EP1801247B1 - Procédé de production des prodiuts finis ou semi-finis à haute densite - Google Patents

Procédé de production des prodiuts finis ou semi-finis à haute densite Download PDF

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Publication number
EP1801247B1
EP1801247B1 EP06026181A EP06026181A EP1801247B1 EP 1801247 B1 EP1801247 B1 EP 1801247B1 EP 06026181 A EP06026181 A EP 06026181A EP 06026181 A EP06026181 A EP 06026181A EP 1801247 B1 EP1801247 B1 EP 1801247B1
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EP
European Patent Office
Prior art keywords
tungsten
density
temperature
molybdenum
forming
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.)
Not-in-force
Application number
EP06026181A
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German (de)
English (en)
Other versions
EP1801247A1 (fr
Inventor
Wolfgang Spielmann
Gerhard Leichtfried
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.)
Metallwerk Plansee GmbH
Original Assignee
Metallwerk Plansee GmbH
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 Metallwerk Plansee GmbH filed Critical Metallwerk Plansee GmbH
Publication of EP1801247A1 publication Critical patent/EP1801247A1/fr
Application granted granted Critical
Publication of EP1801247B1 publication Critical patent/EP1801247B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H01J9/04—Manufacture of electrodes or electrode systems of thermionic cathodes
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/04—Electrodes; Screens; Shields
    • H01J61/06—Main electrodes
    • H01J61/073—Main electrodes for high-pressure discharge lamps
    • H01J61/0735—Main electrodes for high-pressure discharge lamps characterised by the material of the electrode

