DE1067942B - Non-evaporating getter material made of titanium, zirconium, vanadium, niobium and possibly aluminum for electrical discharge vessels and processes for its production - Google Patents
Non-evaporating getter material made of titanium, zirconium, vanadium, niobium and possibly aluminum for electrical discharge vessels and processes for its productionInfo
- Publication number
- DE1067942B DE1067942B DENDAT1067942D DE1067942DA DE1067942B DE 1067942 B DE1067942 B DE 1067942B DE NDAT1067942 D DENDAT1067942 D DE NDAT1067942D DE 1067942D A DE1067942D A DE 1067942DA DE 1067942 B DE1067942 B DE 1067942B
- Authority
- DE
- Germany
- Prior art keywords
- getter material
- niobium
- material according
- vanadium
- titanium
- 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.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims description 13
- 238000001704 evaporation Methods 0.000 title claims description 11
- 229910052782 aluminium Inorganic materials 0.000 title claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims description 7
- 229910052758 niobium Inorganic materials 0.000 title claims description 7
- 239000010955 niobium Substances 0.000 title claims description 7
- 229910052720 vanadium Inorganic materials 0.000 title claims description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium(0) Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 5
- 239000010936 titanium Substances 0.000 title claims description 5
- 229910052719 titanium Inorganic materials 0.000 title claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims description 4
- 229910052726 zirconium Inorganic materials 0.000 title claims description 4
- 238000000034 method Methods 0.000 title description 4
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000005275 alloying Methods 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium(0) Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000004043 responsiveness Effects 0.000 description 3
- 229940023488 Pill Drugs 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N Zirconium(IV) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 239000006187 pill Substances 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- 229910052846 zircon Inorganic materials 0.000 description 2
- 229910000600 Ba alloy Inorganic materials 0.000 description 1
- 229910000636 Ce alloy Inorganic materials 0.000 description 1
- 206010040007 Sense of oppression Diseases 0.000 description 1
- 229910001264 Th alloy Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 238000011068 load Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- ZSLUVFAKFWKJRC-UHFFFAOYSA-N thorium Chemical compound [Th] ZSLUVFAKFWKJRC-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
Classifications
-
- 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
Description
Nicht verdampfender Getterstoff aus Titan, Zirkon, Vanadin, Niob und gegebenenfalls Aluminium für elektrische Entladungsgefäße und Verfahren zu seiner Herstellung Zur Verbesserung und Aufrechterhaltung des Vakuurns in elektrischen Entladungsgefäßen werden bekanntlich Gasfangstoffe (Letter) in das Gefäß eingebracht. Man unterscheidet bekanntlich zwischen verdampfenden und nicht verdampfenden Lettern.Non-evaporating getter material made of titanium, zircon, vanadium, niobium and possibly aluminum for electrical discharge vessels and processes for its Manufacture To improve and maintain the vacuum in electrical As is known, discharge vessels are introduced into the vessel by gas trapping substances (letter). As is well known, a distinction is made between evaporating and non-evaporating letters.
Bei einem Verdampfungsgetter wird ein in einem kleinen Behälter im Innern des Entladungsgefäßes eingebrachtes Reaktionsgemisch, z. B. eine Bariumlegierung, erhitzt. Dabei wird eine bestimmte Menge Barium verdampft, das sich auf der Gefäßwand niederschlägt.With an evaporation getter, an in a small container in the Reaction mixture introduced inside the discharge vessel, e.g. B. a barium alloy, heated. A certain amount of barium is evaporated, which is deposited on the vessel wall precipitates.
Mit einem meist aus Zirkon oder Thorium bestehenden, nicht verdampfenden Letter werden solche Teile des Entladungsgefäßes, z. B. Anode oder Gitter. die während des Betriebes eine hohe Temperatur über 450° C annehmen, versehen. Bei höheren Temperaturen sind die Letter zur Gasaufnahme geeignet. Durch geeignete Legierung von Cer, Thorium und Aluminium gelingt es. die Reaktionstemperatur bis auf etwa 300° C herabzusetzen.With a non-vaporizing one mostly consisting of zirconium or thorium Letter are those parts of the discharge vessel, e.g. B. anode or grid. the during of the plant assume a high temperature of over 450 ° C. At higher temperatures the letters are suitable for gas intake. By a suitable alloy of cerium, thorium and aluminum succeeds. reduce the reaction temperature to about 300 ° C.
