CN1744961A - Refractory metal annealing bands - Google Patents
Refractory metal annealing bands Download PDFInfo
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- CN1744961A CN1744961A CNA2004800032276A CN200480003227A CN1744961A CN 1744961 A CN1744961 A CN 1744961A CN A2004800032276 A CNA2004800032276 A CN A2004800032276A CN 200480003227 A CN200480003227 A CN 200480003227A CN 1744961 A CN1744961 A CN 1744961A
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- 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
- B22F3/16—Both compacting and sintering in successive or repeated steps
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- 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
- B22F5/003—Articles made for being fractured or separated into parts
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- 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
- B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
- C21D9/54—Furnaces for treating strips or wire
- C21D9/56—Continuous furnaces for strip or wire
- C21D9/62—Continuous furnaces for strip or wire with direct resistance heating
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
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- 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
- B22F2005/002—Tools other than cutting tools
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- 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
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- 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
Abstract
The invention relates to a process for making an annealing band, the process comprising (a) producing a refractory metal powder; or refractory metal alloy powder; (b) optionally blending the powder with an oxide component or a carbide component; (c) consolidating the powder or powder blend and forming a consolidated powder component; (d) subjecting the consolidated powder component to thermo-mechanical treatment and forming a sheet, or tube; (e) cutting the sheet into a strip; and (f) forming an annealing band from the strip. Then invention also relates to annealing bands and processes for using annealing bands.
Description
Background technology
The participant of wire rod process industry has recognized the need to better annealing zone for a long time, be used to the better method making the better method of annealing zone and be used for metal wire rod is annealed.In hot candied technical field, general practice is by the resistance heated between the hot candied step copper wire to be carried out online annealing, or as final heat treatment.Be this purpose, wire rod passes through on two wheels (sheet), and described wheel the (sheet) has the voltage that is applied on it.Like that, electric current is heated to its annealing temperature by wire rod with wire rod.When metal wire rod passes through, provide contact area for metal wire rod as the what is called ' annealing zone ' of taking turns (sheet) assembly part on wheel.Annealing wheel (sheet) assembly can be second plate on water-cooled wheel shaft and the assembly that has the annealing zone that covers described wheel shaft at the plate on the side and being bolted to.It is similar with fan belt to pulley that described assembly seems, wire rod is described driving-belt.
Nickel or nickel alloy are used to make annealing zone usually.Regrettably, wire manufacturers report claims that life-span of the annealing zone that uses at present is very short and is necessary to change continually annealing zone.Abrasion mechanism comprises friction and because the arc discharge that the voltage drop between band and the wire rod causes between wheel (sheet) and the wire rod.When changing the annealing zone of wearing and tearing, equipment needs to shut down, and this has constituted two problems: promptly lost manufacturing time and interrupted continuous processing.Some effort have comprised the annealing zone of copper and niobium at production.Yet these effort fail to produce the annealing zone with suitable character.
Because previous reasons needs the improved annealing zone of exploitation.
Because previous reasons needs exploitation to be used to make the improved method of this band.
Because previous reasons needs exploitation to be used for the improved method that metal wire rod is annealed.
Summary of the invention
The present invention relates to a kind of technology that is used to make annealing zone, comprise step (a) production refractory metal powder; (b) powder and oxide component or nitride component or carbide ingredient are mixed; (c) make powder or mixture of powders carry out fixed and form consolidated powder component; (d) make consolidated powder component be subjected to thermal-mechanical treatment and form plate or pipe; (e) plate or pipe are cut into band or ring; And (f) form annealing zone by band, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
The invention still further relates to a kind of member that comprises refractory metal annealing bands, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.The invention still further relates to a kind of technology that metal wire rod is annealed of being used for, comprise that step (a) is provided with two annealing wheel assemblies (annealed sheet), wherein each assembly comprises first annealing wheel (lamellar body), second annealing wheel (sheet plate) and annealing zone, has refractory metal annealing bands between first annealing wheel and second annealing wheel respectively so that be attached to first annealing wheel gone up each other and second annealing wheel, with thinking that wire rod provides contact area; (b) wire rod is passed through on the annealing zone of two annealing wheel assemblies; (c) voltage is applied between first annealing zone (from lamellar body and the electric current by annealing zone) and second annealing zone, and under the condition of the annealing temperature that wire rod is heated at least wire rod, make electric current pass to wire rod thus, and thus wire rod is annealed, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
The invention still further relates to two process that are used to make annealing zone, comprise that step (a) cuts into band with plate; (b) form annealing zone by band; Wherein said metallic plate forms by consolidated powder component is subjected to thermo-mechanical treatment; Described consolidated powder component forms by making refractory metal powder be consolidated into consolidated powder component; And described powder has carried out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, and wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.The invention still further relates to a process that is used to make annealing zone, comprise by band forming annealing zone, wherein said band cuts down on the slave plate, and described plate forms by consolidated powder component is subjected to thermo-mechanical treatment; Described consolidated powder component forms by making refractory metal powder be consolidated into consolidated powder component, wherein said powder carries out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, and wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
The invention still further relates to a kind of member that comprises refractory metal annealing bands, wherein said refractory metal is from comprising (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) are from comprising copper, nickel, titanium, iron, the alloy of the non-refractory metal that chooses in the group of cobalt, and (j) select in the group of its combination, so that annealing zone has the thickness in about 0.01 " to about 0.5 " scope, width in about 0.25 " to about 10 " scope, " arrive the diameter in about 6 feet scopes, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium about 1.5.
