CN101074460A - Method for processing tungsten alloy filament - Google Patents
Method for processing tungsten alloy filament Download PDFInfo
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- CN101074460A CN101074460A CN 200610013763 CN200610013763A CN101074460A CN 101074460 A CN101074460 A CN 101074460A CN 200610013763 CN200610013763 CN 200610013763 CN 200610013763 A CN200610013763 A CN 200610013763A CN 101074460 A CN101074460 A CN 101074460A
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Abstract
A method for machining tungsten-alloy is carried out by dissolving ammonium paratungstate into blue tungsten oxide, adding into K2SiO3 liquid and oxide for improving crystal grain growth, mixing, reducing for two times, pickling, adding rare-earth element solution into pickled raw materials, igniting, screening mixed materials, reducing for two times, screening mixed materials, press forming to obtain briquette strip, sintering in medium-frequency inductive furnace, vertically smelting while sintering, spiral forging, ingoting, re-crystallizing, spiral forging, coiling, eliminating stress, annealing and refining. It has excellent plasticity below Phi0.30 mm, longer utilizing life and better finished product rate.
Description
Technical field:
The present invention relates to a kind of complete processing of tungsten filament, particularly a kind of working method of in tungsten, adding the tungsten alloy filament for preparing behind the rare earth element.
Background technology:
In tungsten, add a certain amount of rare earth element, can change the use properties of tungsten filament, can improve electron emissivity and anti-ablation ability, can improve the processing characteristics of tungsten simultaneously as interpolation cerium or thorium in tungsten.The tungsten alloy filament and the goods that utilize these characteristics to produce are mainly used in tube heater, argon arc welding electrode, pulse tube heater strip.For example: industrial ratio-frequency heating pipe radar modulate emission pipe.Negative electrode as gas discharge lamp in the light source industry also is widely used, though it is high mainly due to the pure tungsten fusing point, but work function height (4.5eV), the trigger voltage height of lamp, and under the ion bombardment of macro-energy easy splatter, make the lifetime of lamp, but added its work function of cerium 2.4eV has just been arranged, having added its work function of thorium just has 2.6eV, and big (for example: when the 1500K, emission can increase by 1.8 * 10 than pure tungsten and tungsten has added after cerium or the thorium its electron emission
5Doubly).Added rhenium in tungsten, can improve the recrystallization temperature of tungsten, improved cold plasticity and high temperature court of a feudal ruler property, improved resistance of oxidation, its resistivity also is improved simultaneously.Be mainly used in electron tube directly-heated wire cathode and well heater, electron tube is deleted the utmost point, picture tube heated filament, pyrometer couple and various hot parts.
Though after having added certain rare earth element, can produce above-mentioned tungsten filament and the goods thereof that various uses is arranged, but the present domestic tungsten cerium alloy of producing (tungsten thorium alloy, W-Re alloys) can't be machined to the filament (the particularly following specification of Φ 0.3mm) of the following specification of Φ 0.8mm.The production technique that mainly is its alloy preform bar falls behind, the base bar foreign matter content of being produced is too high, the distribution of additives of being added is inhomogeneous, density is inconsistent, and domestic used technical process is finished according to the following step: (being selected from " tungsten filament production principle, technology and performance thereof ") 1, become tungstic oxide or calcination au bleu Tungsten oxide 99.999 or low the change to be reduced into blue tungsten oxide the ammonium paratungstate roasting; 2, add cerium (thorium, rhenium etc.); 3, drying, batch mixing, sieve; 4, between 650 ℃-700 ℃, once reduce, between 900 ℃-950 ℃, carry out secondary reduction; 5, the tungstenalloy powder is pressed into the base bar; 6, low temperature presintering; 7, incipient fusion sintering; 8, the processing of swaging; 9, the water-break of annealing again; 10, the processing of swaging; 11, draw processing.
Summary of the invention:
Purpose of the present invention just is to overcome above-mentioned the deficiencies in the prior art, and provide a kind of working method of tungsten alloy filament, the tungsten cerium alloy silk that this method is produced has good plasticity, can be worked into below the Φ 0.30mm, can carry out coiling processing according to different purposes, and its use properties meets international standards fully.
