CN103203601A - Method for producing molybdenum electrode bar by means of die forging - Google Patents

Method for producing molybdenum electrode bar by means of die forging Download PDF

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CN103203601A
CN103203601A CN2013101286020A CN201310128602A CN103203601A CN 103203601 A CN103203601 A CN 103203601A CN 2013101286020 A CN2013101286020 A CN 2013101286020A CN 201310128602 A CN201310128602 A CN 201310128602A CN 103203601 A CN103203601 A CN 103203601A
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molybdenum
hours
heating
bar base
temperature
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CN103203601B (en
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吴兴刚
葛宽余
惠保卫
白秋平
杨德武
惠军胜
苏晓
曹维成
任宝江
仙彬华
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Abstract

The invention discloses a method for producing a molybdenum electrode bar by means of die forging. The method includes the steps of molybdenum powder selection, bar blank pressing, molybdenum bar blank sintering, and forging. The molybdenum electrode bar produced by the method is uniform in size and quality and free of burrs and surface cracks.

Description

Adopt die forging to prepare the method for molybdenum electrode bar
Technical field
The invention belongs to technical field of material, be specifically related to a kind of method that adopts die forging to prepare molybdenum electrode bar.
Background technology
Molybdenum electrode bar be manufactured with two kinds of methods, first kind is to be raw material with sintering molybdenum bar base, adopts the pneumatic hammer die forging; Second kind is to be raw material with the sintering molybdenum bar, adopts precise forging machine to forge.
The granularity of molybdenum powder and Song Bi are the important parameters of determining the molybdenum powder specification, the molybdenum bar base that the molybdenum powder of different grain size and Song Bi is produced, and its physical property is also different, i.e. and the molybdenum bar base specification of the molybdenum powder of different grain size and Song Bi production is different.If the molybdenum bar base employing to different size removes to produce molybdenum electrode bar with a kind of forging mode, just can't guarantee the quality of final molybdenum electrode bar.Be fit to the molybdenum bar base of pneumatic hammer die forging if use instead the finish forge method then exist finish-forging material carrying out flaw detection defective, forge and have that burr increases in shrinkage cavity, the follow-up wire drawing, the problem of surface checking.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts die forging to prepare molybdenum electrode bar, solved in the prior art because the specification of molybdenum bar base and forging mode do not match that the molybdenum bar base finish-forging material carrying out flaw detection that causes is defective, forging exists that burr increases in shrinkage cavity, the follow-up wire drawing, the problem of surface checking.
The technical solution adopted in the present invention is: adopt die forging to prepare the method for molybdenum electrode bar, comprise the steps:
The first step, the choosing of molybdenum powder
Choosing granularity is 3.2~3.9 μ m, and pine is than being 1.05~1.2g/cm 3Molybdenum powder as the raw material of making the molybdenum bar base;
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 180~200Mpa and suppresses, pressurize 8~15 minutes again after the compacting, and making diameter is the molybdenum bar base of 48~150mm;
The 3rd step, sintering molybdenum bar base
The second molybdenum bar base that make of step is packed in the intermediate frequency furnace, and in stove, charge into hydrogen, carry out the segmented sintering then, again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.7~1.0m 3/ h;
In the 4th step, forge
The heating that to carry out multi-pass through the molybdenum bar base that the 3rd step handled forges, and makes molybdenum electrode bar.
Characteristics of the present invention also are,
Segmented sintering in the 3rd step is specially: heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 3~4 hours, was incubated 1.5~2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 2.5~4 hours; Heated 2 hours to 1600 ℃, and be incubated 3.5~4 hours; Heated 2 hours to 1800 ℃, and be incubated 2.5~3.5 hours; Heated 2 hours to 1850 ℃, and be incubated 5~7 hours.
The heating of the multi-pass in the 4th step forges, and be specially: the molybdenum bar base diameter distortion amount of first passage is 8~12mm, and heating-up temperature is 1300 ℃, and be 1~1.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 5~12mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 3~8mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 3~5mm, and heating-up temperature is 1200~1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 5th passage is 2~3mm, and heating-up temperature is 1200~1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 6th passage is 2~3mm, and heating-up temperature is 1200 ℃, and be 0.5 hour heat time heating time; The deflection of the 7th passage is 5~7mm, and heating-up temperature is 1200 ℃, and be 0.5 hour heat time heating time.
