EP0439776B1 - Molybdenum material, in particular for the fabrication of lamps - Google Patents
Molybdenum material, in particular for the fabrication of lamps Download PDFInfo
- Publication number
- EP0439776B1 EP0439776B1 EP90124465A EP90124465A EP0439776B1 EP 0439776 B1 EP0439776 B1 EP 0439776B1 EP 90124465 A EP90124465 A EP 90124465A EP 90124465 A EP90124465 A EP 90124465A EP 0439776 B1 EP0439776 B1 EP 0439776B1
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- EP
- European Patent Office
- Prior art keywords
- molybdenum
- ppm
- lamps
- molybdenum material
- aluminum
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
Definitions
- molybdenum material is to be understood as meaning materials that are used for various purposes in lamp construction.
- the final product of molybdenum production which is initially available as a sintered rod, is then only further processed purely mechanically, so that nothing changes in the chemical composition.
- the desired primary materials are created by rolling, hammering and drawing. More specifically, these processes initially produce pins or wires. Tubes or tape material for the film production are then in turn produced as a semi-finished product from wires or pins.
- molybdenum material which is doped with at least one of the elements Al, Si, K in an amount of 50-7500 ppm (wt.). This can improve the recrystallization behavior of external power supplies for lamps.
- Another task is to use only substances that are harmless to health when producing molybdenum material.
- This positive property is achieved by adding 150-800 ppm by weight aluminum; particularly good results are achieved when using 400-600 ppm.
- a very small amount of potassium, 5-50 ppm, is additionally used as doping to regulate the grain size.
- Such a molybdenum material is particularly well suited as a holder wire in the lamp industry.
- the area of application is primarily in the case of extremely high thermal and chemical loads, as occurs with certain types (PAR lamps, halogen lamps).
- a PAR incandescent lamp with an output of 300 W may be mentioned as an exemplary embodiment.
- the holders for the filament are made of molybdenum wire with a diameter of approx. 125 ⁇ m.
- the molybdenum is doped with 500 ppm (wt.) Al and 15 ppm (wt.) K.
- a molybdenum wire with a doping of 250 ppm aluminum and 15 ppm K may be mentioned as an example. Its constant elongation is around 3.5%.
- the process for producing the molybdenum material is based on the Coolidge process (cf. C. Agte / J. Vacek, Wolfram and Molybdenum, Akademie-Verlag, Berlin, 1959, especially chap. 6):
- the starting material for the production of the molybdenum products is, for example, MoO3 with a purity of 99.97% by weight.
- Aluminum and a small amount of potassium are added to this oxide, which is in powder form, as a dopant.
- the aluminum is added as nitrate (Al (NO3) 3).
- Al (NO3) 3) nitrate
- the subsequent two-stage reduction of the molybdenum oxide is carried out in a manner known per se using an H2 / N2 mixture and pure H2 gas.
- a rotary kiln is advantageously used instead of a feed oven to be equipped with boats.
- the MoO3 is reduced to Mo via MoO2 at temperatures of approx. 500-600 ° C (1st step) or 1000-1100 ° C (2nd step).
- the metal is pressed on hydraulic presses in steel matrices. Sintering takes place in a push-through furnace at low temperatures (1700 ° C). The sintered rod formed is then processed into molybdenum wire by rolling, hammering and drawing. This wire can now be processed into holder wire or core wire, for example.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Vessels And Coating Films For Discharge Lamps (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Luminescent Compositions (AREA)
- Metal Extraction Processes (AREA)
- Glass Compositions (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
Description
Diese Anmeldung steht in engem Zusammenhang mit der Parallelanmeldung EP-A-439 775. Die Erfindung geht aus von einem Molybdänmaterial nach dem Oberbegriff des Anspruchs 1.This application is closely related to the parallel application EP-A-439 775. The invention is based on a molybdenum material according to the preamble of claim 1.
