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WO2002000959A1 - Cathodes destinees au depot cathodique d'alliages de getter et procede de fabrication de ces cathodes - Google Patents

Cathodes destinees au depot cathodique d'alliages de getter et procede de fabrication de ces cathodes Download PDF

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Publication number
WO2002000959A1
WO2002000959A1 PCT/IT2001/000332 IT0100332W WO0200959A1 WO 2002000959 A1 WO2002000959 A1 WO 2002000959A1 IT 0100332 W IT0100332 W IT 0100332W WO 0200959 A1 WO0200959 A1 WO 0200959A1
Authority
WO
WIPO (PCT)
Prior art keywords
alloy
cathode
getter
accordmg
zirconium
Prior art date
Application number
PCT/IT2001/000332
Other languages
English (en)
Inventor
Claudio Boffito
Luca Toia
Alessandro Gallitognotta
Original Assignee
Saes Getters S.P.A.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Saes Getters S.P.A. filed Critical Saes Getters S.P.A.
Priority to AU2001270998A priority Critical patent/AU2001270998A1/en
Publication of WO2002000959A1 publication Critical patent/WO2002000959A1/fr

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/09—Mixtures of metallic powders
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J7/00—Details not provided for in the preceding groups and common to two or more basic types of discharge tubes or lamps
    • H01J7/14—Means for obtaining or maintaining the desired pressure within the vessel
    • H01J7/18—Means for absorbing or adsorbing gas, e.g. by gettering
    • H01J7/183—Composition or manufacture of getters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to cathodes to be used in the cathodic deposition of getter alloys and to the process for the manufacture of these cathodes.
  • Getter materials are used for removing gases such as oxygen, hydrogen, water and carbon oxides in vacuum, in applications such as television and computer kinescopes, field emission-type flat displays (also known as FED), and metal or glass interspaces for thermal insulation. Getter materials can also be used for removing the above gases from other gases such as nitrogen or rare gases, for example in order to keep constant the composition of the working atmosphere of devices such as lamps (mainly fluorescent ones), plasma displays or microelectronic circuits. Getter materials can be pure metals, mainly zirconium, titanium, niobium, vanadium and tantalum; or alloys, mainly based on zirconium or titanium.
  • getter materials require the manufacture of miniaturized getter devices, and particularly of devices having low thickness, of the order of a few microns.
  • the miniaturized getter device can be produced separately and then inserted into the final device; it is mainly the case of getters inside the package of microelectronic circuits, or, for example, laser amplifiers for communications on optical fibers, h other applications the getter device must be produced simultaneously with other components of the final device, such as for example in some kind of FEDs, wherein "islands" of getter material are spread over the whole surface of the display and are exposed to the internal evacuated space; or in the ferroelectric memories of computers, wherein getter material deposits are "embedded” in the structure of the device for protecting the ferroelectric material (generally a ceramic) from the contact with hydrogen which in time would affect its functionality Particularly when the manufacture of the getter device has to be integrated with that of the final device, it is desirable to use the same techniques used for the manufacture of other components of the latter.
  • a vacuum chamber wherein it is possible to create an electric field is used in this technique.
  • a target having generally the shape of a short cylinder
  • the chamber is first evacuated and then backfilled with a noble gas atmosphere, generally argon, at a pressure in the range 10 "3 -10 "5 mbar.
  • a noble gas atmosphere generally argon
  • the species (generally atoms or "clusters" of atoms) derived from the erosion of the target are deposited on the support (as well as on the other available surfaces) thus forming the thin layer.
  • a magnetic field is applied to the plasma zone, which helps to confine the plasma itself and improves the features of erosion of the cathode and of deposit formation; this variant is defined in the field as "magnetron".
  • the deposit can cover the surface of the support completely, thus obtaining a single continuous deposit, or partially, obtaining deposits only on some zones of the support.
  • cathode Since the target is maintained at the cathodic potential, it is also indicated in the field as "cathode", name which will be used in the rest of the description.
  • the most commonly used cathodes have the shape of a disk, with diameter varying between about 2 and 30 cm and thickness varying between a few millimeters and about 20 cm, but in some applications also cathodes having other shapes (for example rectangular) and size are used.
  • Patent application EP-A-572170 describes a use of the technique for the production of getter metal deposits such as Zr or Ti in field emission displays.
  • Patent application EP-A-837502 describes the production of layers of hydrogen getters, formed of nickel, palladium, platinum or oxides thereof by cathodic deposition.
