比利时专利BE1019089A5 HIGH-TEMPERATURE-RESISTANT COATING BRAZING METAL MODIFIED TO REDUCE THE MELT POINT.

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专利摘要:
As part of a brazing filler metal resistant to high temperatures, consisting of a mixture of metals whose main components are molybdenum and ruthenium, in accordance with the invention, in the brazing filler mixture, a metal is dissolved, as a secondary component, in one or more phases which consist mainly of ruthenium or of molybdenum. In particular, the brazing filler metal consists of a single phase, has a melting point which is less than 1900 ° C and is produced as a metallic granulation product. For the manufacture of a preferred high temperature resistant brazing filler metal, a melt is subjected to quenching.
公开号:BE1019089A5
申请号:E2008/0563
申请日:2008-10-13
公开日:2012-03-06
发明作者:Tanja Eckardt；David Francis Lupton
申请人:Heraeus Gmbh W C；
IPC主号:

专利说明:

High temperature resistant MoRu solder metal, modified to lower the melting point
The present invention relates to a use of a mixture of metals as a high temperature resistant solder for the temperature range of 1700 ° C to 1900 ° C, in particular for the brazing of tungsten electrodes and molybdenum fixing rods, discharge lamps, manufacture and use thereof. For this purpose, it is possible to use platinum or rhodium or alloys based on these noble metals, in particular platinum-rhodium alloys. However, platinum and rhodium are very expensive noble metals, so there is a need for lower value solders.
US Pat. No. 2,725,287 discloses a molybdenum solder with a 2.50% boron addition having a melting point of 3950 ° F. (2180 ° C. ) and with silicon addition, a melting point of 3800 ° F (2090 ° C). The low solubility of silicon or boron limits the extent of the decrease in melting point. Mixtures of molybdenum and ruthenium, according to JP 58157593, JP 58016795 or JP 57142765, as well as a molybdenum sealing sheet having a eutectic molybdenum-ruthenium alloy coating, have at least the melting point too much. elevation of the eutectic, rising to 1955 ° C.
WO 2005/15600 discloses an electrode system having a MoRu-based eutectic coating, and DE 2 200 05 03 0113 discloses a solder material consisting of a sintered eutectic alloy with molybdenum / ruthenium base in the form of a wafer. MoRu alloys pose problems when applied in blind holes, while the use of MoRu wafers in the form of a non-flexible molded element and limited in the case of different bore geometries.
JP 16115395 discloses a ruthenium and molybdenum solder material with a titanium additive. However, titanium acts like a getter and weakens the solder connection.
JP 58204436 discloses decreasing the melting point by adding nickel to a eutectic solder consisting of ruthenium and molybdenum. The material is made from a carbonaceous paste which comprises, in addition to the carbonaceous binder, a powder mixture of the respective metals. This carbonaceous paste gives rise, in the commercial field of the lamps, to a blackening of the discharge vessel, giving rise to a lower emission of light.
DE 2 200 05 053 553 discloses a decomposable gel without leaving residues for the manufacture of soft solder pastes.
The object of the present invention is to provide a solder for the range of use of 1700 ° C to 1950 ° C, in particular 1800 ° C to 1900 ° C, without having to take into account the disadvantages. known from the prior art.
For the practice of the present invention, the melting point of a molybdenum and ruthenium metal alloy is reduced by the incorporation of a metal into the MoRu main component network structure, preferably by the addition of a metal having a melting point above 1000 ° C, in particular above 1450 ° C. The reduction of the maximum melting point according to the invention of a mixture of MoRu is reached by saturation. As soon as the solubility of the melting point decreasing component is exceeded in a MoRu alloy network, giving rise to the formation of a new phase, the high temperature strength properties of the solder metal deteriorate. in an undesirable way.
The realization of the object takes place with the features of the independent claims. The subordinate claims describe preferred embodiments.
According to the invention, metal bodies, in particular metal powders, metal granulation products or metal wires, which have a mixture, in particular an alloy of molybdenum, ruthenium and a metal dissolved in at least one of these constituents of the alloy.
In this way, according to the invention, a solder is provided, which consists exclusively of metal and which melt below the MoRu eutectic, in particular at a temperature below 1900 ° C. . Due to the variation in the fraction of the mechanical component decreasing the melting point, the melting point can be modified in a wide range, preferably in a range between 1800 ° C and 1900 ° C, to rise especially at a temperature which is below 1870 ° C. The phenomena of coarse grain growth and loss of strength which occur in the construction elements and the components to be joined, when high brazing temperatures above 1900 ° C are used, are stopped in accordance with the invention or well are removed in a way at least considerable.
The metal dissolved in the solder mixture will have a melting point greater than 1000 ° C, in particular greater than 1450 ° C and will be dissolved in the alloy at a concentration of between 1 and 20% by weight, particularly between 2 and 15% by weight, preferably between 5 and 12% by weight. Suitable metals are scandium, yttrium, vanadium, chromium, manganese, cobalt, copper, and gold, preferably iron and cobalt.
