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WO2008151602A1 - Liquid metal ion source for generating lithium ion beams - Google Patents

Liquid metal ion source for generating lithium ion beams Download PDF

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Publication number
WO2008151602A1
WO2008151602A1 PCT/DE2008/000929 DE2008000929W WO2008151602A1 WO 2008151602 A1 WO2008151602 A1 WO 2008151602A1 DE 2008000929 W DE2008000929 W DE 2008000929W WO 2008151602 A1 WO2008151602 A1 WO 2008151602A1
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Prior art keywords
liquid metal
metal ion
lithium
alloy
emitter
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.)
Ceased
Application number
PCT/DE2008/000929
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German (de)
French (fr)
Inventor
Lothar Bischoff
Shavkat Akhmadaliev
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.)
Helmholtz Zentrum Dresden Rossendorf eV
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Helmholtz Zentrum Dresden Rossendorf eV
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Application filed by Helmholtz Zentrum Dresden Rossendorf eV filed Critical Helmholtz Zentrum Dresden Rossendorf eV
Publication of WO2008151602A1 publication Critical patent/WO2008151602A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J27/00—Ion beam tubes
    • H01J27/02—Ion sources; Ion guns
    • H01J27/26—Ion sources; Ion guns using surface ionisation, e.g. field effect ion sources, thermionic ion sources
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C12/00—Alloys based on antimony or bismuth
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00

Definitions

  • the invention relates to a liquid metal ion source (LMIS) for producing lithium ion beams, in particular the emitter-wetting source material of such an ion source.
  • LMIS liquid metal ion source
  • Liquid metal ion sources are special ion sources, which have a very high directional radiation value compared to other types of ion sources, and which are used in ion microbeams because of this property. These systems enable ion beams to focus less than one micron in diameter and are gaining in importance for ion beam exposure, ion beam milling, microdoping, and sub-micron surface analysis.
  • Lithium is the lightest metal in the periodic table, which is suitable for liquid metal ion sources and can be advantageously used in ion lithography and ion beam analysis. Because of the strong chemical reactivity, it is difficult to handle in sources and operate long-term stable. Other solutions did not lead to an acceptable use.
  • Liquid metal ion sources are available in [P.D. Prewett and G.L.R. Mair, Focused: Ion Beams from Liquid Metal Ion Sources. Research Studies Press Ltd. 1991]. In them, a fine tip made of tungsten, tantalum, carbon or other suitable material serves as an emitter, which is connected to the
  • Source material is wetted. To be able to wet the emitter and during the
  • the source material must be liquid.
  • an electrical resistance heater or an electron beam heater is used.
  • Source material forms and emitted from these ions. In this way it is possible to create a long-term stable ion beam of the elements of the
  • the source material has to be special possess physical and chemical properties. Of particular importance is that the source material is metallic, has a low melting point, is not too high in vapor pressure, is well wetted by the emitter, and is chemically compatible with the emitter material. Therefore, only a few elements, such as indium, gallium and gold are suitable as source material.
  • An effective method to overcome this difficulty and to produce ions of other elements is to use suitable alloys as the source material. It then creates an ion current from all elements contained in the alloy. By means of a subsequent mass separation, the desired type of ion can be separated. The use of lithium is not mentioned, an ion current from all elements contained in the alloy either unwanted or associated with other problems.
  • a liquid metal ion source for producing cobalt ion beams is already known, in which an alloy of the cobalt with elements from the group of the rare earths is used (DE 43 12 028 A1). The principle of this technical solution can not be transferred to a lithium-ion source.
  • the invention has for its object to provide a liquid metal ion source, which ensures a long-term stable operation with sufficiently high emission of the element lithium by equipping with a new lithium source material, in particular an alloy with a sufficiently high proportion of the element lithium.
  • liquid metal ion sources whose emitter is wetted with the defined in the claims alloys as source material.
  • Melting point mean that no chemical reactions occur with the emitter and heater material.
  • the use of the alloying elements is advantageous because thereby the alloy has a low vapor pressure in the temperature range of the melting point. Thus, only a small portion of the source material is vaporized. Both of these facts guarantee a long service life of the liquid metal ion source.
  • Another advantage of the solution according to the invention is the favorable physical properties of the alloy in the liquid phase.
  • the alloy wets the emitter needle easily and completely, there is a sufficient supply of source material from the reservoir to the emitter tip, and a drop of the alloy, which can serve as a reservoir, adheres well and stably to the heater and emitter.
  • the alloy is characterized by a very low corrosion in air.
  • a tungsten emitter is prepared by a known standard method and wetted with the Ga 35 Bi 6 oLi 5 (at.%) Alloy.
  • the emitter is placed in an ion source and examined in an assay booth.
  • the operating temperature is about 300 0 C 1, the heating current about 2.4 A, the emission current 2 ⁇ A.
  • the lithium is separated into the two isotopes (93% 7 Li, 7% 6 Li).
  • the proportions of the ions Bi, Ga, Li in the total current are a function of the emission current and the state of charge.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Electron Sources, Ion Sources (AREA)

