CN106756158B - Tantalum-tungsten alloy blank preparation method - Google Patents
Tantalum-tungsten alloy blank preparation method Download PDFInfo
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- CN106756158B CN106756158B CN201611219592.1A CN201611219592A CN106756158B CN 106756158 B CN106756158 B CN 106756158B CN 201611219592 A CN201611219592 A CN 201611219592A CN 106756158 B CN106756158 B CN 106756158B
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- 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
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- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- 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
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- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A kind of tantalum-tungsten alloy blank preparation method, it is characterised in that include the following steps：1. powder mixes；2. mixed powder is carried out briquet compacting by green compact on moulding press, pressing pressure is 300MPa~400MPa, obtains briquet；3. blank is broken, briquet is put into the ball grinder of high energy ball mill and is crushed, obtain green compact particle, green compact particle size is 0.1mm~0.3mm；4. electric arc melting.Compared with the prior art, the advantages of the present invention are as follows：Whole preparation process flow is few, and preparation efficiency is high, requires tantalum-tungsten alloy batch components that are relatively low and preparing uniform preparation.
Description
Technical field
The present invention relates to a kind of preparation method of metal alloy more particularly to the preparation methods of tantalum-tungsten alloy.
Background technology
Tantalum-tungsten alloy is one kind using tantalum as matrix, adds the alloy that a certain amount of wolfram element is formed.Although both tantalum and tungsten can
It is infinitely dissolved, but work as the plasticity that W content is more than 12at%-14at% alloys to significantly reduce, when W content is relatively low, tantalum tungsten
Alloy had not only maintained the cold plasticity of pure tantalum, but also with higher intensity, anti-oxidant and anti-corrosion capability, therefore relatively low W content
Tantalum-tungsten alloy is widely used in the fields such as Aeronautics and Astronautics, chemical industry, nuclear industry.As Ta-2.5W alloys can be used for manufacture heater,
Cooling coil, heat exchanger and reactor etc.；Ta-7.5W alloys can manufacture anti-corrosion element；Ta-10W can be used as rocket engine
The high-temperature components such as thrust chamber and vacuum high temperature furnace heater.
Currently, the preparation of tantalum-tungsten alloy blank usually requires several processes such as experience batch mixing, green compact, sintering, melting, such as specially
Profit number is the Chinese invention patent of ZL201310579245.X《A kind of preparation method of 2.5 tungsten alloy of tantalum》(Authorization Notice No. is
CN103555975B), tantalum powder and tungsten powder are configured and are put into drum mixer first and mixed for 24 hours by this method in proportion；It will
The powder mixed crosses 120 mesh and sieves to obtain fine powder material；Fine powder material is pressed into rod with 500T hydraulic presses；Alloy rod is put into very
Sintering obtains crude green body ingot in empty sintering furnace；Tantalum-tungsten alloy billet is made through vacuum electron beam melting at least twice in crude green body ingot.Class
As can with application reference number be 201310574775.5 Chinese invention patent application disclose《The preparation side of 10 tungsten alloy of tantalum
Method》(application publication number CN103555981A).
《Material heat treatment journal》Wang Shan, Wang Mingpiao, Chen Chang, Xia Fuzhong, Zuo Bo in 6th phase 2012 open the " tantalum of gentle equal works
And the tissue during tantalum-tungsten alloy cold-rolling deformation and performance " the disclosed method prepared is slightly different with more than, first symmetrically
Measured powder carries out planet high-energy ball milling and sieves to obtain uniformly mixed mixed raw material powder, using isostatic pressed by mixed powder
Compression moulding obtains tantalum-tungsten alloy blank after sintering.
The Chinese invention patent of Patent No. ZL201410118867.7《The preparation method of button blank or aluminum alloy blank》
(Authorization Notice No. CN 103849788B), in the patent by tantalum powder or the compression moulding of tantalum alloy powder and in vacuum sintering furnace into
Row is pre-sintered, then is carried out vacuum vertical sintering and obtain tantalum or tantalum alloy blank, since the process employs vacuum sinterings to burn
Knot technology, obtained blank performance consistency are preferable.
