CN106906396A - A kind of uniform fine grain Tungsten Bar and preparation method thereof - Google Patents
A kind of uniform fine grain Tungsten Bar and preparation method thereof Download PDFInfo
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- CN106906396A CN106906396A CN201710126549.9A CN201710126549A CN106906396A CN 106906396 A CN106906396 A CN 106906396A CN 201710126549 A CN201710126549 A CN 201710126549A CN 106906396 A CN106906396 A CN 106906396A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
Abstract
The present invention relates to tungsten alloy field, specifically a kind of uniform fine grain Tungsten Bar and preparation method thereof.Described uniform fine grain Tungsten Bar, potassium content is 40~80ppm, rhenium content is 0.01%~0.35wt%, and remaining is tungsten, and 1~50mm of diameter, crystal grain are less than 10um, center portion and edge density more than 19.2g/cm3.The preparation method includes successively：The preparation of doped blue tungsten, the preparation of doped tungsten powder, base, sintering, hot rolling.Compared with prior art, composition contains trace elements K to the present invention, and adds a small amount of rhenium element, and the uniform fine grain Tungsten Bar of preparation has superior high-temperature behavior, it is adaptable to the demand of high-end thermal field heater；Using Median frequency sintering technique and the structural homogenity and high-temperature creep resistance of hot rolling technology lifting Tungsten Bar.
Description
Technical field
The present invention relates to field of powder metallurgy, the superior uniform fine grain of specifically a kind of fine grain stabilization, high-temperature behavior
Tungsten Bar and preparation method thereof.
Background technology
Uniform fine grain Tungsten Bar refers to possess that even tissue, crystal grain are tiny, recrystallization temperature is high, high temperature creep property is superior
The features such as tungsten alloy material, be mainly used in the fields such as semiconductor preparation, superhigh temperature equipment, special source, military project.Tungsten Bar
To make the core material including the high temperature thermal field including sapphire crystallization furnace heater, this type high temp temperature of thermal field 1800~
Between 2500 DEG C, and long-time heat preservation is needed, this requires that heating element of tungsten possesses superior Properties of High Temperature Creep and long-time
Stability.
But, during being used as high temperature thermal field heater using traditional Tungsten Bar, because temperature of thermal field is higher than tungsten
The recrystallization temperature (about 2000 DEG C) of bar, tungsten grain coarsening rate is fast, and causing the fragility of tungsten material increases, the use longevity of thermal field
Life is extremely restricted.How tungsten grain even tissue refinement, recrystallization temperature high, Properties of High Temperature Creep good tungsten bar are prepared
Material turns into the key of the high-end thermal field of production.
Chinese patent ZL201210319024.4 discloses a kind of incipient fusion sintering method of tungsten-rhenium alloy, such as in its specification
Announce, tungsten base carries out direct-electrifying sintering after pre-sintering, and the method needs to be clamped in each material in two end electrodes, it is raw
Produce efficiency low；And on the other hand study and show, by the way of Median frequency sintering tungsten alloy, material passes through sensing heating in thermal field
Sintering, by temperature control stage by stage, is more uniformly distributed Tungsten Bar crystal grain, and high-temperature behavior is more preferable.
The content of the invention
It is an object of the present invention to provide a kind of uniform fine grain Tungsten Bar, uneven to solve conventional Tungsten Bar grain structure
The problem that even, recrystallization temperature is low, Properties of High Temperature Creep is poor, while there is provided the preparation method of the uniform fine grain Tungsten Bar.
To solve above technical problem, the technical solution adopted by the present invention is as follows：
Uniform fine grain Tungsten Bar of the present invention, is made up of following component：0.01~0.35wt% of rhenium, potassium 0.0040~
0.0080wt%, remaining is tungsten.
Preferably, described uniform fine grain Tungsten Bar, a diameter of 1~50mm, crystallite dimension are less than 10um, center portion and edge
Density is more than 19.2g/cm3。
The preparation method of uniform fine grain Tungsten Bar of the present invention,
Step includes successively：The preparation of doped blue tungsten, the preparation of doped tungsten powder, base, sintering, hot rolling.
Preferably, the preparation of the doped blue tungsten is concretely comprised the following steps：
Using ammonium paratungstate in H2, reduce at 400-600 DEG C and obtain blue tungsten powder WO2.9, then by blue tungsten powder and rehenic acid ammonium,
Potassium silicate, potassium hydroxide, aluminum nitrate aqueous solution carry out solid-liquid doping, dry 8 hours, prepare doped blue tungsten.
Preferably, the rehenic acid ammonium, potassium silicate, potassium hydroxide, the concentration range of aluminum nitrate aqueous solution be respectively 20~
50g/L, 100~200g/L, 50~100g/L, 10~30g/L.