Technical scheme of the present invention is: a kind of working method of tungsten alloy filament is characterized in that: carry out according to the following step: 1. ammonium paratungstate is fused the au bleu Tungsten oxide 99.999, K then mixes
2SiO3 liquid and can promote crystal grain a large amount of and fast grown oxide carry out batch mixing; 2. above-mentioned raw materials is carried out the reduction first time between 600 ℃-650 ℃, between 800 ℃-850 ℃, carry out the reduction second time; 3. the raw material after will reducing carries out 30 hours-40 hours pickling; 4. add the batch mixing that sieves after the rare earth element solution calcination in the raw material after pickling, between 750 ℃-800 ℃, carry out reduction first time, between 900 ℃-950 ℃, carry out the second time and reduce; 5. batch mixing sieves; 6. after being pressed into the base bar, carry out low temperature presintering; 7. sintering or carry out the incipient fusion sintering twice in medium-frequency induction furnace; 8. carry out rotary blooming, recrystallization annealing temperature, the processing of swaging, recrystallization annealing, the processing of swaging, drawing processing, stress relieving successively; 9. carry out fining-off.
Above-mentioned promote crystal grain a large amount of and fast grown oxide can use silicon-dioxide, aluminum oxide.
Above-mentioned rare earth element can be cerium or thorium or rhenium.
Advantage of the present invention is: 1, the present invention has guaranteed that the crystal boundary axial array of tungsten also makes simultaneously not president too big of its crystal grain, has guaranteed the reasonable dislocation and the ideal number of die of crystal boundary.Among the present invention owing in the doping process, used and can promote the crystal grain multiple additives (salt of wormwood, silicon-dioxide, aluminum oxide) of growing in a large number and fast, these additives are grown crystal in a large number and fast, form the huge interlocking crystal grain with many crystal boundary axial array, the thermostability and the high temperature creep strength of this structure are good.Simultaneously after cerium or thorium or these rare earth elements of rhenium are added in pickling later on; the particle of these oxide compounds enters on the crystal boundary of tungsten; can stop the slippage of crystal boundary; restriction crystal grain is further grown up; improve the recrystallization temperature of tungsten, can keep the fineness of recrystal grain, thereby improved the resistance to deformation of tungsten filament and dislocation (during grain sliding; slippage part and the not boundary of slippage part on slip plane are called " dislocation ") performance.2, add acid cleaning process and removed the most of harmful element in the tungsten powder, made it to reach perfect condition.Analytical results such as following table:
| Title | Fe | Al | Si | Mg | Ca | Ni | O | C |
| Content (%) | 0.0015％ | 0.0006％ | 0.001％ | 0.0006％ | 0.001％ | 0.0006％ | 0.0017％ | 0.002％ |
| Title | P | N | P6 | Bi | Sn | Sb | As | Mo |
| Content (%) | 0.0006％ | 0.0015％ | 0.0001％ | 0.0001％ | 0.0001％ | 0.001％ | 0.001％ | 0.0037％ |
3, the present invention adopts 4 reducing process and the batch mixing that sieves for twice, its objective is and utilizes the reductibility of hydrogen to oxide compound, has reduced the oxygen level in the alloy powder.(too high oxygen level also is the factor that the alloy preform bar can't deep processing) twice batch mixing that sieves makes various additives more even in tungsten powder, and the density of the alloy bar of making could be consistent more.4, the tungsten alloy filament material that processes of the present invention is fit to further deep processing, has good plasticity, can be worked into the following specification of Φ 0.30mm.5, finished product rate height, the long service life of utilizing tungsten alloy filament material that the present invention processes to make.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