  • patent US 5,921,461 describes the production of getter material deposits to be used in the containers of microelectronic devices, indicating as preferred getter materials the metals tantalum, titanium or molybdenum.
  • the production of alloys by cathodic deposition can be carried out starting from several different cathodes, one for each component element of the alloy.
  • every metal has different features of erosion by the Ar + ions, it is difficult by this method to control the composition of the produced alloy. Therefore, it is certainly preferable to start from a single cathode.
  • the various methods that, in principle, could be used for producing a cathode of getter alloy have some drawbacks.
  • a first possibility is producing an ingot by castmg a melt having the composition of the desired alloy; however in most cases the cathode has then to be mechanically worked, in order to clean it from fusion slags or to adapt it to the size of the holder in the deposition chamber and, considering the fragility of the alloys, nearly all the cathodes break during these workings.
  • Another possibility is the production of an ingot by smterization of powders of getter alloy; however, the getter alloys are difficult to be sintered by compression and subsequent thermal treatment and cathodes prepared in this way have nearly always a low mechanical resistance and break easily during transport or mounting in the deposition chamber.
  • Object of the present invention is providing cathodes for the cathodic deposition of getter alloys, as well as a process for the manufacture thereof.
  • the first object is obtained according to the present invention by a cathode made of a composite material, formed of: - powders of a getter alloy; and - a cementing component formed of a titanium or zirconium alloy with at least one element selected among iron, cobalt, nickel and copper; wherein the weight of the getter alloy is between about 50% and 90% of the total weiglit of the cathode and wherein the cementing component has a melting point lower than that of the getter alloy.
  • - fig. 1 shows a cathode according to the present invention
  • - fig. 3 shows a step of the manufacture process of the cathodes according to the invention.
  • FIG 1 represents a cathode 10 according to the invention, shaped as a disk; this cathode can have the typical size that was said before.
  • Cathode 10 has a main surface 11, which is the one subjected to erosion during the deposition of the getter alloy layer.
  • Figure 2 shows h section an enlarged view of a portion of surface 11.
  • the cathodes according to the invention are made of a composite material, and are formed of granules 20 of a getter alloy as the major component, and of a cementing component 21 as the minor component.
  • the cementing component has the features of having in its turn a composition based on zirconium or titanium, thus similar to that of the getter alloys, and of having a melting point lower than the getter alloy and preferably lower than about 1000 °C. It has been found that the use of cementing components having compositions based on zirconium or titanium allows getter alloy deposits to be obtained that, although having a composition slightly different from that of the alloy which forms the cathode, have features of gas sorption which are essentially similar to the latter.
  • the getter alloy used in the cathodes of the invention can be any known getter alloy.
  • binary alloys based on zirconium or titanium with one or more other components selected among aluminum, transition elements or rare earths are used; examples of said alloys are the binary alloys zirconium- vanadium, zirconium-iron, zirconium-nickel, zirconium-aluminum, titanium-vanadium and titanium-nickel; the ternary alloys zirconium- vanadium-iron and zirconium- cobalt-rare earths; or alloys with more components.
  • the cementing component 21 is an alloy of titanium or zirconium with at least one element selected among iron, cobalt, nickel and copper.
  • the cementmg component must have the feature of being more low-melting than the getter alloy, and preferably its melting temperature is lower than about 1000 °C. Suitable for the purposes of the invention are the alloys:
  • Zr-Fe having a zirconium weight content between about 81.5 and 86%, and preferably of about 83%;
  • Zr-Co having a zirconium weight content between about 80 and 86%, and preferably of about 85%;
  • Zr-Ni having a zirconium weight content between about 81 and 84%, and preferably of about 83%
  • Zr-Cu having a zirconium weight content between about 8.5 and 15% or between about 43 and 80%, and preferably the alloy having zirconium weight content of about 53%
  • Ti-Fe having a titanium weight content of about 67%; Ti-Co having a titanium weight content of about 73%; Ti-Ni having a titanium weiglit content between about 62 and 74%, and preferably of about 72.5%;
  • Ti-Cu having a titanium weight content between about 8 and 56%, and preferably of about 21%. h case that the use of the cathode in the previously defined "magnetron" mode is foreseen, it can be preferable to use a cementing component based on copper and not containing the magnetic elements iron, cobalt or nickel, which could interfere with the process.
