CN1876874A - Mo-La-Ce rare earth molybdenum alloy wire and preparation method thereof - Google Patents
Mo-La-Ce rare earth molybdenum alloy wire and preparation method thereof Download PDFInfo
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- CN1876874A CN1876874A CN 200610098707 CN200610098707A CN1876874A CN 1876874 A CN1876874 A CN 1876874A CN 200610098707 CN200610098707 CN 200610098707 CN 200610098707 A CN200610098707 A CN 200610098707A CN 1876874 A CN1876874 A CN 1876874A
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Abstract
The invention relates to a Mo-La-Ce rare-earth molybdenum alloy wire and its process for preparing. The invention is characterized in that the said molybdenum alloy wire contains 0.4 %-1.0% lanthanum oxide and cerium oxide(mass %) and the proportion by weight of lanthanum oxide and cerium oxide is 4:1. The process for preparing is different from the traditional powder metallurgy productive technology, which includes performing vacuum drying and liquid-solid doping for molybdenum dioxide, lanthanum nitrate and cerium nitrate solution, then performing secondary reduction to prepare binary rare-earth doping molybdenum powder, finally preparing rare-earth doping molybdenum wire with Mo-La-Ce of 0.5-0.8mm diameter by impression, agglomeration and pressure processing procedure. The raw materials of this invention is cheap and facile, and the prepared molybdenum wire is of high tensile strength, strong abrasive resistance and simple process and is inflexible, and has high rate of finished products, good compatibility and long durability.
Description
Technical field
Mo-La-Ce rare earth molybdenum alloy wire and preparation method thereof relates to a kind of component, metal processing that is used for special bulb and electric lighting device and cuts molybdenum alloy wire of heater strip in silk and the kiln and preparation method thereof.
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 metal processing industry, be widely used as line cutting molybdenum filament, 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.In the metal processing industry, need line cutting molybdenum filament to have performances such as high strength, high-wearing feature, inductile, long service life, by contrast the intensity of pure molybdenum filament low, wear no resistance, plasticity is higher, work-ing life is short, can not satisfy mechanical industry user's demand.
Summary of the invention
The object of the present invention is to provide that a kind of good processability, tensile strength height, recrystallization temperature height, wear resisting property are strong, technology simply, the Mo-La of not flexible brittle failure, yield rate height, material high conformity, long service life
2O
3-CeO
2The preparation method of rare earth molybdenum alloy wire.
The objective of the invention is to be achieved through the following technical solutions.
The Mo-La-Ce rare earth molybdenum alloy wire is characterized in that containing in this molybdenum alloy wire that to account for weight alloy per-cent be 0.4%～1.0%La
2O
3And CeO
2, and La
2O
3: CeO
2Weight ratio be 4: 1.
The preparation method of Mo-La-Ce rare earth molybdenum alloy wire is characterized in that its preparation process is followed successively by:
A. be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate;
B. get La
2O
3, CeO
2Two kinds of rare earth oxides dissolve with concentrated nitric acid and to make La (NO
3)
3, Ce (NO
3)
4Solution;
C. with molybdenum dioxide and La (NO
3)
3, Ce (NO
3)
4Solution carries out vacuum drying after evenly mixing under vacuum;
D. will mix the oven dry after the titanium dioxide molybdenum powder, carry out the secondary hydrogen reducing and make the Mo-La-Ce doped molybdenum; Carry out the rear-earth-doped molybdenum bar base of isostatic cool pressing compacting Mo-La-Y again; Presintering 1 hour under 1150-1350 ℃ of temperature earlier; 1850 ℃ of-1950 ℃ of sintering temperatures 6 hours, obtain the molybdenum bar that mixes again;
E. the doping molybdenum bar is carried out earlier rollingly together under 1450-1650 ℃ of temperature, under 1350 ℃ of-1450 ℃ of temperature, carry out two road rolling-coggings again and make molybdenum rod, be drawn into assorted molybdenum filament through deep bid again; After annealing under 1250 ℃ of-1350 ℃ of temperature, carry out the mid-game drawing again, obtain the rear-earth-doped molybdenum filament of Mo-La-Ce.
The rear-earth-doped molybdenum filament of Mo-La-Ce of the present invention wherein contains La
2O
3And CeO
2Two kinds of rare earth oxides and pure molybdenum are compared, and the high-temperature behavior of product is good, the recrystallization temperature height, improved more than 400～600 ℃ than pure molybdenum, had premium propertiess such as high strength, high-wearing feature, inductile, long service life, in mechanical processing industry, had widely and use.