Wherein, blue tungsten powder and rehenic acid ammonium, potassium silicate, potassium hydroxide, aluminum nitrate consumption can according to component composition requirement and
Rehenic acid ammonium, potassium silicate, potassium hydroxide, aluminum nitrate aqueous solution concentration are calculated.
Preferably, the preparation of the doped tungsten powder is concretely comprised the following steps：
Four sections of temperature-control reductions of the doped blue tungsten, four sections of temperature are respectively 670 DEG C, 720 DEG C, 770 DEG C and 820 DEG C, often
Section soaking time is 60-80min, boat charge 300g, and reducing atmosphere is hydrogen, and hydrogen flowing quantity is 15~30m3/ h, must adulterate
Tungsten powder.
Preferably, the doped tungsten powder granularity is 1.3-1.8um.
Preferably, the base is concretely comprised the following steps：
By the doped tungsten powder through pickling, drying and processing, doped tungsten powder is suppressed using isostatic cool pressing method, unit
Pressure 150-200MPa, is made pressed compact, 1.5~15kg of substance.
Preferably, the sintering is concretely comprised the following steps：
By the pressed compact pre-sintered 20 minutes in 1200~1300 DEG C of hydrogen pre-burning stoves, it is set tentatively to possess certain strong
Degree, then carries out high temperature sintering, 0.5~200m of hydrogen flowing quantity in intermediate frequency furnace3/ h, obtains sintered blank, sintered blank diameter
16~65mm, density is 17.0-18.5g/cm3, sintering temperature is 1900~2500 DEG C.
Preferably, the hot rolling is concretely comprised the following steps：
The sintered blank is heated to be swaged after 1200~1500 DEG C to 17mm, then through 10 passage continuous rollings, is obtained
The uniform fine grain Tungsten Bar of a diameter of 1~50mm, rolling temperature is 1500~2000 DEG C, and mill speed is 1~2.5m/s.
Compared with prior art, the invention has the advantages that：
1) composition contains trace elements K, and adds a small amount of rhenium element, and the uniform fine grain Tungsten Bar of preparation has superior
High-temperature behavior, it is adaptable to the demand of high-end thermal field heater；
2) using Median frequency sintering technique and the structural homogenity and high-temperature creep resistance of hot rolling technology lifting Tungsten Bar.
Brief description of the drawings
Accompanying drawing 1 is the bar center portion metallograph of a diameter of 40mm in the present invention.
Accompanying drawing 2 is the bar edge metallograph of a diameter of 40mm in the present invention.
Accompanying drawing 3 is the bar edge metallograph of a diameter of 40mm in the present invention.
Accompanying drawing 4 is the bar edge metallograph of a diameter of 10mm in the present invention.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
The preparation method of tungsten alloy bar of the present invention, step is followed successively by：
(1) preparation of doped blue tungsten
Using ammonium paratungstate in H2, reduce at 400 DEG C and obtain blue tungsten powder WO2.9, then by blue tungsten powder and rehenic acid ammonium, silicic acid
Potassium, potassium hydroxide, aluminum nitrate aqueous solution carry out solid-liquid doping, rhenium in rehenic acid ammonium, potassium silicate, potassium hydroxide, aluminum nitrate aqueous solution
The concentration of sour ammonium is 20g/L, the concentration of potassium silicate is 100g/L, the concentration of potassium hydroxide is 50g/L, the concentration of aluminum nitrate is
10g/L, dries 8 hours, prepares doped blue tungsten, and the requirement according to component composition and solution concentration can calculate rehenic acid ammonium, silicic acid
The consumption of potassium, potassium hydroxide.
(2) preparation of doped tungsten powder
Doped blue tungsten obtained in step (1) is reduced using the technique of four sections of temperature controls, four sections of temperature are respectively 670
DEG C, 720 DEG C, 770 DEG C and 820 DEG C, every section of soaking time is 60min, boat charge 300g, and reducing atmosphere is hydrogen, hydrogen stream
It is 15m to measure3/ h, is obtained doped tungsten powder, and the doped tungsten powder granularity is 1.3~1.8um after testing.
(3) base
Doped tungsten powder obtained in step (2), through pickling, drying and processing, is carried out doped tungsten powder using isostatic cool pressing method
Compacting, unit pressure 150MPa is made pressed compact, substance 1.5kg.
(4) sinter
Pressed compact obtained in step (3) is pre-sintered 20 minutes in 1200 DEG C of hydrogen pre-burning stoves, it is tentatively possessed necessarily
Intensity, high temperature sintering, hydrogen flowing quantity 0.5m are then carried out in intermediate frequency furnace3/ h, obtains sintered blank, sintered blank diameter
16mm, density is 17.0-18.5g/cm3, sintering temperature is 1900 DEG C.
