CN100482835C - Lanthanum microdoped molybdenum alloy wire preparation method - Google Patents
Lanthanum microdoped molybdenum alloy wire preparation method Download PDFInfo
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- CN100482835C CN100482835C CNB2006101707513A CN200610170751A CN100482835C CN 100482835 C CN100482835 C CN 100482835C CN B2006101707513 A CNB2006101707513 A CN B2006101707513A CN 200610170751 A CN200610170751 A CN 200610170751A CN 100482835 C CN100482835 C CN 100482835C
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Abstract
The invention discloses a making method of high-temperature metal molybdenum filament with trace lanthanum, which comprises the following steps: reducing molybdenum oxide in the vacuum twice; punching; sintering; rolling; drawing; obtaining the Mo-La alloy filament.
Description
Technical field
The preparation method of lanthanum microdoped molybdenum alloy wire relates to a kind of production method of hot metal molybdenum filament, the preparation method of special lanthanum microdoped molybdenum alloy wire
Background technology
Because refractory metal molybdenum has higher high temperature strength, favorable conductive thermal conductivity, the lower coefficient of expansion and workability, thereby in special bulb such as automobile halogen tungsten lamp, high-pressure mercury lamp, tubular halogen tungsten lamp and electric lighting device, be extensive use of the molybdenum filament material make their required bulbs hook, around filament with component such as heart yearn, guide rod, outlet line and plasticity supports, in the kiln industry, be used as the hydrogen furnace heater strip.But in part with high-temperature behavior requirement; element as high temperature lamps scaffolding thread, high-temperature electric resistance furnace (under gas shield or vacuum) heating element all needs molybdenum filament to have high temperature use properties preferably; the recrystallization temperature of pure molybdenum filament has only 1000～1200 ℃; thereby fragility and fracture often appear; its hot strength is also low and yielding, can not satisfy the service requirements of above-mentioned industry far away.This is because its recrystal grain is grown up and formed due to the equiaxial crystalline-granular texture behind recrystallize at this moment.
Summary of the invention
The objective of the invention is to the deficiency that exists at above-mentioned prior art, provide a kind of good processability, technology is simple, yield rate is high, material high conformity, not flexible brittle failure, long service life, recrystallization temperature height, La content are the preparation method of the lanthanum microdoped molybdenum alloy wire of 300 ± 50ppm.
The objective of the invention is to be achieved through the following technical solutions.
The preparation method of lanthanum microdoped molybdenum alloy wire adopts the powder metallurgy process preparation; It is characterized in that it being to carry out secondary reduction after carrying out that bipyramid vacuum-drying liquid one is solid and mix in the powder molybdenum dioxide stage to produce the lanthanum microdoped molybdenum alloy powder, repressed again, sintering, rolling, drawing procedure are prepared little lanthanum Mo-La alloy silk of mixing.
The preparation method of lanthanum microdoped molybdenum alloy wire of the present invention is characterized in that poly-comprising in step of its preparation process:
A. be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate;
B. by taking by weighing La
2O
3Dissolve standby; With molybdenum dioxide and La (NO
3)
3Solution mixes in pot is mixed in bipyramid vacuum-drying;
C. molybdenum dioxide is carried out secondary hydrogen reducing Cheng Wei in four pipe high temperature retort furnaces and mix lanthanum Mo-La molybdenum powder;
D. little lanthanum Mo-La molybdenum powder of mixing is carried out isostatic cool pressing and is pressed into alloy bar, carry out presintering and high temperature sintering and obtain the sintered alloy rod;
E. the sintered alloy rod is rolled cogging, obtains little lanthanum rolled alloy bar of mixing respectively; Rod of metal alloy is carried out the deep bid drawing obtain the alloy silk;
F. the alloy silk is carried out high temperature annealing, carry out the mid-game drawing after the elimination internal stress, obtain alloy and change wire drawing;
G. the alloy silk changes to be pulled in and carries out high temperature annealing under the hydrogen shield, carries out mechanical property behind the cool to room temperature and detects and microstructure analysis.
