CN1066367C - Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method - Google Patents
Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method Download PDFInfo
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- CN1066367C CN1066367C CN98124722A CN98124722A CN1066367C CN 1066367 C CN1066367 C CN 1066367C CN 98124722 A CN98124722 A CN 98124722A CN 98124722 A CN98124722 A CN 98124722A CN 1066367 C CN1066367 C CN 1066367C
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Abstract
The present invention relates to a method for making molybdenum electrode blanks and molybdenum head piece blanks by using an electron-beam smelting method. A product is made by the method that rod-shaped molybdenum is used as raw material and is smelted in an electron-beam smelting furnace of electromagnetic focusing; the pressure intensity in the furnace body is from 5*10<-1> to 1*10<-3> Pa; the pressure intensity in an electron gun chamber is from 1*10<-2> to 1*10<-4> Pa; the voltage of the electron gun is from 20 to 25 thousand volts; the current of the electron gun is from 2 to 7 amperes. The product produced by the method has the advantages of high density, high purity, flushing and corrosion resistance of smelting high-temperature material, long service life, recycled raw material, simple technology and low cost.
Description
The present invention relates to the technology that the electronic torch melting manufactured is used for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base.
Molybdenum electrode is the electrode of the conduction usefulness of aluminosilicate refractory fiber electric melting furnace, glass melting electric furnace and fuse salt re metal electrolyzing groove.Said molybdenum head piece is the flow export as the alumina silicate of the molten condition in the silicate refractory fibre electric melting furnace.
At present, the metal molybdenum bar of molybdenum electrode base both domestic and external, molybdenum head piece base all adopts powder metallurgic method.Be exactly with molybdenum powder through die mould, sinter the metal molybdenum bar of molybdenum electrode base, molybdenum head piece base into after, make molybdenum electrode and molybdenum head piece through forging and pressing, the processing of car bits again.Because the metal molybdenum bar of molybdenum electrode, molybdenum head piece base is to make with powder metallurgic method, the density of base is low, and is generally about 9 grams per cubic centimters, not fine and close, and the space is arranged between particle, and it is many to contain gaseous impurity.So after making base with powder metallurgic method, the density of molybdenum electrode of making again and molybdenum head piece is also low, they in electric melting furnace or fused salt electrolysis groove high temperature resistant fusion material wash away and the corrosive nature of high temperature resistant fusion material poor, therefore service life is short, generally only can use several days also super only 30 days at the most.
Purpose of the present invention just is to work out the method for the metal molybdenum bar of a kind of new preparation molybdenum electrode base and molybdenum head piece base, the metal molybdenum bar cost of feasible molybdenum electrode base of making in this way and molybdenum head piece base is low, the density height, washing away of molybdenum electrode that this base is made after processing and the high temperature resistant fusion thing of molybdenum head piece, corrosion resistance and good, long service life.
The metal molybdenum bar of electronic torch melting manufactured molybdenum electrode base and molybdenum head piece base is (to be electron bombardment furnace again) to carry out in the electromagnetic focusing electron beam furnace.Its principle be utilize the electromagnetic focusing electron gun at the electron beam that makes high-speed motion under the high vacuum high voltage behind electromagnetic focusing repeatedly, bombardment molybdenum material and do not have the liquid level of the molten metal bath in the end water jacketed copper crucible, the kinetic energy of the electronics of high-speed motion is transformed into heat energy, make metalliferous material be heated into liquid of fusion to the metal bath that does not have end water jacketed copper crucible, make the metal bath on the upper strata of water jacketed copper crucible of the no end keep the liquid condition of fusion, metal liquid in its molten bath a suitable thickness arranged, the sweet crucible of no end water-cooled copper earthenware bottom is the metal that solidifies.Drip along with the fusing of metalliferous material on the liquid level of melt metal to the metal bath that does not have water jacketed copper crucible top, the end, the metal that solidifies of water jacketed copper crucible bottom of the no end down draws, make its crystallization gradually, be frozen into the round metal bars base, then become molybdenum pole base if make material with metal molybdenum, metal molybdenum bar base is as excellent base, the molybdenum electrode that processes from strand and the molybdenum head piece of the base of the base of molybdenum electrode and molybdenum head piece.