Description of drawings
In conjunction with the accompanying drawings, and with reference to the following description and the appended claims, these and other feature of the present invention, aspect and advantage will become and be easier to understand, wherein:
Fig. 1 is the side view of annealing zone;
Fig. 2 is the cross-sectional view of annealing zone shown in Figure 1;
Fig. 3 is the side view that comprises the annealing wheel assembly of annealing zone;
Fig. 4 is the cross-sectional view of annealing wheel assembly shown in Figure 3;
Fig. 5 is the side view of continuous no gap of the present invention annealing zone;
Fig. 6 shows the annealing zone that has in the gap of non-destructive position; With
Fig. 7 shows the annealing zone that has in the gap of destructive position.
The specific embodiment
The present invention relates to a kind of technology that is used to make annealing zone.Described technology comprises step (a) production refractory metal powder; (b) powder and oxide component or nitride component or carbide ingredient are mixed; (c) make powder or mixture of powders carry out fixed and form consolidated powder component; (d) make consolidated powder component be subjected to thermal-mechanical treatment and form plate or pipe; (e) plate or pipe are cut into band or ring; (f) form annealing zone by band, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.The refractory metal powder of using among the present invention can be any refractory metal powder, and described refractory metal powder is produced annealing zone of the present invention when carrying out treatment step of the present invention.The example of suitable refractory metal powder comprises the alloy of the non-refractory metal that those are chosen by (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) and (j) refractory metal powder made of its composition from the group that comprises copper, nickel, titanium, iron, cobalt.As used herein, term " refractory metal " is applicable to the composition of refractory metal, refractory metal alloy or refractory metal and refractory metal alloy.
Powder has abundant low oxygen content so that powder can carry out fixed and be subjected to thermo-mechanical treatment.In one embodiment, refractory metal powder comprises having less than about 300ppm, preferably is lower than 200ppm and more preferably less than the powder of the alloy of tantalum, niobium or the tantalum of the oxygen content of 100ppm or niobium.This powder can be made by a kind of technology, described technology comprises that step (i) provides the hydride powder of first metal of-100 orders (or-60 orders), described first metal is from comprising tantalum, a kind of in the alloy that niobium and these metals form each other or these metals or all with in the group of the alloy of other metal formation select, (ii) existence have affinity than first metal higher for the situation of the metal of the affinity of oxygen under the hydride of heating first metal in single heating cycle, to remove dehydrogenation and oxygen, (iii) from metal, remove subsequently and describedly have the metal of higher affinity for oxygen and (iv) form first metal dust that has less than the oxygen content of 300ppm thus.In U.S. Patent No. 6,261, this powder has been carried out further description in 337, the integral body of described patent is cited as a reference at this.
Optionally, refractory metal powder carries out mixing with oxide component or nitride component or carbide ingredient before fixed at it.Suitable oxide is included in the steady oxide in the selected metal system.The example of steady oxide includes but not limited to the combination of magnesia, silica, yittrium oxide, zirconia, lanthana, calcium oxide and these oxides.The spendable amount of these oxides is at least about 5ppm and can be at about 5ppm in the scope of about 1000ppm or in about 10ppm arrives the scope of about 500ppm.Suitable nitride is included in the stable nitride in the selected metal system.The example of suitable nitride includes but not limited to niobium nitride, tantalum nitride, zirconium nitride, hafnium nitride and their mixture.The spendable amount of these nitride is at least about 5ppm and can be at about 5ppm in the scope of about 1000ppm or in about 10ppm arrives the scope of about 500ppm.Suitable carbide is included in those stable in selected metal system carbide.The example of stable carbide includes, but are not limited to: the combination of TaC, NbC, WC, HfC, ZrC, TiC and these carbide.The spendable amount of these carbide is at least about 10ppm and can be at about 5ppm in the scope of about 1000ppm or in about 10ppm arrives the scope of about 500ppm.
Can by any make refractory metal powder can be subjected to treatment step of the present invention that powder is carried out is fixed so that can make the technology of annealing zone of the present invention.The example of suitable technology comprises the combination of expressing technique, heat and other static pressuring processes, compacting and sintering process and aforementioned technology.
When selecting expressing technique, powder carries out fixed under the temperature of about room temperature (25 ℃) in about 3300 (about 1815 ℃) scopes.Before extruding and the area of the technology after extruding reduce can be at about 5: 1 in about 20: 1 scope.In a preferred embodiment, extrude before and extrude after the area of technology be reduced to about 9: 1.