The invention has the beneficial effects as follows: the molybdenum electrode bar that the method for preparing molybdenum electrode bar of the present invention makes, have the barred body structured size, quality is even, no burr, the advantage of no surface checking.
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment.
Embodiment 1
The first step, the choosing of molybdenum powder
Choosing granularity is 3.2 μ m, and pine is than being 1.05g/cm 3Molybdenum powder as the die forging raw material.
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 180Mpa and suppresses, pressurize 8 minutes again after the compacting, and making diameter is the molybdenum bar base of 55mm;
The 3rd step, sintering molybdenum bar base
Second two kinds of molybdenum bar bases making of step are packed in the intermediate frequency furnace, and charge into hydrogen in stove, carry out the segmented sintering then, heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 3 hours, was incubated 1.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 2.5 hours; Heated 2 hours to 1600 ℃, and be incubated 3.5 hours; Heated 2 hours to 1800 ℃, and be incubated 2.5 hours; Heated 2 hours to 1850 ℃, and be incubated 5 hours; Again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.7m 3/ h;
In the 4th step, forge
The heating of the molybdenum bar base of handling through the 3rd step being carried out four-pass forges, and the molybdenum bar base diameter distortion amount of first passage is 8mm, and heating-up temperature is 1300 ℃, and be 1 hour heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 5mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 3mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 3mm, and heating-up temperature is 1200~1250 ℃, and be 0.5 hour heat time heating time; Making diameter is the 36mm molybdenum electrode bar.
Get the molybdenum electrode bar that present embodiment makes and detect, the barred body structured size, quality is even, no burr, no surface checking, density is 9.8g/cm 3, number of die is 2100/cm 2
Embodiment 2
The first step, the choosing of molybdenum powder
Choosing granularity is 3.9 μ m, and pine is than being 1.2g/cm 3Molybdenum powder as the die forging raw material.
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 200Mpa and suppresses, pressurize 15 minutes again after the compacting, and making diameter is the molybdenum bar base of 90mm;
The 3rd step, sintering molybdenum bar base
Second two kinds of molybdenum bar bases making of step are packed in the intermediate frequency furnace, and charge into hydrogen in stove, carry out the segmented sintering then, heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 4 hours, was incubated 2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 3.5 hours; Heated 2 hours to 1600 ℃, and be incubated 3.5 hours; Heated 2 hours to 1800 ℃, and be incubated 3.5 hours; Heated 2 hours to 1850 ℃, and be incubated 5 hours; Again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 1.0m 3/ h;
In the 4th step, forge
The heating of the molybdenum bar base of handling through the 3rd step being carried out five passages forges, and the molybdenum bar base diameter distortion amount of first passage is 12mm, and heating-up temperature is 1300 ℃, and be 1 hour heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 5mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 3mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 3mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The 5th passage molybdenum bar base diameter distortion amount be 2mm, heating-up temperature is 1200 ℃, be that to make diameter in 0.5 hour be the 65mm molybdenum electrode bar heat time heating time.
Get the molybdenum electrode bar that present embodiment makes and detect, the barred body structured size, quality is even, no burr, no surface checking, density is 9.7g/cm 3, number of die is 2150/cm 2
Embodiment 3
The first step, the choosing of molybdenum powder
Choosing granularity is 3.5 μ m, and pine is than being 1.12g/cm 3Molybdenum powder as the die forging raw material.
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 190Mpa and suppresses, pressurize 10 minutes again after the compacting, and making diameter is the molybdenum bar base of 120mm;
The 3rd step, sintering molybdenum bar base
Second two kinds of molybdenum bar bases making of step are packed in the intermediate frequency furnace, and charge into hydrogen in stove, carry out the segmented sintering then, heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 4 hours, was incubated 2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 3.5 hours; Heated 2 hours to 1600 ℃, and be incubated 3.5 hours; Heated 2 hours to 1800 ℃, and be incubated 3.5 hours; Heated 2 hours to 1850 ℃, and be incubated 6 hours; Again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.8m 3/ h;
In the 4th step, forge