  • the weight of the getter alloy is between 50% and 90% of the total weight of the cathode. With contents of alloy higher than 90% there is too little cementing component, and the mechanical resistance of the catiiode decreases, while for contents of getter alloy lower than about 50% there is an excessive quantity of cementing component which can lead to a composition of the getter layer deposited sensibly different from that of the starting getter alloy.
  • the weight of the getter alloy in the cathode is comprised between about 70 and 85%.
  • the getter alloy is present in the cathode in powder with granules 20 having size comprised between about 50 and 200 ⁇ m, whereas the cementing component 21 forms a continuous matrix which binds the granules of the getter alloy.
  • the invention in a second aspect thereof relates to a process for the manufacture of the previously described cathodes.
  • the process will be described with reference to figure 3, which shows an important step thereof.
  • a mechanical mixture, 30, of powders 20 of the getter alloy and powders 31 of the cementing component is used as starting material of the process; in the drawing the size of the granules 20 of the alloy is increased for the sake of clarity.
  • the mixture 30 is introduced in a mould of suitable shape for the manufacture of the catiiode 10 and brought to a temperature higher than the melting temperature of the cementmg component but lower than the melting temperature of the getter alloy; in this operation the cementing component melts, thus forming a liquid that wets the granules of the getter alloy 20.
  • the assembly is allowed to cool and the cementmg component solidifies, thus forming a substantially cylindrical body formed of the matrix 21 which conglomerates the granules 20, which can form the cathode 10 itself or a precursor thereof.
  • the two components 20 and 31 are mixed in the weight ratio corresponding to the desired percentage of getter alloy in the final cathode.
  • the granules of getter alloy, 20, have the above cited particle size, while the granules of the cementing component, 31, have a size comprised between about 20 and 100 ⁇ m. It has been found that the use of a cementmg component in powder form having an average particle size lower than that of the getter alloy allows to obtain more homogeneous cathodes which have better mechanical properties.
  • the mould has been made in two portions, a cylindrical portion 32 and a base 32', easily separable at the end of the process; this structure favors the cathode extraction from the mould.
  • the walls of the container are made of a material which does not interact with the cementing component in the melted state; to this end it is possible to use graphite, refractories or metals such as for example molybdenum or iron, the latter being preferred for its low cost; alternatively, it is possible to use other materials, by coating the surfaces which will come into contact with the melt with a material which is inert with respect to it.
  • the melting step is carried out by placing the mould containing the mixture 30 in a vacuum oven, with a pressure during the operation lower than 10 "2 mbar. hi this way it is avoided the possibility that the getter alloy reacts with gases present in the working atmosphere, as well as the formation of cavities in the cathode due to gas bubbles.
  • the melting step it is also possible to cover the mixture 30 with a weight, having an external diameter equal to the internal diameter of the mould (this possibility is not shown in the drawing); this weight favors the achievement of a more planar and regular upper surface of the cylindrical body, protects the mixture from contact with traces of gases present in the melting oven and avoids the presence of residual porosity in the final product.
  • the weight is made by the same measures and materials used for the mould.
  • the cylindrical body itself extracted from the mould can form the cathode 10; this cathode has the advantage of being easily machinable, for example by turning, hi order to adapt it to the holder.
  • the body extracted from the mould can form a precursor of the cathodes of the invention; as a consequence of the machinability of the composite materials formed of granules of getter alloy in the cementmg matrix, a body having multiple height with respect to that of the desired cathode can be produced; this body can be subsequently divided into several parts, with cuts parallel to each other and perpendicular to the body axis, thus obtaining several equal cathodes from a single fusion.
  • the cathodes according to the invention can be used for the production by cathodic deposition of layers of getter alloys on the most different substrates, such as metals, semiconductors (among which mainly silicon), ceramics, glass and plastics. Moreover, these cathodes can be used in deposition processes which may imply the application of a magnetic field ("magnetron" mode) or not; in the first case, the use of cathodes with a cementing component based on copper is preferred.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Vessels, Lead-In Wires, Accessory Apparatuses For Cathode-Ray Tubes (AREA)