From the above tantalum-tungsten alloy blank preparation method it is found that due to the use of plurality of devices involved in preparation process and multiple
Technique causes the production cycle longer.
Invention content
The technical problem to be solved by the present invention is to provide that a kind of flow is short for the above-mentioned state of the art and blank at
Divide uniform tantalum-tungsten alloy blank preparation method.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of tantalum-tungsten alloy blank preparation method,
It is characterized in that including the following steps：
1. powder mix, the tungsten powder that the tantalum powder and average particle size for being 3 μm~5 μm using average particle size are 3 μm as raw material and by
Required ratio mixes after being weighed, and mixed powder is positioned in the ball grinder of high energy ball mill and is uniformly mixed, is mixed
Powder；
2. mixed powder is carried out briquet compacting by green compact on moulding press, pressing pressure is 300MPa~400MPa, is obtained
Briquet；
3. blank is broken, briquet is put into the ball grinder of high energy ball mill and is crushed, obtain green compact particle, green compact
Particle size is 0.1mm~0.3mm；
4. green compact particle is put into arc-melting furnace crucible and closes fire door, is evacuated to pressure in the burner hearth by electric arc melting
It vacuumizes, is vacuumized after being filled with high-purity argon gas to 0.05MPa, the above vacuum step is in triplicate less than stopping after 0.003Pa
Melting is carried out afterwards obtains tantalum-tungsten alloy blank.
Preferably, 1. the described ball milling condition is as follows for step：Ball-milling medium is self-control diameter 6mm tantalum balls, the tantalum being put into
Ball quality is 1 with powder quality ratio:3~1:4, high energy ball mill rotating speed is 400r/min~600r/min, turns to adjustment time
5min~10min, Ball-milling Time are 60min~120min.
Preferably, step 2. described in green compact may be used and bi-directionally or uni-directionally suppress.
Preferably, step 3. described in ball milling condition it is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, is put into
Tantalum ball quality is 1 with powder quality ratio:3~1:4, high energy ball mill rotating speed is 50r/min~60r/min, turns to adjustment time
2min~3min, Ball-milling Time are 10min~20min.
Preferably, step 4. described in electric arc melting condition it is as follows：Melting electric current 400A~500A, smelting time
3min~5min, melting number 3~4 times overturn sample after primary per melting.
Compared with the prior art, the advantages of the present invention are as follows：Whole preparation process flow is few, and preparation efficiency is high, at low cost,
Require tantalum-tungsten alloy batch components that are relatively low and preparing uniform preparation.
Specific implementation mode
Present invention is further described in detail with reference to embodiments.
Embodiment 1, the tungsten powder that the tantalum powder and average particle size for being 3 μm -5 μm using average particle size are 3 μm is raw material, by Ta-
2.5W alloying components carry out tantalum powder respectively and tungsten powder weighs, and two kinds of powders are mixed to be positioned in the ball grinder of high energy ball mill and are mixed
It closes uniformly, ball-milling technology is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, and the tantalum ball quality being put into is 1 with powder quality ratio:
3, high energy ball mill rotating speed is 400r/min, turns to adjustment time 5min, Ball-milling Time 120min；Using automatically automatically at
Swaging machine by uniformly mixed pressed by powder at briquet, using two-way compacting, pressing pressure 300MPa；The briquet that will be obtained again
It is put into the ball grinder of high energy ball mill and is crushed to obtain green compact particle, ball-milling technology is as follows：Ball-milling medium is self-control diameter
6mm tantalum balls, the tantalum ball quality being put into are 1 with powder quality ratio:3, high energy ball mill rotating speed is 50r/min, turns to adjustment time