The heating of the molybdenum bar base of handling through the 3rd step being carried out six passages forges, and the molybdenum bar base diameter distortion amount of first passage is 8mm, and heating-up temperature is 1300 ℃, and be 1 hour heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 12mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 5mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 5mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The 5th passage molybdenum bar base diameter distortion amount be 3mm, heating-up temperature is 1200 ℃, be 0.5 hour heat time heating time; The 6th passage molybdenum bar base diameter distortion amount be 3mm, heating-up temperature is 1200 ℃, be that to make diameter in 0.5 hour be the 84mm molybdenum electrode bar heat time heating time.
Get the molybdenum electrode bar that present embodiment makes and detect, the barred body structured size, quality is even, no burr, no surface checking, density is 9.9g/cm 3, number of die is 2000/cm 2
Embodiment 4
The first step, the choosing of molybdenum powder
Choosing granularity is 3.4 μ m, and pine is than being 1.1g/cm 3Molybdenum powder as the die forging raw material.
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 195Mpa and suppresses, pressurize 13 minutes again after the compacting, and making diameter is the molybdenum bar base of 150mm;
The 3rd step, sintering molybdenum bar base
Second two kinds of molybdenum bar bases making of step are packed in the intermediate frequency furnace, and charge into hydrogen in stove, carry out the segmented sintering then, heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 4 hours, was incubated 2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 4 hours; Heated 2 hours to 1600 ℃, and be incubated 4 hours; Heated 2 hours to 1800 ℃, and be incubated 3.5 hours; Heated 2 hours to 1850 ℃, and be incubated 7 hours; Again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.8m 3/ h;
In the 4th step, forge
The heating of the molybdenum bar base of handling through the 3rd step being carried out seven passages forges, and the molybdenum bar base diameter distortion amount of first passage is 10mm, and heating-up temperature is 1300 ℃, and be 1.5 hours heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 10mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 8mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 3mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The 5th passage molybdenum bar base diameter distortion amount be 2mm, heating-up temperature is 1200 ℃, be 0.5 hour heat time heating time; The 6th passage molybdenum bar base diameter distortion amount be 2mm, heating-up temperature is 1200 ℃, be 0.5 hour heat time heating time; The 7th passage molybdenum bar base diameter distortion amount be 5mm, heating-up temperature is 1200 ℃, be that to make diameter in 0.5 hour be the 110mm molybdenum electrode bar heat time heating time.
Get the molybdenum electrode bar that present embodiment makes and detect, the barred body structured size, quality is even, no burr, no surface checking, density is 9.7g/cm 3, number of die is 2160/cm 2
Embodiment 5
The first step, the choosing of molybdenum powder
Choosing granularity is 3.9 μ m, and pine is than being 1.05g/cm 3Molybdenum powder as the die forging raw material.
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 185Mpa and suppresses, pressurize 15 minutes again after the compacting, and making diameter is the molybdenum bar base of 95mm;
The 3rd step, sintering molybdenum bar base
Second two kinds of molybdenum bar bases making of step are packed in the intermediate frequency furnace, and charge into hydrogen in stove, carry out the segmented sintering then, heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 4 hours, was incubated 2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 3.6 hours; Heated 2 hours to 1600 ℃, and be incubated 3.8 hours; Heated 2 hours to 1800 ℃, and be incubated 3.7 hours; Heated 2 hours to 1850 ℃, and be incubated 6.5 hours; Again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.9m 3/ h;
In the 4th step, forge
The heating of the molybdenum bar base of handling through the 3rd step being carried out six passages forges, and the molybdenum bar base diameter distortion amount of first passage is 10mm, and heating-up temperature is 1300 ℃, and be 1.5 hours heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 10mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 6mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 4mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The 5th passage molybdenum bar base diameter distortion amount be 2.5mm, heating-up temperature is 1200 ℃, be 0.5 hour heat time heating time; The 6th passage molybdenum bar base diameter distortion amount be 2.5mm, heating-up temperature is 1200 ℃, be that to make diameter in 0.5 hour be the 60mm molybdenum electrode bar heat time heating time.
Get the molybdenum electrode bar that present embodiment makes and detect, the barred body structured size, quality is even, no burr, no surface checking, density is 9.7g/cm 3, number of die is 2200/cm 2