Für die Getterung von kleinen, wenig belasteten Eletrottenröhren verbietet sich häufig die Anwendung von Verdampfungsgettern. Dies hat darin seinen Grund, daß durch das Kondensieren von Bariumdampf an unerwünschten Stellen zusätzlich Kapazitäten, Strombrücken und Emissionsbehinderungen der Kathode auftreten und daß die Austrittsarbeit gerade auf solchen Elektroden ungewollt erniedrigt wird, die z. B. zur Unterdrückung des Rückstromes bei Hochspannungsgleichrichtern eine hohe Austrittsarbeit besitzen müssen. Auch bei nicht verdampfenden Lettern liegt die Reaktionstemperatur zur sicheren Aufrechterhaltung des notwendigen Vakuums zu hoch, so daß das Gasbindungsvermögen des Getters bei den kleinen, im Betrieb kalt bleibenden Röhren nicht ausreicht.Prohibited for the gettering of small, lightly loaded electric tubes often the use of evaporation getters. This is because that through the condensation of barium vapor at undesired places additional capacities, Current bridges and emission restrictions of the cathode occur and that the work function is inadvertently lowered precisely on such electrodes that z. B. for oppression of the reverse current in high-voltage rectifiers have a high work function have to. Even with letters that do not evaporate, the reaction temperature is safe Maintaining the necessary vacuum too high, so that the gas binding capacity of the getter is not sufficient for the small tubes that remain cold during operation.
Aus diesen Gründen werden bei kleinen. wenig belasteten Elektronenröhren nicht verdampfende Letter angewendet. Zur Herstellung von Lettern dieser Art wird von den bekannten Gasbindern ausgegangen, deren gasbindender Bestandteil ganz oder vorwiegend aus Aluminium und aus einem oder .mehreren hochschmelzenden Metallen besteht, die nicht gasförmige Hydride bilden können. wie Titan, Zirkon. Niob und Vanadin.For these reasons, small. little stressed electron tubes non-evaporating letter applied. For the production of letters of this type started from the known gas binders, the gas-binding constituent wholly or mainly made of aluminum and one or more refractory metals exists that cannot form gaseous hydrides. like titanium, zircon. Niobium and Vanadium.
Ein nicht verdampfender Getterstoff, der bereits bei Zimmertemperatur oder niedrigeren Temperaturen wirksam ist, wird dadurch gewonnen, daß in dem nicht verdampfenden Getterstoff aus Titan, Zirkon, Vanadin, Niob und gegebenenfalls Aluminium, nach der Erfindung metallisches Vanadin und/oder Niob mit oder ohne Zusatz von Aluminium in einem Gewichtsverhältnis von 3 bis 25% vorhanden sind. Der Vorteil dieses Getters liegt besonders in der leichteren Herstellbarkeit und darin, daß der Getterstoff mit gasbindender Wirkung in solchen Röhren verwendet oder an solchen Stellen von Röhren angebracht werden kann, die im Betrieb kalt bleiben.A non-evaporating getter substance that is already available at room temperature or lower temperatures is effective, is achieved in that not evaporating getter material made of titanium, zirconium, vanadium, niobium and possibly aluminum, according to the invention, metallic vanadium and / or niobium with or without the addition of aluminum are present in a weight ratio of 3 to 25%. The advantage of this getter lies particularly in the ease of manufacture and in the fact that the getter material used with a gas-binding effect in such tubes or in such places of Tubes can be attached that remain cold during operation.
Die Mischung kann z. B. durch Zusammenbringen der Metalle in Pulverform erfolgen. Durch Behandlung bei erhöhter Temperatur kann die gewünschte Legierungsbildung durch thermische Diffusion einer Pulvermischung erreicht werden.The mixture can e.g. B. by bringing the metals together in powder form take place. The desired alloy formation can be achieved by treatment at elevated temperature can be achieved by thermal diffusion of a powder mixture.
Das so erhaltene :Metallpulver kann in an sich bekannter Weise zu einer Tablette verpreßt und in Pillenform in das elektrische Entladungsgefäß eingebaut werden. Die Anbringung kann jedoch auch in an sich bekannter Weise durch Aufstreichen einer Suspension des Metallpulvers auf einen Träger und Aufsinterung im Vakuum, im Wasserstoff oder in einer Edelgasatmosphäre erfolgen.The metal powder obtained in this way can be added in a manner known per se compressed into a tablet and built into the electrical discharge vessel in pill form will. However, it can also be attached in a manner known per se by painting a suspension of the metal powder on a carrier and sintering in a vacuum, take place in hydrogen or in a noble gas atmosphere.
