CN104190937B - A kind of preparation method of ultra-large type carefully brilliant molybdenum electrode - Google Patents
A kind of preparation method of ultra-large type carefully brilliant molybdenum electrode Download PDFInfo
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- CN104190937B CN104190937B CN201410275354.7A CN201410275354A CN104190937B CN 104190937 B CN104190937 B CN 104190937B CN 201410275354 A CN201410275354 A CN 201410275354A CN 104190937 B CN104190937 B CN 104190937B
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Abstract
The preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2,500 3000, take molybdenum powder and load in glued membrane, hydrostatic profile, it is placed under intermediate frequency furnace, hydrogen atmosphere after sintering rod base into, inserts in mould, forge mould, after insert tempering furnace, form fine grained texture, take out cleaning afterwards, prepare product after drying.Instant invention overcomes sintering and the defective workmanship forged, technique is simple, and easy industrial production control reduces and pollutes, and low cost, Quality advance, production efficiency is greatly improved.
Description
Technical field
The present invention relates to the preparation method of a kind of molybdenum electrode, the preparation method of a kind of ultra-large type made with pure molybdenum powder carefully brilliant molybdenum electrode.
Background technology
nullAt present，Glass fiber manufacturing enterprise often to use molybdenum electrode，Molybdenum electrode is put in frit，Glass is melted into liquid and heat-preservation cotton fiber is made in wire drawing，This kind of molybdenum electrode requires possess higher heat-resisting quantity、Compactness and thinner grain size，And simultaneously used in this field generally a diameter of 500 700，The ultra-large type molybdenum electrode of a length of 2500-3000，Conventional preparation method is mainly for the preparation of the less molybdenum electrode of diameter，The moulding process of extruding or drawing is mainly used to be processed molding，The most thermally treated，The molybdenum bar that machining is formed，Such method is high to equipment requirements，Complex process，Relatively costly，Simultaneously because molybdenum electrode size is bigger，The method is used to prepare big molybdenum electrode the most difficult，And the molybdenum bar resistance to elevated temperatures prepared is poor、Compactness is poor and grain size is the biggest，Do not meet the requirement of big molybdenum electrode used by this field completely.
Some enterprises attempt using the technique sintering, forging molding, the steps include: that high temperature sintering-cooling forges-lonneal-polish after processing-heating up.The technique needing to use cooling water circulation to process after high temperature burns till all is have employed when Mo is processed.Although the processing method of this kind of technique is helpful to the compactness increasing material, but all can not form fine grained texture.
It addition, prior art there is also a significant deficiency, both during forging, all use the surface directly forging rod base, and uncontrollable to the deflection of material in forging, its forging method has had a strong impact on formation and the quality of fine grained texture.
Further, in prior art, the temperature of tempering all uses lonneal, and temperature is all at 450-500 DEG C, owing to temperature is relatively low, and the heavy damage formation of product fine grained texture, have impact on product quality.
Summary of the invention
The purpose of the present invention aims to solve the problem that the deficiency of above-mentioned technical problem, the preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode is provided, the thin brilliant molybdenum electrode length made increases (length 2500-3000), enlarged diameter (diameter 500 700), use the method to be greatly improved formation and the stability of fine grained texture, improve intensity and the density of product.
The technical solution adopted in the present invention is: the preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000,
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, use 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 1900-2000 DEG C and sinter 55-65 hour, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, temperature 1350-1400 DEG C of control rod base, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6 Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
In the present invention, described sintering, can sinter under vacuo, during vacuum-sintering, temperature progressively heats up from zero degree to 2000 DEG C.
During described step one sintering, maintain the temperature at 1900 DEG C in intermediate frequency furnace and sinter 60 hours, burn till rod base.
In described step 2, the temperature of control rod base 1400 DEG C before forging.
In described step 3, take out the rod member forging molding, insert in the tempering furnace of 1200 DEG C, keep 2 hours, stablize fine grained texture.