Abstract

L'invention concerne des cathodes composites destinées au dépôt cathodique d'alliages de getter, constituées de poudres d'un alliage de getter (20) dans une matrice d'un composant de liage (21). L'invention concerne également un procédé de fabrication desdites cathodes.
PCT/IT2001/000332 2000-06-28 2001-06-26 Cathodes destinees au depot cathodique d'alliages de getter et procede de fabrication de ces cathodes WO2002000959A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001270998A AU2001270998A1 (en) 2000-06-28 2001-06-26 Cathodes for cathodic deposition of getter alloys and a process for the manufacture thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITMI2000A001453 2000-06-28
IT2000MI001453A IT1318061B1 (it) 2000-06-28 2000-06-28 Catodi per deposizione catodica di leghe getter e processo per la loro produzione.

Publications (1)

Publication Number Publication Date
WO2002000959A1 true WO2002000959A1 (fr) 2002-01-03

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AU (1) AU2001270998A1 (fr)
IT (1) IT1318061B1 (fr)
WO (1) WO2002000959A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002089174A3 (fr) * 2001-05-01 2003-02-27 Koninkl Philips Electronics Nv Lampe a decharge
WO2002061168A3 (fr) * 2000-10-24 2003-03-13 Honeywell Int Inc Procedes de preparation de materiaux metalliques melanges a base de titane et a base de zirconium et cibles de pulverisation
WO2003044827A3 (fr) * 2001-11-12 2004-03-18 Getters Spa Cathode creuse a getter integre pour lampes a decharge et procedes de realisation correspondant
GB2523583A (en) * 2014-02-28 2015-09-02 Castings Technology Internat Ltd Forming a composite component
CN113136504A (zh) * 2021-04-24 2021-07-20 杨阳 吸气合金及其应用、吸气靶材及吸气薄膜
CN115185169A (zh) * 2022-09-07 2022-10-14 上海晶维材料科技有限公司 一种用于空间氢原子钟上具有抗粉化能力的吸附泵
EP4338866A1 (fr) * 2022-09-15 2024-03-20 Honeywell International Inc. Getter evaporable stabilisé pour une poigneabilité accrue

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB723306A (en) * 1949-03-17 1955-02-09 American Electro Metal Corp Method of manufacturing a titanium-rich alloy body
EP0837502A2 (fr) * 1996-10-15 1998-04-22 Texas Instruments Inc. Améliorations relatives au piégeage d'hydrogène
US6027986A (en) * 1994-12-02 2000-02-22 Saes Getters S.P.A. Process for producing high-porosity non-evaporable getter materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB723306A (en) * 1949-03-17 1955-02-09 American Electro Metal Corp Method of manufacturing a titanium-rich alloy body
US6027986A (en) * 1994-12-02 2000-02-22 Saes Getters S.P.A. Process for producing high-porosity non-evaporable getter materials
EP0837502A2 (fr) * 1996-10-15 1998-04-22 Texas Instruments Inc. Améliorations relatives au piégeage d'hydrogène

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6833058B1 (en) 2000-10-24 2004-12-21 Honeywell International Inc. Titanium-based and zirconium-based mixed materials and sputtering targets
WO2002061168A3 (fr) * 2000-10-24 2003-03-13 Honeywell Int Inc Procedes de preparation de materiaux metalliques melanges a base de titane et a base de zirconium et cibles de pulverisation
US6943497B2 (en) 2001-05-01 2005-09-13 Koninklijke Philips Electronics N.V. Discharge lamp provided with a getter
US6800998B2 (en) 2001-05-01 2004-10-05 Koninklijke Philips Electronics N.V. Discharge lamp provided with a getter
WO2002089174A3 (fr) * 2001-05-01 2003-02-27 Koninkl Philips Electronics Nv Lampe a decharge
WO2003044827A3 (fr) * 2001-11-12 2004-03-18 Getters Spa Cathode creuse a getter integre pour lampes a decharge et procedes de realisation correspondant
US6916223B2 (en) 2001-11-12 2005-07-12 Saes Getters S.P.A. Discharge lamps using hollow cathodes with integrated getters and methods for manufacturing same
GB2523583A (en) * 2014-02-28 2015-09-02 Castings Technology Internat Ltd Forming a composite component
GB2523583B (en) * 2014-02-28 2016-09-14 Castings Tech Int Ltd Forming a composite component
CN113136504A (zh) * 2021-04-24 2021-07-20 杨阳 吸气合金及其应用、吸气靶材及吸气薄膜
CN115185169A (zh) * 2022-09-07 2022-10-14 上海晶维材料科技有限公司 一种用于空间氢原子钟上具有抗粉化能力的吸附泵
EP4338866A1 (fr) * 2022-09-15 2024-03-20 Honeywell International Inc. Getter evaporable stabilisé pour une poigneabilité accrue
US12281896B2 (en) 2022-09-15 2025-04-22 Honeywell International Inc. Stabilized evaporable getter for increased handleability

Also Published As

Publication number Publication date
AU2001270998A1 (en) 2002-01-08
ITMI20001453A0 (it) 2000-06-28
IT1318061B1 (it) 2003-07-21
ITMI20001453A1 (it) 2001-12-28

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