A kind of manufacturing of the present invention is used for the method for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base, and the bar-shaped metal molybdenum of raw material is packed in the feed box of electromagnetic focusing electron beam furnace (being electron bombardment furnace again); After ingot installed at the bottom of bar-shaped metal molybdenum of raw material and the traction molybdenum, the burner hearth of envelope cipher telegram magnetic focusing electron beam furnace carried out exhaust and vacuumizes, and making the pressure in the body of heater is 5 * 10
-1～1 * 10
-3Pressure in the Pa, gun chamber is 1 * 10
-2～1 * 10
-4Behind the Pa, start electron gun and draw electron beam, electron gun voltage is transferred to 20000～25000 volts, making its electron beam current is the 2-7 ampere, make the bar-shaped metal molybdenum of raw material be melted the temperature of end and the temperature in molybdenum molten bath is 2700-3500 ℃, ingot links to each other with dragging spindle blade at the bottom of making the traction molybdenum, the liquid molybdenum of the bar-shaped metal molybdenum melting end of raw material drips at the bottom of the traction molybdenum on water jacketed copper crucible upper strata, the no end in the molybdenum molten bath on the ingot, along with the liquid metal molybdenum of the bar-shaped metal molybdenum melting end of raw material drips in the molybdenum molten bath, drag spindle blade drag the traction molybdenum at the bottom of ingot move down, make copper crucible lower floor molten metal molybdenum gradually crystallization and freezing become the metal molybdenum pole.
The bar-shaped metal molybdenum of used raw material can prepare in order to the below method: (1) with the molybdenum bar, molybdenum waste material (the molybdenum waste materials of different shapes such as bar, rod, plate, sheet) is bundled into bar-shaped with molybdenum filament, and (2) after cleaning, drying, use 2000 kilograms per centimeter with molybdenum car bits
2The pressure die mould after, be welded into bar-shapedly, (3) are with the useless molybdenum electrode welding rod of growing up.
After ingot installs at the bottom of bar-shaped metal molybdenum of raw material and the traction molybdenum, behind the burner hearth (burner hearth of electron bombardment furnace) of envelope cipher telegram magnetic focusing electron beam furnace, start oil-sealed rotary pump and carry out exhaust and vacuumize, and then start booster pump and carry out exhaust with diffusion pump and vacuumize, making the interior pressure of body of heater is 5 * 10
-1～1 * 10
-3Pressure in the Pa, gun chamber is 1 * 10
-2～1 * 10
-4Behind the Pa, start electron gun and draw electron beam, the voltage of electron gun is transferred to 20000～25000 volts, electron beam current 2-7 ampere, making the temperature of the bar-shaped metal molybdenum melting end of raw material and the temperature in molybdenum molten bath is 2700-3500 ℃.The size of electron beam current is decided with the bar-shaped metal molybdenum material of raw material and the size of water jacketed copper crucible diameter of the no end, is generally the 2-7 ampere.To draw at the bottom of the molybdenum ingot and drag spindle blade with the pin pin joint.Drag spindle blade drag at the bottom of the traction molybdenum speed that moves down of ingot with 20～50 centimetres/hour for well, the diameter of water jacketed copper crucible is decided on the no end, the diameter of crucible is little, the speed that moves down is with regard to soon; Crucible diameter is big, and the speed that moves down is just slow.Its speed that moves down is also relevant with the content of gas in the kind of raw material and the raw material, and the speed that the impurity content of gas greatly then moves down in the raw material is just slow.The degree of depth of the molybdenum molten bath fusion molybdenum of ingot is good with 8～15 millimeters at the bottom of the traction molybdenum on water jacketed copper crucible upper strata, the no end.Dragging spindle blade is to be made by the copper pipe of water-cooled.
The molybdenum electrode base of being produced by said method and the metal molybdenum bar of molybdenum head piece base through car bits machining, are processed into molybdenum electrode and the molybdenum head piece of different size by certain geomery, and the molybdenum car bits that Vehicle Processing is come out can be used as raw material and reclaim use.
During the metal molybdenum bar with electronic torch melting manufactured molybdenum electrode base and molybdenum head piece base of the present invention, it is commercially available that used electromagnetic focusing electron beam furnace is electron bombardment furnace again, sees Fig. 1, and it is made of body of heater 1 and feed box 2 and electron gun 3.