Method of the present invention, the molybdenum source is an ammonium dimolybdate, raw material is cheap and easy to get, employed additive La
2O
3Cheap, to operator's not injury of health; Production technique is easy to control, and is easy and simple to handle, safe, reliable, need not big input and transformation on equipment, is suitable for scale operation; Employing liquid one is consolidated adulterating method and is consolidated adulterating method and compare, the alloying element that is added being evenly distributed in material, good product consistency; The pressure processing craft that adopts is that Y370, Y250 twice rolling-cogging and rotary blooming technology are compared, and the loss of product is low, and fibrous tissue is obvious.
The inventive method, little lanthanum Mo-La rare earth molybdenum alloy wire of mixing of preparation, its material contains oxide compound La
2O
3, wherein La is at the silk material
In weight percent be 0.03%.Compare with pure molybdenum, the high-temperature behavior of products obtained therefrom of the present invention is good, and the recrystallization temperature height has improved 500 ℃ than pure molybdenum, premium propertiess such as products obtained therefrom intensity height of the present invention, recrystallization temperature height, long service life.
Embodiment
The preparation method of lanthanum microdoped molybdenum alloy wire, poly-comprising in the step of its preparation process: a. are that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate; B. by taking by weighing La
2O
3Dissolve standby; With molybdenum dioxide and La (NO
3)
3Solution mixes in pot is mixed in bipyramid vacuum-drying; C. molybdenum dioxide is carried out secondary hydrogen reducing Cheng Wei in four pipe high temperature retort furnaces and mix lanthanum Mo-La molybdenum powder; D. little lanthanum Mo-La molybdenum powder of mixing is carried out isostatic cool pressing and is pressed into alloy bar, carry out presintering and high temperature sintering and obtain the sintered alloy rod; E. the sintered alloy rod is rolled cogging, obtains little lanthanum rolled alloy bar of mixing respectively; Rod of metal alloy is carried out the deep bid drawing obtain the alloy silk; F. the alloy silk is carried out high temperature annealing, carry out the mid-game drawing after the elimination internal stress, obtain alloy and change wire drawing; G. the alloy silk changes to be pulled in and carries out high temperature annealing under the hydrogen shield, carries out mechanical property behind the cool to room temperature and detects and microstructure analysis.
Concrete with the ammonium dimolybdate is, and raw material adds that hydrogen once reduces obtains molybdenum dioxide; Take by weighing La according to weight percent
2O
3Dissolve standby; With molybdenum dioxide and La (NO
3)
3Solution mixes in pot is mixed in bipyramid vacuum-drying, and wherein the pressure of air compressor pump is 0.18MPa, and the bake out temperature of the pot that mixes is 90 ℃, and the inner vacuum tightness of pot of mixing need be controlled at more than the 0.7MPa; Molybdenum dioxide is carried out the secondary hydrogen reducing in four pipe high temperature retort furnaces, hydrogen flowing quantity is 8.0M
3/ H, boat charge is the 1.8kg/ boat, pushing away boat speed is 2 boats/45min; Little lanthanum Mo-La molybdenum powder of mixing is carried out isostatic cool pressing and is pressed into, obtain
Little lanthanum Mo-La alloy bar of mixing, the pressing pressure of isostatic cool pressing is 185MPa, and the dwell time is 8min, and a release time is 45s, and the secondary release time is 5s; And carry out 1250 ℃ of retort furnace presintering and 1900 ℃ of intermediate frequency high temperature sinterings obtain
Little lanthanum Mo-La sintered alloy rod of mixing; Will
Little lanthanum Mo-La sintered alloy rod of mixing carries out 1650 ℃ of Y370 milling trains and the cogging of 1250 ℃ of Y250 Kocos mill millings, obtains respectively
With
Little lanthanum rolled alloy bar of mixing; Will
Littlely mix that lanthanum Mo-La rod of metal alloy is carried out R1800, R1500, R1200, the drawing of R1000 deep bid obtains
Little lanthanum Mo-La alloy silk of mixing; Will
Little lanthanum Mo-La alloy silk of mixing carries out the online annealing of high temperature, and online annealing temperature is 1250 ℃; Carry out the mid-game drawing after eliminating internal stress, obtain
Little lanthanum Mo-La alloy of mixing changes wire drawing.In order to investigate
Little high-temperature behavior of mixing the lanthanum molybdenum filament will
Little lanthanum Mo-La alloy silk of mixing changes and is pulled to
And under hydrogen shield, carry out high temperature annealing respectively at 1300 ℃, 1400 ℃, 1500 ℃ insulation 60min, carry out mechanical property behind the cool to room temperature and detect and microstructure analysis.
