CN103056357A - Method for preparing 5N purity tungsten bar or tungsten wire - Google Patents
Method for preparing 5N purity tungsten bar or tungsten wire Download PDFInfo
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- CN103056357A CN103056357A CN2012104971532A CN201210497153A CN103056357A CN 103056357 A CN103056357 A CN 103056357A CN 2012104971532 A CN2012104971532 A CN 2012104971532A CN 201210497153 A CN201210497153 A CN 201210497153A CN 103056357 A CN103056357 A CN 103056357A
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Abstract
The invention discloses a method for preparing a 5N purity tungsten bar or tungsten wire. The method includes the following steps that (1) tungsten powders with above 5N purity are filled in a soft mold to be subjected to isostatic cool pressing to obtain an isostatic cool pressing blank; and (2) the isostatic cool pressing blank obtained in the step (1) is subjected to bar or wire manufacturing to obtain the 5N purity tungsten bar or tungsten wire. The tungsten bar or tungsten wire prepared by the method has the advantages that the purity can reach to above 5N (99.999%), and the tungsten bar or tungsten wire can be used for producing an electrode of a long service life gas discharge lamp. The method is high in production efficiency, stable in product qualities and suitable for industrialized production.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to a kind of preparation method of tungsten bar or tungsten filament of 5N purity.
Background technology
Along with the technological progress of electric light source and the update of illuminating product, gas-discharge lamp has obtained using more and more widely.The electrode of gas-discharge lamp uses tungsten bar and tungsten filament to make mostly, these materials comprise thorium tungsten, Doped Tungsten, lanthanum tungsten, barium tungsten, Rare-Earth Tungsten, pure tungsten etc., wherein, the purity of Doped Tungsten and pure tungsten is higher, the content of tungsten can reach 99.95%(3N5 respectively) and 99.99%(4N), be merely able to reach 99%(2N and the content of tungsten is the highest in thorium tungsten, barium tungsten and the Rare-Earth Tungsten).The life-span of gas-discharge lamp electrode is depended on the height of the purity of tungsten in the electrode material, the higher then life-span of tungsten purity that is electrode is longer, and along with on the market to the more and more higher requirement of gas-discharge lamp life-span, above-mentioned material can't satisfy such demand because tungsten purity is not enough.
Summary of the invention
The object of the invention is to overcome the prior art defective, a kind of preparation method of tungsten bar or tungsten filament of 5N purity is provided.
Technical scheme of the present invention is as follows:
A kind of tungsten bar of 5N purity or the preparation method of tungsten filament comprise the steps:
(1) tungsten powder of purity more than 5N packed into carries out isostatic cool pressing in the soft mode, get the isostatic cool pressing base;
(2) with step (2) gained isostatic cool pressing base rod processed or throwing, get tungsten bar or the tungsten filament of 5N purity.
In a preferred embodiment of the invention, described step (1) is Ф 20～Ф 100mm for carrying out isostatic cool pressing to diameter in the soft mode that the tungsten powder of purity more than 5N packed under the pressure more than the 150MPa, gets the isostatic cool pressing base.
In a preferred embodiment of the invention, described step (2) comprises the steps:
A, step (1) gained isostatic cool pressing base is sintered to density at 17.5g/cm
3More than, get sintered blank;
B, with the sintered blank of step a forge to density at 19.0g/cm
3More than, must forge striking adobe;
C, with step b forge striking adobe cut and polish after namely get the tungsten bar of 5N purity.
In a preferred embodiment of the invention, described step a is: step (1) gained isostatic cool pressing base is sintered to density at 17.5g/cm in 1800 ~ 2100 ℃ under hydrogen atmosphere
3More than, get sintered blank.
In a preferred embodiment of the invention, described step b is: with the sintered blank of step a in 1500 ~ 1700 ℃ forge to density at 19.0g/cm
3More than, must forge striking adobe.
In a preferred embodiment of the invention, described step c is: with step b forge striking adobe cut with centreless mill after namely get the tungsten bar of 5N purity.