When selecting isostatic pressing process, powder optionally is subjected to pressing step.Preferably by powder is placed on optionally scribble the barrier layer for example in the high temperature insostatic pressing (HIP) jar of molybdenum, described jar of emptying, described jar is placed in the high temperature insostatic pressing (HIP) container and described container is subjected under about 1500 (about 815 ℃) temperature in about 2600 (about 1427 ℃) scopes, assign at about 1 hour to about 10 hours to the pressure in the scope of about 45ksi at about 10ksi, preferably under 2300 °F (about 1260 ℃), reach about 6 hours at least about 30ksi, the high temperature insostatic pressing (HIP) condition, implement the high temperature insostatic pressing (HIP) step.
When powder is undertaken may using the combination of single shaft pressing process, isostatic cool pressing technology and these technologies when fixed by compacting and sintering step.In one embodiment, replace making that pressed powder carries out sintering step is, described pressed powder is subjected to the electrical resistance sintering condition, thereby wherein electric current carries out sintering to produce enough heats to metal dust by described powder.
The size of consolidated powder component can change according to application.Generally, the length of consolidated powder component is at least about 4 " (about 10cm), the width of consolidated powder component is at least about 2 " (about 5cm), and the height of consolidated powder component is at least about 2 " (about 5cm).In another embodiment, the length of consolidated powder component is in the scope of about 4 " (about 10cm) is to about 40 " (about 101cm), and " (about 10cm) is in the scope of about 30 feet (914cm) preferably about 4.In another embodiment, the width of consolidated powder component is in the scope of about 0.5 " (about 1.3cm) is to about 3 " (about 7.6cm), preferably in about 0.5 " (about 1.3cm) is to about 40 " scope (1219cm).In another embodiment, the height of consolidated powder component is in about 0.5 " (about 1.3cm) is to about 3 " scope (7.6cm), preferably in about 0.5 " (about 1.3 ") to about 40 " in the scope of (about 1219cm).
Hot mechanical treatment step comprises the combination of forging, rolling and annealing steps.
Can implement to forge step under any condition of annealing zone of the present invention making it possible to form.In one embodiment, under the temperature in from about room temperature to about 1800 scopes, preferably at room temperature implement to forge step, forge the thickness that has in about 0.5 " to about 15 " (about 1.3cm is to about 38cm) scope, the width in about 2 " to about 60 " (about 5cm arrives about 152cm) scope and " arrive the sheet billet of the about 30 feet length in (about 5cm arrives about 914cm) scopes about 2.In another embodiment, sheet billet has about 1.5 inches thickness, about 4.5 inches width and the length of about 40 inches (102cm).
Can implement rolling step under any condition of annealing zone of the present invention making it possible to form.Rolling step generally include with sheet billet be rolled into the thickness that has in about 0.010 " to about 0.5 " (about 0.03cm is to about 1.3cm) scope, in about 0.25 " to about 60 " (about 0.64cm arrives about 152cm) scope width and " arrive the plate of the about 100 feet length in (about 12.7cm arrives about 3048cm) scopes about 5.In another embodiment, plate has about 4 millimeters thickness, about 30 inches width and the length of about 5 feet (about 152.4cm).
Can implement annealing steps making it possible to form under any condition of annealing zone of the present invention.Generally, about 850 ℃ in about 2000 ℃ scope, preferably under about 1000 temperature in about 1400 ℃ of scopes, implement annealing steps.
In one embodiment, described technology further comprises at least one intermediate annealing step.Described annealing steps preferably is implemented after about total deformation of 70% to 90%.For example, when consolidated powder component is rolled and its thickness is reduced to the about 80% time of its original depth, can before forging step, implement the intermediate annealing step.
Plate is cut into the thickness that has in about 0.01 " (about 0.03cm) is to about 0.5 " (about 1.3cm) scope, the width in about 0.25 " (about 0.64cm) arrives about 10 " (about 305cm) scope and " (about 12.7cm) arrives the band of the length in about 20 feet (about 610cm) scopes about 5.In one embodiment, band is the niobium band with the hardness in about 60 Vickers hardnesses arrive about 200 Vickers hardness scopes.In another embodiment, band is the molybdenum band with the hardness in about 190 Vickers hardnesses arrive about 400 Vickers hardness scopes.In another embodiment, band is the tungsten rod band with the hardness in about 300 Vickers hardnesses arrive about 600 Vickers hardness scopes.
By band being placed on 3 benders (three point bender) are gone up or can forming annealing zone by the method that band forms annealing zone by any other.
In one embodiment, annealing zone of the present invention can be made by ingot metallurgy (I/M) technology.
The alloy of the non-refractory metal that annealing zone of the present invention is chosen from the group that comprises copper, nickel, titanium, iron, cobalt by (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) and (j) their combination make.Annealing zone can be attached on the annealing wheel assembly of online annealing device.When annealing zone was used in the online annealing device, it was surpassing in continued operation period of annealing device of 36 hours effectively, or surpassed 160 hours or in continued operation period of longer annealing device effectively.In one embodiment, annealing zone is remained valid surpassing in continued operation period of 36 to about 160 hours annealing devices in the scope.
When claiming annealing zone to be " effectively ", it means that annealing zone can anneal continuously to the wire rod in the online annealing device, and does not need to change annealing zone and need not make online annealing device (or processing line) shutdown.
Annealing zone of the present invention preferably has high arc resistance, and described high arc resistance is relevant with high-melting-point and be considered to favorable properties in the annealing zone.