Claims (3)

1. adopt die forging to prepare the method for molybdenum electrode bar, it is characterized in that, comprise the steps:
The first step, the choosing of molybdenum powder
Choosing granularity is 3.2~3.9 μ m, and pine is than being 1.05~1.2g/cm 3Molybdenum powder as the raw material of making the molybdenum bar base;
Second step, pressed bar
The molybdenum powder that the first step is chosen is packed in the cylindrical mold, the mould that will install molybdenum powder is again put into cold isostatic press and is suppressed, and the pressure of cold isostatic press is set to 180~200Mpa and suppresses, pressurize 8~15 minutes again after the compacting, and making diameter is the molybdenum bar base of 48~150mm;
The 3rd step, sintering molybdenum bar base
The second molybdenum bar base that make of step is packed in the intermediate frequency furnace, and in stove, charge into hydrogen, carry out the segmented sintering then, again the molybdenum bar base is cooled off behind the sintering; In sintering and the cooling procedure, the flow of hydrogen is 0.7~1.0m 3/ h;
In the 4th step, forge
The heating that to carry out multi-pass through the molybdenum bar base that the 3rd step handled forges, and makes molybdenum electrode bar.
2. employing die forging as claimed in claim 1 prepares the method for molybdenum electrode bar, it is characterized in that, the segmented sintering described in the 3rd step is specially: heating earlier made furnace temperature rise to 1000 ℃ from 20 ℃ in 3~4 hours, was incubated 1.5~2.5 hours then; Heated 1.5 hours to 1250 ℃, and be incubated 2.5 hours; Heated 1.5 hours to 1400 ℃, and be incubated 2.5~4 hours; Heated 2 hours to 1600 ℃, and be incubated 3.5~4 hours; Heated 2 hours to 1800 ℃, and be incubated 2.5~3.5 hours; Heated 2 hours to 1850 ℃, and be incubated 5~7 hours.
3. employing die forging as claimed in claim 1 or 2 prepares the method for molybdenum electrode bar, it is characterized in that the heating of multi-pass described in the 4th step forges, be specially: the molybdenum bar base diameter distortion amount of first passage is 8~12mm, heating-up temperature is 1300 ℃, and be 1~1.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of second passage is 5~12mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 3rd passage is 3~8mm, and heating-up temperature is 1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of four-pass is 3~5mm, and heating-up temperature is 1200~1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 5th passage is 2~3mm, and heating-up temperature is 1200~1250 ℃, and be 0.5 hour heat time heating time; The molybdenum bar base diameter distortion amount of the 6th passage is 2~3mm, and heating-up temperature is 1200 ℃, and be 0.5 hour heat time heating time; The deflection of the 7th passage is 5~7mm, and heating-up temperature is 1200 ℃, and be 0.5 hour heat time heating time.
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CN104190937A (en) * 2014-06-19 2014-12-10 洛阳科威钨钼有限公司 A preparation method of an ultra large fine-grain molybdenum electrode
CN107914016A (en) * 2017-11-08 2018-04-17 金堆城钼业股份有限公司 A kind of production method of molybdenum bar
CN109014189A (en) * 2018-08-27 2018-12-18 广州市石基耐火材料厂 Molybdenum electrode and preparation method thereof
CN110640246A (en) * 2019-09-02 2020-01-03 江苏弘亚钨钼科技有限公司 Preparation method of H-shaped molybdenum wire

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CN104190937A (en) * 2014-06-19 2014-12-10 洛阳科威钨钼有限公司 A preparation method of an ultra large fine-grain molybdenum electrode
CN107914016A (en) * 2017-11-08 2018-04-17 金堆城钼业股份有限公司 A kind of production method of molybdenum bar
CN107914016B (en) * 2017-11-08 2020-12-15 金堆城钼业股份有限公司 Production method of molybdenum strip
CN109014189A (en) * 2018-08-27 2018-12-18 广州市石基耐火材料厂 Molybdenum electrode and preparation method thereof
CN109014189B (en) * 2018-08-27 2020-11-06 广州市石基耐火材料厂 Molybdenum electrode and preparation method thereof
CN110640246A (en) * 2019-09-02 2020-01-03 江苏弘亚钨钼科技有限公司 Preparation method of H-shaped molybdenum wire

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