The preparation method is different with traditional powder metallurgical production technique, is with molybdenum dioxide La (NO
3)
3, Ce (NO
3)
4Gu solution carries out vacuum-drying liquid-doping, then carry out secondary reduction and produce the binary rare-earth doped molybdenum, operation such as repressed again, sintering, press working, preparing specification is the rear-earth-doped molybdenum filament of 0.5～0.8mmMo-La-Ce.Raw material raw material cheapness of the present invention, be easy to get, prepared molybdenum wire tensile strength height, wear resisting property are strong, technology simply, not flexible brittle failure, yield rate height, high conformity, long service life.
Method of the present invention, raw material is cheap and easy to get.The molybdenum source is an ammonium dimolybdate, the additive La of use
2O
3, CeO
2Cheap, 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; Gu compare the alloying element that is added being evenly distributed in material, good product consistency Gu adopt liquid-adulterating method and solid-adulterating method; 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.
Description of drawings
Accompanying drawing is the process flow diagram of method of the present invention.
Embodiment
The Mo-La-Ce rare earth molybdenum alloy wire, containing weight percent in this molybdenum alloy wire is 0.4%～1.0%La
2O
3And CeO
2, and La
2O
3: CeO
2Weight ratio be 4: 1.Its preparation process is followed successively by: a. is that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate; B. get La
2O
3, CeO
2Two kinds of rare earth oxides dissolve with concentrated nitric acid and to make La (NO
3)
3, Ce (NO
3)
4Solution; C. with molybdenum dioxide and La (NO
3)
3, Ce (NO
3)
4Solution carries out vacuum drying after evenly mixing under vacuum; D. will mix the oven dry after the titanium dioxide molybdenum powder, carry out the secondary hydrogen reducing and make the Mo-La-Ce doped molybdenum; Carry out the rear-earth-doped molybdenum bar base of isostatic cool pressing compacting Mo-La-Y again; Presintering 1 hour under 1150 ℃ of-1350 ℃ of temperature earlier 1850 ℃ of-1950 ℃ of sintering temperatures 6 hours, obtains the molybdenum bar that mixes again; E. the doping molybdenum bar is carried out earlier rollingly together under 1450 ℃ of-1650 ℃ of temperature, under 1350 ℃ of-1450 ℃ of temperature, carry out two road rolling-coggings again and make molybdenum rod, be drawn into assorted molybdenum filament through deep bid again; After annealing under 1250 ℃ of-1350 ℃ of temperature, carry out the mid-game drawing again, obtain the rear-earth-doped molybdenum filament of Mo-La-Ce.
Embodiment 1
Preparation process is to be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate; Weight percent according to tabulation 1 alloy designs composition takes by weighing two kinds of rare earth oxides respectively and dissolves standby with concentrated nitric acid; With molybdenum dioxide and La (NO
3)
3, Ce (NO
3)
4Solution mixes in pot is mixed in bipyramid vacuum-drying, and wherein the pressure of air compressor pump is 0.2MPa, and the bake out temperature of the pot that mixes is 70 ℃, and the inner vacuum tightness of pot of mixing need be controlled at more than the 0.06MPa; Molybdenum dioxide is carried out the secondary hydrogen reducing in four pipe high temperature retort furnaces, hydrogen flowing quantity is 2.2M
3/ H, boat charge is the 1.0kg/ boat, pushing away boat speed is 4 boats/60min; The Mo-La-Ce doped molybdenum is carried out isostatic cool pressing be pressed into, obtain the rear-earth-doped molybdenum bar of 48mmMo-La-Y, the pressing pressure of isostatic cool pressing is 175MPa, and the dwell time is 10min, and a release time is 45s, and the secondary release time is 5s; And carried out 1250 ℃ of retort furnace presintering 1 hour and 1950 ℃ of 6 hours intermediate frequency high temperature sinterings obtain 48mmMo-La-Ce sintering doping molybdenum bar; 48mmMo-La-Ce sintering doping molybdenum bar is carried out 1650 ℃ of Y370 milling trains and the cogging of 1250 ℃ of Y250Kocos mill millings, obtain 14.5mm and the rolling molybdenum rod of 6.0mm respectively; With the rear-earth-doped molybdenum rod of 6.0mmMo-La-Ce carry out R1800, R1500, R1200, the drawing of R1000 deep bid obtains the rear-earth-doped molybdenum filament of 1.75mmMo-La-Ce; The rear-earth-doped molybdenum filament of 1.75mmMo-La-Ce is carried out high temperature annealing, and annealing temperature is 1250 ℃, and soaking time is 30min; Carry out the mid-game drawing after eliminating internal stress, obtain the rear-earth-doped molybdenum filament of 0.5～ 0.8mmMo-La-Ce.