Abstract

The invention relates to a liquid metal ion source (LMIS), for generating lithium ion beams, in particular, the source material wetting the emitter of such an ion source. The invention includes liquid metal ion sources the emitter o which is wetted with a particular alloy of lithium and one or more elements gallium, indium and bismuth as source material. It is possible with liquid metal ion sources of this type to obtain a long lasting stable ion stream made up to an adequate degree of lithium ions. The components of the alloy in combination with the low melting point bring it about that no chemical reactions with the emitter and heater material occur and that the alloy surface corrodes relatively slowly in air.

Description

Flüssigmetall-Ionenquelle zur Erzeugung von Lithium-Ionenstrahlen Liquid metal ion source for generating lithium-ion beams

Die Erfindung betrifft eine Flüssigmetall-Ionenquelle (LMIS) zur Erzeugung von Lithiumionenstrahlen, insbesondere das den Emitter benetzende Quellenmaterial einer derartigen lonenquelle.The invention relates to a liquid metal ion source (LMIS) for producing lithium ion beams, in particular the emitter-wetting source material of such an ion source.

Flüssigmetali-Ionenquellen sind spezielle lonenquellen, die gegenüber anderen Typen von lonenquellen einen sehr hohen Richtstrahlwert besitzen, und die auf Grund dieser Eigenschaft in lonenmikrostrahlanlagen Verwendung finden. Diese Anlagen ermöglichen es, lonenstrahlen auf weniger als einem Mikrometer Durchmesser zu fokussieren, und sie erlangen zunehmende Bedeutung für die lonenstrahlbelichtung, lonenstrahlfräsen, Mikrodotierung und Oberflächenanalyse im Submikrometerbereich.Liquid metal ion sources are special ion sources, which have a very high directional radiation value compared to other types of ion sources, and which are used in ion microbeams because of this property. These systems enable ion beams to focus less than one micron in diameter and are gaining in importance for ion beam exposure, ion beam milling, microdoping, and sub-micron surface analysis.

Lithium ist das leichteste Metall im Periodensystem, das für Flüssigmetall- lonenquellen geeignet ist und vorteilhaft in der lonenlithographie und der lonenstrahl-Analytik eingesetzt werden kann. Wegen der starken chemischen Reaktivität lässt es sich nur schwierig in Quellen handhaben und langzeitstabil betreiben. Auch andere Lösungsansätze führten nicht zu einem akzeptablen Einsatz.Lithium is the lightest metal in the periodic table, which is suitable for liquid metal ion sources and can be advantageously used in ion lithography and ion beam analysis. Because of the strong chemical reactivity, it is difficult to handle in sources and operate long-term stable. Other solutions did not lead to an acceptable use.

Flüssigmetall-Ionenquellen sind in [P.D. Prewett and G.L.R. Mair, Focused: Ion Beams from Liquid Metal Ion Sources. Research Studies Press Ltd. 1991] ausführlich beschrieben. In ihnen dient eine aus Wolfram, Tantal, Kohlenstoff oder anderem geeigneten Material hergestellte feine Spitze als Emitter, der mit demLiquid metal ion sources are available in [P.D. Prewett and G.L.R. Mair, Focused: Ion Beams from Liquid Metal Ion Sources. Research Studies Press Ltd. 1991]. In them, a fine tip made of tungsten, tantalum, carbon or other suitable material serves as an emitter, which is connected to the

Quellenmaterial benetzt ist. Um den Emitter benetzen zu können und während desSource material is wetted. To be able to wet the emitter and during the

Betriebs der lonenquelle muss das Quellenmaterial flüssig sein. Dazu wird eine elektrische Widerstandsheizung oder eine Elektronenstrahlheizung verwendet.Operation of the ion source, the source material must be liquid. For this purpose, an electrical resistance heater or an electron beam heater is used.