Embodiment 1: preparation tungsten cerium alloy silk:
A kind of working method of tungsten cerium alloy silk, carry out according to the following step: 1. ammonium paratungstate is fused the au bleu Tungsten oxide 99.999, K then mixes
2SiO3 liquid and Al (NO
3)
3Liquid, batch mixing; The content of potassium should be controlled at 50-80PPm.2. above-mentioned raw materials is carried out the reduction first time between 600 ℃-650 ℃, between 800 ℃-850 ℃, carry out the reduction second time; 3. the raw material after will reducing carries out 30 hours pickling; (deionized water wash repeatedly makes 80 ℃-120 ℃ of pH values=7 vacuum-dryings) 4. adds the cerous nitrate solution batch mixing that sieves in the raw material after pickling after 300 ℃ of-500 ℃ of calcinations, between 750 ℃-800 ℃, carry out the reduction first time, between 900 ℃-950 ℃, carry out the reduction second time; 5. batch mixing sieves; 6. after being pressed into the base bar, carry out low temperature presintering (1100 ℃); 7. carry out the incipient fusion sintering twice; The incipient fusion sintering is warmed up to 1500-1600 ℃ for the first time, is incubated 12-15 minute, fusing current 80-90%, and the incipient fusion sintering is warmed up to 1700-1900 ℃ for the second time, is incubated 12-15 minute, fusing current 80-90%, and the density of tungsten rod is guaranteed at 17.4～17.9g/cm
38. carry out rotary blooming, recrystallization annealing temperature, the processing of swaging, recrystallization annealing, the processing of swaging, drawing processing, stress relieving successively; 9. carry out fining-off.
Claims (3)
1, a kind of working method of tungsten alloy filament is characterized in that: carry out according to the following step: 1. with ammonium paratungstate powder fusion au bleu Tungsten oxide 99.999, K then mixes
2SiO3 liquid and can promote crystal grain a large amount of and fast grown oxide carry out batch mixing; 2. above-mentioned raw materials is carried out the reduction first time between 600 ℃-650 ℃, between 800 ℃-850 ℃, carry out the reduction second time; 3. the raw material after will reducing carries out 30 hours-40 hours pickling; 4. add the batch mixing that sieves after the rare earth element solution calcination in the raw material after pickling, between 750 ℃-800 ℃, carry out reduction first time, between 900 ℃-950 ℃, carry out the second time and reduce; 5. batch mixing sieves; 6. after being pressed into the base bar, carry out low temperature presintering; 7. in medium-frequency induction furnace, carry out sintering or carry out the incipient fusion sintering twice; 8. carry out rotary blooming, recrystallization annealing temperature, the processing of swaging, recrystallization annealing, the processing of swaging, drawing processing, stress relieving successively; 9. carry out fining-off.
2, the working method of tungsten alloy filament according to claim 1 is characterized in that: above-mentioned promote crystal grain a large amount of and fast grown oxide can use silicon-dioxide, aluminum oxide.
3, the working method of tungsten alloy filament according to claim 1 is characterized in that: above-mentioned rare earth element can be cerium or thorium or rhenium.
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| CN 200610013763 CN101074460A (en) | 2006-05-19 | 2006-05-19 | Method for processing tungsten alloy filament |
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| CN 200610013763 CN101074460A (en) | 2006-05-19 | 2006-05-19 | Method for processing tungsten alloy filament |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009171A (en) * | 2010-09-30 | 2011-04-13 | 厦门虹鹭钨钼工业有限公司 | Magnetron coil material powder for magnetron cathode and preparation method thereof |