(5) hot rolling
Just sintered blank obtained in step (3) is swaged to 17mm after being heated to 1200 DEG C, then through 10 passage continuous rollings,
Uniform fine grain Tungsten Bar is obtained, rolling temperature is 1500 DEG C, and mill speed is 1m/s.
Embodiment 2
The preparation method of tungsten alloy bar of the present invention, step is followed successively by：
(1) preparation of doped blue tungsten
Using ammonium paratungstate in H2, reduce at 600 DEG C and obtain blue tungsten powder WO2.9, then by blue tungsten powder and rehenic acid ammonium, silicic acid
Potassium, potassium hydroxide, aluminum nitrate aqueous solution carry out solid-liquid doping, rhenium in rehenic acid ammonium, potassium silicate, potassium hydroxide, aluminum nitrate aqueous solution
The concentration of sour ammonium is 50g/L, the concentration of potassium silicate is 200g/L, the concentration of potassium hydroxide is 100g/L, the concentration of aluminum nitrate is
30g/L, dries 8 hours, prepares doped blue tungsten, and the requirement according to component composition and solution concentration can calculate rehenic acid ammonium, silicic acid
The consumption of potassium, potassium hydroxide.
(2) preparation of doped tungsten powder
Doped blue tungsten obtained in step (1) is reduced using the technique of four sections of temperature controls, four sections of temperature are respectively 670
DEG C, 720 DEG C, 770 DEG C and 820 DEG C, every section of soaking time is 80min, boat charge 300g, and reducing atmosphere is hydrogen, hydrogen stream
It is 30m to measure3/ h, is obtained doped tungsten powder, and the doped tungsten powder granularity is 1.3~1.8um after testing.
(3) base
Doped tungsten powder obtained in step (2), through pickling, drying and processing, is carried out doped tungsten powder using isostatic cool pressing method
Compacting, unit pressure 200MPa is made pressed compact, and tungsten base substance is in 15kg.
(4) sinter
Pressed compact obtained in step (3) is pre-sintered 20 minutes in 1300 DEG C of hydrogen pre-burning stoves, it is tentatively possessed necessarily
Intensity, high temperature sintering, hydrogen flowing quantity 200m are then carried out in intermediate frequency furnace3/ h, obtains sintered blank, sintered blank diameter
65mm, density is 17.0-18.5g/cm3, sintering temperature is 2500 DEG C.
(5) hot rolling
Just sintered blank obtained in step (4) is swaged to 17mm after being heated to 1500 DEG C, then through 10 passage continuous rollings,
Uniform fine grain Tungsten Bar is obtained, rolling temperature is 1500 DEG C, and mill speed is 2.5m/s.
Tungsten Bar such as Fig. 1~4 prepared by the method for embodiment 1 and embodiment 2, group is grouped into：Rhenium 0.01~
0.35wt%, potassium, 0.0040~0.0080wt%, remaining is tungsten, a diameter of 1~50mm, crystallite dimension less than 10um, center portion and
Edge density is more than 19.2g/cm3。
Claims (10)
1. a kind of uniform fine grain Tungsten Bar, it is characterised in that be made up of following component：0.01~0.35wt% of rhenium, potassium 0.0040
~0.0080wt%, remaining is tungsten.
2. uniform fine grain Tungsten Bar according to claim 1, it is characterised in that a diameter of 1~50mm, crystallite dimension are less than
10um, center portion and edge density are more than 19.2g/cm3。
3. a kind of preparation method of uniform fine grain Tungsten Bar according to claim 1, it is characterised in that
Step includes successively：The preparation of doped blue tungsten, the preparation of doped tungsten powder, base, sintering, hot rolling.
4. the preparation method of uniform fine grain Tungsten Bar according to claim 3, it is characterised in that
The preparation of the doped blue tungsten is concretely comprised the following steps：
Using ammonium paratungstate in H2, reduce at 400-600 DEG C and obtain blue tungsten powder WO2.9, then by blue tungsten powder and rehenic acid ammonium, silicic acid
Potassium, potassium hydroxide, aluminum nitrate aqueous solution carry out solid-liquid doping, dry 8 hours, prepare doped blue tungsten.
5. the preparation method of uniform fine grain Tungsten Bar according to claim 4, it is characterised in that
The rehenic acid ammonium, potassium silicate, potassium hydroxide, the concentration range of aluminum nitrate aqueous solution be respectively 20~50g/L, 100~
200g/L, 50~100g/L, 10~30g/L.
