CN102198507A - Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament - Google Patents
Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament Download PDFInfo
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- CN102198507A CN102198507A CN 201110125548 CN201110125548A CN102198507A CN 102198507 A CN102198507 A CN 102198507A CN 201110125548 CN201110125548 CN 201110125548 CN 201110125548 A CN201110125548 A CN 201110125548A CN 102198507 A CN102198507 A CN 102198507A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 92
- 239000010937 tungsten Substances 0.000 title claims abstract description 92
- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 24
- 150000002367 halogens Chemical class 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011591 potassium Substances 0.000 claims abstract description 28
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 239000008187 granular material Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000004927 fusion Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 22
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 8
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005056 compaction Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000011799 hole material Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 2
- 239000006260 foam Substances 0.000 abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 238000012545 processing Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 206010000269 abscess Diseases 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- CGGMOWIEIMVEMW-UHFFFAOYSA-N potassium tungsten Chemical compound [K].[W] CGGMOWIEIMVEMW-UHFFFAOYSA-N 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention provides a method for producing a tungsten bar serving as a halogen tungsten lamp tungsten filament, comprising the following steps of: material selecting, pre-reducing, high potassium doping, reducing, acid rinsing, powder preparing, cold static pressure shaping, high temperature sintering and the like. Compared with the conventional technology, the method is characterized in that two crystal ammonium paratungstates are utilized to prepared raw materials, high potassium doping is adopted, preparation of middle granule tungsten powder is added, a powder distribution scheme is optimized by the middle granule tungsten and a unique incipient fusion high temperature sintering process is utilized. In the method, the granularity distribution of the tungsten powder avoids the peak or double peak phenomenon and has good normal distribution, after being sintered at high temperature, the cross section crystal of the tungsten bar is thin and uniform; the tungsten bar is pressed by a powder mixing scheme; according to a forming mechanism of potassium foams, the number of tungsten bar cross section crystal grains is increased; and the partial growth of the crystal grains is avoided so that the potassium foam is small in aperture, large in density, multiple in crystal boundary, long in line and uniform in distribution.
Description
Technical field
The present invention relates to the tungsten powder metallurgical technology, especially a kind of tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament.
Background technology
Along with the fast development of Domestic Automotive Industry, electronics industry, space flight and aviation industry, the demand of halogen tungsten lamp is with the speed increment in every year 20%.Halogen tungsten lamp is mainly used in the illuminator of above-mentioned industry.There is the characteristic of shock and vibration in halogen tungsten lamp because of environment for use, therefore require that its core material---the recrystallized structure of tungsten filament can form good dovetail bridging arrangement, length-width ratio is greater than 12, i.e. elevated temperature strength height under the high temperature burning-point state, and high temperature sink-resistance performance and anti-deformation are good.The technological process of production of tungsten filament is long, but after the process that changes sintered state (tungsten rod) from powdered form into is finished, the chemical composition and the structure property of tungsten filament are established, follow-up calendering processing is very small to the improvement and the castering action of tungsten filament high temperature sink-resistance performance, and therefore how obtaining the good high potassium tungsten rod of institutional framework becomes the key point that the wolfram filament for halogen tungsten lamp quality promotes.China's tungsten filament production technology is started late, and the domestic blank that still belongs to of the production line of wolfram filament for halogen tungsten lamp adopts common process, can only obtain low and middle-grade wolfram filament for halogen tungsten lamp by the production line screening of common tungsten filament, causes the yield rate of its product low, the production cost height; This wolfram filament for halogen tungsten lamp is low because of its start-stop recrystallization temperature simultaneously, length-width ratio is little, make that its elevated temperature strength is low, high temperature sink-resistance performance and anti-deformation is poor, service life short, quality and external product gap are bigger, at present mainly by satisfying domestic demand from external high price import halogen tungsten lamp or wolfram filament for halogen tungsten lamp.Therefore, improve the tungsten rod quality, particularly urgent from improving the start with needs that satisfy the wolfram filament for halogen tungsten lamp quality of material property.
