CN106735280A - A kind of preparation method of spherical TiTa alloy powders - Google Patents
A kind of preparation method of spherical TiTa alloy powders Download PDFInfo
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- CN106735280A CN106735280A CN201611037627.XA CN201611037627A CN106735280A CN 106735280 A CN106735280 A CN 106735280A CN 201611037627 A CN201611037627 A CN 201611037627A CN 106735280 A CN106735280 A CN 106735280A
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
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Abstract
The invention discloses a kind of preparation method of spherical TiTa alloy powders, the method is：First, Ti powder, Ta powder are placed in batch mixer and are mixed, obtain mixed-powder；2nd, mixed-powder is pressed into base；3rd, pre-sintered treatment is carried out to pressed compact；4th, being placed in pressed compact carries out melting in vaccum consumable electrode electric arc furnace, obtain bar stock；5th, it is forged to strip off the skin, punch, after tapping process, being processed into the final alloy bar of PREP powder；6th, final alloy bar described in step 5 is made spherical TiTa alloyed powders through PREP technique.Operating process of the present invention is simple, production efficiency is high, the made contaminated risk reduction of TiTa alloy powders; oxygen content≤0.1wt.%; raw material saving at least more than 30%; the manufacturing cost 50% of spherical TiTa alloy powders can be effectively reduced, and then meets low cost, the large-scale production of the spherical TiTa alloy powders of high-quality.
Description
Technical field
The invention belongs to powder metallurgy preparing technical field, and in particular to a kind of preparation side of spherical TiTa alloy powders
Method.
Background technology
Relative to biomedical alloys such as traditional TC4, NiTi, TiTa alloys possess more excellent bio-compatible because of it
The characteristic such as property, excellent corrosion resistance, low elastic modulus, becomes one of presently most preferable biological and medicinal implant material
And demand rapid growth.Meanwhile, it is at full speed with 3D printing technique (laser rapid manufacturing, electron beam selective melting technology)
Development, the high performance spherical titanium tantalum alloy powder that good fluidity, stomata are mingled with less, impurity content is low will be as the biological doctor of 3D printing
With the important foundation raw material of implant, it is expected to more be widely applied.
PREP powder-making technique is one of the main method for preparing spherical high-temperature alloy powder at present.Should
It is to be made bar gained by the multiple melting of vaccum consumable electrode electric arc furnace that technology is raw materials used.Application No.
Spherical titanium alloy powder and spherical niobium are described in 201610220596.5 and 201610219834.0 patent in detail
The preparation method and device of powder.But, for high-melting-point is poor, for the high density difference complete solid solution alloy of Ti-Ta binary, the skill
Art is related to multiple (5~6 times) the repetitions melting of bar, and every melting is once needed to do and once strip off the skin treatment, and wastage of material is very big,
Loss rate of raw materials reaches 40%, and production cost increased 1.5 times.Also, raw material pole in the pilot process for be repeated several times melting
It is vulnerable to pollution, there is a problem of that purity is low, oxygen content is higher so as to cause made powder.Additionally, easily producing titanium during melting
Volatilization and element between layering, so as to be easily caused component segregation, and the uniformity of alloy ingot melting is directly affected
The structural constituent of PREP powder, size distribution.
The content of the invention
The technical problems to be solved by the invention are for above-mentioned the deficiencies in the prior art, there is provided a kind of spherical TiTa
The preparation method of alloy powder.The preparation method operating process is simple, and production efficiency is high, the made contaminated wind of TiTa alloy powders
Danger reduces, oxygen content≤0.1wt.%, the uniform segregation-free of composition；And raw material saving at least more than 30%, can effectively reduce
The manufacturing cost 50% of spherical TiTa alloy powders, and then meet low cost, the scale of the spherical TiTa alloy powders of high-quality
Production.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of preparation of spherical TiTa alloy powders
Method, it is characterised in that the method is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
80r/min~120r/min, the mixing time of the batch mixer is 12h~18h, steel ball and the mixed powder in the batch mixer
The weight ratio at end is (2~4):1；
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 160MPa~200MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 4.0 × 10 are not less than in vacuum- 2Pre-sintered treatment is carried out under conditions of Pa, the temperature of the pre-sintered treatment is 1500 DEG C~1600 DEG C, the pre-sintered treatment
Time be 30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in melting is carried out in vaccum consumable electrode electric arc furnace,
Obtain the bar stock of a diameter of 60mm；The melting electric current is 2kA~3kA, and the melting voltage is 20V~40V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 6, final alloy bar described in step 5 is made spherical TiTa through PREP technique
Alloyed powder, the particle diameter of the TiTa alloyed powders is 30 μm~250 μm.