Definitions

  • the invention relates to a method for producing a semifinished product or component from a material of the group molybdenum, molybdenum alloy, tungsten, tungsten alloy with an average relative density> 98.5% and a relative core density> 98.3%.
  • the refractory metals molybdenum, tungsten and their alloys are usually produced by powder metallurgy.
  • the starting material here are ore concentrates, which are chemically processed into intermediates and then reduced to metallic powder.
  • the reducing agent is hydrogen. Alloy elements can be added before, during or after the reduction.
  • Typical molybdenum alloys are TZM (Ti-Zr-C alloyed Mo), Mo-La 2 O 3 , Mo-Y 2 O 3 and Mo-Si-B.
  • AKS-W K-doped tungsten
  • W-ThO 2 W-La 2 O 3 , W-Ce 2 O 3 , WY 2 O 3 and AKS-W-ThO 2 are mentioned.
  • AKS-W and AKS-W-ThO 2 are used especially in lighting technology and here again mainly for filaments and electrodes.
  • the potassium additives present in the AKS-W which are in the form of bubbles, thereby stabilize the grain growth, whereby a stable structure is maintained even at very high operating temperatures and long times. This is especially true for the service life of electrodes for highly loaded lamps, such as Metal halide and short arc lamps, where the surface temperature is up to 2,600 ° C, of essential importance.
  • the powder is compacted by die pressing or cold isostatic pressing. Large sized semi-finished product is preferably produced by cold isostatic pressing. For wire rods and small billets, both die pressing and cold isostatic pressing are used.
  • Fisher molybdenum powder with a typical Fisher particle size of 2 to 5 microns and tungsten powder having a typical Fisher particle size of 1.5 to 4.5 microns
  • fractional bulk densities in the range of 0.11 to 0.17 (molybdenum) and 0.13 to 0.22 (tungsten).
  • tungsten fractional bulk densities in the range of 0.11 to 0.17 (molybdenum) and 0.13 to 0.22 (tungsten).
  • tungsten Using a compacting pressure in the range of 200 to 500 MPa, fractional green densities are achieved in the range of 0.6 to 0.68 for both molybdenum and tungsten.
  • the green compacts are sintered.
  • the sintering process is carried out in such a way that the sintered body has a low porosity associated with a fine-grained microstructure.
  • Molybdenum and tungsten are usually sintered in hydrogen with a dew point ⁇ 0 ° C.
  • the usual sintering temperatures for molybdenum are 1,800 ° C to 2,200 ° C, for tungsten 2,100 ° C to 2,700 ° C. Usual sintering times are 1 to 24 hours. Since the sintering process is determined by grain boundary diffusion, sintering can be carried out at a lower temperature with a smaller particle size. However, the particle size also determines the pore size in the sintered semifinished product. Thus, the pore size can be reduced by a factor of 3 when the particle size of Fisher of the molybdenum powder used is reduced from 10 microns to 2.6 microns.
  • a disadvantage of fine-grained powder is the higher proportion of adsorbed gases, in particular oxygen. During the sintering process, this oxygen reacts with the hydrogen of the sintering gas to form water vapor. Due to the low gas permeability of the green compact, which is further reduced during the sintering process, the water vapor, in particular from the center of the sintered body, can not be removed sufficiently. This is especially the case when fine-grained powder having a particle size of Fisher ⁇ 4.5 ⁇ m is used.
  • a high water vapor content in the interior of the sintered body triggers a CVT (Chemical Vapor Transport) reaction.
  • This CVT reaction leads, through material transport through the gas phase, to a destruction of specific surface area and thus a reduction in the driving forces for sintering, in particular in the interior of the sintered body.
  • This process is exacerbated in molybdenum and tungsten alloys, where additives release an oxygen-containing species during sintering, resulting in increased water vapor formation, such as in AKS-W, Mo-La 2 O 3 or W-La 2 O 3 Case is.
  • Gas phase reactions therefore limit the dimension of the sintered body, especially in these alloys. With sintered bodies with larger dimensions or with the use of very fine-grained powder, the achievable sintering density, in particular in the center of the sintered body, is lower than in the case of small sintered bodies or when coarser powder is used.
  • thermomechanical treatment achieves the desired shape, reduction / elimination of porosity, and adjustment of the desired mechanical and microstructural properties. With increasing degree of deformation, the density increases up to the theoretical density and the grain size decreases. The reduction of the grain size depends strongly on the selected forming temperature and the intermediate annealing temperatures.
  • the use of fine-grained powders or, in the case of alloys containing a species which splits off oxygen or water vapor during the sintering process is limited in the size of the sintered body. If a product having larger dimensions is produced from this sintered body, then the possible degree of deformation for closing the porosity, in particular in the center of the sintered body, may not be sufficient.
  • AKS tungsten which is used as electrode material in lamps.
  • the production of lamp electrodes from W is, for example AT-U-006,240 known.
  • Anodes with a diameter of up to 55 mm are used especially for short arc lamps.
  • a life-determining property of such electrodes is their dimensional stability.
  • the deformation of the electrodes is triggered by thermally induced voltages. These thermally induced voltages can, for example, lead to elevations in the region of the electrode plateau. The arc is then concentrated on these bumps, resulting in localized overheating. This can lead to the melting of the electrode in this area.