In a preferred embodiment of the invention, described step (1) is Ф 20～Ф 24mm for carrying out isostatic cool pressing to diameter in the soft mode that the tungsten powder of purity more than 5N packed under the pressure more than the 150MPa, gets the isostatic cool pressing base.
In a preferred embodiment of the invention, described step (2) comprises the steps:
A, step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density at 18.0g/cm
3More than, get the incipient fusion base;
B, with the incipient fusion base of step a revolve hammer and wire drawing to density at 19.1g/cm
3More than, diameter of phi 0.02mm～Φ 12mm, get the wire drawing base;
C, the wire drawing base of step b carried out namely getting after surface treatment and the annealing tungsten filament of 5N purity.
In a preferred embodiment of the invention, described step a is: step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density at 18.0g/cm in 2300 ~ 2600 ℃ under hydrogen atmosphere
3More than, get the incipient fusion base.
In a preferred embodiment of the invention, described step c is: the tungsten filament that the wire drawing base of step b is carried out namely getting after surface treatment and 1400 ~ 1600 ℃ of annealing 5N purity.
In a preferred embodiment of the invention, the oxygen content of the tungsten powder of described purity more than 5N is lower than 500ppm, and carbon content, nitrogen content, sulfur content, hydrogen content all are lower than 50ppm, and Fisher particle size is 1.5～5.0 μ m.
The invention has the beneficial effects as follows:
1, the purity of the tungsten bar silk material for preparing of method of the present invention is to 5N(99.999%) more than, can be used in the production of long-life gas discharge lamp electrode;
2, high, the constant product quality of method production efficiency of the present invention is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of the tungsten powder of purity used in the present invention more than 5N;
Fig. 2 is the metallograph of forging striking adobe of the tungsten bar of the prepared 5N purity of the embodiment of the invention 1;
Fig. 3 is the metallograph of the tungsten filament of the prepared 5N purity of the embodiment of the invention 2, and this tungsten filament is also annealed;
Fig. 4 is the metallograph after the tungsten filament annealing of the prepared 5N purity of the embodiment of the invention 2;
Fig. 5 is the metallograph of the tungsten filament of the prepared 5N purity of the embodiment of the invention 3, and this tungsten filament is also annealed;
Fig. 6 is the metallograph after the tungsten filament annealing of the prepared 5N purity of the embodiment of the invention 3;
The specific embodiment
Below by the specific embodiment in connection with accompanying drawing, technical scheme of the present invention is further detailed and describes.
The purity of used tungsten powder is more than 5N in following examples, and commercialization can be available from Honglu Tungsten Molybdenum Industry Co., Ltd., Shiamen.
The ultra micro mechanism of this tungsten powder as shown in Figure 1, its Fisher particle size is 2.4 μ m, its impurities analysis is as shown in the table:
Tungsten powder in following examples replaces with the tungsten powder with following characteristics, and all can reach identical technique effect: oxygen content is lower than 500ppm, and it is 1.5～5.0 μ m that carbon content, nitrogen content, sulfur content, hydrogen content all are lower than the 50ppm Fisher particle size.
Embodiment 1
Step (1): it is about Ф 56mm that the tungsten powder of purity more than 5N packed in the soft mode carrying out isostatic cool pressing to diameter under the 200MPa pressure, gets the isostatic cool pressing base;
Step (2):
A, step (1) gained isostatic cool pressing base is sintered to density at 17.5g/cm in 2100 ℃ under hydrogen atmosphere
3More than, get sintered blank;
B, the sintered blank of step a is forged to density 19.15g/cm with pneumatic hammer in 1600 ℃
3, diameter Ф 29mm, must forge striking adobe, its deflection is 64%, this forges the inside grain structure of striking adobe tiny evenly (as shown in Figure 2);
C, with step b forge that striking adobe cuts and the centreless mill after namely get the tungsten bar of 5N purity, inner grain structure is tiny, and evenly it is of a size of Ф 27 * 47mm, the impurities analysis of this tungsten bar sees the following form:
Embodiment 2
Step (1): the tungsten powder of purity more than 5N packed into, and to carry out isostatic cool pressing to diameter in the soft mode under the pressure of 200MPa be Ф 23mm, gets the isostatic cool pressing base.
