EP0104973B1 - Vorrichtung zur Ionisierung eines Materials durch Hochtemperaturheizung - Google Patents

Vorrichtung zur Ionisierung eines Materials durch Hochtemperaturheizung Download PDF

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Publication number
EP0104973B1
EP0104973B1 EP83401692A EP83401692A EP0104973B1 EP 0104973 B1 EP0104973 B1 EP 0104973B1 EP 83401692 A EP83401692 A EP 83401692A EP 83401692 A EP83401692 A EP 83401692A EP 0104973 B1 EP0104973 B1 EP 0104973B1
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EP
European Patent Office
Prior art keywords
tube
rod
temperature
heating
ionization
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP83401692A
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English (en)
French (fr)
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EP0104973A1 (de
Inventor
Yves Boulin
Jean Cesario
Bernard Landeau
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.)
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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Publication of EP0104973A1 publication Critical patent/EP0104973A1/de
Application granted granted Critical
Publication of EP0104973B1 publication Critical patent/EP0104973B1/de
Expired legal-status Critical Current

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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
    • H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission

Definitions

  • the present invention relates to a device for ionizing a material by heating this material to an elevated temperature.
  • Such an ionization device is used in particular in mass spectrometers used to measure the isotopic abundance ratios in a given chemical element.
  • mass spectrometers used to measure the isotopic abundance ratios in a given chemical element.
  • geochronology uses these spectrometers to measure the isotopic abundance ratios in a given chemical element.
  • the hot metallic surface In order to increase the yield, the hot metallic surface must therefore be made of a material having both a high working function W and a very high melting point.
  • a refractory metal is chosen from the group comprising rhenium, tungsten and tantalum.
  • the working function W of these metals being between 4.2 V and 5.1 V, it is therefore necessary to heat the metal surface as much as possible when the material to be ionized has an ionization potential greater than these values.
  • devices for ionizing solid materials using the principle of thermionization generally comprise three tungsten or rhenium ribbons (or filaments) carried by conductive rods passing through an insulating support plate.
  • the material to be ionized is deposited on one of the ribbons which, with a ribbon opposite, serves to vaporize the material.
  • the third ribbon, which forms a U with the first two, provides the ionization proper.
  • the three ribbons are heated by the Joule effect to a maximum temperature of 2,500 ° C.
  • the deposition of the material is very difficult to carry out, given the very reduced sizing, in particular to prevent part of the material from being deposited on the other ribbons.
  • the ribbons must be manually welded to the rods which support them, which results in poor reproducibility and a high cost price.
  • the geometrical arrangement of the filaments is such that a small part of the atoms formed collides with the intermediate filament ensuring ionization.
  • the ionization efficiency of this device is therefore rather poor.
  • Document US-A-3 229 157 discloses an ionization device in which the material to be ionized is placed in a cavity extended by a tube in which a temperature gradient is established.
  • the present invention specifically relates to a device for ionizing a material by heating at high temperature which does not have the drawbacks of known devices and which is characterized both by a high ionic yield, the production of an ion current intense for a reasonable period and great simplicity of placing the material to be ionized.
  • a device for ionizing a solid material comprising a tube open at its two ends and means for heating a first end of the tube at a temperature allowing the ionization of said material, the second end of the tube being maintained at a lower temperature, so as to create a temperature gradient between said ends of the tube,
  • this device being characterized in that it comprises furthermore a movable rod at one end of which said material is deposited and means for introducing the end of the rod carrying said material through the second end of the tube and for moving said rod in a controlled manner inside the tube, so to control the ion current emitted by the device.