Embodiment
Be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate, it is standby to get molybdenum dioxide 50kg; Take by weighing 13.9gLa according to weight percent
2O
3Dissolve standby; With molybdenum dioxide and La (NO
3)
3Solution mixes in pot is mixed in bipyramid vacuum-drying, and wherein the pressure of air compressor pump is 0.18MPa, and the bake out temperature of the pot that mixes is 90 ℃, and the inner vacuum tightness of pot of mixing need be controlled at more than the 0.7MPa, obtains molybdenum dioxide 49.0kg after the doping; Molybdenum dioxide is carried out the secondary hydrogen reducing in four pipe high temperature retort furnaces, hydrogen flowing quantity is 8.0M
3/ H, boat charge is the 1.8kg/ boat, pushing away boat speed is 2 boats/45min, obtains little lanthanum Mo-La alloy powder 34.5kg that mixes; Little lanthanum Mo-La molybdenum powder of mixing is carried out isostatic cool pressing and is pressed into, and obtaining substance is 11.5kg's
Little lanthanum Mo-La alloy bar of mixing, the pressing pressure of isostatic cool pressing is 185MPa, and the dwell time is 8min, and a release time is 45s, and the secondary release time is 5s; And carry out 1250 ℃ of retort furnace presintering and 1900 ℃ of intermediate frequency high temperature sinterings obtain
Little lanthanum Mo-La sintered alloy rod of mixing; Will
Little lanthanum Mo-La sintered alloy rod of mixing carries out 1650 ℃ of Y370 milling trains and the cogging of 1250 ℃ of Y250Kocos mill millings, obtains respectively
With
Little lanthanum rolled alloy bar of mixing; Will
Littlely mix that lanthanum Mo-La rod of metal alloy is carried out R1800, R1500, R1200, the drawing of R1000 deep bid obtains
Little lanthanum Mo-La alloy silk of mixing; Will
Little lanthanum Mo-La alloy silk of mixing carries out the online annealing of high temperature, and online annealing temperature is 1250 ℃; Carry out the mid-game drawing after eliminating internal stress, obtain
Little lanthanum Mo-La alloy of mixing changes wire drawing.In order to investigate
Little high-temperature behavior of mixing the lanthanum molybdenum filament will
Little lanthanum Mo-La alloy silk of mixing changes and is pulled to
And under hydrogen shield, carry out high temperature annealing respectively at 1300 ℃, 1400 ℃, 1500 ℃ insulation 60min, carry out mechanical property behind the cool to room temperature and detect and microstructure analysis.Shown in detection data in the process see the following form.