Zwischen einer Gegenelektrode und der Emitterspitze wird eine elektrischeBetween a counter electrode and the emitter tip is an electrical

Spannung angelegt. Die hohe elektrische Feldstärke an der Emitterspitze führt dazu, dass sich an dieser eine noch feinere Spitze aus dem flüssigenVoltage applied. The high electric field strength at the emitter tip causes this at an even finer peak from the liquid

Quellenmaterial bildet und aus dieser Ionen emittiert werden. Auf diese Weise ist es möglich, einen auf lange Zeit stabilen lonenstrahl der Elemente desSource material forms and emitted from these ions. In this way it is possible to create a long-term stable ion beam of the elements of the

Quellenmaterials zu erzeugen. Das Quellenmaterial muss dazu spezielle physikalische und chemische Eigenschaften besitzen. Von besonderer Wichtigkeit ist, dass sich das Quellenmaterial metallisch verhält, einen niedrigen Schmelzpunkt besitzt, sein Dampfdruck nicht zu hoch ist, den Emitter gut benetzt und mit dem Emittermaterial chemisch verträglich ist. Daher sind nur wenige Elemente, z.B. Indium, Gallium und Gold als Quellenmaterial geeignet. Ein wirkungsvolles Verfahren um diese Schwierigkeit zu überwinden und Ionen anderer Elemente erzeugen zu können, besteht in der Verwendung geeigneter Legierungen als Quellenmaterial. Es entsteht dann ein lonenstrom aus allen in der Legierung enthaltenen Elementen. Mittels einer nachfolgenden Massenseparation kann die gewünschte lonensorte abgetrennt werden. Die Verwendung von Lithium ist nicht erwähnt, ein lonenstrom aus allen in der Legierung enthaltenen Elementen entweder nicht gewünscht oder mit weiteren Problemen verbunden.To generate source material. The source material has to be special possess physical and chemical properties. Of particular importance is that the source material is metallic, has a low melting point, is not too high in vapor pressure, is well wetted by the emitter, and is chemically compatible with the emitter material. Therefore, only a few elements, such as indium, gallium and gold are suitable as source material. An effective method to overcome this difficulty and to produce ions of other elements is to use suitable alloys as the source material. It then creates an ion current from all elements contained in the alloy. By means of a subsequent mass separation, the desired type of ion can be separated. The use of lithium is not mentioned, an ion current from all elements contained in the alloy either unwanted or associated with other problems.

Es ist bereits eine Flüssigmetall-Ionenquelle zur Erzeugung von Kobalt- Ionenstrahlen bekannt, bei der eine Legierung des Kobalts mit Elementen aus der Gruppe der Seltenen Erden eingesetzt wird (DE 43 12 028 A1). Das Prinzip dieser technischen Lösung lässt sich für eine Lithium-Ionenquelle nicht übertragen.A liquid metal ion source for producing cobalt ion beams is already known, in which an alloy of the cobalt with elements from the group of the rare earths is used (DE 43 12 028 A1). The principle of this technical solution can not be transferred to a lithium-ion source.

Der Erfindung liegt die Aufgabe zugrunde, eine Flüssigmetall-Ionenquelle zu schaffen, die durch Ausstattung mit einem neuen Lithium-Quellenmaterial, insbesondere einer Legierung mit ausreichend hohem Anteil des Elements Lithium einen insgesamt langzeitig stabilen Betrieb mit ausreichend hoher Emission des Elements Lithium gewährleistet.The invention has for its object to provide a liquid metal ion source, which ensures a long-term stable operation with sufficiently high emission of the element lithium by equipping with a new lithium source material, in particular an alloy with a sufficiently high proportion of the element lithium.

Erfindungsgemäß wird die Aufgabe mit Flüssigmetall-Ionenquellen gelöst, deren Emitter mit den in den Patentansprüchen definierten Legierungen als Quellenmaterial benetzt ist.According to the invention the object is achieved with liquid metal ion sources whose emitter is wetted with the defined in the claims alloys as source material.

Mit derart ausgestatteten Flüssigmetall-Ionenquellen ist es möglich, langzeitig einen stabilen lonenstrom, der im ausreichenden Maße aus Lithiumionen besteht, zu erhalten.With such equipped liquid metal ion sources, it is possible to obtain a long-term stable ion current, which consists to a sufficient extent of lithium ions.