  • the means for moving the rod inside the tube may in particular comprise a screw-nut assembly, one of the elements of which is fixed and the other of which is integral with the rod.
  • the solid material can be easily deposited at the end of the rod. either by electrodeposition on a point formed at this end, or by fixing the material on a ball of ion-exchange resin housed in a closed recess at the end of the rod, or by any other means.
  • the means for heating the first end of the tube preferably comprise an electronic bombardment device comprising a turn surrounding the first end of the tube, means for supplying power to the turn and means for applying a potential difference between the turn and the tube.
  • the latter is preferably mounted by its unheated end on a fixed interchangeable plate of conductive material.
  • Figure 1 there is shown very schematically a possible application of the invention to a mass spectrometer 10 for measuring the isotopic abundance ratios in a given chemical element.
  • the invention can be used in all cases where it is desired to have an ionization device by high temperature heating with a high yield, whatever the use. ions (bombardment of another material, for example).
  • the ionization device 12 constitutes a source of ions 14 accelerated and focused by successive electrodes 16, in the usual way, before coming to pass through the sorting device and measuring ions 18, also well known.
  • the ionization device 12 firstly comprises a rectilinear ionization tube 20, open at its two ends, and which can be produced, for the reasons mentioned above , in any material sufficiently electrically conductive and having a high working function in the ionization zone and, for example, in a refractory metal such as rhenium, tungsten or tantalum.
  • This tube 20 is embedded by its left end by considering FIG. 2 in a wafer or patch 22 made of a material which is a good conductor of electricity and heat, such as stainless steel.
  • This plate facilitates the handling of the tube and serves as a thermal flywheel, so as to maintain the corresponding end of the tube at a temperature of a few hundred degrees Celsius.
  • the tube 20 is heated to a very high temperature, slightly lower than the melting temperature of the tube (that is to say of the order of 3000 ° C), by suitable heating means 24. From this local heating, a thermal gradient is created along the tube 20, the heat escaping both by radiation around the tube and by conduction along the tube and the brochure. If necessary, this thermal gradient can be accentuated by cooling the left end of the tube by considering figure 2.
  • the heating means 24 are constituted by an electronic bombardment device comprising a turn 26 surrounding the tube 20 near its straight end, terminals 28 electrically connected to the turn 26 and making it possible to heat the turn by means of a power supply (not shown) and means (not shown) for establishing a high potential difference between the coil 26 and the tube 20.
  • the electronic current emitted by the coil can be 60 mA and the potential difference between the turn and the tube of 1000 V. We then obtain a power of 60 Watts allowing to heat at 3000 ° C the end of the tube.
  • a shield represented schematically at 30 is preferably provided around the tube 20 and the turn 26.
  • This shield can take, for example, the form of two half-shells.
  • the zone in which the heating takes place by the coil 26 must be located as close as possible to this end in order to increase the probability that the ions formed exit the tube, that is to say the ionic yield of the device.
  • the tube will be heated to less than 1.5 to 2 mm from its end.
  • the device further comprises a straight cylindrical rod 32, arranged coaxially with the tube 20 and whose external diameter is slightly less than the internal diameter of the tube.
  • the diameter of the rod 32 can be 1 mm if the internal diameter of the tube 20 is 1.2 mm.
  • the material of the rod must be very pure, refractory, chemically inert and preferably electrically conductive in order to allow the electrodeposition of the material to be ionized.
  • it may be graphite, tantalum or ceramics rendered, if necessary, superficially conductive.
  • the rod 32 can be translated along its axis so as to be introduced by the cold end (left end in FIG. 2) inside the tube. To this end, the rod 32 is carried by a micrometric screw 34 screwed into a nut 36 fixedly connected to a part 38 carrying the tube 20 by columns 40.