Unter dem Begriff Molybdänmaterial sollen im folgenden Vormaterialien verstanden werden, die für verschiedene Zwecke im Lampenbau angewendet werden. Das zunächst als Sinterstab vorliegende Endprodukt der Molybdänherstellung wird anschließend nur noch rein mechanisch weiterverarbeitet, so daß sich an der chemischen Zusammensetzung nichts mehr ändert. Durch Walzen, Hämmern und Ziehen entstehen die gewünschten Vormaterialien. Genauer gesagt entstehen bei diesen Prozessen zunächst Stifte oder Drähte. Röhrchen oder Bandmaterial für die Folienherstellung werden dann als Halbzeug wiederum aus Drähten oder Stiften hergestellt.In the following, the term molybdenum material is to be understood as meaning materials that are used for various purposes in lamp construction. The final product of molybdenum production, which is initially available as a sintered rod, is then only further processed purely mechanically, so that nothing changes in the chemical composition. The desired primary materials are created by rolling, hammering and drawing. More specifically, these processes initially produce pins or wires. Tubes or tape material for the film production are then in turn produced as a semi-finished product from wires or pins.
Aus der JP-A- 60 194 043 ist ein Molybdänmaterial bekannt, das mit mindestens einem der Elemente Al, Si, K in einer Menge von 50 - 7500 ppm (Gew.) dotiert ist. Damit läßt sich das Rekristallisationsverhalten von äußeren Stromzuführungen bei Lampen verbessern.From JP-A-60 194 043 a molybdenum material is known which is doped with at least one of the elements Al, Si, K in an amount of 50-7500 ppm (wt.). This can improve the recrystallization behavior of external power supplies for lamps.
Die Dotierung von Molybdänmaterial mit Eisen und/oder Kobalt ist aus der DD-PS 49 592 bekannt. Diese Maßnahme dient dazu, eine höhere Bruchdehnung und eine höhere Bruchfestigkeit zu erzielen. Es hat sich jedoch in der Zwischenzeit herausgestellt, daß Kobalt ein die Gesundheit gefährdender Stoff ist, für den inzwischen strenge Vorschriften am Arbeitsplatz gelten (MAK-Werte). Weiterhin hat sich gezeigt, daß die gewünschten Eigenschaften der Dehnung und Festigkeit nur mit großer Streubreite erzielt werden können, so daß bei der Herstellung ein hoher Ausschuß verkraftet werden muß.The doping of molybdenum material with iron and / or cobalt is known from DD-PS 49 592. This measure serves to achieve a higher elongation at break and a higher breaking strength. In the meantime, however, it has been found that Cobalt is a substance that is hazardous to health and has now been subject to strict workplace regulations (MAK values). Furthermore, it has been shown that the desired properties of elongation and strength can only be achieved with a wide spread, so that a high scrap must be handled during manufacture.
Es ist Aufgabe der vorliegenden Erfindung eine Qualitätsverbesserung der Materialeigenschaften von Molybdän-Halbzeug, insbesondere für die Lampenindustrie, zu erzielen und den Ausschuß zu senken.It is an object of the present invention to improve the quality of the material properties of semi-finished molybdenum, in particular for the lamp industry, and to reduce rejects.
Eine weitere Aufgabe ist es, bei Herstellung von Molybdänmaterial ausschließlich gesundheitlich unbedenkliche Stoffe zu verwenden.Another task is to use only substances that are harmless to health when producing molybdenum material.
Diese Aufgaben werden durch die kennzeichnenden Merkmale des Anspruchs 1 gelöst. Eine besonders vorteilhafte Ausgestaltung der Erfindung findet sich in Anspruch 2.These objects are achieved by the characterizing features of claim 1. A particularly advantageous embodiment of the invention can be found in claim 2.
In den letzten Jahren haben sich die Anforderungen an die thermische und mechanische Belastbarkeit des Molybdänmaterials ständig erhöht, insbesondere im Zusammenhang mit der Entwicklung von PAR-Lampen und von Halogenglühlampen. Dies führte zunächst zu einer weitgehenden Spezialisierung der Molybdänmaterialien für verschiedene Einsatzgebiete. Beispielsweise wurden verschiedene Molybdänmaterialien für Kerndrähte, gasdichte Einschmelzstifte, Halterdrähte und Dichtungsfolien hergestellt. Insbesondere bei Halterdrähten, die eine zwischen Stromzuführungen aufgespannte Wendel stützen (vgl. z.B. DE-OS 27 46 850) ist eine hohe und konstante Dehnung die wichtigste Eigenschaft. Weiterhin kommt es auch auf eine hohe Bruchfestigkeit und eine hohe Rekristallisationstemperatur an.In recent years, the requirements for the thermal and mechanical resilience of the molybdenum material have increased continuously, especially in connection with the development of PAR lamps and halogen incandescent lamps. This initially led to extensive specialization of molybdenum materials for various areas of application. For example, various molybdenum materials for core wires, gas-tight sealing pins, holder wires and sealing foils were produced. Particularly in the case of holder wires which support a helix stretched between current leads (see, for example, DE-OS 27 46 850), there is a high and constant elongation the most important property. Furthermore, a high breaking strength and a high recrystallization temperature are also important.