Die Bestandteile der Legierung im Zusammenspiel mit dem niedrigenThe components of the alloy in interaction with the low

Schmelzpunkt führen dazu, dass keine chemischen Reaktionen mit dem Emitter- und Heizermaterial auftreten. Die Verwendung der Legierungselemente ist vorteilhaft, da dadurch die Legierung im Temperaturbereich des Schmelzpunktes einen niedrigen Dampfdruck besitzt. Somit wird nur ein geringer Anteil des Quellenmaterials verdampft. Beide genannten Sachverhalte garantieren eine lange Lebensdauer der Flüssigmetall-Ionenquelle.Melting point mean that no chemical reactions occur with the emitter and heater material. The use of the alloying elements is advantageous because thereby the alloy has a low vapor pressure in the temperature range of the melting point. Thus, only a small portion of the source material is vaporized. Both of these facts guarantee a long service life of the liquid metal ion source.

Ein weiterer Vorteil der erfindungsgemäßen Lösung besteht in den günstigen physikalischen Eigenschaften der Legierung in der flüssigen Phase. Die Legierung benetzt die Emitternadel leicht und vollständig, es erfolgt ein ausreichender Nachfluss von Quellenmaterial aus dem Reservoir zur Emitterspitze, und ein Tropfen der Legierung, welcher als Reservoir dienen kann, haftet gut und stabil am Heizer und Emitter. Die Legierung zeichnet sich durch eine sehr geringe Korrosion an Luft aus.Another advantage of the solution according to the invention is the favorable physical properties of the alloy in the liquid phase. The alloy wets the emitter needle easily and completely, there is a sufficient supply of source material from the reservoir to the emitter tip, and a drop of the alloy, which can serve as a reservoir, adheres well and stably to the heater and emitter. The alloy is characterized by a very low corrosion in air.

Die Erfindung wird nachfolgend anhand eines Ausführungsbeispiels näher erläutert.The invention will be explained in more detail with reference to an embodiment.

Ein Wolframemitter wird nach einem bekannten Standardverfahren hergestellt und mit der Legierung aus Ga35Bi6oLi5 (at. %) benetzt. Der Emitter wird in eine lonenquelle eingesetzt und in einem Analyseteststand untersucht. Die Betriebstemperatur beträgt ca. 3000C1 der Heizstrom etwa 2.4 A, der Emissionsstrom 2 μA. Das Lithium ist aufgetrennt in die beiden Isotope (93% 7Li, 7% 6Li). Die Anteile der Ionen Bi, Ga, Li am Gesamtstrom sind eine Funktion des Emissionsstromes und des Ladungszustandes.A tungsten emitter is prepared by a known standard method and wetted with the Ga 35 Bi 6 oLi 5 (at.%) Alloy. The emitter is placed in an ion source and examined in an assay booth. The operating temperature is about 300 0 C 1, the heating current about 2.4 A, the emission current 2 μA. The lithium is separated into the two isotopes (93% 7 Li, 7% 6 Li). The proportions of the ions Bi, Ga, Li in the total current are a function of the emission current and the state of charge.

Für Li konnte durch die Massenabhängigkeit der Energiebreite von m1/3 des Projektilions ein Wert von nur 2 eV gefunden werden. Für reine Li-LMIS betrug dieser Parameter 4 eV durch die hohe Winkelintensität und der dadurch entstehenden Coulomb - Abstoßung. Im Falle der Legierungsquelle wird eine normale Winkelverteilung erwartet. Diese kleine Energiebreite gestattet auch kleinere Strahldurchmesser eines fokussierten lonenstrahls durch die verringerte chromatische Aberration. For Li, a value of only 2 eV could be found by the mass dependence of the energy width of m 1/3 of the projectile. For pure Li-LMIS this parameter was 4 eV due to the high angle intensity and the resulting Coulomb repulsion. In the case of the alloy source, a normal angular distribution is expected. This small energy width also allows smaller beam diameters of a focused ion beam due to the reduced chromatic aberration.