Further, annealing zone preferably not with contact high temperature under the wire rod of annealing zone, for example copper wire dissolves each other.
The size of annealing zone is such so that annealing zone can be used for using the wire rod of annealing zone to make in the machine.Annealing zone preferably has thickness in about 0.01 " to about 0.5 " scope, the width in about 0.25 " to about 10 " scope and " arrives the diameter in about 6 feet scopes about 1.5.In one embodiment, annealing zone have the thick thickness of about 4mm, about 20 in about 25mm scope width and at about 350 diameters that arrive in about 500mm scope.Annealing zone can be that (i) is open-ended, (ii) is welded together, or (iii) open-ended and have an end, inclined-plane of overlapping.
Advantageously, annealing zone of the present invention preferably has uniform microstructure.For example, when annealing zone spreads all over (1) refractory metal in the annealing zone and (2) non-refractory metal for example copper or nickel or titanium or iron or cobalt is made by distributing equably.Another kind of optional mode is that when annealing zone of the present invention was made by the combination of refractory metal, the chemical composition of alloy was uniform in annealing zone.And when annealing zone was made by single refractory metal, the microstructure of annealing zone was uniform in annealing zone.The uniformity of distribution mutually, chemical composition and microstructure is corresponding to uniform physical property, the feature paid attention to for wire manufacturers.
In use, explained hereafter of the present invention goes out suitable refractory metal powder.Described powder optionally mixes with oxide component or nitride component or carbide ingredient, and described powder or mixture of powders carry out fixed so that consolidated powder component forms.Consolidated powder component is subjected to thermo-mechanical treatment, and forms plate.Plate is cut into band and annealing zone is formed by band.
When powder formation step, powder consolidation step and plate formation step have been carried out in advance, for example, when these steps are carried out by the service provider, the present invention includes two process that are used to make annealing zone, comprise that step (a) cuts into band with plate; (b) form annealing zone by band, wherein said metallic plate forms by consolidated powder component is subjected to thermo-mechanical treatment, and wherein said consolidated powder component forms by making refractory metal powder be consolidated into consolidated powder component, so that powder carries out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it.
When powder forms step, the powder consolidation step, when plate formation step and plate cutting step have been carried out in advance, the present invention includes the single stage technology that is used to make annealing zone, comprise by band and form annealing zone, wherein said band cuts down on the slave plate, described plate forms by consolidated powder component is subjected to thermo-mechanical treatment, and wherein said consolidated powder component is shaped by making refractory metal powder be consolidated into consolidated powder component, so that powder carries out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
For the wire rod manufacturing process, the present invention includes and be used for technology that metal wire rod is annealed, wherein be provided with two annealing wheel assemblies.Each annealing wheel (sheet) assembly comprises first annealing wheel (lamellar body), second annealing wheel (plate) and annealing zone, wherein be attached to described first annealing wheel (body) and second annealing wheel (plate) gone up each other and have the refractory metal annealing bands that is positioned between first annealing wheel (body) and second annealing wheel (plate) respectively, with thinking that wire rod provides contact area.Annealing zone can for example be attached on annealing wheel (sheet) assembly by annealing zone being clipped in annealing wheel (sheet) assembly by any suitable technology.Wire rod on the annealing zone of two annealing wheel assemblies by and voltage be applied between first annealing zone and second annealing zone so that electric current passes through wire rod under the condition of the annealing temperature that wire rod is heated at least wire rod.Transmitting the voltage that comes out from annealing device can change according to application.
The wire rod that can carry out this annealing conditions comprises copper wire, copper alloy silk, aluminium wire, aluminum-alloy wire, steel wire, steel alloy silk and their combination.The size of spendable wire rod can be in about 0.002 " (about 0.006cm) is to about 0.1 " (about .23cm) scope.Certainly, the wire rod with other size also can be used.
Referring to accompanying drawing, Fig. 1 shows the side view of open-ended annealing zone 5.Hatching 1 and 3 among Fig. 1 refers to the cross-sectional view of annealing zone shown in Figure 2; Fig. 3 shows the annealing wheel assembly 11 that comprises annealing zone 13; Refer to cross-sectional view shown in Figure 4 with hatching 7 and 9, wherein annealing zone 15 is attached on annealing wheel 17 and 19.
In one embodiment, annealing zone of the present invention has the gap.Yet in another embodiment, annealing zone of the present invention is continuous and does not comprise the gap.Fig. 5 shows continuous no gap annealing zone constructed in accordance.Fig. 6 shows the annealing zone in the gap (gap does not overlap with the wire rod that leaves band) that has in non-destructive position.Fig. 7 shows the annealing zone in the gap (gap overlaps with the wire rod that leaves band) that has in destructive position.What be not bound by theory is to it is believed that when annealing zone has the gap it has destroyed circuit (in described circuit, electric current is transferred into wire rod from annealing zone), and increased the possibility (band is subjected to undesirable erosion) of arc discharge or arc discharge.The use of band has reduced arc discharge continuously.