  • the local overheating leads to an increased evaporation of the electrode material.
  • the vaporized electrode material settles on the lamp bulb and drastically reduces the light flux.
  • a feinkömiges electrode material has a longer life. This is due to the fact that with coarse-grained material, the damage concentrates on a few grain boundaries, whereby there is a self-reinforcing effect by a concentration of the arc.
  • the object of the invention is therefore to provide semi-finished products or components with a high density, especially in the center, connected to a fine-grained structure.
  • the object is achieved by a method having the features according to claim 1.
  • the method according to the invention it is possible to produce semi-finished products or components made of molybdenum, tungsten and their alloys with an average relative density> 98.5% and a relative core density> 98.3%.
  • average relative density is the average density relative to the specific To understand weight. Under Kem ashamed the expert understands the density in the center of a semifinished product or component. Since the core volume is not specified in relation to the total volume, the core volume for the determination of the core density is defined as follows for the following data: The center-nearest 10% of the total area transverse to the deformation direction x extension in the direction of deformation.
  • the semifinished product or the component, in the deformed state preferably has a comm number> 100 grains / mm 2 transversely to its deformation direction.
  • the sintering takes place at a temperature of 0.55 to 0.92 x solidus temperature.
  • the sintering temperature is chosen so that a sintering density of 90% to 98.5% of the theoretical density, preferably a proportion of the closed pores based on the total porosity of> 0.8 is set. If the relative density exceeds 98.5%, the objective, namely the production of a component or semi-finished product with a count of> 100 grains / mm 2 , can not be achieved.
  • ⁇ is defined by: ( Initial cross-sectional area - Cross-sectional area after the forming process ) / Initial cross-sectional area ⁇ 100th
  • the hot isostatic pressing is carried out without using a jug and is carried out at a temperature of 0.40 to 0.65 x solidus temperature at a pressure of 50 to 300 MPa. If the temperature is below 0.4 x solidus temperature, the target, a mean relative density of> 98.5% and a relative core density of> 98.3% in the component or semi-finished product, can not be achieved. If the temperature is above 0.65 x solidus temperature, undesirable coarsening occurs due to normal or abnormal grain growth. If the pressure is below 50 MPa, the density target can not be achieved either. At pressures above 300 MPa, the inventive method can no longer be economically represented.
  • the hot isostatically pressed part is reshaped.
  • the degree of deformation ⁇ is 15 to 90%. If the degree of deformation ⁇ is less than 15%, the goal of a relative density> 98.3% can not be achieved. If the degree of deformation is more than 90%, again the process can not be economically represented, since dense products can also be produced without the hot isostatic pressing according to the invention.
  • the method according to the invention is particularly useful for the production of electrodes in the diameter range of 15 to 55 mm, which are used in discharge lamps. If the diameter is less than 15 mm, such electrodes can be produced more economically by means of conventional production methods. The upper limit of 55 mm results from the border wattage of such lamps.
  • the starting material for the electrodes is preferably formed by radial forging or rolling.
  • an AKS-W powder with a particle size of Fisher of 4.1 ⁇ m was used for the production of an AKS-W electrode.
  • the powder was compacted by cold isostatic pressing at a pressure of 200 MPa into a green compact.
  • the sintering was carried out at a temperature of 2,250 ° C in hydrogen.
  • the sintered rods thus produced had an average specific gravity, as determined by buoyancy, of 92.0%.
  • the proportion of closed porosity was> 95%, the measurement being carried out by means of mercury porosimetry.
  • the sintered bodies were hot isostatically compacted in the subsequent step at a temperature of 1750 ° C and a pressure of 195 MPa for 3 hours.
  • the relative mean density after the hot isostatic pressing process was 97.9%.
  • the rods were reshaped on a radial forging machine.
  • the degree of deformation ⁇ was 67%.
  • the average relative density of the bars after the forming process was 99.66% and the relative density was 99.63%.
  • the grain size was determined in the formed state and after annealing at 1,800 ° C / 4 hours. In the formed state, it was about 10,000 grains / mm 2 both in the center and in the edge region of the rods. In the annealed state, a very fine-grained microstructure was still found, with a mean number in the center of the rods of about 800 and in the border area of 850 grains / mm 2 .
  • the chemical analysis of the rods gave the following result: potassium 15 ⁇ g / g, silicon 6 ⁇ g / g, carbon ⁇ 5 ⁇ g / g, oxygen 7 ⁇ g / g.
  • Anodes for 2.5 kW short arc lamps for cinema projection were produced from the material produced according to the invention.
  • the determined average service life was 2,060 hours.
  • a material was also used which, after the sintering process, was not subjected to any subsequent densification by a hot isostatic pressing process, with otherwise identical production process. This resulted in an average service life of 1,710 hours.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Discharge Lamp (AREA)