6. the preparation method of uniform fine grain Tungsten Bar according to claim 4, it is characterised in that
The preparation of the doped tungsten powder is concretely comprised the following steps：
Four sections of temperature-control reductions of the doped blue tungsten, four sections of temperature are respectively 670 DEG C, 720 DEG C, 770 DEG C and 820 DEG C, every section of guarantor
The warm time is 60~80min, boat charge 300g, and reducing atmosphere is hydrogen, and hydrogen flowing quantity is 15~30m3/ h, obtains Doped Tungsten
Powder.
7. the preparation method of uniform fine grain Tungsten Bar according to claim 6, it is characterised in that
The doped tungsten powder granularity is 1.3~1.8um.
8. the preparation method of uniform fine grain Tungsten Bar according to claim 7, it is characterised in that
The base is concretely comprised the following steps：
By the doped tungsten powder through pickling, drying and processing, doped tungsten powder is suppressed using isostatic cool pressing method, unit pressure
150~200MPa, is made pressed compact, 1.5~15kg of substance.
9. the preparation method of uniform fine grain Tungsten Bar according to claim 8, it is characterised in that
The sintering is concretely comprised the following steps：
The pressed compact is pre-sintered 20 minutes in 1200~1300 DEG C of hydrogen pre-burning stoves, it is tentatively possessed certain intensity,
Then high temperature sintering, 0.5~200m of hydrogen flowing quantity are carried out in intermediate frequency furnace3/ h, acquisition sintered blank, sintered blank diameter 16~
65mm, density is 17.0-18.5g/cm3, sintering temperature is 1900~2500 DEG C.
10. the preparation method of uniform fine grain Tungsten Bar according to claim 9, it is characterised in that
The hot rolling is concretely comprised the following steps：
The sintered blank is heated to be swaged after 1200~1500 DEG C to 17mm, then through 10 passage continuous rollings, diameter is obtained
It is the uniform fine grain Tungsten Bar of 1~50mm, rolling temperature is 1500~2000 DEG C, and mill speed is 1~2.5m/s.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109306420A (en) * | 2017-11-09 | 2019-02-05 | 安泰天龙钨钼科技有限公司 | A kind of High Performance W alloy bar material and preparation method thereof |
| CN110000387A (en) * | 2019-05-20 | 2019-07-12 | 安泰天龙钨钼科技有限公司 | A kind of big specification fine grain tungsten bar and its two rolling preparation methods |
| CN111041317A (en) * | 2019-12-19 | 2020-04-21 | 厦门钨业股份有限公司 | Micro-nano composite reinforced tungsten alloy material and preparation method thereof |
| 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 |
| CN113186439A (en) * | 2021-01-20 | 2021-07-30 | 厦门虹鹭钨钼工业有限公司 | Alloy wire and preparation method and application thereof |
| CN114774749A (en) * | 2022-04-26 | 2022-07-22 | 上海超淼争锋生物科技有限公司 | High-toughness tungsten-based alloy, preparation process and application thereof |
| CN116770148A (en) * | 2023-06-20 | 2023-09-19 | 西华大学 | Block tungsten alloy with high thermal conductivity and low-temperature toughness and preparation method thereof |
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| CN109306420A (en) * | 2017-11-09 | 2019-02-05 | 安泰天龙钨钼科技有限公司 | A kind of High Performance W alloy bar material and preparation method thereof |
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| CN110000387A (en) * | 2019-05-20 | 2019-07-12 | 安泰天龙钨钼科技有限公司 | A kind of big specification fine grain tungsten bar and its two rolling preparation methods |
| CN110000387B (en) * | 2019-05-20 | 2021-06-01 | 安泰天龙钨钼科技有限公司 | Large-size fine-grain tungsten rod and two-roller rolling preparation method thereof |
| CN111041317A (en) * | 2019-12-19 | 2020-04-21 | 厦门钨业股份有限公司 | Micro-nano composite reinforced tungsten alloy material and preparation method thereof |
| 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 |
| CN113186439A (en) * | 2021-01-20 | 2021-07-30 | 厦门虹鹭钨钼工业有限公司 | Alloy wire and preparation method and application thereof |
| CN114774749A (en) * | 2022-04-26 | 2022-07-22 | 上海超淼争锋生物科技有限公司 | High-toughness tungsten-based alloy, preparation process and application thereof |
| CN116770148A (en) * | 2023-06-20 | 2023-09-19 | 西华大学 | Block tungsten alloy with high thermal conductivity and low-temperature toughness and preparation method thereof |
| CN116770148B (en) * | 2023-06-20 | 2024-03-08 | 西华大学 | Block tungsten alloy with high thermal conductivity and low-temperature toughness and preparation method thereof |
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Application publication date: 20170630 |