Claims (1)
1. the preparation method of lanthanum microdoped molybdenum alloy wire, little lanthanum Mo-La rare earth molybdenum alloy wire of mixing of preparation contains oxide compound La
2O
3, wherein the weight percent of La in the silk material is 0.03%, adopts the powder metallurgy process preparation; Gu it is characterized in that it being to carry out secondary reduction after carrying out bipyramid vacuum-drying liquid-doping in the powder molybdenum dioxide stage to produce the lanthanum microdoped molybdenum alloy powder, repressed again, sintering, rolling, drawing procedure are prepared little lanthanum Mo-La alloy silk of mixing; Poly-comprising in the step of its preparation process:
A. be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate;
B. by taking by weighing La
2O
3Dissolve standby; With molybdenum dioxide and La (NO
3)
3Solution mixes in pot is mixed in bipyramid vacuum-drying;
C. molybdenum dioxide is carried out secondary hydrogen reducing Cheng Wei in four pipe high temperature retort furnaces and mix lanthanum Mo-La molybdenum powder;
D. little lanthanum Mo-La molybdenum powder of mixing is carried out isostatic cool pressing and is pressed into alloy bar, carry out 1250 ℃ of temperature presintering and 1900 ℃ of high temperature sinterings obtain the sintered alloy rod;
E. the sintered alloy rod is carried out 1650 ℃ of Y370 milling trains and the cogging of 1250 ℃ of Y250 Kocos mill millings, obtain little lanthanum rolled alloy bar of mixing respectively; Rod of metal alloy is carried out the deep bid drawing obtain the alloy silk;
F. the alloy silk is carried out high temperature annealing under 1250 ℃ of temperature, carry out the mid-game drawing after the elimination internal stress, obtain alloy and change wire drawing;
G. alloy changes wire drawing under hydrogen shield, is incubated 60min respectively and carries out high temperature annealing under 1300 ℃, 1400 ℃, 1500 ℃ temperature, carries out mechanical property behind the cool to room temperature and detects and microstructure analysis.
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| CNB2006101707513A CN100482835C (en) | 2006-12-22 | 2006-12-22 | Lanthanum microdoped molybdenum alloy wire preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110605398A (en) * | 2019-10-11 | 2019-12-24 | 北京北钨科技有限公司 | Preparation method of lanthanum-micro-doped high-temperature molybdenum wire |
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| CN203501764U (en) * | 2012-08-31 | 2014-03-26 | 北京天龙钨钼科技有限公司 | Partition plate assembly used for tungsten sintering furnace |
| CN104392892A (en) * | 2013-11-15 | 2015-03-04 | 朱惠冲 | Light distribution screen in automobile headlight and preparation materials of light distribution screen |
| CN106086747B (en) * | 2016-07-04 | 2018-04-24 | 江阴恩特莱特镀膜科技有限公司 | A kind of B alloy wire for cast rotating tin target prime coat and preparation method thereof |
| CN106591786B (en) * | 2016-11-11 | 2019-02-15 | 洛阳科威钨钼有限公司 | A kind of preparation method of doping type molybdenum target material |
| CN106756157B (en) * | 2016-11-25 | 2018-03-30 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum-rhenium lanthanum alloy material |
| CN107931355A (en) * | 2017-11-17 | 2018-04-20 | 金堆城钼业股份有限公司 | A kind of production method of spray molybdenum wires |
| CN109894621A (en) * | 2019-01-16 | 2019-06-18 | 天长市润源金属制品有限公司 | A kind of medical wire rod of high molybdenum filament and its processing method |
| CN111560551B (en) * | 2019-06-10 | 2021-05-18 | 中国兵器工业第五九研究所 | Preparation method of high-compactness special-shaped molybdenum-based composite material part |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1269426A (en) * | 1999-04-06 | 2000-10-11 | 株洲硬质合金厂 | Preparation of doped molybdenum-base alloy |
| CN1693513A (en) * | 2005-05-26 | 2005-11-09 | 自贡硬质合金有限责任公司 | Production method of molybdenum alloy |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1269426A (en) * | 1999-04-06 | 2000-10-11 | 株洲硬质合金厂 | Preparation of doped molybdenum-base alloy |
| CN1693513A (en) * | 2005-05-26 | 2005-11-09 | 自贡硬质合金有限责任公司 | Production method of molybdenum alloy |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110605398A (en) * | 2019-10-11 | 2019-12-24 | 北京北钨科技有限公司 | Preparation method of lanthanum-micro-doped high-temperature molybdenum wire |
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Owner name: JINDUICHENG MOLYBDENUM CO., LTD. Free format text: FORMER OWNER: JINDUICHENG ALUMINIUM INDUSTRY GROUP CO., LTD. Effective date: 20070907 |
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Effective date of registration: 20070907 Address after: 714102 Shaanxi province Huaxian Jin Dui Zhen Applicant after: Jinduicheng Molybdenum Industry Co., Ltd. Address before: 714102 Shaanxi province Huaxian Jin Dui Zhen Applicant before: Jinduicheng Molybdenum Group Co., Ltd. |
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