The advantage of method that manufacturing of the present invention is used for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base just is:
1. owing to make the metal molybdenum bar of molybdenum electrode base and molybdenum head piece base with electron-beam process, the density of the metal molybdenum bar of molybdenum electrode base of producing and molybdenum head piece base is big, the purity height, the impurity content of gas is few, the matrix compact crystallization, washing away of the high-temperature material that molybdenum electrode of making and molybdenum head piece refractory melt, corrosion resistance is strong, long service life.Service life is relevant with melting species and operating condition.Its life-span of the product that method of the present invention is made is generally between 40-90 days.
2. method of the present invention can use the molybdenum waste material to make raw material, and the molybdenum car that produced when being machined to molybdenum electrode and molybdenum head piece bits also can be used as raw material and reclaim and use, and technology is simple, product with low cost.
Fig. 1 electromagnetic focusing electron beam furnace schematic diagram
Among the figure, 1 is body of heater, 2 is feed box, and 3 is the electromagnetic focusing electron gun, has or not end water jacketed copper crucible 4 in the body of heater 1,5 molybdenum electrode base or molybdenum head piece billets for generation, 6 are ingot at the bottom of the traction molybdenum, and 7 drag spindle blade for what made by the copper pipe of water-cooled, drag spindle blade 7 and traction molybdenum at the bottom of ingot 6 link to each other by the pin pin joint, 8 is the molybdenum molten bath, 9 is the melting end of the rod of the bar-shaped metal molybdenum of raw material facing to the metal molybdenum molten bath of water jacketed copper crucible of the no end, and 10 is the magnetic scanning lens, and 11 is electronic beam current, 12 is the secondary magnetic focusing lens, 13 is the hurdle orifice plate, and 14 is a magnetic focusing lens, and 15 is accelerating anode, 16 are the poly-fast utmost point, 17 is the tantalum cathode piece, and 18 is tungsten cathode, and 19 is gun chamber, 20 are the bar that gets stuck of the bar-shaped metal molybdenum of clamping raw material, and 21 is the bar-shaped metal molybdenum of raw material.
Below with embodiment method of the present invention is further described, will help the present invention and advantage thereof are done further to understand, protection scope of the present invention is not subjected to the qualification of embodiment, protection scope of the present invention is decided by claims.
To clean, dried molybdenum car crumb pressure 2000 kilograms per centimeter
2Die mould is welded into the bar-shaped molybdenum electrode welding growth rod that maybe will give up, and the molybdenum bar that maybe will give up is bundled into bar-shaped as the bar-shaped metal molybdenum of raw material.
Raw material is held in both hands shape metal molybdenum 21, in the feed box 2 in the electromagnetic focusing electron beam furnace of packing into; After bar-shaped metal molybdenum of raw material 21 and ingot 6 at the bottom of the traction molybdenum installed, behind the burner hearth of envelope cipher telegram magnetic focusing electronics smelting furnace, start oil-sealed rotary pump and carry out exhaust and vacuumize, start booster pump and diffusion pump then and carry out exhaust and vacuumize, making the interior pressure of body of heater is 1 * 10
-1Pressure in the Pa, gun chamber is 8 * 10
-3Pa.Start electron gun and draw electron beam, transfer voltage to 21000 volt of electron gun, make 5 amperes of its electron beam currents; The temperature that makes the melting end 9 of the bar-shaped metal molybdenum 21 of raw material is 3000 ℃, and also making the temperature in the molybdenum molten bath 8 of ingot 6 at the bottom of the traction molybdenum on upper strata of water jacketed copper crucible of the no end 4 is 3000 ℃.Like this, the liquid molybdenum of the bar-shaped metal molybdenum melting end 9 of raw material drips in the molybdenum pond 8 of water jacketed copper crucible of the no end, makes the degree of depth of the molten aluminum in molybdenum molten bath remain on 10 millimeters, will draw molybdenum at the bottom of ingot 6 link to each other with dragging spindle blade 7 usefulness pin pin joints.In the molybdenum molten bath 8 along with the liquid metal molybdenum drench of bar-shaped metal molybdenum 21 melting ends 9 of raw material ingot 6 at the bottom of the traction molybdenum on water jacketed copper crucible 4 upper stratas, 75 millimeters no ends of diameter, ingot 6 moves down at the bottom of dragging spindle blade 7 to drag the traction molybdenum, its speed that moves down is 38 centimetres/hour, make the metal molybdenum crystallization gradually of the molten of no end water jacketed copper crucible lower floor, be frozen into the metal molybdenum pole that is used for production molybdenum electrode base and molybdenum head piece base.