  • the screw 34 includes a slotted head 34a making it possible to carry out the controlled introduction of the rod 32 into the tube 20 by means of an insulating tool sealingly passing through the vacuum enclosure containing the source.
  • this introduction can be done automatically, for example using a stepping motor controlled by a processor.
  • the sample of solid material to be ionized 42 is deposited at the end by which the rod enters the tube (right end in FIG. 2).
  • the end of the rod has a pointed shape in the variant embodiment shown.
  • This shape makes it possible to proceed in a simple, rapid and perfectly controlled manner to an electrodeposition of the material 42, as shown in FIG. 3.
  • a solution 46 of the material that one wishes to deposit on the end of the rod 32 and to pass a current by means of a source 45 between the tank and the rod.
  • It may especially be a nitric solution of the material to be ionized. Soak to a perfectly controlled depth the pointed end 32a of the rod in the solution 46 and electrolysis is carried out.
  • a deposit 42 of the material to be ionized is thus obtained. In a known manner, this deposit will transform into oxide as soon as it is brought to a temperature of a few hundred degrees Celsius inside the tube 20.
  • the material to be ionized can be fixed on a ball of ion exchange resin.
  • the end of the rod 32 then has a different shape which is characterized by a recess, for example of conical shape, in which the resin ball is deposited on which the material to be ionized is fixed.
  • the device according to the invention allows the deposition of the material to be ionized to be carried out without difficulty, which constitutes significant progress compared with known devices.
  • the plate 22 is detachably fixed on a support 48, in order to allow the replacement of the tube 20-plate assembly 22 after manipulation, if necessary.
  • This characteristic makes it possible in particular to avoid any risk of disturbance of a manipulation by the previous one.
  • the support 48 also made of an electrically conductive material, is fixed to the part 38 by screws 52.
  • the turn 26, the shield 30 and the terminals 28 are mounted in an insulating part 50 held by the part 48.
  • the fixed part 38 made of stainless steel, has a part 38a which covers the insulating part 50.
  • This part 38a is provided with a hole 54 in the extension of the straight end of the tube through which the ions exit. Part 38a thus constitutes the first electrode of the acceleration device 16 of FIG. 1.
  • a sample of the material is first deposited on the end of the rod 32 by one of the methods described above and the rod is mounted on the screw 34. After having introduced this assembly as well as, if necessary, a tube 20 mounted on its plate 22, there is a vacuum in the enclosure.
  • the opposite end of the tube 20 is heated by means of the electronic bombardment device 24.
  • This heating is carried out initially weakly so that the degassing of the walls of the tube can be made, then at full power, the right end of the tube 20 considering Figure 2 then being brought as we have seen to a temperature of about 3000 ° C (the temperature limit being only fixed by the tube melting temperature).
  • the tube 20 in fact constitutes a fourtubular along which a temperature gradient ranging from approximately 300 ° C. to approximately 3000 ° C. is then established.
  • the end of the rod carrying the sample is continued to be moved towards the hot end of the tube, until the formation of ions is detected by means of the device. 18 ( Figure 1).
  • the displacement of the rod being able to be perfectly controlled by the micrometric screw 34, or by any other equivalent means, it is possible to continue the progressive displacement of the sample until the ion current observed allows a suitable measurement to be made.
  • the rod 32 is then held in this position and the measurements are carried out in the usual way.
  • the device according to the invention it can be seen that the creation of a temperature gradient along the tube 20, combined with the controlled displacement of the solid sample inside the tube, makes it possible to achieve a perfectly controlled ionization of this sample.
  • the rod 32 forms a piston which practically closes the end of the tube opposite the normal outlet end of the ions, and that the location of the heating means 24 in the immediate vicinity of this outlet end increases the probability that an ion re-evaporated by the surface of the tube leaves by this end.
  • the intensity of the ion current and the ion yield are also improved.