Darüber hinaus ergab sich lange Zeit ein scheinbar unlösbares Problem in der hohen Streubreite dieser Eigenschaften, die, um einen hohen Ausschuß zu vermeiden, dazu zwang, ständig die Maschinenparameter nachzuregeln.In addition, for a long time there appeared to be an insoluble problem in the wide range of these properties, which, in order to avoid high rejects, made it necessary to continuously readjust the machine parameters.
Durch eine geeignete Dotierung mit Aluminium anstelle von Eisen und/oder Kobalt ist es nun gelungen, diese Schwierigkeiten zu überwinden. Außerdem wird eine sehr geringe Menge an Kalium zugesetzt. Dazu ist jedoch eine extrem hohe Reinheit des Molybdänausgangsmaterials Voraussetzung; sie muß bei mindestens 99,97 Gew.-% allgemein und bei mindestens 99,999 Gew.-% in bezug auf Kalium liegen.Appropriate doping with aluminum instead of iron and / or cobalt has now succeeded in overcoming these difficulties. A very small amount of potassium is also added. However, an extremely high purity of the molybdenum starting material is a prerequisite for this; it must be at least 99.97% by weight in general and at least 99.999% by weight with respect to potassium.
Aluminium verdampft während des Herstellungsprozesses - im Gegensatz zu Kalium - nicht. Somit verhindert die Zugabe von Aluminium die Streuung der Materialeigenschaften.Unlike potassium, aluminum does not evaporate during the manufacturing process. The addition of aluminum thus prevents the material properties from spreading.
Diese positive Eigenschaft wird erzielt durch die Zugabe von 150-800 Gew.-ppm Aluminium; besonders gute Ergebnisse werden bei Verwendung von 400-600 ppm erzielt. Aus fertigungstechnischen Gründen wird für die Regulierung der Korngröße zusätzlich eine sehr geringe Menge an Kalium, 5-50 ppm, als Dotierung eingesetzt.This positive property is achieved by adding 150-800 ppm by weight aluminum; particularly good results are achieved when using 400-600 ppm. For reasons of manufacturing technology, a very small amount of potassium, 5-50 ppm, is additionally used as doping to regulate the grain size.
Ein derartiges Molybdänmaterial ist besonders gut als Halterdraht in der Lampenindustrie geeignet. Das Einsatzgebiet liegt vor allem bei extrem hoher thermischer und chemischer Belastung, wie sie bei bestimmten Typen (PAR-Lampen, Halogenlampen) auftritt. Als Ausführungsbeispiel sei eine PAR-Glühlampe mit einer Leistung von 300 W angeführt. Die Halter für den Leuchtkörper sind aus Molybdändraht gefertigt mit einem Durchmesser von ca. 125 µm. Das Molybdän ist mit 500 ppm (Gew.) Al und 15 ppm (Gew.) K dotiert.Such a molybdenum material is particularly well suited as a holder wire in the lamp industry. The area of application is primarily in the case of extremely high thermal and chemical loads, as occurs with certain types (PAR lamps, halogen lamps). A PAR incandescent lamp with an output of 300 W may be mentioned as an exemplary embodiment. The holders for the filament are made of molybdenum wire with a diameter of approx. 125 µm. The molybdenum is doped with 500 ppm (wt.) Al and 15 ppm (wt.) K.