Claims (9)

  1. Procédé de fabrication d'un composant ou d'un produit semi-fini constitué d'un matériau de l'ensemble constitué du molybdène, des alliages de molybdène, du tungstène et des alliages du tungstène dont la densité relative moyenne est > 98,5 % et la densité moyenne de l'âme > 98,3 %, dans lequel la fabrication comprend au moins les étapes de traitement qui consistent à :
    - préparer une poudre dont les particules ont une taille de Fisher de 0,5 à 10 µm,
    - comprimer la poudre sous une pression de 100 à 500 MPa,
    - la fritter à une température de 0,55 à 0,92 x température du solidus jusqu'à une densité relative D, avec 90 % < D < 98,5 %,
    - la comprimer en conditions isostatiques à chaud sans recourir à un récipient, à une température de 0,40 à 0,65 x température du solidus et sous une pression de 50 à 300 MPa et
    - déformer à un degré de déformation ϕ avec 15 % < ϕ < 90 %.
  2. Procédé selon la revendication 1, caractérisé en ce que le composant ou le produit semi-fini présente à l'état non déformé un indice moyen de grains > 100 grains/mm2.
  3. Procédé selon les revendications 1 ou 2, caractérisé en ce qu'avant la compression isostatique à chaud, le corps fritté subit une déformation supplémentaire avec 2 % < ϕ < 60 %.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que le corps fritté présente une proportion de pores fermés de > 0,8 par rapport à la porosité globale.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le composant ou le produit semi-fini est constitué de tungstène dopé au K (AKS-W) et en ce que sa teneur en K est comprise entre 5 et 70 µg/g.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que la déformation s'effectue par forgeage radial ou laminage et qu'elle fournit un barreau.
  7. Procédé selon la revendication 6, caractérisé en ce que le barreau a un diamètre de 15 à 55 mm.
  8. Procédé selon les revendications 6 ou 7, caractérisé en ce que l'on réalise une électrode de lampe à partir du barreau.
  9. Procédé selon la revendication 8, caractérisé en ce que l'électrode de lampe est utilisée dans une lampe à court arc lumineux.
EP06026181A 2005-12-23 2006-12-18 Procédé de production des prodiuts finis ou semi-finis à haute densite Not-in-force EP1801247B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT0088805U AT9340U1 (de) 2005-12-23 2005-12-23 Verfahren zur herstellung eines hochdichten halbzeugs oder bauteils

Publications (2)

Publication Number Publication Date
EP1801247A1 EP1801247A1 (fr) 2007-06-27
EP1801247B1 true EP1801247B1 (fr) 2008-03-12

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EP06026181A Not-in-force EP1801247B1 (fr) 2005-12-23 2006-12-18 Procédé de production des prodiuts finis ou semi-finis à haute densite

Country Status (6)

Country Link
US (1) US20070148031A1 (fr)
EP (1) EP1801247B1 (fr)
JP (1) JP5265867B2 (fr)
CN (1) CN101007350B (fr)
AT (2) AT9340U1 (fr)
DE (1) DE502006000455D1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7973476B2 (en) 2006-12-22 2011-07-05 Osram Gesellschaft mit beschränkter Haftung High-pressure mercury discharge lamp

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090011266A1 (en) * 2007-07-02 2009-01-08 Georgia Tech Research Corporation Intermetallic Composite Formation and Fabrication from Nitride-Metal Reactions
KR101246754B1 (ko) * 2007-09-21 2013-03-26 오스람 게엠베하 직류 방전 램프
RU2461910C2 (ru) * 2007-09-21 2012-09-20 Осрам Аг Газоразрядная лампа постоянного тока
DE102008014096A1 (de) * 2008-03-05 2009-09-10 Osram Gesellschaft mit beschränkter Haftung Wolframelektrode für Hochdruckentladungslampen und Hochdruckentladungslampe mit einer Wolframelektrode
US9992917B2 (en) 2014-03-10 2018-06-05 Vulcan GMS 3-D printing method for producing tungsten-based shielding parts
CN105478772B (zh) * 2014-09-15 2018-12-04 安泰科技股份有限公司 一种钼平面靶材的制造方法

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Also Published As

Publication number Publication date
JP5265867B2 (ja) 2013-08-14
CN101007350A (zh) 2007-08-01
US20070148031A1 (en) 2007-06-28
AT9340U1 (de) 2007-08-15
DE502006000455D1 (de) 2008-04-24
EP1801247A1 (fr) 2007-06-27
ATE389040T1 (de) 2008-03-15
CN101007350B (zh) 2012-07-04
JP2007169789A (ja) 2007-07-05

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