The preparation method of above-mentioned a kind of spherical TiTa alloy powders, it is characterised in that batch mixer described in step one is V
Type batch mixer.
The preparation method of above-mentioned a kind of spherical TiTa alloy powders, it is characterised in that melting described in step 4 time
Number is 2 times.
The preparation method of above-mentioned a kind of spherical TiTa alloy powders, it is characterised in that TiTa alloys described in step 6
In powder the weight/mass percentage composition of Ta be 40%~80%, in the TiTa alloyed powders weight/mass percentage composition of Ti be 20%~
60%.
The preparation method of above-mentioned a kind of spherical TiTa alloy powders, it is characterised in that plasma described in step 6 revolves
Turn electrode atomized technique detailed process be：Final alloy bar is clamped on electric machine main shaft first, spray chamber is taken out
Vacuum, makes the vacuum of spray chamber be not less than 4.0 × 10-2Pa, then to be filled with spray chamber argon gas protect；Then, motor master
Axle drives final alloy bar to start rotation at a high speed, after rotating speed reaches 10000r/min~15000r/min, plasma tungsten electrode
Rifle loads the current arc of 1200A~1500A, and the end face of final alloy bar is melted, and forms molten bath, in high speed rotation
Under centrifugal action, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, while molten drop is because of its surface
The effect of power and there is nodularization, and final rapid solidification forms spherical TiTa alloy powders；The bulk purity of the high-purity argon gas
It is 99.99%, the feed speed of the final alloy bar is 1.0mm/min~1.4mm/min.
The present invention has advantages below compared with prior art：
1st, present invention preparation TiTa alloy powders process is simple, reduces melting number of times so as to avoid repeating the waste original that strips off the skin
Material, economizes in raw materials more than 30%.The reduction of melting number of times simultaneously, additionally it is possible to effectively reduce being manufactured into for spherical TiTa alloy powders
This 50%, the production efficiency of raising powder.
2nd, the contaminated risk of powder that prepared by the present invention reduces, and wherein oxygen element content is greatly lowered, made powder
Oxygen content≤0.1wt.%, powder sphericity is high, disclosure satisfy that low cost, the scale metaplasia of the spherical TiTa alloy powders of high-quality
Produce and require.
3rd, the present invention thoroughly solves that high-melting-point is poor, the high density difference complete solid solution alloy of Ti-Ta binary low cost is equal
Even melting problem, and breach the high efficiency of spherical TiTa alloy powders, the rotating electrode atomized technology of preparing of low cost plasma.
Technical scheme is described in further detail below by accompanying drawing, embodiment and comparative example.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Fig. 2 is the SEM figures of spherical Ti-65Ta alloy powders prepared by the embodiment of the present invention 1.
Fig. 3 is that the X-ray of Ti-50Ta final alloy bars prepared by the embodiment of the present invention 4, comparative example 1 and comparative example 2 is spread out
Penetrate collection of illustrative plates.
Fig. 4 is the micro-organization chart of Ti-50Ta final alloy bars prepared by the embodiment of the present invention 4.
Fig. 5 is the micro-organization chart of Ti-50Ta final alloy bars prepared by comparative example of the present invention 1.
Fig. 6 is the micro-organization chart of Ti-50Ta final alloy bars prepared by comparative example of the present invention 2.
Specific embodiment
Embodiment 1
The method that the present embodiment prepares spherical Ti-65Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
90r/min, the mixing time of the batch mixer is 15h, and steel ball and the weight ratio of the mixed-powder are 3 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 65%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 35%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 190MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 3.2 × 10 are not less than in vacuum- 2Carry out pre-sintered treatment under conditions of Pa, the temperature of the pre-sintered treatment is 1570 DEG C, the time of the pre-sintered treatment is
30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in vaccum consumable electrode electric arc furnace and is melted twice
Refining, obtains the bar stock of a diameter of 60mm；The melting electric current is 2.5kA, and the melting voltage is 30V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 6, final alloy bar described in step 5 is made spherical Ti- through PREP technique
65Ta alloyed powders；
The specific embodiment that the PREP prepares Ti-65Ta alloy powders is：First by finished product
Alloy bar material is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then to mist
Argon gas protection is filled with change room；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 14000r/min, plasma tungsten electrode rifle loads the current arc of 1400A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.1mm/min.