To avoid undesired phase formation, the alloy can be quenched from the melt. This produces a solder having a melting point congru.
According to the invention, a new quality of solder connections is obtained in discharge lamps having tungsten electrodes and molybdenum fixing rods, since these brazing filler metals are more temperature resistant than comparable brazing filler metals based on platinum or rhodium. Compared to mixtures of the molybdenum and ruthenium eutectic, the advantage of easier manufacture and braze bonding is obtained in the context of a reduction in the melting point of the Binary eutectic of 1955 ° C at a temperature below 1900 ° C, preferably up to a temperature below 1870 ° C, in particular up to a temperature below 1850 ° C. The brazing process at a temperature below 100 ° C. simplifies the manufacture of the solder joints themselves, respectively the discharge lamps, so that, according to the invention, there is also provided a simplified method for the manufacture of a solder connection between a tungsten electrode and a molybdenum attachment rod, therefore a simplified manufacture of a discharge lamp. For tungsten-doped electrodes and for molybdenum-doped fixation rods, the aforementioned advantages can also be implemented.
The use of organic binder based carbon is avoided in accordance with the invention, as well as an addition of boron or silicon compounds.
By way of exception, a solder paste comprising a gel which decomposes without leaving residues can be prepared, in particular according to DE 10 2005 053 553, which does not give rise to blackening of the ampoule. the lamp. The main constituents of the gels volatilize or decompose at relatively low temperatures of 150 ° C to 250 ° C. In this range, it is not yet confronted with an oxidation worthy of mention of the brazing construction elements, respectively of the solder. After removal of the organic constituents, it is possible to heat under the protection of an inert gas up to the brazing temperature, without any residual present disturbing the operation of the lamp.
High temperature resistant pastes according to the invention consist of an alloy consisting of a molybdenum-ruthenium matrix, a metal component dissolved therein and a flux which decomposes without leaving residues.
The brazing filler metal according to the invention is generally suitable for the brazing of refractory metals, in particular molybdenum, tungsten, tantalum and niobium. For this purpose, considerable advantages are expected in the field of energy technology, for example for heat exchangers in fuel cells operating at high temperatures, in furnace construction and in glass processing. .
Hereinafter, the invention is explained in more detail with reference to examples.
Figures 1 and 2 show the arrangement of the granulation product 3 according to the invention between the electrode heads 1 and the fixing rods 2.
FIG. 3 represents the brazing temperature of the MoRu granulation product as a function of the metal additive.
Example 1
An alloy consisting of 57% by weight of molybdenum and 43% by weight of ruthenium is heated to induction melting in a zirconium oxide crucible and cobalt is added to the molten mass in the amount of 9.2% by weight. The melt is poured into a copper shell cooled with water and is then analyzed. X-ray fluorescence spectrometry gives weight fractions of 9.0% by weight for cobalt, 39% by weight for ruthenium and 52% by weight for molybdenum. X-ray fluorescence spectrometry indicates a network structure of the MoRu intermetallic phase with a shift towards lower lattice steps, indicating the incorporation of a smaller cobalt atom into the MoRu lattice. The melting point is decreased relative to that of the pure MoRu alloy by about 110 ° C.
Example 2
In a similar manner to Example 1, with a cobalt content of 4.6% by weight, a melting point decrease of approximately 80 ° C. can be obtained.
Example 3
In a similar manner to Example 1, with a iron content of 9.0% by weight, a melting point decrease of about 110 ° C. can be obtained.
The solder is prepared in the form of a granulation product so that it can be adapted to the use, respectively to the respective geometry. The granulation product is prepared by sieving with particle sizes of 0.2 to 0.7 mm.
For the brazing of refractory materials in which a cylindrical rod 2 in a blind hole must be connected to a larger component, such as for example an electrode head 1, the blind hole is filled with a defined quantity of the granulation product 3 and the combination of materials is then heated by induction under vacuum or argon atmosphere, and until the brazing filler metal melts and fills the free space between the parts to be connected.
The granulation product may for example be prepared in the following manner: 1. Processing by machining bars or round bars melted, for example by turning, planing or milling; 2. Pouring the molten metal into a liquid, for example water; 3. Propulsion of the melt by means of a stream of gas in a nozzle (Laval); 4. Liquid metal spill onto a strongly cooled rotating cylinder (melt spinning).
The granulation product may also be adjusted to obtain defined particulate fractions by sieving, grading, or the like. The use of a granulation product offers particular advantages as regards the flexible implementation in variable geometries of the construction elements to be welded. Alternatively, the solder is prepared in the form of wire, wire section, washers, cut round bars, sheets, etc.