Advantageously, the use of continuous annealing band allows wearing and tearing by the whole length that distributes and spread all over band equably.The use of continuous annealing band has applied continuous electric field in entire belt, and the arc discharge that therefore distributes equably in entire belt, and the potential possibility of having removed the excessive arc discharge that is caused by the gap in the band.At present, in common annealing band (comprising the gap), arc discharge concentrates on 14% be with, and has just surpassed the gap.
The life-span of continuous annealing band constructed in accordance is longer and significantly longer than the life-span of annealing zone constructed in accordance (having the gap) usually.Generally, compare with annealing zone (having the gap) constructed in accordance, continuous annealing band of the present invention has and exceeds at least about 50% to about 80% or surpass for 80% life-span.Compare with common annealing band (not using material of the present invention to make), continuous annealing band of the present invention continues in common use at least about 100%, or surpasses approximately 200%, or surpasses for 300% life-span.In one embodiment, with the common annealing band, for example nickel strap is compared, and continuous annealing band of the present invention continues from about 100% to about 1000%, or the longer life-span.
Continuous annealing band of the present invention can be made by any proper method.Generally, length by determining band and circularity and as mentioned above after manufacturing the two ends of connecting band make the continuous annealing band.The shaping of band can utilize standard metal processing practice and finish, and the end connects and also can utilize standard metal processing practice, for example 3 bendings and welding and realize.Other possible manufacture method to produce have enough diameters and thickness and cross-sectional width pipe to produce continuous band.
Advantageously, the invention provides improved annealing zone, be used to the improved method making the improved method of this band and be used for wire rod is annealed.The period that annealing zone of the present invention can replace the conventional annealing band and allow wire manufacturers that the running of operation annealing device is prolonged.Safeguard and equipment downtime because the use of annealing zone can reduce, so the present invention is particularly useful for the online annealing device in the wire rod manufacturing.When using niobium annealing zone of the present invention, but the comparable conventional nickel strap durability of niobium band is high more than 10 times.
In following illustrative examples the present invention is further described, unless otherwise mentioned, all parts and percentage are all calculated by weight in described example.
Example
Example 1
Technical process
When multiple material being cut, its cutting rate (seeing the following form) is measured by discharge processing (EDM).In this example, wire rod is used as cutting element (wire rod-discharge processing).For discharge processing, workpiece is immersed in oil product or the water.Voltage is applied between workpiece and the wire rod, and make wire rod so near workpiece so that cause electric arc from wire rod to workpiece.Each arc evaporation the very a spot of material in surface of the work place.When workpiece is etched by arc discharge, the wire rod cut workpiece.Utilizing the accessible cutting rate of this method is the indication of material arc resistance.The high arc resistance of slow cutting rate representation.Following table has been listed the cutting rate that is quantized as " cutting area/hour " (square inch/hour).Can see that niobium has than the much lower cutting rate of any other test material.
Discharge processing (EDM) test shows the slow cutting speed (seeing the following form 1) of Nb.
Table 1
| Material | Cutting rate (In 2/hr) |
| CuCrNb | 4.512 |
| CuCrNb | 3.600 |
| Glidcop TM | 3.510 |
| Copper | 3.066 |
| Cu18Nb | 2.832 |
| Ni201 | 2.646 |
| Glidcop TM | 2.160 |
| Glidcop TM&Nb | 1.962 |
| Niobium | 0.936 |
" Glidcop
TM" be oxide dispersion intensifying (ODS) copper alloy that OMG company produces.
Infer that from these results niobium has the repellence for electron discharge higher than other material.Because electron discharge is one of main abrasion mechanism of annealing zone, infer further that therefore the annealing zone made by Nb will get slower and they will have the life-span longer than other band than the belt wear of being made by other material.
Example 2
Technical process
Determine the Vickers hardness measurement according to ASTM E92-82, how described ASTM E92-82 carries out the well-known standard that Vickers hardness is measured for having described in detail very much.Table 2 shows the Vickers hardness that obtains for the different materials rank.
Table 2
| Material grade | Vickers hardness number |
| I/M Nb | 70 |
| P/M Nb | 110 |
(I/M): ingot metallurgy
(P/M): powder metallurgy
The result shows that other Nb of P/M level is obviously hard than other Nb of I/M level.Infer that from these results P/M Nb has the repellence for mechanical erosion higher than I/M Nb.Because mechanical erosion is one of main abrasion mechanism of annealing zone, infer further that therefore the annealing zone made by P/M Nb will get slower and they will have than the longer life-span of I/MNb band than the belt wear of being made by I/M Nb.
Although in conjunction with preferred embodiments more of the present invention the present invention is described in detail, other modification also is possible.Therefore, the spirit and scope of claims should not be subject to the description to the embodiment that comprises at this.
Claims (51)
1, a kind of technology that is used to make annealing zone, described technology comprises:
(a) production refractory metal powder;
(b) described powder and oxide component or nitride component or carbide ingredient are mixed;
(c) make the fixed and formation consolidated powder component of described powder or mixture of powders;
(d) make described consolidated powder component be subjected to thermal-mechanical treatment and form plate;
(e) described plate is cut into band; And
(f) form annealing zone by described band, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
2, technology according to claim 1, wherein said refractory metal are from alloy that comprises the non-refractory metal that (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) choose from the group that comprises copper, nickel, titanium, iron, cobalt and the component that (j) chooses in the group of their combination.