Fig. 2 is the SEM figures of spherical Ti-65Ta alloy powders manufactured in the present embodiment.As can be seen that Ti-65Ta from figure
Alloy powder is spherical, and sphericity is higher.The particle diameter of spherical Ti-65Ta alloyed powders manufactured in the present embodiment is 30 μm~250 μm,
And the yield of particle diameter≤150 μm is 0.08wt.% for the oxygen content of 72%, Ti-65Ta alloyed powders, is preparing spherical Ti-
The loss late that strips off the skin of alloy bar stock is only 5% during 65Ta alloyed powders.
Embodiment 2
The method that the present embodiment prepares spherical Ti-40Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
80r/min, the mixing time of the batch mixer is 12h, and steel ball and the weight ratio of the mixed-powder are 2 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 40%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 60%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 160MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 3.0 × 10 are not less than in vacuum- 2Carry out pre-sintered treatment under conditions of Pa, the temperature of the pre-sintered treatment is 1500 DEG C, the time of the pre-sintered treatment is
30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in vaccum consumable electrode electric arc furnace and is melted twice
Refining, obtains the bar stock of a diameter of 60mm；The melting electric current is 2.0kA, and the melting voltage is 20V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 6, final alloy bar described in step 5 is made spherical Ti- through PREP technique
40Ta alloyed powders；
The specific embodiment that the PREP prepares Ti-40Ta alloy powders is：First by finished product
Alloy bar material is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then to mist
Argon gas protection is filled with change room；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 10000r/min, plasma tungsten electrode rifle loads the current arc of 1200A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.4mm/min.
The particle diameter of spherical Ti-40Ta alloyed powders manufactured in the present embodiment is 30 μm~250 μm, and particle diameter≤150 μm
Yield is that the oxygen content of 74%, Ti-40Ta alloyed powders is 0.08wt.%, is closed during spherical Ti-40Ta alloyed powders are prepared
The loss late that strips off the skin of golden bar stock is only 5%.
Embodiment 3
The method that the present embodiment prepares spherical Ti-80Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
120r/min, the mixing time of the batch mixer is 18h, and steel ball and the weight ratio of the mixed-powder are 4 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 80%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 20%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 200MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 2.0 × 10 are not less than in vacuum- 2Carry out pre-sintered treatment under conditions of Pa, the temperature of the pre-sintered treatment is 1600 DEG C, the time of the pre-sintered treatment is
30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in vaccum consumable electrode electric arc furnace and is melted twice
Refining, obtains the bar stock of a diameter of 60mm；The melting electric current is 3.0kA, and the melting voltage is 40V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 6, final alloy bar described in step 5 is made spherical Ti- through PREP technique
80Ta alloyed powders；
The specific embodiment that the PREP prepares Ti-80Ta alloy powders is：First by finished product
Alloy bar material is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then to mist
Argon gas protection is filled with change room；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 15000r/min, plasma tungsten electrode rifle loads the current arc of 1500A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.0mm/min.
The particle diameter of spherical Ti-80Ta alloyed powders manufactured in the present embodiment is 30 μm~250 μm, and particle diameter≤150 μm
Yield is that the oxygen content of 70%, Ti-80Ta alloyed powders is 0.09wt.%, is closed during spherical Ti-80Ta alloyed powders are prepared
The loss late that strips off the skin of golden bar stock is only 5%.
Embodiment 4
The method that the present embodiment prepares spherical Ti-50Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
100r/min, the mixing time of the batch mixer is 15h, and steel ball and the weight ratio of the mixed-powder are 3 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 50%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 50%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 180MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 3.0 × 10 are not less than in vacuum- 2Carry out pre-sintered treatment under conditions of Pa, the temperature of the pre-sintered treatment is 1550 DEG C, the time of the pre-sintered treatment is
30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in vaccum consumable electrode electric arc furnace and is melted twice
Refining, obtains the bar stock of a diameter of 60mm；The melting electric current is 2.5kA, and the melting voltage is 30V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 6, final alloy bar described in step 5 is made spherical Ti- through PREP technique
50Ta alloyed powders；
The specific embodiment that the PREP prepares spherical Ti-50Ta alloy powders is：First will
Final alloy bar is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then
Protected to argon gas is filled with spray chamber；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 12000r/min, plasma tungsten electrode rifle loads the current arc of 1300A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.3mm/min.