Step (2):
A, step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density at 18.4g/cm in 2500 ℃ under hydrogen atmosphere
3About, diameter Ф 18mm, get the incipient fusion base;
B, with the incipient fusion base of step a revolve hammer and wire drawing to density at 19.18g/cm3, diameter of phi 1.1mm, get the wire drawing base, the impurities analysis of this wire drawing base sees the following form:
C, above-mentioned wire drawing base is carried out after centreless mill, alignment, the cutting getting the polishing tungsten filament of size Ф 1.0 * 1000mm, its inside is elongated bacillar structure (as shown in Figure 3); This polishing tungsten filament is namely got tungsten filament, its inner perfect recrystallization, uniform crystal particles and tiny (as shown in Figure 4) of 5N purity after 1600 ℃ of annealing.
Embodiment 3
Step (1): the tungsten powder of purity more than 5N packed into, and to carry out isostatic cool pressing to diameter in the soft mode under the pressure of 200MPa be Ф 23mm, gets the isostatic cool pressing base.
Step (2):
A, step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density at 18.4g/cm in 2500 ℃ under hydrogen atmosphere
3About, diameter Ф 18mm, get the incipient fusion base;
B, with the incipient fusion base of step a revolve hammer and wire drawing to density at 19.18g/cm
3, diameter of phi 0.265mm, get the wire drawing base, the impurities analysis of this wire drawing base sees the following form:
C, above-mentioned wire drawing base is carried out electrolytic cleaned, get the white tungsten filament of electrolytic cleaned of diameter of phi 0.25mm, its inside is elongated bacillar structure (as shown in Figure 5);
D, the tungsten filament, its inner perfect recrystallization, uniform crystal particles and tiny (as shown in Figure 6) that the white tungsten filament of above-mentioned electrolytic cleaned are namely got 5N purity after 1600 ℃ of annealing.
The above only is preferred embodiment of the present invention, so can not limit according to this scope of the invention process, the equivalence of namely doing according to claim of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (10)
1. the preparation method of the tungsten bar of a 5N purity or tungsten filament is characterized in that: comprise the steps:
(1) tungsten powder of purity more than 5N packed into carries out isostatic cool pressing in the soft mode, get the isostatic cool pressing base;
(2) with step (2) gained isostatic cool pressing base rod processed or throwing, get tungsten bar or the tungsten filament of 5N purity.
2. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 1 or tungsten filament, it is characterized in that: described step (1) is Ф 20～Ф 100mm for carrying out isostatic cool pressing to diameter in the soft mode that the tungsten powder of purity more than 5N packed under the pressure more than the 150MPa, gets the isostatic cool pressing base.
3. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 2 or tungsten filament, it is characterized in that: described step (2) comprises the steps:
A, step (1) gained isostatic cool pressing base is sintered to density at 17.5g/cm
3More than, get sintered blank;
B, with the sintered blank of step a forge to density at 19.0g/cm
3More than, must forge striking adobe;
C, with step b forge striking adobe cut and polish after namely get the tungsten bar of 5N purity.
3, the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 3 or tungsten filament is characterized in that: described step a is: step (1) gained isostatic cool pressing base is sintered to density at 17.5g/cm in 1800 ~ 2100 ℃ under hydrogen atmosphere
3More than, get sintered blank.
4. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 3 or tungsten filament, it is characterized in that: described step b is: with the sintered blank of step a in 1500 ~ 1700 ℃ forge to density at 19.0g/cm
3More than, must forge striking adobe.
5. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 3 or tungsten filament, it is characterized in that: described step c is: with step b forge striking adobe cut with the centreless mill after namely get the tungsten bar of 5N purity.
6. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 1 or tungsten filament, it is characterized in that: described step (1) is Ф 20～Ф 24mm for carrying out isostatic cool pressing to diameter in the soft mode that the tungsten powder of purity more than 5N packed under the pressure more than the 150MPa, gets the isostatic cool pressing base.
7. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 6 or tungsten filament, it is characterized in that: described step (2) comprises the steps:
A, step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density more than 18.0g/cm3, get the incipient fusion base;
B, with the incipient fusion base of step a revolve hammer and wire drawing to density at 19.1g/cm
3More than, diameter of phi 0.02mm～Φ 12mm, get the wire drawing base;
C, the wire drawing base of step b carried out namely getting after surface treatment and the annealing tungsten filament of 5N purity.
8. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 7 or tungsten filament, it is characterized in that: described step a is: step (1) gained isostatic cool pressing base is carried out incipient fusion and sinters to density at 18.0g/cm in 2300 ~ 2600 ℃ under hydrogen atmosphere
3More than, get the incipient fusion base.
9. the preparation method of the tungsten bar of a kind of 5N purity as claimed in claim 7 or tungsten filament, it is characterized in that: described step 2 is: the tungsten filament that the wire drawing base of step b is carried out namely getting after surface treatment and 1400 ~ 1600 ℃ of annealing 5N purity.
10. such as the tungsten bar of the described a kind of 5N purity of arbitrary claim or the preparation method of tungsten filament in the claim 1 to 9, it is characterized in that: the oxygen content of the tungsten powder of described purity more than 5N is lower than 500ppm, carbon content, nitrogen content, sulfur content, hydrogen content all are lower than 50ppm, and Fisher particle size is 1.5～5.0 μ m.
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| CN2012104971532A CN103056357A (en) | 2012-11-28 | 2012-11-28 | Method for preparing 5N purity tungsten bar or tungsten wire |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588531A (en) * | 2018-04-27 | 2018-09-28 | 厦门虹鹭钨钼工业有限公司 | A kind of anode material and preparation method thereof |
| CN111136264A (en) * | 2020-01-14 | 2020-05-12 | 西安瑞福莱钨钼有限公司 | Method for producing ultra-thick tungsten plate by upsetting tungsten rod |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6328927B1 (en) * | 1998-12-24 | 2001-12-11 | Praxair Technology, Inc. | Method of making high-density, high-purity tungsten sputter targets |
| CN101157997A (en) * | 2007-11-15 | 2008-04-09 | 赣州虹飞钨钼材料有限公司 | Preparation method of wolfram filament for halogen tungsten lamp |
| CN102198507A (en) * | 2011-05-16 | 2011-09-28 | 赣州虹飞钨钼材料有限公司 | Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament |
| CN102277558A (en) * | 2011-08-23 | 2011-12-14 | 洛阳科威钨钼有限公司 | Process for manufacturing tungsten spin-coated sputtering tube target |
-
2012
- 2012-11-28 CN CN2012104971532A patent/CN103056357A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6328927B1 (en) * | 1998-12-24 | 2001-12-11 | Praxair Technology, Inc. | Method of making high-density, high-purity tungsten sputter targets |
| CN101157997A (en) * | 2007-11-15 | 2008-04-09 | 赣州虹飞钨钼材料有限公司 | Preparation method of wolfram filament for halogen tungsten lamp |
| CN102198507A (en) * | 2011-05-16 | 2011-09-28 | 赣州虹飞钨钼材料有限公司 | Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament |
| CN102277558A (en) * | 2011-08-23 | 2011-12-14 | 洛阳科威钨钼有限公司 | Process for manufacturing tungsten spin-coated sputtering tube target |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588531A (en) * | 2018-04-27 | 2018-09-28 | 厦门虹鹭钨钼工业有限公司 | A kind of anode material and preparation method thereof |
| CN111136264A (en) * | 2020-01-14 | 2020-05-12 | 西安瑞福莱钨钼有限公司 | Method for producing ultra-thick tungsten plate by upsetting tungsten rod |
| CN111136264B (en) * | 2020-01-14 | 2022-03-15 | 西安瑞福莱钨钼有限公司 | Method for producing ultra-thick tungsten plate by upsetting tungsten rod |
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Application publication date: 20130424 |