3, technology according to claim 1, wherein said annealing zone has uniform microstructure.
4, technology according to claim 1, wherein said powder have abundant low oxygen content so that described powder can carry out fixed and be subjected to thermo-mechanical treatment.
5, technology according to claim 1, wherein said refractory metal powder has the oxygen content less than about 300ppm.
6, technology according to claim 1, wherein said oxide is selected from the group that comprises magnesia, silica, yittrium oxide, zirconia, lanthana, hafnium oxide, calcium oxide and their combination.
7, technology according to claim 1, wherein said carbide ingredient comprise the carbide that chooses the group of stable carbide outside comprising TaC, WC, HfC, TiC, NbC, ZrC, aforementioned carbide and their combination.
8, technology according to claim 1, wherein said powder is undertaken fixed by the technology that chooses from the group of the combination that comprises expressing technique, heat and other static pressuring processes, compacting and sintering process and aforementioned technology.
9, technology according to claim 1, wherein said powder carries out fixedly under the temperature of about room temperature in about 3300 scopes by extruding, and described technology has before about 9: 1 the extruding and the area after extruding reduces.
10, technology according to claim 1, the described powder that wherein optionally is subjected to pressing step is undertaken fixed by high temperature insostatic pressing (HIP).
11, technology according to claim 10, wherein by described powder is placed in the high temperature insostatic pressing (HIP) jar that optionally scribbles the barrier layer, emptying is described jar, described jar is placed in the high temperature insostatic pressing (HIP) container and described container is under about 1500 temperature in about 2600 scopes, under the pressure in about 10ksi arrives the scope of about 45ksi, reach the high temperature insostatic pressing (HIP) condition in about 1 hour to about 10 hours scope, implement described high temperature insostatic pressing (HIP) step.
12, technology according to claim 1, wherein said powder is undertaken fixed by compacting and sintering step, and described pressing step is selected from the group that comprises single shaft pressing process, isostatic cool pressing technology and their combination.
13, technology according to claim 10, replace wherein making that described pressed powder carries out sintering step is, described pressed powder is in the electrical resistance sintering condition, thereby wherein electric current carries out sintering to produce sufficient heat to described metal dust by described powder.
14, technology according to claim 1, wherein said hot mechanical treatment step comprise the combination of forging, rolling and annealing steps.
15, technology according to claim 14, wherein under the temperature of about room temperature in about 1800 ℃ of scopes, implement described forging step, forge the thickness that becomes to have in about 0.5 " to about 15 " scope, the width in about 2 " to about 60 " scope and " arrive the sheet billet of the length in about 30 feet scopes about 2.
16, technology according to claim 15, wherein said sheet billet have about 1.5 inches thickness, about 4.5 inches width and about 40 inches length.
17, technology according to claim 14, wherein said rolling step comprise with sheet billet be rolled into the thickness that has in about 0.010 " to about 0.5 " scope, in about 0.25 " to about 60 " scope width and " arrive the plate of the length in about 100 feet scopes about 5.
18, technology according to claim 17, wherein said plate have about 4 millimeters thickness, about 30 inches width and about 5 feet length.
19, technology according to claim 14 is wherein implemented described annealing steps under about 850 ℃ of temperature that arrive in about 2000 ℃ of scopes.
20, technology according to claim 14, wherein said technology further comprise at least one intermediate annealing step.
21, technology according to claim 14, wherein said plate are cut into the thickness that has in about 0.01 " to about 0.5 " scope, the width in about 0.25 " to about 10 " scope and " arrive the band of the length in about 20 feet scopes about 5.
22, technology according to claim 21, wherein said band are the niobium band with the hardness in about 60 Vickers hardnesses arrive about 200 Vickers hardness scopes.
23, technology according to claim 21, wherein said band are the molybdenum band with the hardness in about 190 Vickers hardnesses arrive about 400 Vickers hardness scopes.
24, technology according to claim 21, wherein said band are the tungsten rod band with the hardness in about 300 Vickers hardnesses arrive about 600 Vickers hardness scopes.
25, technology according to claim 1 is wherein by being placed on described band on 3 benders or forming the annealing zone described annealing zone that is shaped by any other manufacturing process and with described band.
26, technology according to claim 1, wherein said annealing zone have the thickness in about 0.01 " to about 0.5 " scope.
27, technology according to claim 1, wherein said annealing zone have the width in about 0.25 " to about 10 " scope.
28, technology according to claim 1, wherein said annealing zone has about 1.5 " arrives the diameter in about 6 feet scopes.
29, technology according to claim 1, wherein said annealing zone have the thick thickness of about 4mm, about 20 in about 25mm scope width and at about 350 diameters that arrive in about 500mm scope.
30, technology according to claim 1, wherein said technology further comprise described annealing zone are attached on the annealing wheel assembly of online annealing device.
31, technology according to claim 1, wherein said annealing zone are that (i) is open-ended, (ii) is welded together, or (iii) open-ended and have an end, inclined-plane of overlapping.
32, the annealing zone that adopts technology according to claim 1 to produce.