Die Dehnung (Δl/l) dieses Molybdändrahtes, in der einzigen Figur dargestellt, ist etwas höher (ca. 21,5 %) als die eines entsprechenden Molybdändrahtes, der mit 500 ppm (Gew.) Kobalt dotiert ist (ca. 20,8 %). Von besonderer Bedeutung ist jedoch der Umstand, daß die Streubreite der Dehnung bei der Aluminiumdotierung erheblich gegenüber einer Kobaltdotierung reduziert ist. Sie beträgt etwa 2 % gegenüber ca. 5 % (s. Figur). Auch andere Eigenschaften sind gegenüber den bekannten Dotierungen verbessert. So beträgt beispielsweise die Rekristallisationstemperatur jetzt ca. 1700 °C gegenüber nur 1100 °C beim Stand der Technik.The elongation (Δl / l) of this molybdenum wire, shown in the single figure, is somewhat higher (approx. 21.5%) than that of a corresponding molybdenum wire which is doped with 500 ppm (wt.) Cobalt (approx. 20.8 %). Of particular importance, however, is the fact that the spread of elongation in aluminum doping is considerably reduced compared to cobalt doping. It is about 2% compared to about 5% (see figure). Other properties are also improved compared to the known doping. For example, the recrystallization temperature is now approximately 1700 ° C compared to only 1100 ° C in the prior art.
Für reduzierte Anforderungen können andere, insbesondere geringere Dotierungen verwendet werden. Als Beispiel sei ein Molybdändraht mit einer Dotierung von 250 ppm Aluminium und 15 ppm K genannt. Seine Dehnungskonstanz liegt bei etwa 3,5 %.Other, in particular lower, doping can be used for reduced requirements. A molybdenum wire with a doping of 250 ppm aluminum and 15 ppm K may be mentioned as an example. Its constant elongation is around 3.5%.
Das Verfahren zur Herstellung des Molybdänmaterials läuft im Prinzip nach dem Coolidge-Verfahren ab (vgl. hierzu C. Agte/J. Vacek, Wolfram und Molybdän, Akademie-Verlag, Berlin, 1959, insbes. Kap. 6): Ausgangsstoff für die Herstellung der Molybdänerzeugnisse ist beispielsweise MoO₃ mit einer Reinheit von 99,97 Gew.-%. Diesem als Pulver vorliegenden Oxid wird als Dotierstoff Aluminium und eine geringe Menge an Kalium zugegeben. Das Aluminium wird als Nitrat (Al (NO₃)₃) beigefügt. Denkbar wäre auch die Verwendung einer anderen instabilen Aluminiumverbindung, z.B. AlCl₃. Hingegen ist eine Verbindung hoher Stabilität, z.B. Al₂O₃, ungeeignet, da das Aluminium bei der anschließenden thermischen Behandlung nicht freigesetzt würde.In principle, the process for producing the molybdenum material is based on the Coolidge process (cf. C. Agte / J. Vacek, Wolfram and Molybdenum, Akademie-Verlag, Berlin, 1959, especially chap. 6): The starting material for the production of the molybdenum products is, for example, MoO₃ with a purity of 99.97% by weight. Aluminum and a small amount of potassium are added to this oxide, which is in powder form, as a dopant. The aluminum is added as nitrate (Al (NO₃) ₃). It would also be conceivable to use another unstable aluminum compound, for example AlCl₃. On the other hand, a compound of high stability, for example Al₂O₃, is unsuitable since the aluminum would not be released during the subsequent thermal treatment.
Die anschließende zweistufige Reduktion des Molybdänoxids wird in an sich bekannter Weise mit einem H₂/N₂-Gemisch und reinem H₂-Gas durchgeführt. Vorteilhaft wird ein Drehrohrofen statt eines mit Schiffchen zu bestückenden Vorschubofens verwendet. In zwei Schritten wird das MoO₃ über MoO₂ zu Mo reduziert bei Temperaturen von ca. 500-600 °C (1. Schritt) bzw. 1000-1100 °C (2. Schritt).The subsequent two-stage reduction of the molybdenum oxide is carried out in a manner known per se using an H₂ / N₂ mixture and pure H₂ gas. A rotary kiln is advantageously used instead of a feed oven to be equipped with boats. In two steps, the MoO₃ is reduced to Mo via MoO₂ at temperatures of approx. 500-600 ° C (1st step) or 1000-1100 ° C (2nd step).
Um die gewünschten duktilen Materialien herstellen zu können, wird das Metall auf hydraulischen Pressen in Stahlmatrizen verpreßt. Die Sinterung erfolgt in einem Durchschubofen bei niedrigen Temperaturen (1700 °C). Der dabei gebildete Sinterstab wird anschließend durch Walzen, Hämmern und Ziehen zu Molybdändraht verarbeitet. Dieser Draht kann nun beispielsweise zu Halterdraht oder auch Kerndraht verarbeitet werden.In order to be able to produce the desired ductile materials, the metal is pressed on hydraulic presses in steel matrices. Sintering takes place in a push-through furnace at low temperatures (1700 ° C). The sintered rod formed is then processed into molybdenum wire by rolling, hammering and drawing. This wire can now be processed into holder wire or core wire, for example.