Claims

Patentansprüche claims 1. Flüssigmetall-Ionenquelle zur Erzeugung von Lithium-Ionenstrahlen, gekennzeichnet durch die Zusammensetzung des den Emitter benetzenden1. liquid metal ion source for generating lithium-ion beams, characterized by the composition of the emitter wetting Quellenmaterials als Legierung aus Lithium und einem oder mehreren der Elemente Gallium, Indium und Wismut.Source material as an alloy of lithium and one or more of the elements gallium, indium and bismuth. 2. Flüssigmetall-Ionenquelle nach Anspruch 1 , dadurch gekennzeichnet, dass die Legierung aus 5 bis 10 Atomprozent Lithium, 33 bis 43 Atomprozent Gallium und 56 bis 66 Atomprozent Wismut besteht.2. liquid metal ion source according to claim 1, characterized in that the alloy consists of 5 to 10 atomic percent lithium, 33 to 43 atomic percent gallium and 56 to 66 atomic percent bismuth. 3. Flüssigmetall-Ionenquelle nach Anspruch 1 , dadurch gekennzeichnet, dass die Legierung aus 5 bis 10 Atomprozent Lithium und 90 bis 95 Atomprozent Gallium besteht.3. liquid metal ion source according to claim 1, characterized in that the alloy consists of 5 to 10 atomic percent lithium and 90 to 95 atomic percent gallium. 4. Flüssigmetall-Ionenquelle nach Anspruch 1 , dadurch gekennzeichnet, dass die Legierung aus 5 bis 10 Atomprozent Lithium und 90 bis 95 Atomprozent4. liquid metal ion source according to claim 1, characterized in that the alloy of 5 to 10 atomic percent lithium and 90 to 95 atomic percent Indium besteht.Indium exists. 5. Flüssigmetall-Ionenquelle nach Anspruch 1, dadurch gekennzeichnet, dass die Legierung aus 5 bis 10 Atomprozent Lithium, 75 bis 80 Atomprozent Indium und 20 bis 25 Atomprozent Wismut besteht. 5. liquid metal ion source according to claim 1, characterized in that the alloy consists of 5 to 10 atomic percent lithium, 75 to 80 atomic percent indium and 20 to 25 atomic percent bismuth.
PCT/DE2008/000929 2007-06-12 2008-06-05 Liquid metal ion source for generating lithium ion beams Ceased WO2008151602A1 (en)

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DE200710027097 DE102007027097B4 (en) 2007-06-12 2007-06-12 Liquid metal ion source for generating lithium-ion beams
DE102007027097.8 2007-06-12

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Citations (3)

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US4088919A (en) * 1976-04-13 1978-05-09 United Kingdom Atomic Energy Authority Ion source including a pointed solid electrode and reservoir of liquid material
US4367429A (en) * 1980-11-03 1983-01-04 Hughes Aircraft Company Alloys for liquid metal ion sources
US4752692A (en) * 1985-04-26 1988-06-21 Hughes Aircraft Company Liquid metal ion source

Family Cites Families (2)

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Publication number Priority date Publication date Assignee Title
DE4312028A1 (en) 1993-04-13 1994-10-20 Rossendorf Forschzent Liquid metal ion source for generating cobalt ion beams
US7608178B2 (en) * 2003-11-10 2009-10-27 Polyplus Battery Company Active metal electrolyzer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4088919A (en) * 1976-04-13 1978-05-09 United Kingdom Atomic Energy Authority Ion source including a pointed solid electrode and reservoir of liquid material
US4367429A (en) * 1980-11-03 1983-01-04 Hughes Aircraft Company Alloys for liquid metal ion sources
US4752692A (en) * 1985-04-26 1988-06-21 Hughes Aircraft Company Liquid metal ion source

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
BELL A E ET AL: "Lithium ion emission from a liquid metal ion source of LiNO3", INTERNATIONAL JOURNAL OF MASS SPECTROMETRY AND ION PROCESSES NETHERLANDS, vol. 88, no. 1, 1 March 1989 (1989-03-01), pages 59 - 68, XP007906090, ISSN: 0168-1176 *
BISCHOFF I L ET AL: "An alloy liquid metal ion source for lithium", JOURNAL OF PHYSICS D: APPLIED PHYSICS IOP PUBLISHING LTD. UK, vol. 41, no. 5, 7 March 2008 (2008-03-07), pages 052001 - 1, XP007906083, ISSN: 0022-3727 *
MACKENZIE R A D ET AL: "BIBLIOGRAPHY; Focused ion beam technology: a bibliography", NANOTECHNOLOGY, IOP, BRISTOL, GB, vol. 1, no. 2, 1 October 1990 (1990-10-01), pages 163 - 201, XP020067444, ISSN: 0957-4484 *

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DE102007027097B4 (en) 2010-12-30

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