33, a kind of member that comprises refractory metal annealing bands, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
34, annealing zone according to claim 32, wherein said refractory metal is selected in the group of their combination from the alloy that comprises the non-refractory metal that (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) choose from the group that comprises copper, nickel, titanium, iron, cobalt with (j).
35, annealing zone according to claim 34, wherein said annealing zone has uniform microstructure.
36, annealing zone according to claim 34, wherein said annealing zone have thickness in about 0.01 " to about 0.5 " scope, the width in about 0.25 " to about 10 " scope and " arrive the diameter in about 6 feet scopes about 1.5.
37, annealing zone according to claim 34, wherein when described annealing zone is used in the online wire annealing device, wherein said annealing zone is remained valid surpassing in continued operation period of annealing device of 36 hours.
38, annealing zone according to claim 34, wherein when described annealing zone is used in the online wire annealing device, described annealing zone is remained valid surpassing in continued operation period of annealing device of 160 hours.
39, a kind of technology that metal wire rod is annealed of being used for comprises:
(a) two annealing wheel assemblies are set, each assembly comprises first annealing wheel, second annealing wheel and annealing zone;
Wherein be attached to described first annealing wheel gone up each other and described second annealing wheel and have refractory metal annealing bands between described first annealing wheel and described second annealing wheel respectively, with thinking that wire rod provides contact area;
(b) wire rod is passed through on the described annealing zone of two annealing wheel assemblies;
(c) voltage is applied between described first annealing zone and described second annealing zone, and therefore under the condition of the annealing temperature that described wire rod is heated at least described wire rod with current delivery to described wire rod, thus described wire rod is annealed, wherein at least one annealing zone has been got rid of the annealing zone that comprises copper and niobium.
40, according to the described technology of claim 39, wherein said wire rod is selected from the group that comprises copper wire, copper alloy silk, aluminium wire, aluminum-alloy wire, steel wire, steel alloy silk and their combination.
41, according to the described technology of claim 39, wherein said refractory metal is selected in the group of their combination from the alloy that comprises the non-refractory metal that (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) choose from the group that comprises copper, nickel, titanium, iron, cobalt with (j).
42, according to the described technology of claim 39, wherein said annealing zone has uniform microstructure.
43, a kind of technology that is used to make annealing zone comprises:
(a) plate is cut into band; With
(b) form annealing zone by described band;
Wherein said metallic plate is shaped by consolidated powder component is subjected to thermo-mechanical treatment;
Wherein said consolidated powder component forms by making refractory metal powder be consolidated into consolidated powder component; With
Wherein said powder has carried out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, and wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
44, according to the described technology of claim 43, wherein said annealing zone has uniform microstructure.
45, a kind of technology that is used to make annealing zone comprises by described band forming annealing zone;
Wherein said band cuts down on the slave plate, and described plate forms by described consolidated powder component is subjected to thermo-mechanical treatment;
Wherein said consolidated powder component forms by making refractory metal powder be consolidated into consolidated powder component; With
Wherein said powder carries out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, and wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
46, according to the described technology of claim 45, wherein said annealing zone has uniform microstructure.
47, a kind of member that comprises refractory metal annealing bands with uniform microstructure, wherein said refractory metal is selected in the group of their combination from the alloy that comprises the non-refractory metal that (a) niobium, (b) tantalum, (c) molybdenum, (d) tungsten, (e) niobium alloy, (f) tantalum alloy, (g) molybdenum alloy, (h) tungsten alloy, (i) (1) refractory metal and (2) choose from the group that comprises copper, nickel, titanium, iron, cobalt with (j), and
Wherein said annealing zone has thickness, the width in about 0.25 " to about 10 " scope in about 0.01 " to about 0.5 " scope, " arrive the diameter in about 6 feet scopes, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium about 1.5.
48, according to the described annealing zone of claim 47, wherein said annealing zone is made by a kind of technology, and described technology comprises:
(a) production refractory metal powder;
(b) described powder and oxide component or nitride component or carbide ingredient are mixed;
(c) make described powder or mixture of powders carry out fixed and form consolidated powder component;
(d) make described consolidated powder component be subjected to thermal-mechanical treatment and form plate or pipe;
(e) described plate or pipe are cut into band or ring; With
(f) form described annealing zone by described band or ring, wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
49, according to the described annealing zone of claim 47, wherein said annealing zone is made by a kind of technology, and described technology comprises:
(a) plate is cut into band; With
(b) form annealing zone by described band;
Wherein said metallic plate forms by described consolidated powder component is subjected to thermo-mechanical treatment;
Wherein said consolidated powder component is by making refractory metal powder or refractory metal alloy powder consolidation become consolidated powder component to form; With
Wherein said powder has carried out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it.
50, according to the described annealing zone of claim 47, wherein said annealing zone is made by a kind of technology, and described technology comprises by band and forms annealing zone;
Wherein said band cuts down on the slave plate, and described plate forms by described consolidated powder component is subjected to thermo-mechanical treatment; With
Wherein said consolidated powder component is by making refractory metal powder or refractory metal alloy powder consolidation become consolidated powder component to form,
Wherein said powder carries out optionally mixing with oxide component or nitride component or carbide ingredient before fixed at it, and wherein said annealing zone has been got rid of the annealing zone that comprises copper and niobium.