X ray diffracting spectrum with the present embodiment final alloy bar in Fig. 3, Fig. 4 is the present embodiment Ti-50Ta finished products
The micro-organization chart of alloy bar material, can be seen that Ta powder and Ti powder are well mixed with reference to Fig. 3 and Fig. 4.Be marked on Fig. 4 simultaneously
A regions and b regions carry out energy spectrum analysis (such as table 1), and the result of table 1 is further proved, final made TiTa alloying components are uniform
And realize complete alloying.The yield of spherical Ti-50Ta alloy powders particle diameter≤150 μm manufactured in the present embodiment is 73%,
Oxygen content is 0.09wt.%, and the loss late that strips off the skin of alloy bar stock is only 5% during spherical Ti-50Ta alloyed powders are prepared.
The EDAX results of Ti-50Ta final alloy bars in the embodiment 4 of table 1
| Region | Ta (wt.%) | Ti (wt.%) |
| A regions | 50.1 | 49.9 |
| B regions | 50.0 | 50.0 |
Comparative example 1
The method that this comparative example prepares spherical Ti-50Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
100r/min, the mixing time of the batch mixer is 15h, and steel ball and the weight ratio of the mixed-powder are 3 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 50%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 50%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 180MPa；
Step 3, the pressed compact that will be suppressed in step 2 is placed in that melting twice is carried out in vaccum consumable electrode electric arc furnace, obtains
To the bar stock of a diameter of 60mm；The melting electric current is 2.5kA, and the melting voltage is 30V；
Bar stock described in step 4, step 3 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 5, final alloy bar described in step 4 is made spherical Ti- through PREP technique
50Ta alloyed powders；
The specific embodiment that the PREP prepares spherical Ti-50Ta alloy powders is：First will
Final alloy bar is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then
Protected to argon gas is filled with spray chamber；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 12000r/min, plasma tungsten electrode rifle loads the current arc of 1300A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.3mm/min.
Fig. 3 is the X ray diffracting spectrum of this comparative example final alloy bar, and Fig. 5 is this comparative example Ti-50Ta final alloys
The micro-organization chart of bar, can be seen that Ta powder and the mixing of Ti powder are uneven with reference to Fig. 3 and Fig. 5.C is marked on Fig. 5 simultaneously
Region and d regions carry out energy spectrum analysis (such as table 2), and the result of table 2 further proves that TiTa alloying components are produced obtained in 2 meltings
Macrosegregation is given birth to.
The EDAX results of Ti-50Ta final alloy bars in the comparative example 1 of table 2
| Region | Ta (wt.%) | Ti (wt.%) |
| C regions | 50.3 | 49.7 |
| D regions | 60.7 | 39.3 |
Form substantial amounts of bulk granulated slag during PREP, powder diameter≤150 μm are received
Rate is only 10%, and oxygen content is 0.09wt.%.It can be seen that the material composition of 2 meltings is extremely uneven, not yet complete alloying, because
And high-melting-point alloy is thrown out of in the form of bulk granulated slag in rotation electrode pulverizing process.
Comparative example 2
The method that this comparative example prepares spherical Ti-50Ta alloy powders is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is
100r/min, the mixing time of the batch mixer is 15h, and steel ball and the weight ratio of the mixed-powder are 3 in the batch mixer:
1；The batch mixer is V-type batch mixer；The weight/mass percentage composition of Ta is 50%, Ti in the mixed-powder in the mixed-powder
Weight/mass percentage composition be 50%.
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold
The pressing pressure of isostatic pressed is 180MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vaccum consumable electrode electric arc furnace carries out five meltings, obtains
To the bar stock of a diameter of 60mm；The melting electric current is 2.5kA, and the melting voltage is 30V；
Bar stock described in step 4, step 3 is forged to strip off the skin, punches, after tapping process, be processed into plasma electric rotating
The final alloy bar of pole powder by atomization；
Step 5, final alloy bar described in step 4 is made spherical Ti- through PREP technique
50Ta alloyed powders；
The specific embodiment that the PREP prepares spherical Ti-50Ta alloy powders is：First will
Final alloy bar is clamped on electric machine main shaft, is vacuumized that (vacuum is not less than 4.0 × 10 to spray chamber-2Pa), then
Protected to argon gas is filled with spray chamber；Then, electric machine main shaft drives final alloy bar to start rotation at a high speed, when rotating speed reaches
After 12000r/min, plasma tungsten electrode rifle loads the current arc of 1300A, the end face of final alloy bar is melted, and formed
Molten bath, under the centrifugal action of high speed rotation, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, together
When molten drop there is nodularization because of the effect of its surface tension, and final rapid solidification forms spherical TiTa alloy powders；Wherein institute
It is 99.99% to state the bulk purity of high-purity argon gas, and the feed speed of the final alloy bar is 1.3mm/min.