2min, Ball-milling Time 20min obtain the green compact particle that size is 0.3mm；Load weighted green compact particle is put into electric arc melting
Fire door is closed in stove crucible, open mechanical pump and molecular pump be evacuated to pressure in the burner hearth less than stop after 0.003Pa mechanical pump and
Molecular pump vacuumizes after being filled with high-purity argon gas to 0.05MPa, and the above vacuum step carries out electric arc melting afterwards in triplicate, melts
Sweetening process is as follows：Melting electric current 400A, smelting time 5min, melting number 4 times (overturning sample after primary per melting), finally
The uniform Ta-2.5W alloy blanks of ingredient are obtained, test result is as follows for alloying component：
Each region W content of alloy billet that 1 embodiment 1 of table obtains
Embodiment 2, the tungsten powder that the tantalum powder and average particle size for being 3 μm -5 μm using average particle size are 3 μm is raw material, by Ta-
2.5W alloying components carry out tantalum powder respectively and tungsten powder weighs, and two kinds of powders are mixed to be positioned in the ball grinder of high energy ball mill and are mixed
It closes uniformly, ball-milling technology is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, and the tantalum ball quality being put into is 1 with powder quality ratio:
4, high energy ball mill rotating speed is 600r/min, turns to adjustment time 10min, Ball-milling Time 60min；Using automatically automatically at
Swaging machine at briquet, suppresses uniformly mixed pressed by powder, pressing pressure 500MPa using unidirectional；The briquet that will be obtained again
It is put into the ball grinder of high energy ball mill and is crushed to obtain green compact particle, ball-milling technology is as follows：Ball-milling medium is self-control diameter
6mm tantalum balls, the tantalum ball quality being put into are 1 with powder quality ratio:3, high energy ball mill rotating speed is 60r/min, turns to adjustment time
3min, Ball-milling Time 15min obtain the green compact particle that size is 0.25mm；Load weighted green compact particle is put into electric arc to melt
Fire door is closed in furnace crucible, opens mechanical pump and molecular pump is evacuated to after pressure in the burner hearth is less than 0.003Pa and stops mechanical pump
And molecular pump, it being vacuumized after being filled with high-purity argon gas to 0.05MPa, the above vacuum step carries out electric arc melting afterwards in triplicate,
Smelting technology is as follows：Melting electric current 500A, smelting time 3min, melting number 3 times (overturning sample after primary per melting), most
After obtain the uniform Ta-2.5W alloy blanks of ingredient, test result is as follows for alloying component：
Each region W content of alloy billet that 2 embodiment 2 of table obtains
Embodiment 3
The tungsten powder that the tantalum powder and average particle size for being 3 μm -5 μm using average particle size are 3 μm is raw material, by Ta-10W alloying components
Tantalum powder is carried out respectively and tungsten powder weighs, and two kinds of powders are mixed and are positioned over uniformly mixed in the ball grinder of high energy ball mill, ball milling
Technique is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, and the tantalum ball quality being put into is 1 with powder quality ratio:4, high energy ball mill
Rotating speed is 500r/min, turns to adjustment time 8min, Ball-milling Time 100min；It will be mixed using full-automatic automatic forming press
Uniform pressed by powder is at briquet, using two-way compacting, pressing pressure 450MPa；Obtained briquet is put into high-energy ball milling again
It is crushed to obtain green compact particle in the ball grinder of machine, ball-milling technology is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, is put into
Tantalum ball quality and powder quality ratio be 1:3, high energy ball mill rotating speed is 60r/min, turns to adjustment time 3min, Ball-milling Time
For 15min, the green compact particle that size is 0.20mm is obtained；Load weighted green compact particle is put into arc-melting furnace crucible and is closed