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  • 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)
  • Electron Sources, Ion Sources (AREA)

Claims (7)

1. Vorrichtung zur Ionisierung eines festen Materials, enthaltend ein an seinen zwei Enden offenes Rohr (20) und eine Einrichtung (24) zum Erwärmen eines ersten Endes des Rohres auf eine Temperatur, die die lonisierung des genannten Materials erlaubt, wobei das zweite Ende des Rohres auf einer tieferen Temperatur gehalten wird, um einen Temperaturgradienten zwischen den genannten Enden des Rohres zu erzeugen, wobei die Vorrichtung dadurch gekennzeichnet ist, daß sie darüber hinaus einen beweglichen Stab (32) aufweist, an dessen einem Ende das genannte Material (42) niedergeschlagen ist, und Einrichtungen, um das Ende des Stabes, das das genannte Material enthält, durch das zweite Ende des Rohres einzuführen und um den genannten Stab im Innern des Rohres in gesteuerter Weise zu verschieben, um den von der Einrichtung abgegebenen lonenstrom zu beeinflussen.
2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, daß die Einrichtung zum Verschieben des Stabes im Innern des Rohres eine Schraube/Mutter-Anordnung (34, 36) enthält, von denen das eine (36) der Elemente feststehend ist und das andere (34) fest mit dem Stab verbunden ist.
3. Vorrichtung nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, daß das genannte Ende des Stabes eine Spitze (32a) aufweist, auf welcher das Material (42) durch Galvanostegie niedergeschlagen ist.
4. Vorrichtung nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, daß das genannte Ende des Stabes eine Aushöhlung aufweist, in welcher in Kügelchen aus ionenaustauschendem Harz angeordnet ist, das das genannte Material festhält.
5. Vorrichtung nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Erwärmungseinrichtung für das erste Ende des Rohres eine Vorrichtung (26, 28) zur elektronischen Bombardierung aufweist.
6. Vorrichtung nach Anspruch 5, dadurch gekennzeichnet, daß die Vorrichtung zur elektronischen Bombardierung eine Drahtwindung (26) ist, die das erste Ende des Rohres umgibt, und weiterhin Einrichtungen (28) zur elektrischen Versorgung der Drahtwindung und Einrichtungen zum Anlegen einer Potentialdifferenz zwischen die Drahtwindung und das Rohr aufweist.
7. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß das Rohr (20) an seinem zweiten Ende an einer festen, unbeweglichen Platte (22) aus leitfähigem Material befestigt ist.
EP83401692A 1982-08-30 1983-08-22 Vorrichtung zur Ionisierung eines Materials durch Hochtemperaturheizung Expired EP0104973B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8214774 1982-08-30
FR8214774A FR2532470A1 (fr) 1982-08-30 1982-08-30 Dispositif d'ionisation d'un materiau par chauffage a haute temperature

Publications (2)

Publication Number Publication Date
EP0104973A1 EP0104973A1 (de) 1984-04-04
EP0104973B1 true EP0104973B1 (de) 1987-05-27

Family

ID=9277108

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83401692A Expired EP0104973B1 (de) 1982-08-30 1983-08-22 Vorrichtung zur Ionisierung eines Materials durch Hochtemperaturheizung

Country Status (5)

Country Link
US (1) US4595835A (de)
EP (1) EP0104973B1 (de)
JP (1) JPS5963651A (de)
DE (1) DE3371836D1 (de)
FR (1) FR2532470A1 (de)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4783595A (en) * 1985-03-28 1988-11-08 The Trustees Of The Stevens Institute Of Technology Solid-state source of ions and atoms
US4833319A (en) * 1987-02-27 1989-05-23 Hughes Aircraft Company Carrier gas cluster source for thermally conditioned clusters
DE3739253A1 (de) * 1987-11-19 1989-06-01 Max Planck Gesellschaft Mit kontaktionisation arbeitende einrichtung zum erzeugen eines strahles beschleunigter ionen
FR2657723A1 (fr) * 1990-01-26 1991-08-02 Nermag Ste Nouvelle Spectrometre de masse a filtre quadripolaire et tiroir mobile d'acces a la source ionique.
US5220167A (en) * 1991-09-27 1993-06-15 Carnegie Institution Of Washington Multiple ion multiplier detector for use in a mass spectrometer
US6202870B1 (en) 1999-03-29 2001-03-20 Woodrow W. Pearce Venting cap
US20080083874A1 (en) * 2006-10-10 2008-04-10 Prest Harry F Vacuum interface for mass spectrometer

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2682611A (en) * 1953-01-29 1954-06-29 Atomic Energy Commission Ion source
US3229157A (en) * 1963-09-30 1966-01-11 Charles M Stevens Crucible surface ionization source
FR2045097A5 (en) * 1969-05-30 1971-02-26 Commissariat Energie Atomique Lithium ion source
DE2548891C3 (de) * 1975-10-31 1983-04-28 Finnigan MAT GmbH, 2800 Bremen Probenwechsler für Massenspektrometer
JPS583592B2 (ja) * 1978-09-08 1983-01-21 日本分光工業株式会社 質量分析計への試料導入方法及び装置

Also Published As

Publication number Publication date
JPS5963651A (ja) 1984-04-11
US4595835A (en) 1986-06-17
EP0104973A1 (de) 1984-04-04
FR2532470B1 (de) 1985-05-17
FR2532470A1 (fr) 1984-03-02
DE3371836D1 (en) 1987-07-02

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