| CN102672175A (en) * | 2012-05-15 | 2012-09-19 | 赣州海盛钨钼集团有限公司 | Preparation method of potassium-containing round-tungsten-doped aluminum strip |
| CN101716708B (en) * | 2009-12-23 | 2012-11-14 | 北京钨钼材料厂 | Method and device for annealing and rotary swaging multiplex composite rare-earth tungsten electrode |
| CN103346054A (en) * | 2013-06-21 | 2013-10-09 | 威海多晶钨钼科技有限公司 | Thorium tungsten wire used for winding microwave oven magnetron and manufacturing method of thorium tungsten wire |
| CN103658655A (en) * | 2013-12-25 | 2014-03-26 | 株洲硬质合金集团有限公司 | Method for producing xenon lamp tungsten anode |
| CN105385897A (en) * | 2015-11-04 | 2016-03-09 | 重庆材料研究院有限公司 | Thermocouple material for temperature measurement of reactor core of nuclear reactor and preparation method |
| CN105506255A (en) * | 2015-12-11 | 2016-04-20 | 朱惠冲 | Breakage-preventing machining process for tungsten-base alloy wire rods |
| CN107068514A (en) * | 2017-04-18 | 2017-08-18 | 江苏圣亚有色金属材料有限公司 | A kind of preparation method of electron gun filament |
| CN110102869A (en) * | 2019-05-16 | 2019-08-09 | 广东省焊接技术研究所（广东省中乌研究院） | A kind of agitating friction weldering stirring head material and preparation method thereof |
| CN110164751A (en) * | 2018-02-05 | 2019-08-23 | 北京欧美中科学技术研究院 | A kind of preparation method of graphene high-efficiency energy-saving lamp |
| CN113174521A (en) * | 2021-01-15 | 2021-07-27 | 厦门虹鹭钨钼工业有限公司 | Tungsten-rhenium alloy wire and preparation method thereof |
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2006
- 2006-05-19 CN CN 200610013763 patent/CN101074460A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716708B (en) * | 2009-12-23 | 2012-11-14 | 北京钨钼材料厂 | Method and device for annealing and rotary swaging multiplex composite rare-earth tungsten electrode |
| CN102009171A (en) * | 2010-09-30 | 2011-04-13 | 厦门虹鹭钨钼工业有限公司 | Magnetron coil material powder for magnetron cathode and preparation method thereof |
| CN102009171B (en) * | 2010-09-30 | 2012-08-22 | 厦门虹鹭钨钼工业有限公司 | Magnetron coil material powder for magnetron cathode and preparation method thereof |
| CN102672175A (en) * | 2012-05-15 | 2012-09-19 | 赣州海盛钨钼集团有限公司 | Preparation method of potassium-containing round-tungsten-doped aluminum strip |
| CN103346054B (en) * | 2013-06-21 | 2015-06-10 | 威海多晶钨钼科技有限公司 | Thorium tungsten wire used for winding microwave oven magnetron and manufacturing method of thorium tungsten wire |
| CN103346054A (en) * | 2013-06-21 | 2013-10-09 | 威海多晶钨钼科技有限公司 | Thorium tungsten wire used for winding microwave oven magnetron and manufacturing method of thorium tungsten wire |
| CN103658655A (en) * | 2013-12-25 | 2014-03-26 | 株洲硬质合金集团有限公司 | Method for producing xenon lamp tungsten anode |
| CN103658655B (en) * | 2013-12-25 | 2015-12-09 | 株洲硬质合金集团有限公司 | A kind of production method of xenon lamp tungsten anode |
| CN105385897A (en) * | 2015-11-04 | 2016-03-09 | 重庆材料研究院有限公司 | Thermocouple material for temperature measurement of reactor core of nuclear reactor and preparation method |
| CN105385897B (en) * | 2015-11-04 | 2018-06-19 | 重庆材料研究院有限公司 | Nuclear reactor thermocouple for measuring temperature material and preparation method |
| CN105506255A (en) * | 2015-12-11 | 2016-04-20 | 朱惠冲 | Breakage-preventing machining process for tungsten-base alloy wire rods |
| CN107068514A (en) * | 2017-04-18 | 2017-08-18 | 江苏圣亚有色金属材料有限公司 | A kind of preparation method of electron gun filament |
| CN110164751A (en) * | 2018-02-05 | 2019-08-23 | 北京欧美中科学技术研究院 | A kind of preparation method of graphene high-efficiency energy-saving lamp |
| CN110102869A (en) * | 2019-05-16 | 2019-08-09 | 广东省焊接技术研究所（广东省中乌研究院） | A kind of agitating friction weldering stirring head material and preparation method thereof |
| CN113174521A (en) * | 2021-01-15 | 2021-07-27 | 厦门虹鹭钨钼工业有限公司 | Tungsten-rhenium alloy wire and preparation method thereof |
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Open date: 20071121 |