Fire door, opens mechanical pump and molecular pump is evacuated to pressure in the burner hearth less than mechanical pump and molecular pump is stopped after 0.003Pa, is filled with height
It is vacuumized after pure argon to 0.05MPa, the above vacuum step carries out electric arc melting afterwards in triplicate, and smelting technology is as follows：It is molten
Electric current 500A, smelting time 5min are refined, and it is uniform to finally obtain ingredient for melting number 4 times (sample being overturn after primary per melting)
Ta-10W alloy blanks, test result is as follows for alloying component：
Each region W content of alloy billet that 3 embodiment 3 of table obtains
Claims (2)
1. a kind of tantalum-tungsten alloy blank preparation method, it is characterised in that include the following steps：
1. powder mixes, the tungsten powder that the tantalum powder and average particle size for being 3 μm~5 μm using average particle size are 3 μm is as raw material and by required
Ratio mixes after being weighed, and mixed powder is positioned in the ball grinder of high energy ball mill and is uniformly mixed, obtains mixed powder；
2. mixed powder is carried out briquet compacting by green compact on moulding press, pressing pressure is 300MPa~400MPa, obtains base
Block；
3. blank is broken, briquet is put into the ball grinder of high energy ball mill and is crushed, obtain green compact particle, green compact particle ruler
Very little is 0.1mm~0.3mm；
4. green compact particle is put into arc-melting furnace crucible and closes fire door by electric arc melting, it is evacuated to pressure in the burner hearth and is less than
Stop vacuumizing after 0.003Pa, be vacuumized after being filled with high-purity argon gas to 0.05MPa, the above vacuum step is laggard in triplicate
Row melting obtains tantalum-tungsten alloy blank；
1. the described ball milling condition is as follows for step：Ball-milling medium is self-control diameter 6mm tantalum balls, the tantalum ball quality being put into and powder matter
Amount is than being 1:3~1:4, high energy ball mill rotating speed is 400r/min~600r/min, turns to adjustment time 5min~10min, ball
Time consuming is 60min~120min；
Step 3. described in ball milling condition it is as follows：Ball-milling medium is self-control diameter 6mm tantalum balls, the tantalum ball quality and powder being put into
Mass ratio is 1:3~1:4, high energy ball mill rotating speed is 50r/min~60r/min, turns to adjustment time 2min~3min, ball milling
Time is 10min~20min；
Step 4. described in electric arc melting condition it is as follows：Melting electric current 400A~500A, smelting time 3min~5min, melting
Number 3~4 times overturns sample after primary per melting.
2. tantalum-tungsten alloy blank preparation method according to claim 1, it is characterised in that step 2. described in green compact adopt
With bi-directionally or uni-directionally suppressing.
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| CN108436074B (en) * | 2018-04-17 | 2019-10-01 | 中南大学 | Tantalum-tungsten alloy foil preparation method and tantalum-tungsten alloy foil |
| CN111763838A (en) * | 2020-07-09 | 2020-10-13 | 宝鸡恒业有色金属科技有限公司 | Preparation process of tantalum-tungsten alloy wire |
| CN111763839A (en) * | 2020-07-09 | 2020-10-13 | 宝鸡恒业有色金属科技有限公司 | Tantalum-tungsten alloy plate machining and forming process capable of improving yield |
| CN113088718B (en) * | 2021-03-31 | 2022-08-12 | 中南大学 | Short-process non-consumable arc melting preparation method of high-density high-melting-point tungsten alloy |
| CN113484181B (en) * | 2021-06-18 | 2024-04-02 | 安徽工业大学 | Method for detecting setting forming capability of trapped refractory blank |
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| US5918104A (en) * | 1997-12-24 | 1999-06-29 | H.C. Starck, Inc. | Production of tantalum-tungsten alloys production by powder metallurgy |
| CN1560300A (en) * | 2004-03-09 | 2005-01-05 | 株洲硬质合金集团有限公司 | Preparation method of Taw Yalloy bar |
| CN103555981A (en) * | 2013-11-15 | 2014-02-05 | 宝鸡市众邦稀有金属材料有限公司 | Preparation method of tantalum 10 tungsten alloy |
| CN103849788B (en) * | 2014-03-20 | 2016-01-13 | 宁夏东方钽业股份有限公司 | The preparation method of tantalum blank or tantalum alloy blank |
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