DieReaktionsfähigkeit desGetterstoffes kann durch einmaliges oder mehrfaches Hydrieren und Dehydrieren gesteigert werden. Die dadurch erzielte Gitteraufweitung des Fangstoffes ist besonders wirksam, wenn die Ad- und Desorption bei möglichst tiefer Temperatur durchgeführt wird.The reactivity of the getter substance can be determined by a single or multiple hydration and dehydration can be increased. The resulting lattice expansion of the catching material is particularly effective when the adsorption and desorption at as possible is carried out at a lower temperature.
Eine Steigerung der Reaktionsfähigkeit kann auch dadurch erreicht werden, daß der pulverförmigen Gettermischung ein Pulver von Metallen mit hohem Dampfdruck zugemischt oder zulegiert wird, die bereits bei niedrigen Temperaturen wieder ausgedampft werden können. Derartige Metalle sind z. B. Magnesium, die Erdalkalimetalle, Zink oder Kadmium. Auch in diesem Fall läßt sich die Steigerung der Reaktionsfähigkeit durch eine bleibende Aufweitung der Gitterstruktur erklären.An increase in responsiveness can also be achieved in this way be that the powdery getter mixture is a powder of metals with high Vapor pressure is added or alloyed, which is already at low temperatures evaporated again can be. Such metals are z. B. Magnesium, the alkaline earth metals, zinc or cadmium. In this case, too, the increase explain the reactivity by a permanent expansion of the lattice structure.
Die Handhabung der beschriebenen Getter stößt infolge ihrer bereits- bei Zimmertemperatur hohen Rtaktionsfähigkeit auf gewisse Schwierigkeiten. Zum Schutze gegen N.#orzeitige Reaktion und damit verbundene Erschöpfung des Getters wird das Getterpulver oder die fertige Getterpille vor dem Einbau zweckmäßig mit einer geringen Menge Wasserstoff beladen. Durch diesen Vorgang wird eine zwischenzeitliche Herabsetzung der Reaktionsfähigkeit erreicht. Zur endgültigen Aktivierung des Getters muß der aufgenommene Wasserstoff im Vakuum vor dem Abschmelzen der Röhre durch eine Wärmehehandlung wieder ausgetrieben werden.The handling of the getters described comes across as a result of their already- high reactivity to certain difficulties at room temperature. For protection against N. # early reaction and the associated exhaustion of the getter that will Getter powder or the finished getter pill before installation, expediently with a small amount Load amount of hydrogen. This process results in a temporary reduction responsiveness achieved. For the final activation of the getter the absorbed hydrogen in a vacuum before the tube is melted by a heat treatment to be driven out again.
Die beschriebenen, auch bei Zimmertemperatur reagierenden Fangstoffe können sowohl in Hochvakuumröhren als auch in gasgefüllten Entladungsröhren Verwendung finden. In mit Quecksilber oder Mischgas gefüllten Röhren zeigen sie gegenüber den bisher üblichen Barium-Verdampfungsgettern gewisse Vorteile, da ihre Wirksamkeit in viel geringerem Maße durch die Einwirkung des Quecksilberdampfes herabgesetzt wird.The traps described, which also react at room temperature can be used in high vacuum tubes as well as in gas-filled discharge tubes Find. In tubes filled with mercury or mixed gas, they point towards the barium vaporization getters that have been customary up to now have certain advantages because of their effectiveness reduced to a much lesser extent by the action of mercury vapor will.
Durch den Legierungszusatz gemäß der Erfindung erhöht sich die Einbausicherheit der Getterstoffe beträchtlich. Die Lagerfähigkeit der so hergestellten Getter gegenüber den nach anderen Verfahren hergestellten Titan- bzw. Zirkon-Legierungsgettern, insbesondere für solche, die bei tiefen Temperaturen arbeiten sollen, wird durch den Legierungszusatz mach der Erfindung wesentlich erhöht.The addition of alloys according to the invention increases the reliability of installation the getter substances considerably. Compared to the shelf life of the getter produced in this way the titanium or zirconium alloy getters produced by other processes, in particular for those who are supposed to work at low temperatures, the alloy is added make the invention significantly increased.