Summary of the invention
Purpose of the present invention just provides a kind of tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament, tungsten rod potassium content 〉=0.0085%, the density 〉=17.20g/cm that prepare with this method
3, grain size 〉=6000/mm
2, adopt existing routine techniques to carry out pressure processing, can produce the recrystallized structure structure and be good dovetail overlap joint, length-width ratio is greater than 12, steady quality, yield rate height, and under high temperature burning-point state the elevated temperature strength height, the wolfram filament for halogen tungsten lamp that high temperature sink-resistance performance and anti-deformation are good.
The tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament of the present invention may further comprise the steps:
1, select materials, the monocline ammonium paratungstate mixes in the ratio of 3:1～1.5 with spherical ammonium paratungstate, is raw material with the mixture of gained;
2, prereduction adopts routine techniques that above-mentioned raw materials is passed through four-tape warm area reduction furnace, and hydrogen reducing generation oxygen content is 20～20.5% blue tungsten oxide;
3, high potassium mixes, with common process the blue tungsten oxide wet method is mixed potassium silicate, aluminum nitrate solution, potassium, silicon, aluminium are adsorbed in the blue tungsten hole, and potassium, silicon, aluminium content are respectively 0.18～0.20%, 0.30～0.35%, 0.010～0.013% in the doped blue tungsten;
4, reduction generates Fisher particle size with conventional reduction technology by secondary reduction with doped blue tungsten and is the fine grained tungsten powder of 2.0～2.6um, and is standby; Doped blue tungsten is generated Fisher particle size with the direct once reduction of conventional reduction technology be the coarse granule tungsten powder of 3.4～4.0um, standby; Adopting six warm area reduction furnaces that doped blue tungsten is generated Fisher particle size through secondary reduction is the middle particle tungsten powder of 2.7～3.3um, standby, in the process conditions of particle tungsten powder preparation be: once also the reason doped blue tungsten temperature for preparing tungsten dioxide is 530,550,580,620,650,670 ℃, and hydrogen flowing quantity is 2.0～3.0m
3/ h, dew point of hydrogen≤-60 ℃, boat charge is 300～350g, push away speed and be 25min, output tungsten dioxide oxygen content is 12～14%, and the process conditions of particle tungsten powder in the secondary reduction preparation: temperature is 700,750,800,830,860,860 ℃, and hydrogen flowing quantity is 3.0～5.0m
3/ h, dew point of hydrogen≤-60 ℃, boat charge is 280～320g, pushes away speed and is 30min;
5, pickling, with thin, in, the coarse granule tungsten powder is adulterant and the impurity that surplus is removed in 5～6% hydrochloric acid, 5～6% hydrofluoric acid washes with concentration respectively, the effective potassium content of gained acid-washed tungsten powder is respectively 0.016～0.018%, 0.012～0.014%, 0.008～0.010%;
6, join powder, thin, in, the coarse granule acid-washed tungsten powder mixes 25～30min by the weight ratio of 20～25:60～50:20～25 in batch mixer;
7, cold isostatic compaction, adopting routine techniques that 2000g is cooperated the tungsten powder diameter of packing into is in the elasticity die sleeve of 23 ± 0.2mm, uses the cold isostatic press press forming, and the maximal pressure pressing pressure is 150～160Mpa, be shaped the back tungsten strip under hydrogen shield, through 1300 ± 50 ℃ of presintering 40～45min;
8, high temperature sintering; under hydrogen shield; tungsten strip directly energising heat-agglomerating in the incipient fusion machine after the presintering; sintering schedule is three sections intensifications, two sections insulations; electric current/time parameter is (the 0-2000A)/5min that heats up, intensification (2000-3800A)/15min, insulation 3800A/15min, intensification (3800-4900A)/2min, insulation 4900A/20min; the crystallization of output tungsten rod section is tiny and even, potassium content 〉=0.0085%, density 〉=17.20g/cm
3, grain size 〉=6000/mm
2
The tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament of the present invention, distinguish preparation, the middle particle tungsten powder of the high potassium doping of the ammonium paratungstate mixed preparing, the employing that are two kinds of crystalline forms of raw material employing, newly-increased a kind of middle particle tungsten powder with common process and optimized the incipient fusion high temperature sintering system of joining powder scheme and employing uniqueness, its action principle and advantage are:
1, by the ammonium para-tungstate crystal pattern is influenced discovering of product performance, the crystalline form resulting a certain specific ammonium paratungstate of arranging in pairs or groups can make the every performance of wolfram filament for halogen tungsten lamp all good, and the change of single crystalline form ammonium paratungstate ratio, the performance of gained tungsten filament changes thereupon;
2, the more conventional doping of blue tungsten doping of the present invention is high by 30～40%, and conventional method is if adopt the doping gained tungsten rod density＜17.0g/cm of this method
3, grain size＜1000/mm
2, be difficult to processing, yield rate is low, and cause the institutional framework deterioration, mould-crisp transition temperature height, problem such as high temperature sink-resistance performance difference.