51, according to the described annealing zone of claim 47, wherein said annealing zone is continuous no gap annealing zone.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US44400403P | 2003-01-31 | 2003-01-31 | |
| US60/444,004 | 2003-01-31 |
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| US (1) | US20060115372A1 (en) |
| EP (1) | EP1594645A2 (en) |
| JP (1) | JP2006517615A (en) |
| KR (1) | KR20050094472A (en) |
| CN (1) | CN1744961A (en) |
| AU (1) | AU2004209010A1 (en) |
| BR (1) | BRPI0407168A (en) |
| CA (1) | CA2514118A1 (en) |
| IL (1) | IL169536A0 (en) |
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| CN109402541A (en) * | 2017-08-15 | 2019-03-01 | 核工业西南物理研究院 | A kind of dispersed particle-strengthened tungsten block materials preparation method |
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| US20130264314A1 (en) * | 2010-10-18 | 2013-10-10 | Nippon Tungsten Co., Ltd. | Electrode for electric discharge machining |
| CN104046822B (en) * | 2014-07-08 | 2016-01-13 | 西北有色金属研究院 | A kind of solution strengthening preparation has the method for the tantalum-base alloy of gradient-structure |
| EP3346017B1 (en) * | 2017-01-10 | 2021-09-15 | Heraeus Deutschland GmbH & Co. KG | Method for cutting refractory metals |
| CN109306421B (en) * | 2018-09-18 | 2019-09-17 | 厦门虹鹭钨钼工业有限公司 | A kind of anti-erosion molybdenum alloy electrode and its manufacturing method |
| DE102019005944A1 (en) * | 2019-08-23 | 2021-02-25 | Grohe Ag | Method for producing a component, in particular for a sanitary fitting |
| CN111334679B (en) * | 2020-04-23 | 2021-11-30 | 合肥工业大学 | Processing method of tungsten-yttrium oxide composite material with excellent thermal stability |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR1459895A (en) * | 1965-08-23 | 1966-06-17 | Kennecott Copper Corp | Process for manufacturing metal strips and metal strips thus obtained |
| GB1406317A (en) * | 1972-10-11 | 1975-09-17 | Standard Telephones Cables Ltd | Thermal conditioning of wire |
| US3989923A (en) * | 1972-10-11 | 1976-11-02 | International Standard Electric Corporation | Wire heat treating apparatus |
| US4549754A (en) * | 1983-06-20 | 1985-10-29 | Reed Tubular Products Company | Tool joint |
| AT386612B (en) * | 1987-01-28 | 1988-09-26 | Plansee Metallwerk | CRISP-RESISTANT ALLOY FROM MELTING-MELTING METAL AND METHOD FOR THEIR PRODUCTION |
| AT389326B (en) * | 1987-11-09 | 1989-11-27 | Plansee Metallwerk | METHOD FOR PRODUCING SEMI-FINISHED PRODUCTS FROM Sintered Refractory Metal Alloys |
| AT392432B (en) * | 1989-05-03 | 1991-03-25 | Plansee Metallwerk | METHOD FOR THE PRODUCTION OF WARM-CRAWL-RESISTANT SEMI-FINISHED PRODUCTS OR MOLDED PARTS FROM HIGH-MELTING METALS |
| ES2020131A6 (en) * | 1989-06-26 | 1991-07-16 | Cabot Corp | Powders and products of tantalum, niobium and their alloys |
| US5242481A (en) * | 1989-06-26 | 1993-09-07 | Cabot Corporation | Method of making powders and products of tantalum and niobium |
| US6375708B1 (en) * | 1994-12-22 | 2002-04-23 | Osram Sylvania Inc. | Alloy for electrical contacts and electrodes and method of making |
| US6521173B2 (en) * | 1999-08-19 | 2003-02-18 | H.C. Starck, Inc. | Low oxygen refractory metal powder for powder metallurgy |
| US6467818B1 (en) * | 1999-10-01 | 2002-10-22 | Grant Prideco, L.P. | Drill collar box |
| MXPA04007104A (en) * | 2002-01-23 | 2004-10-29 | Starck H C Inc | Stabilized grain size refractory metal powder metallurgy mill products. |
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| CN109402541A (en) * | 2017-08-15 | 2019-03-01 | 核工业西南物理研究院 | A kind of dispersed particle-strengthened tungsten block materials preparation method |
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| Publication number | Publication date |
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| EP1594645A2 (en) | 2005-11-16 |
| KR20050094472A (en) | 2005-09-27 |
| JP2006517615A (en) | 2006-07-27 |
| AU2004209010A1 (en) | 2004-08-19 |
| ZA200515979B (en) | 2006-11-29 |
| WO2004069453A3 (en) | 2004-12-09 |
| CA2514118A1 (en) | 2004-08-19 |
| MXPA05008067A (en) | 2005-09-21 |
| BRPI0407168A (en) | 2006-02-07 |
| IL169536A0 (en) | 2007-07-04 |
| WO2004069453A2 (en) | 2004-08-19 |
| US20060115372A1 (en) | 2006-06-01 |
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