The composition and the index of table 1 Mo-La-Ce rare earth molybdenum alloy wire
| Synthetic silk composition (wt.%) | Silk footpath (mm) | Brinell hardness number | Density | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) | ||
| La 2O 3 | CeO 2 | Mo | ||||||
| 0.32 | 0.08 | 99.96 | ￠0.7 | 203 | 10.16 | 1379 | 14 | 200 |
| 0.16 | 0.04 | 99.8 | ￠0.7 | 189 | 10.18 | 1156 | 17 | 200 |
| 0.8 | 0.2 | 99.00 | ￠0.7 | 217 | 10.16 | 1583 | 9 | 200 |
The mechanical property of table 2 3.17mmMo-La-Ce doped molybdenum wire
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 883.19 | 3.6 | 50 |
| MLC-2 | 933.13 | 2.3 | 50 |
| MLC-3 | 956.91 | 16.6 | 50 |
| MLC-4 | 945.36 | 7.9 | 50 |
| MLC-5 | 942.30 | 15.1 | 50 |
The mechanical property of table 3 2.0mmMo-La-Ce doped molybdenum wire
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 1303.11 | 2.60 | 50 |
| 1313.35 | 5.40 | 50 | |
| 1323.59 | 3.04 | 50 | |
| MLC-2 | 1076.33 | 3.13 | 50 |
| 1068.29 | 4.13 | 50 | |
| 1070.63 | 4.39 | 50 | |
| MLC-3 | 1106.80 | 3.23 | 50 |
| 1133.26 | 3.47 | 50 | |
| 1129.57 | 4.23 | 50 |
Mechanical property after the annealing of table 4 1.75mmMo-La-Ce doped molybdenum wire
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 897.29 | 17.86 | 50 |
| 900.19 | 15.58 | 50 | |
| 940.53 | 16.57 | 50 | |
| MLC-2 | 994.51 | 13.39 | 50 |
| 1051.38 | 8.06 | 50 | |
| 1015.98 | 10.07 | 50 | |
| MLC-3 | 1017.72 | 14.24 | 50 |
| 1027.88 | 8.59 | 50 | |
| 1001.76 | 16.39 | 50 |
The mechanical property of table 5 0.90mmMo-La-Ce doped molybdenum wire
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 1340.37 | 5.19 | 50 |
| 1366.30 | 2.51 | 50 | |
| 1385.74 | 3.05 | 50 | |
| MLC-2 | 1251.17 | 2.06 | 50 |
| 1250.79 | 6.18 | 50 | |
| 1247.36 | 4.56 | 50 | |
| MLC-3 | 1242.40 | 2.69 | 50 |
| 1258.03 | 4.75 | 50 | |
| 1255.36 | 2.15 | 50 |
The mechanical property of table 6 0.70mmMo-La-Ce doped molybdenum wire
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 1393.68 | 8.68 | 200 |
| 1362.54 | 7.36 | 200 | |
| 1377.07 | 8.47 | 200 | |
| MLC-2 | 1491.25 | 7.89 | 200 |
| 1528.62 | 7.95 | 200 | |
| 1435.89 | 7.45 | 200 | |
| MLC-3 | 1374.31 | 8.35 | 200 |
| 1368.77 | 6.26 | 200 | |
| 1431.05 | 6.84 | 200 |
Behind the table 7 0.70mmMo-La-Ce doped molybdenum wire medium annealing (1500 ℃ * 3h) mechanical property
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 914.67 | 23.01 | 200 |
| MLC-2 | 913.64 | 18.25 | 200 |
| MLC-3 | 928.08 | 18.81 | 200 |
Behind the table 8 0.70mmMo-La-Ce doped molybdenum wire medium annealing (1840 ℃ * 6h) mechanical property
| Lot number | Tensile strength (MPa) | Unit elongation (%) | Gauge length (mm) |
| MLC-1 | 563.25 | 0.99 | 200 |
| MLC-2 | 523.70 | 2.68 | 200 |
| MLC-3 | 562.90 | 0.99 | 200 |
Claims (2)
1.Mo-La-Ce rare earth molybdenum alloy wire, it is characterized in that containing in this molybdenum alloy wire the weight percent that accounts for alloy is 0.4%～1.0%La
2O
3And CeO
2, and La
2O
3: CeO
2Weight ratio be 4: 1.
2.Mo-La-Ce the preparation method of rare earth molybdenum alloy wire is characterized in that its preparation process is followed successively by:
A. be that raw material adds hydrogen and once reduces and obtain molybdenum dioxide with the ammonium dimolybdate;
B. get La
2O
3, CeO
2Two kinds of rare earth oxides dissolve with concentrated nitric acid and to make La (NO
3)
3, Ce (NO
3)
4Solution;
C. with molybdenum dioxide and La (NO
3)
3, Ce (NO
3)
4Solution carries out vacuum drying after evenly mixing under vacuum;
D. will mix the oven dry after the titanium dioxide molybdenum powder, carry out the secondary hydrogen reducing and make the Mo-La-Ce doped molybdenum; Carry out the rear-earth-doped molybdenum bar base of isostatic cool pressing compacting Mo-La-Y again; Earlier again under 1150 ℃ of-1350 ℃ of temperature, sintering 1 hour; 1850 ℃ of-1950 ℃ of sintering temperatures 6 hours, obtain the molybdenum bar that mixes again;
E. the doping molybdenum bar is carried out earlier rollingly together under 1450 ℃ of-1650 ℃ of temperature, under 1250 ℃ of-1350 ℃ of temperature, carry out two road rolling-coggings again and make molybdenum rod, be drawn into assorted molybdenum filament through deep bid again; After annealing under 1200 ℃ of-1300 ℃ of temperature, carry out the mid-game drawing again, obtain the rear-earth-doped molybdenum filament of Mo-La-Ce.