Claims (2)
- Molybdenum material, particularly for making lamps, the molybdenum having a purity of at least 99.97 % by weight, characterized in that only aluminium and potassium are present as doping material, the aluminium content being between 150 and 800 ppm by weight, and the molybdenum material being additionally doped with a small quantity of potassium which is between 5 and 50 ppm, the K content being small as compared with the Al content.
- Molybdenum material according to Claim 1, characterized in that the aluminium content is between 400 and 600 ppm.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4002973 | 1990-02-01 | ||
| DE4002973A DE4002973A1 (en) | 1990-02-01 | 1990-02-01 | Molybdenum material esp. for lamp mfr. - contains aluminium as sole dopant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0439776A1 EP0439776A1 (en) | 1991-08-07 |
| EP0439776B1 true EP0439776B1 (en) | 1994-10-26 |
Family
ID=6399218
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP90124465A Expired - Lifetime EP0439776B1 (en) | 1990-02-01 | 1990-12-17 | Molybdenum material, in particular for the fabrication of lamps |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP0439776B1 (en) |
| JP (1) | JPH04297543A (en) |
| KR (1) | KR910021489A (en) |
| AT (1) | ATE113319T1 (en) |
| DE (2) | DE4002973A1 (en) |
| ES (1) | ES2060914T3 (en) |
| HU (1) | HU210093B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19603300C2 (en) * | 1996-01-30 | 2001-02-22 | Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh | Electric lamp with molybdenum foil bushings for a lamp vessel made of quartz glass |
| DE19603301C2 (en) * | 1996-01-30 | 2001-02-22 | Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh | Electric lamp with molybdenum foil bushings for a lamp vessel made of quartz glass |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3676083A (en) * | 1969-01-21 | 1972-07-11 | Sylvania Electric Prod | Molybdenum base alloys |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD49592A (en) * | ||||
| DE1211402B (en) * | 1960-04-29 | 1966-02-24 | Egyesuelt Izzolampa | Process for the production of tungsten wires, in particular for pipe grids |
| CH503114A (en) * | 1966-12-21 | 1971-02-15 | Egyesuelt Izzolampa | Group vi re contg alloys as for use in - making filaments or electrode plates |
| AT329889B (en) * | 1974-01-18 | 1976-06-10 | Plansee Metallwerk | Process for the production of molybdenum wires and sheets with a stacking wire structure |
| JPS604548B2 (en) * | 1976-10-21 | 1985-02-05 | ゼネラル エレクトリツク コンパニ− | light bulb mount |
-
1990
- 1990-02-01 DE DE4002973A patent/DE4002973A1/en not_active Withdrawn
- 1990-12-03 HU HU908036A patent/HU210093B/en not_active IP Right Cessation
- 1990-12-17 AT AT90124465T patent/ATE113319T1/en not_active IP Right Cessation
- 1990-12-17 ES ES90124465T patent/ES2060914T3/en not_active Expired - Lifetime
- 1990-12-17 DE DE59007563T patent/DE59007563D1/en not_active Expired - Fee Related
- 1990-12-17 EP EP90124465A patent/EP0439776B1/en not_active Expired - Lifetime
-
1991
- 1991-01-23 JP JP916191A patent/JPH04297543A/en active Pending
- 1991-02-01 KR KR1019910001736A patent/KR910021489A/en not_active Application Discontinuation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3676083A (en) * | 1969-01-21 | 1972-07-11 | Sylvania Electric Prod | Molybdenum base alloys |
Also Published As
| Publication number | Publication date |
|---|---|
| ES2060914T3 (en) | 1994-12-01 |
| KR910021489A (en) | 1991-12-20 |
| ATE113319T1 (en) | 1994-11-15 |
| HU908036D0 (en) | 1991-06-28 |
| DE4002973A1 (en) | 1991-08-08 |
| HU210093B (en) | 1995-02-28 |
| EP0439776A1 (en) | 1991-08-07 |
| HUT62339A (en) | 1993-04-28 |
| DE59007563D1 (en) | 1994-12-01 |
| JPH04297543A (en) | 1992-10-21 |
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