Bei dem im fertigen Entladungsgefäß durchgeführten Aktivieren, das bei diesen Gettern erforderlich ist, bewirken die Legierungsbestandteile gemäß der Erfindung ein schnelles Lösen bereits vorhandener adsorbierter Gasmengen im Gefüge der Legierung. Dadurch wird die ursprüngliche Reaktionsbereitschaft wiederhergestellt.During the activation carried out in the finished discharge vessel, the is required in these getter, effect the alloy components according to Invention a rapid dissolution of already existing amounts of adsorbed gas in the structure the alloy. This will restore the original responsiveness.
Claims (6)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1067942B true DE1067942B (en) | 1959-10-29 |
Family
ID=593363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT1067942D Pending DE1067942B (en) | Non-evaporating getter material made of titanium, zirconium, vanadium, niobium and possibly aluminum for electrical discharge vessels and processes for its production |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1067942B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1189212B (en) * | 1961-02-04 | 1965-03-18 | Getters Spa | Getter device with getter material that is not evaporated |
| DE3235681A1 (en) * | 1981-11-02 | 1983-05-11 | Maja Feodos'evna Bojarina | Non-vaporisable getter |
| WO1998003987A1 (en) * | 1996-07-23 | 1998-01-29 | Saes Getters S.P.A. | Method for the manufacture of supported thin layers of non-evaporable getter material and getter devices thereby manufactured |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB410614A (en) * | 1932-02-10 | 1934-05-24 | King Lab Inc | Improvements in and relating to methods of manufacturing getters |
| DE745134C (en) * | 1936-06-21 | 1944-02-26 | Aeg | Water-cooled transmitter tubes |
| DE809223C (en) * | 1944-03-11 | 1951-07-26 | Philips Nv | Electric discharge tubes with artificially cooled anode |
| DE811008C (en) * | 1946-10-05 | 1951-08-16 | Philips Nv | Process for the arrangement of gas-binding layers in discharge tubes |
| DE888431C (en) * | 1949-10-04 | 1953-08-31 | Loewe Opta Ag | Gettering process and process for producing the getter substance |
| DE924335C (en) * | 1952-07-18 | 1955-02-28 | Leitz Ernst Gmbh | Procedure for evacuating a vessel |
| FR1094616A (en) * | 1955-05-23 | |||
| DE939042C (en) * | 1952-10-24 | 1956-02-16 | Telefunken Gmbh | Vaporizable getter material for electrical discharge vessels, which contains a permanent barium alloy and an additive |
| DE946076C (en) * | 1945-02-03 | 1956-07-26 | Lorenz C Ag | Process for the production of highly active getter substances |
-
0
- DE DENDAT1067942D patent/DE1067942B/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1094616A (en) * | 1955-05-23 | |||
| GB410614A (en) * | 1932-02-10 | 1934-05-24 | King Lab Inc | Improvements in and relating to methods of manufacturing getters |
| DE745134C (en) * | 1936-06-21 | 1944-02-26 | Aeg | Water-cooled transmitter tubes |
| DE809223C (en) * | 1944-03-11 | 1951-07-26 | Philips Nv | Electric discharge tubes with artificially cooled anode |
| DE946076C (en) * | 1945-02-03 | 1956-07-26 | Lorenz C Ag | Process for the production of highly active getter substances |
| DE811008C (en) * | 1946-10-05 | 1951-08-16 | Philips Nv | Process for the arrangement of gas-binding layers in discharge tubes |
| DE888431C (en) * | 1949-10-04 | 1953-08-31 | Loewe Opta Ag | Gettering process and process for producing the getter substance |
| DE924335C (en) * | 1952-07-18 | 1955-02-28 | Leitz Ernst Gmbh | Procedure for evacuating a vessel |
| DE939042C (en) * | 1952-10-24 | 1956-02-16 | Telefunken Gmbh | Vaporizable getter material for electrical discharge vessels, which contains a permanent barium alloy and an additive |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1189212B (en) * | 1961-02-04 | 1965-03-18 | Getters Spa | Getter device with getter material that is not evaporated |
| DE3235681A1 (en) * | 1981-11-02 | 1983-05-11 | Maja Feodos'evna Bojarina | Non-vaporisable getter |
| WO1998003987A1 (en) * | 1996-07-23 | 1998-01-29 | Saes Getters S.P.A. | Method for the manufacture of supported thin layers of non-evaporable getter material and getter devices thereby manufactured |
| US6016034A (en) * | 1996-07-23 | 2000-01-18 | Saes Getters S.P.A. | Method for forming supported thin layers of non-evaporable getter material and getter devices formed thereby |
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