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|---|---|---|---|
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|---|---|---|---|
| CN 200610098707 CN1876874A (en) | 2006-07-06 | 2006-07-06 | Mo-La-Ce rare earth molybdenum alloy wire and preparation method thereof |
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|---|---|---|---|---|
| CN100439522C (en) * | 2006-12-15 | 2008-12-03 | 西部金属材料股份有限公司 | Process for preparing molybdenum-lanthanum alloy |
| CN100439523C (en) * | 2006-12-15 | 2008-12-03 | 西部金属材料股份有限公司 | Process for preparing high-performance molybdenum bar |
| CN101956112A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Mo-Ce alloy wire and preparation method thereof |
| CN103706802A (en) * | 2013-12-18 | 2014-04-09 | 金堆城钼业股份有限公司 | Method for preparing lanthanum-doped alloy molybdenum powder |
| CN104511591A (en) * | 2014-12-27 | 2015-04-15 | 金堆城钼业股份有限公司 | Preparation method of composite rare earth oxide reinforced molybdenum alloy piercing mandrel |
| CN109913791A (en) * | 2017-12-13 | 2019-06-21 | 现代自动车株式会社 | Friction member and its coating method with wear-resistant coating |
| CN110548771A (en) * | 2019-08-14 | 2019-12-10 | 江苏弘亚钨钼科技有限公司 | Preparation method of W-shaped molybdenum wire |
| 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 |
| 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 |
| CN110846528A (en) * | 2019-10-17 | 2020-02-28 | 自贡硬质合金有限责任公司 | Preparation method of molybdenum plate blank |
| CN110976900A (en) * | 2019-11-21 | 2020-04-10 | 金堆城钼业股份有限公司 | Production method of composite alloy molybdenum powder |
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2006
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439523C (en) * | 2006-12-15 | 2008-12-03 | 西部金属材料股份有限公司 | Process for preparing high-performance molybdenum bar |
| CN100439522C (en) * | 2006-12-15 | 2008-12-03 | 西部金属材料股份有限公司 | Process for preparing molybdenum-lanthanum alloy |
| CN101956112B (en) * | 2010-09-30 | 2014-06-18 | 金堆城钼业股份有限公司 | Mo-Ce alloy wire and preparation method thereof |
| CN101956112A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Mo-Ce alloy wire and preparation method thereof |
| CN103706802B (en) * | 2013-12-18 | 2015-07-29 | 金堆城钼业股份有限公司 | Mix the preparation method of lanthanum alloy molybdenum powder |
| CN103706802A (en) * | 2013-12-18 | 2014-04-09 | 金堆城钼业股份有限公司 | Method for preparing lanthanum-doped alloy molybdenum powder |
| CN104511591A (en) * | 2014-12-27 | 2015-04-15 | 金堆城钼业股份有限公司 | Preparation method of composite rare earth oxide reinforced molybdenum alloy piercing mandrel |
| CN109913791A (en) * | 2017-12-13 | 2019-06-21 | 现代自动车株式会社 | Friction member and its coating method with wear-resistant coating |
| CN110548771A (en) * | 2019-08-14 | 2019-12-10 | 江苏弘亚钨钼科技有限公司 | Preparation method of W-shaped molybdenum wire |
| 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 |
| 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 |
| CN110846528A (en) * | 2019-10-17 | 2020-02-28 | 自贡硬质合金有限责任公司 | Preparation method of molybdenum plate blank |
| CN110976900A (en) * | 2019-11-21 | 2020-04-10 | 金堆城钼业股份有限公司 | Production method of composite alloy molybdenum powder |
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Owner name: JINDUICHENG MOLYBDENUM CO., LTD. Free format text: FORMER OWNER: JINDUICHENG ALUMINIUM INDUSTRY GROUP CO., LTD. Effective date: 20070914 |
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Effective date of registration: 20070914 Address after: 714102 Shaanxi province Huaxian County in northern Shaanxi Province Jin Dui Zhen Applicant after: Jinduicheng Molybdenum Industry Co., Ltd. Address before: 714102 Shaanxi province Huaxian County in northern Shaanxi Province Jin Dui Zhen Applicant before: Jinduicheng Molybdenum Group Co., Ltd. |
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