3, the preparation of the newly-increased a kind of middle particle tungsten powder of the present invention, after the cooperation, the size distribution of tungsten powder has been avoided needle pattern or bimodal phenomenon, is good normal distribution, behind the high temperature sintering, makes the section crystallization of tungsten rod tiny and even.
4, by the tungsten strip that cooperates the compacting of powder scheme, when assurance is purified metals and is obtained the well processed tissue, formation mechanism according to the potassium bubble, the sintering current system heats up at a slow speed by beginning, three sections intensifications, two sections INSULATION DESIGN, to increase tungsten rod section number of die and to avoid the crystal grain part to grow up, reach that potassium abscess footpath is little, density is big, crystal boundary is many, potassium bubble row are long, purpose is evenly distributed, and be good dovetail bridging arrangement through the pressure processing gained wolfram filament for halogen tungsten lamp recrystallized structure of tungsten rod, length-width ratio 〉=12 of potassium bubble, the high temperature sink-resistance performance is good etc.
The specific embodiment
Embodiment one:
A kind of tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament may further comprise the steps:
1, in the bipyramid batch mixer, mixes 20min in the 3:1.5 ratio with spherical ammonium paratungstate with the monocline ammonium paratungstate;
2, prereduction, by four-tape warm area reduction furnace, reduction generates blue tungsten oxide with above-mentioned raw materials;
3, the high potassium of blue tungsten mixes, and the 200kg blue tungsten oxide is added in the doping machine, and by blue tungsten weight, wet method is mixed 0.18% potassium, 0.32% silicon and 0.012% aluminium, obtains the blue tungsten of high potassium after stirring, mixing, steam drying;
4, reduction, Fisher particle size are the fine grained tungsten powder of 2.0～2.6um and coarse granule tungsten powder that Fisher particle size is 3.4～4.0um explained hereafter routinely,
Fisher particle size is the middle particle tungsten powder manufacturing condition of 2.7～3.3um: once also the reason doped blue tungsten temperature for preparing tungsten dioxide is 530,550,580,620,650,670 ℃, and hydrogen flowing quantity is 2.2m
3/ h, dew point of hydrogen are-72 ℃, and boat charge is 302g, push away speed and are 25min.Output tungsten dioxide oxygen content is 13.2%, and the temperature of particle tungsten powder is 700,750,800,830,860,860 ℃ in the secondary reduction preparation, and hydrogen flowing quantity is 3.80m
3/ h, dew point of hydrogen are-70 ℃, and boat charge is 300g, push away speed and are 30min, and the output tungsten powder particle-size is 3.05um;
5, tungsten powder pickling, with thin, in, the coarse granule tungsten powder is adulterant and the impurity that surplus is removed in 5～6% hydrochloric acid, 5～6% hydrofluoric acid washes with concentration respectively;
6, thin, in, the coarse granule acid-washed tungsten powder fully mixes 30min by the weight ratio of 20:60:20 at " V " type batch mixer, cooperation powder potassium content is 0.0125%;
7, cooperate powder through cold isostatic compaction;
8, high temperature sintering, sintering current system (electric current/time) is pressed
(0-2000A)/5min+ (2000-3800A)/15min+3800A/15min+ (3800-4900A)/2min+4900A/20min carries out;
The potassium content of output tungsten rod is 0.0088%, density is 17.30g/cm
3, grain size is 6800/mm
2
Tungsten rod through swage processing and follow-up conventional crin, filament processing technology to the finished product wolfram filament for halogen tungsten lamp of Φ 0.20mm, its tensile strength 0.81N/mg, tolerance+0.5%, coiling performance T type, recrystallized structure is good dovetail bridging arrangement, length-width ratio is 26.