With the metal molybdenum bar of molybdenum electrode base or molybdenum head piece base, be machined into molybdenum electrode or molybdenum head piece through the car bits.
The density of the molybdenum electrode base made from the method for present embodiment or the metal molybdenum bar of molybdenum head piece base is 10.2 gram per centimeters
3, reached solid density.The purity height, gaseous impurity is few, matrix crystallization, densification.Make molybdenum electrode or molybdenum head piece with above-mentioned base again,, reach 80 days service life through in aluminosilicate refractory fiber smelting furnace, glass melting electric furnace or fuse salt re metal electrolyzing groove, showing with electrode or head piece experiment as conduction.
Claims (3)
1. a manufacturing is used for the method for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base, it is characterized in that,
(1) the bar-shaped metal molybdenum of raw material is packed in the feed box of electromagnetic focusing electron beam furnace,
(2) with after ingot installs at the bottom of bar-shaped metal molybdenum of raw material and the traction molybdenum, the burner hearth of envelope cipher telegram magnetic focusing electron beam furnace,
(3) carry out exhaust and vacuumize, making the pressure in the body of heater is 5 * 10
-1～1 * 10
-3Pressure in the Pa, gun chamber is 1 * 10
-2～1 * 10
-4Pa,
(4) start electron gun and draw electron beam, the voltage of electron gun is transferred to the 20000-25000 volt, making its electron beam current is the 2-7 ampere, makes the bar-shaped metal molybdenum of raw material be melted the temperature of end and the temperature in molybdenum molten bath is 2700-3500 ℃,
(5) make the traction molybdenum at the bottom of ingot link to each other with dragging spindle blade, the liquid molybdenum of the bar-shaped metal molybdenum melting end of raw material drips in the molybdenum molten bath of ingot at the bottom of the traction molybdenum on water jacketed copper crucible upper strata, the no end, along with the liquid metal molybdenum of the bar-shaped metal molybdenum melting end of raw material drips in the molybdenum molten bath, ingot moves down at the bottom of dragging spindle blade to drag the traction molybdenum
(6) make copper crucible lower floor molten metal molybdenum gradually crystallization and freezing become the metal molybdenum pole.
2. be used for the method for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base according to a kind of manufacturing of claim 1, it is characterized in that, drag spindle blade to drag that the speed that moves down of ingot is 20-50 centimetre/hour at the bottom of the traction molybdenum.
3. be used for the method for the metal molybdenum bar of production molybdenum electrode base and molybdenum head piece base according to a kind of manufacturing of claim 1, it is characterized in that, the degree of depth of the aluminum metal bath fusion molybdenum at the bottom of the traction molybdenum on water jacketed copper crucible upper strata, the no end on the ingot is the 8-15 millimeter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124722A CN1066367C (en) | 1998-11-12 | 1998-11-12 | Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124722A CN1066367C (en) | 1998-11-12 | 1998-11-12 | Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method |
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| CN1253865A CN1253865A (en) | 2000-05-24 |
| CN1066367C true CN1066367C (en) | 2001-05-30 |
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| CN98124722A Expired - Lifetime CN1066367C (en) | 1998-11-12 | 1998-11-12 | Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127741A (en) * | 2011-02-11 | 2011-07-20 | 韩伟东 | Method for preparing high-purity molybdenum target for thin film solar cell |
| CN103021780A (en) * | 2012-11-16 | 2013-04-03 | 云南钛业股份有限公司 | EB (electron beam) gun air flow rate control method during EB furnace smelting process |
| CN104894388A (en) * | 2014-03-06 | 2015-09-09 | 北京工业大学 | Method for preparing vanadium target material through electron beam melting |
| CN105567991A (en) * | 2014-10-17 | 2016-05-11 | 宁波创润新材料有限公司 | Smelting device |
| CN104765385A (en) * | 2015-03-29 | 2015-07-08 | 西安赛隆金属材料有限责任公司 | Electron beam selected area melting atmosphere adjust and control system and method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0285741A1 (en) * | 1987-04-10 | 1988-10-12 | W.C. Heraeus GmbH | Process for the production of a highly ductile semi-finished tantalum product |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0285741A1 (en) * | 1987-04-10 | 1988-10-12 | W.C. Heraeus GmbH | Process for the production of a highly ductile semi-finished tantalum product |
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