The present invention, uses Mo to make, and owing to molybdenum is the most close with the character of tungsten, its floating-point and electric conductivity highlight, and coefficient of linear thermal expansion is little, and relatively tungsten is easily worked.The thermal conductivity of molybdenum [135 watts/(rice is opened)] and specific heat [0.276 kilojoule (kilogram open)] are in optimal collocation, its fusing point: 2620 DEG C, intensity and density more than tungsten, and molybdenum still has high intensity at 1200 DEG C, and molybdenum has the ability doubling tungsten.
Molybdenum, under the temperature and pressure that vacuum drying oven works, has extremely low vapour pressure, and therefore, molybdenum is to working in stove or the pollution minimum of operation material, and evaporation loss will not restrict the service life of the molybdenum matter hot parts such as heating element heater and heat insulation encapsulating.
The present invention uses the molybdenum powder that purity is higher, and the molybdenum electrode length made increases (length 2500-3000), enlarged diameter (a diameter of 500 700), and adds the grain formation fine grained texture making molybdenum man-hour in forging, is greatly improved the service life of molybdenum electrode.
The present invention, based on the feature that molybdenum powder intensity is high, uses mould that molybdenum powder is made hollow opaque molybdenum pipe, changes external extruding or the moulding process of drawing.
The present invention, when the base of molding sinters, eliminates cooling process (particularly cooling water circulation operation).It has been investigated that, temperature-fall period can destroy the formation of the fine grained texture of material.Use after high temperature sintering and directly forge, the formation of fine grained texture can be kept, the effect that this technique produces be prior it is not expected that.
The present invention, changes and forges technique, and conventional forging the most directly forges the surface of rod base, and its defect is: forge uneven, it is impossible to controlling deflection, poor product quality, qualification rate is low, is also highly vulnerable to breakage the crystallization of rod base.The present invention uses and inserts in mould by rod base, directly forges mould, effectively controls the deflection (control of deflection of the present invention is for less than 50%) of rod base, neither destroys fine grained texture, and properties of product are greatly improved, and qualification rate can realize 100%.
The present invention, changes tempering process, and conventional tempering all uses low temperature (450-500 DEG C), it has been investigated that, lonneal is the biggest to fine grained texture's destructiveness of molybdenum, it is impossible to ensure product quality.Temperature of the present invention uses 1000-1200 DEG C, substantially increases formation and the stability of fine grained texture, greatly improves quality and the life-span of product, and it is the most unexpected that this technique is told on.
Beneficial effects of the present invention:
First, instant invention overcomes the defect that in the past can only produce less than 1700 length molybdenum electrodes, the length of molybdenum electrode is increased to 2500-3000, enlarged diameter 500 700.
Its two, instant invention overcomes the defect of sintering difficulty, after changing conventional sintering, need to use a difficult problem for cooling water circulation.The present invention eliminates temperature reduction technology in high-sintering process, directly forges after using high temperature sintering, and this process advan, in the compactness of increase material, forms fine grained texture.
They are three years old, instant invention overcomes and forge that technique compactness is poor, forge uneven defect, directly forge the surface of rod base during forging in the past, change into rod base is loaded the technique forging mould in mould, effectively control the deflection ＜ 50% forged, effectively accelerate formation and the Quality advance of fine grained texture.
They are four years old, instant invention overcomes the defect being tempered the STRESS VARIATION that uneven and lonneal causes after forging molding, change conventional lonneal (450-500 DEG C) into high tempering (1000-1300 DEG C), greatly ensure that material performance under tempered condition, effectively stabilizing material still has high intensity and density at 1200 DEG C, after fine grained texture is formed, guarantee that molybdenum has extremely low vapour pressure under the temperature and pressure that vacuum drying oven works, make it to working in stove or the pollution minimum of operation material, and evaporation loss will not restrict the service life of the molybdenum matter hot parts such as heating element heater and heat insulation encapsulating.
