on one face of the ionization cage, outside a frontal region F of the ionization cage 10 situated opposite the first inlet slot 11.
  • frontal region F corresponds to the projection on the opposite face of the surface of the entrance slot 11 along the normal to the plane containing it.
  • the second emergency filament 22 is arranged facing the second entrance slot 26, and therefore in a peripheral region distinct from the frontal region F situated opposite the first entrance slot 11.
  • the second entrance slot 26 is for example disposed in a peripheral region defined by a perimeter P away from a distance of at least one millimeter around the perimeter of the frontal region F located opposite the the first input slot 11 (see for example the figure 3 ).
  • the emergency filament 22 is not altered by the first working filament 13.
  • the time required for the tilting of filament is thus significantly reduced because the interactions between the first working filament and the second emergency filament are reduced.
  • each entrance slot 11, 26 are designed according to the disposition of the deflection and selection means. Taking the example of realization of the mass spectrometer of the figure 2 the longitudinal axes L and L 'of the first and second inlet slots 11, 26 are substantially parallel to each other and parallel to an edge of the ionization cage 10.
  • the horizontal plane (X, Y) is defined by the plane containing the exit slot 15.
  • the first and second input slots 11, 26 are for example arranged on opposite faces 27, 28 of the ionization cage 10. There is then sufficient space on either side of the ionization cage For arranging the filaments 13, 22 and their respective supports 25.
  • FIGS. 2 to 4 illustrate a first embodiment in which the first and second ends of the first and second entrance slots 11, 26 are contained in two planes respectively parallel to each other and parallel to a lateral face 28 of the ionization cage 10.
  • the second emergency filament 22 is disposed in a peripheral region situated below a frontal region F situated opposite the first entrance slot 11.
  • This example is better visible on the figure 3 where one distinguishes the second entry slot 26 in dashed lines on an opposite face 28 of the ionization cage 10, shifted below the frontal region F , located opposite the first entry slot 11 .
  • the figure 5 illustrates a second embodiment of the ionization cage 10.
  • the longitudinal axes L and L 'of the first and second input slots 11, 26 are substantially parallel to each other, and parallel at a horizontal edge of the ionization cage 10.
  • the first and second inlet slots 11, 26 are disposed on opposite side faces 27, 28 of the ionization cage 10.
  • the first and second entry slots 11, 26 define a plane substantially parallel to the plane defined by the side 16 of the ionization cage 10, containing the exit slot 15 for the passage of the particles. ionized.
  • the figure 6 illustrates a third embodiment similar to the two previous examples, for which the peripheral region containing the second input slot 26 is shifted from the front region F , both along an axis Y parallel to the longitudinal axis L of the first inlet slot 11 and along an axis Z perpendicular to the longitudinal axis L of the first inlet slot 11.
  • the second inlet slit 26 is disposed on the opposite face 28 and is offset both horizontally along the horizontal axis Y and vertically along the vertical axis Z , of the frontal region F located opposite the the first entrance slot 11.
  • the first and second inlet slits 11, 26 are arranged on the same face 27 of the ionization cage 10.
  • the figure 8 thus illustrates a fifth embodiment for which the longitudinal axes L and L ' of the input slots 11, 26 are respectively parallel to the vertical axis Z.
  • the inlet slots 11, 26 may be arranged on opposite faces 27, 28 of the ionization cage 10.
  • the first and second ends of the first and the second inlet slots 11, 26 are for example contained in two plans respectively parallel to each other.
  • the ionisation cell 9 thus makes it possible to shift the second emergency filament 22 from the frontal region F in which interactions can take place, so that the waiting time required for the tilting of the first working filament 13 to fail at the second emergency filament 22 is reduced.

Landscapes

  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)
  • Examining Or Testing Airtightness (AREA)
EP10714937.9A 2009-03-11 2010-03-10 Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant Active EP2406811B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0901114A FR2943173B1 (fr) 2009-03-11 2009-03-11 Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant
PCT/FR2010/050407 WO2010103235A1 (fr) 2009-03-11 2010-03-10 Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant

Publications (2)

Publication Number Publication Date
EP2406811A1 EP2406811A1 (fr) 2012-01-18
EP2406811B1 true EP2406811B1 (fr) 2017-11-08

Family

ID=41066492

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10714937.9A Active EP2406811B1 (fr) 2009-03-11 2010-03-10 Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant

Country Status (6)

Country Link
US (1) US8803104B2 (zh)
EP (1) EP2406811B1 (zh)
JP (1) JP5289589B2 (zh)
CN (1) CN102439686B (zh)
FR (1) FR2943173B1 (zh)
WO (1) WO2010103235A1 (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9666422B2 (en) 2013-08-30 2017-05-30 Atonarp Inc. Analyzer
JP6320197B2 (ja) * 2014-06-26 2018-05-09 ヤマハファインテック株式会社 イオン発生装置およびガス分析器

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1516614A (fr) * 1966-03-23 1968-03-08 Varian Associates Source d'ions à deux filaments pour spectromètre de masse
GB1338213A (en) * 1971-06-18 1973-11-21 Scient Research Instr Corp Dual mode chemical or electron impact ionization source for mass spectrometer
JPS5719949A (en) * 1980-07-09 1982-02-02 Hitachi Ltd Dual filament ion source
JP2943226B2 (ja) * 1990-03-29 1999-08-30 株式会社島津製作所 ガスクロマトグラフ質量分析計のイオン源
JPH07169427A (ja) * 1993-12-14 1995-07-04 Nissin Electric Co Ltd イオン源装置
US5600136A (en) * 1995-06-07 1997-02-04 Varian Associates, Inc. Single potential ion source
US6629508B2 (en) * 1999-12-10 2003-10-07 Epion Corporation Ionizer for gas cluster ion beam formation
US6686595B2 (en) * 2002-06-26 2004-02-03 Semequip Inc. Electron impact ion source
KR100505040B1 (ko) * 2003-12-19 2005-07-29 삼성전자주식회사 이온 소스 및 이를 갖는 이온 주입 장치
US6974957B2 (en) * 2004-02-18 2005-12-13 Nanomat, Inc. Ionization device for aerosol mass spectrometer and method of ionization
EP1807859A2 (en) * 2004-10-25 2007-07-18 TEL Epion Inc. Ionizer and method for gas-cluster ion-beam formation
US7459677B2 (en) * 2006-02-15 2008-12-02 Varian, Inc. Mass spectrometer for trace gas leak detection with suppression of undesired ions
US7427751B2 (en) * 2006-02-15 2008-09-23 Varian, Inc. High sensitivity slitless ion source mass spectrometer for trace gas leak detection

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
WO2010103235A1 (fr) 2010-09-16
JP5289589B2 (ja) 2013-09-11
US20110315875A1 (en) 2011-12-29
CN102439686A (zh) 2012-05-02
US8803104B2 (en) 2014-08-12
FR2943173B1 (fr) 2016-03-18
FR2943173A1 (fr) 2010-09-17
CN102439686B (zh) 2015-04-08
JP2012520542A (ja) 2012-09-06
WO2010103235A9 (fr) 2010-11-18
EP2406811A1 (fr) 2012-01-18

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