权利要求:
Claims (10)
[1]
1. Use of a mixture of metals having a melting point of less than 1900 ° C consisting of molybdenum and ruthenium as the main components and a secondary component which is dissolved in one or more phases which consist primarily of ruthenium or molybdenum, the secondary component representing a melting point reducing metal which is selected from the group consisting of cobalt, iron, manganese, chromium and vanadium, as a high temperature resistant solder.
[2]
2. Use of a high temperature resistant solder according to claim 1, which consists of a single phase.
[3]
Use of a high temperature resistant solder according to claim 1 or 2, characterized in that the high temperature resistant solder is a metal granulation product.
[4]
4. Use of a high temperature resistant solder according to any one of claims 1 to 3, comprising 30 to 60% by weight of molybdenum; ruthenium in the amount of 30 to 60% by weight; and another metal of from 2 to 20% by weight. i
[5]
5. A process for producing a high temperature resistant solder of a mixture of metals having a melting point of less than 1900 ° C consisting of molybdenum and ruthenium as the major components and a a secondary component which is dissolved in one or more phases which consist mainly of ruthenium or molybdenum, the secondary component representing a melting point reducing metal which is selected from the group consisting of cobalt, iron, manganese, chromium and vanadium, characterized in that a melt of this mixture is subjected to quenching.
[6]
A process for producing a solder connection between a tungsten-based electrode and a molybdenum-based fixation rod, characterized in that welding is carried out at a temperature below 1900 ° C with a solder metal based on a mixture of molybdenum-ruthenium and with an additional metal dissolved therein.
[7]
A method for manufacturing a discharge lamp, characterized in that an electrode and a fixing rod are welded to each other according to claim 6.
[8]
A brazing bond which connects a tungsten-based electrode to a molybdenum-based fixation rod, characterized by a brazing filler metal of a mixture of metals having a melting point of less than 1900 ° C consisting of molybdenum and ruthenium as main components and by a secondary component which is dissolved in one or more phases which consist mainly of ruthenium or molybdenum, the secondary component representing a melting point decreasing metal which is selected from the group consisting of group comprising cobalt, iron, manganese, chromium and vanadium.
[9]
9. A discharge lamp comprising a tungsten-based electrode and a molybdenum-based fixation rod, characterized in that the tungsten electrode and the molybdenum fixation rod are welded to each other at the same time. using a solder of a mixture of metals having a melting point of less than 1900 ° C consisting of molybdenum and ruthenium as the main components and a secondary component that is dissolved in one or more which consist mainly of ruthenium or molybdenum, the secondary component being a melting point reducing metal which is selected from the group consisting of cobalt, iron, manganese, chromium and vanadium.
[10]
10. Non-residue decomposing gel-containing paste and a high temperature resistant solder of a mixture of metals having a melting point below 1900 ° C of molybdenum and ruthenium of major components and by a secondary component which is dissolved in one or more phases which consist mainly of ruthenium or molybdenum, the secondary component representing a melting point reducing metal which is selected from the group consisting of cobalt, iron , manganese, chromium and vanadium.

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同族专利:

公开号 | 公开日

HU0800625A2|2009-05-28|

DE102007050487A1|2009-04-30|

HU0800625D0|2008-12-29|

引用文献:

公开号 | 申请日 | 公开日 | 申请人 | 专利标题

US2725287A|1952-11-26|1955-11-29|Raytheon Mfg Co|Molybdenum solder powder|

DE1225023B|1962-12-17|1966-09-15|Snecma|Process for the production of a hard solder connection between two graphite parts or a graphite part and a part made of difficult-to-melt material|

US3292255A|1964-06-25|1966-12-20|James C Marshall|Brazing alloys for tungsten and molybdenum|

IL34931A|1969-07-28|1973-04-30|Gillette Co|Metal articles with protective metal layers and methods and apparatus for their manufacture|

NL7300381A|1973-01-11|1974-07-15|

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JPH0223258B2|1982-03-16|1990-05-23|Nikoraeuitsuchi Mirofu Urajimiiru|

JP3727914B2|1996-11-20|2005-12-21|株式会社東芝|Antiferromagnetic film, magnetoresistive effect element and magnetic device using the same|

DE10336087A1|2003-08-06|2005-03-03|Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH|Electrode system with novel connection, associated lamp with this foil and method of making the connection|

DE102005030113A1|2005-06-28|2007-01-25|Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH|Electrode system for a lamp|

DE102005053553A1|2005-11-08|2007-05-16|Heraeus Gmbh W C|Solder pastes with resin-free flux|

法律状态:
2014-04-30| RE| Patent lapsed|Effective date: 20131031 |

优先权:

申请号 | 申请日 | 专利标题

DE102007050487|2007-10-19|

DE102007050487A|DE102007050487A1|2007-10-19|2007-10-19|High temperature solder for the production of discharge lamp by a solder connection between a tungsten-based electrode and molybdenum-based supporting bar, comprises molybdenum and ruthenium as main component, and further metals|

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