Its five, present invention process is simple, and easy industrial production control reduces pollution.
Its six, present invention reduces production cost, improve quality, production efficiency is greatly improved.
Detailed description of the invention
The preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000,
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, use 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 1900-2000 DEG C and sinter 55-65 hour, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, temperature 1350-1400 DEG C of control rod base, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6 Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
Described sintering, can sinter under vacuo, and during vacuum-sintering, temperature progressively heats up from zero degree to 2000 DEG C.
Embodiment one,The preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000,
Step one, take the molybdenum powder of granularity 2.8 μm, load in the rubber die sleeve made in advance, use 160MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 1900 DEG C and sinter 55 hours, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, the temperature of control rod base 1350 DEG C, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1000 DEG C, keep 1 hour, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6 Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
Embodiment two,The preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000,
Step one, take the molybdenum powder of granularity 3 μm, load in the rubber die sleeve made in advance, use 180MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 1950 DEG C and sinter 60 hours, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, the temperature of control rod base 1380 DEG C, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1100 DEG C, keep 2 hours, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6 Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
Embodiment three,The preparation method of a kind of ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000,
Step one, take the molybdenum powder of granularity 3.8 μm, load in the rubber die sleeve made in advance, use 200MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 2000 DEG C and sinter 65 hours, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, the temperature of control rod base 1400 DEG C, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1200 DEG C, keep 3 hours, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6 Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
Claims (4)
1. a preparation method for ultra-large type carefully brilliant molybdenum electrode, uses the molybdenum powder of purity ＞ 99.95% to prepare, wherein, a diameter of the 500 700 of molybdenum electrode, a length of 2500-3000, it is characterised in that:
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, use 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, in a hydrogen atmosphere, maintain the temperature at 1900 DEG C and sinter 55-65 hour, after burning till rod base, standby；
Step 2, the excellent base burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, temperature 1350-1400 DEG C of control rod base, forge rod mold tool, the deflection ＜ 50% of control rod base when forging, forges into length 2500-3000, the rod member of a diameter of 500 700；
Step 3, lay down mould, take out the rod member forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, rod member being carried out machining, both ends cut flat with, and screwed hole is beaten in a side end face, and rear polishing makes surface roughness reach Ra1.6-Ra3.2 μm；
Through cleaning after step 5, machining, it is dried, prepared ultra-large type carefully brilliant molybdenum electrode.
The preparation method of a kind of ultra-large type the most according to claim 1 carefully brilliant molybdenum electrode, it is characterised in that: during described step one sintering, maintain the temperature at 1900 DEG C in intermediate frequency furnace and sinter 60 hours, burn till rod base.
The preparation method of a kind of ultra-large type the most according to claim 1 carefully brilliant molybdenum electrode, it is characterised in that: in described step 2, the temperature of control rod base 1400 DEG C before forging.
The preparation method of a kind of ultra-large type the most according to claim 1 carefully brilliant molybdenum electrode, it is characterised in that: in described step 3, take out the rod member forging molding, insert in the tempering furnace of 1200 DEG C, keep 2 hours, stablize fine grained texture.
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| CN109014189B (en) * | 2018-08-27 | 2020-11-06 | 广州市石基耐火材料厂 | Molybdenum electrode and preparation method thereof |
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| CN100566921C (en) * | 2008-04-25 | 2009-12-09 | 胡延槽 | The preparation method of high-density molybdenum tube |
| CN102699328B (en) * | 2012-01-04 | 2015-05-13 | 洛阳科威钨钼有限公司 | Process for manufacturing large molybdenum electrode |
| CN103157795B (en) * | 2013-03-26 | 2014-12-24 | 金堆城钼业股份有限公司 | Preparation method of large-scale molybdenum plate blank |
| CN103203601B (en) * | 2013-04-12 | 2015-07-29 | 金堆城钼业股份有限公司 | Die forging is adopted to prepare the method for molybdenum electrode bar |
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