Embodiment two:
A kind of tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament may further comprise the steps:
1, in the bipyramid batch mixer, mixes 20min in the 3:1.2 ratio with spherical ammonium paratungstate with the monocline ammonium paratungstate;
2, prereduction, by four-tape warm area reduction furnace, reduction generates blue tungsten oxide with above-mentioned raw materials;
3, the high potassium of blue tungsten mixes, and the 200kg blue tungsten oxide is added in the doping machine, and by blue tungsten weight, wet method is mixed 0.2% potassium, 0.35% silicon and 0.013% aluminium, obtains the blue tungsten of high potassium after stirring, mixing, steam drying;
4, reduction, Fisher particle size are the fine grained tungsten powder of 2.0～2.6um and coarse granule tungsten powder that Fisher particle size is 3.4～4.0um explained hereafter routinely,
In particle tungsten powder manufacturing condition: once also the reason doped blue tungsten temperature for preparing tungsten dioxide is 530,550,580,620,650,670 ℃, and hydrogen flowing quantity is 2.6m
3/ h, dew point of hydrogen are-68 ℃, and boat charge is 322g, push away speed and are 25min.Output tungsten dioxide oxygen content is 12.8%, and the temperature of particle tungsten powder is 700,750,800,830,860,860 ℃ in the secondary reduction preparation, and hydrogen flowing quantity is 4.30m
3/ h, dew point of hydrogen are-63 ℃, and boat charge is 315g, push away speed and are 30min, and the output tungsten powder particle-size is 3.21um;
5, tungsten powder pickling, with thin, in, the coarse granule tungsten powder is adulterant and the impurity that surplus is removed in 5～6% hydrochloric acid, 5～6% hydrofluoric acid washes with concentration respectively;
6, thin, in, the coarse granule acid-washed tungsten powder fully mixes 30min by the weight ratio of 22:56:22 at " V " type batch mixer, cooperation powder potassium content is 0.0134%;
7, cooperate powder through cold isostatic compaction;
8, high temperature sintering, identical with embodiment one,
Output tungsten rod potassium content 0.0091%, density 〉=17.52g/cm
3, grain size 〉=6450/mm
2
Claims (1)
1. tungsten rod preparation method who is used to make the halogen tungsten lamp tungsten filament is characterized in that: may further comprise the steps:
(1), select materials, the monocline ammonium paratungstate mixes in the ratio of 3:1～1.5 with spherical ammonium paratungstate, is raw material with the mixture of gained;
(2), prereduction, adopt routine techniques with above-mentioned raw materials by four-tape warm area reduction furnace, it is 20～20.5% blue tungsten oxide that hydrogen reducing generates oxygen content;
(3), high potassium mixes, with common process the blue tungsten oxide wet method is mixed potassium silicate, aluminum nitrate solution, potassium, silicon, aluminium are adsorbed in the blue tungsten hole, and potassium, silicon, aluminium content are respectively 0.18～0.20%, 0.30～0.35%, 0.010～0.013% in the doped blue tungsten;
(4), reduction, doped blue tungsten is the fine grained tungsten powder of 2.0～2.6um with conventional reduction technology by secondary reduction generation Fisher particle size, standby; Doped blue tungsten is generated Fisher particle size with the direct once reduction of conventional reduction technology be the coarse granule tungsten powder of 3.4～4.0um, standby;
Adopting six warm area reduction furnaces that doped blue tungsten is generated Fisher particle size through secondary reduction is the middle particle tungsten powder of 2.7～3.3um, standby, in the process conditions of particle tungsten powder preparation be: once also the reason doped blue tungsten temperature for preparing tungsten dioxide is 530,550,580,620,650,670 ℃, and hydrogen flowing quantity is 2.0～3.0m
3/ h, dew point of hydrogen≤-60 ℃, boat charge is 300～350g, push away speed and be 25min, output tungsten dioxide oxygen content is 12～14%, and the process conditions of particle tungsten powder in the secondary reduction preparation: temperature is 700,750,800,830,860,860 ℃, and hydrogen flowing quantity is 3.0～5.0m
3/ h, dew point of hydrogen≤-60 ℃, boat charge is 280～320g, pushes away speed and is 30min;
(5), pickling, with thin, in, the coarse granule tungsten powder is adulterant and the impurity that surplus is removed in 5～6% hydrochloric acid, 5～6% hydrofluoric acid washes with concentration respectively;
(6), join powder, thin, in, the coarse granule acid-washed tungsten powder mixes 25～30min by the weight ratio of 20～25:60～50:20～25 in batch mixer;
(7), cold isostatic compaction, adopting routine techniques that 2000g is cooperated the tungsten powder diameter of packing into is in the elasticity die sleeve of 23 ± 0.2mm, use the cold isostatic press press forming, the maximal pressure pressing pressure is 150～160Mpa, be shaped the back tungsten strip under hydrogen shield, through 1300 ± 50 ℃ of presintering 40～45min;
(8), high temperature sintering; under hydrogen shield; tungsten strip directly energising heat-agglomerating in the incipient fusion machine after the presintering; sintering schedule is three sections intensifications, two sections insulations, and electric current/time parameter is (the 0-2000A)/5min that heats up, intensification (2000-3800A)/15min, insulation 3800A/15min, intensification (3800-4900A)/2min, insulation 4900A/20min.
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| CN103056357A (en) * | 2012-11-28 | 2013-04-24 | 厦门虹鹭钨钼工业有限公司 | Method for preparing 5N purity tungsten bar or tungsten wire |
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| CN111790915A (en) * | 2020-03-03 | 2020-10-20 | 威海多晶钨钼科技有限公司 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
| CN115074794A (en) * | 2022-05-13 | 2022-09-20 | 重庆材料研究院有限公司 | Preparation method of gold-plated tungsten wire for gas detector |
| CN116352100A (en) * | 2023-05-31 | 2023-06-30 | 赣州海盛钨业股份有限公司 | Production process of high-performance doped tungsten bar |
| CN119282127A (en) * | 2024-10-11 | 2025-01-10 | 青岛华钨新材料有限公司 | Potassium-doped tungsten rod for high-flexibility tungsten wire rope and its manufacturing method |
| CN119304197A (en) * | 2024-10-18 | 2025-01-14 | 青岛华钨新材料有限公司 | Nanocrystalline potassium-doped tungsten material and preparation method thereof |
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| 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 |
| CN103056357A (en) * | 2012-11-28 | 2013-04-24 | 厦门虹鹭钨钼工业有限公司 | Method for preparing 5N purity tungsten bar or tungsten wire |
| 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 |
| CN109014231A (en) * | 2018-08-15 | 2018-12-18 | 赣州虹飞钨钼材料有限公司 | A kind of preparation method of compound rare-earth tungsten powder |
| CN109014231B (en) * | 2018-08-15 | 2021-09-10 | 赣州虹飞钨钼材料有限公司 | Preparation method of composite rare earth tungsten powder |
| CN111790915A (en) * | 2020-03-03 | 2020-10-20 | 威海多晶钨钼科技有限公司 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
| CN111790915B (en) * | 2020-03-03 | 2021-09-24 | 威海多晶钨钼科技有限公司 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
| CN115074794A (en) * | 2022-05-13 | 2022-09-20 | 重庆材料研究院有限公司 | Preparation method of gold-plated tungsten wire for gas detector |
| CN116352100A (en) * | 2023-05-31 | 2023-06-30 | 赣州海盛钨业股份有限公司 | Production process of high-performance doped tungsten bar |
| CN116352100B (en) * | 2023-05-31 | 2023-07-28 | 赣州海盛钨业股份有限公司 | Production process of high-performance doped tungsten bar |
| CN119282127A (en) * | 2024-10-11 | 2025-01-10 | 青岛华钨新材料有限公司 | Potassium-doped tungsten rod for high-flexibility tungsten wire rope and its manufacturing method |
| CN119304197A (en) * | 2024-10-18 | 2025-01-14 | 青岛华钨新材料有限公司 | Nanocrystalline potassium-doped tungsten material and preparation method thereof |
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