X ray diffracting spectrum with this comparative example final alloy bar in Fig. 3, Fig. 6 is this comparative example Ti-50Ta finished products
The micro-organization chart of alloy bar material, can be seen that Ta powder and Ti powder are well mixed with reference to Fig. 3 and Fig. 6.Be marked on Fig. 6 simultaneously
E regions and f regions carry out energy spectrum analysis (such as table 3), and the result of table 3 is further proved, by the TiTa alloys after 5 meltings into
Point uniformity is improved, and realizes complete alloying.
The EDAX results of Ti-50Ta final alloy bars in the comparative example 2 of table 3
| Region | Ta (wt.%) | Ti (wt.%) |
| E regions | 50.1 | 49.9 |
| F regions | 50.0 | 50.0 |
The yield of spherical Ti-50Ta alloy powders particle diameter≤150 μm prepared by this comparative example is 72%.But, five times are molten
Stripped off the skin repeatedly during refining so that significant loss 35%, powder production cost improves 50%, and oxygen content is up to
0.18wt.%.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention
Protection domain in.
Claims (5)
1. a kind of preparation method of spherical TiTa alloy powders, it is characterised in that the method is comprised the following steps：
Step one, by Ti powder, Ta powder be placed in batch mixer mix, obtain mixed-powder；The rotating speed of the batch mixer is 80r/min
~120r/min, the mixing time of the batch mixer is 12h~18h, the weight of steel ball and the mixed-powder in the batch mixer
Amount is than being (2~4):1；
Step 2, mixed-powder described in step one is fitted into compacting tool set, base is pressed into isostatic cool pressing, it is described cold etc. quiet
The pressing pressure of pressure is 160MPa~200MPa；
Step 3, the pressed compact that will be suppressed in step 2 are placed in vacuum sintering furnace, and 4.0 × 10 are not less than in vacuum-2Pa's
Under the conditions of carry out pre-sintered treatment, the temperature of the pre-sintered treatment is 1500 DEG C~1600 DEG C, the pre-sintered treatment when
Between be 30min；
Step 4, the pressed compact after pre-sintered treatment in step 3 is placed in melting is carried out in vaccum consumable electrode electric arc furnace, obtained
The bar stock of a diameter of 60mm；The melting electric current is 2kA~3kA, and the melting voltage is 20V~40V；
Bar stock described in step 5, step 4 is forged to strip off the skin, punches, after tapping process, be processed into plasma rotating electrode mist
Change the final alloy bar of powder processed；
Step 6, final alloy bar described in step 5 is made spherical TiTa alloys through PREP technique
Powder, the particle diameter of the TiTa alloyed powders is 30 μm~250 μm.
2. a kind of preparation method of spherical TiTa alloy powders according to claim 1, it is characterised in that institute in step one
Batch mixer is stated for V-type batch mixer.
3. a kind of preparation method of spherical TiTa alloy powders according to claim 1, it is characterised in that institute in step 4
The number of times for stating melting is 2 times.
4. a kind of preparation method of spherical TiTa alloy powders according to claim 1, it is characterised in that institute in step 6
It is 40%~80% to state the weight/mass percentage composition of Ta in TiTa alloyed powders, and the weight/mass percentage composition of Ti is in the TiTa alloyed powders
20%~60%.
5. a kind of preparation method of spherical TiTa alloy powders according to claim 1, it is characterised in that institute in step 6
The detailed process for stating PREP technique is：Final alloy bar is clamped on electric machine main shaft first, to mist
Change room to be vacuumized, the vacuum of spray chamber is not less than 4.0 × 10-2Pa, then to be filled with spray chamber argon gas protect；With
Afterwards, electric machine main shaft drives final alloy bar to start rotation at a high speed, after rotating speed reaches 10000r/min~15000r/min, etc.
Ion tungsten electrode rifle loads the current arc of 1200A~1500A, and the end face of final alloy bar is melted, and forms molten bath, in height
Speed rotation centrifugal action under, the liquid metal of fusing is thrown away at a high speed further forms tiny molten drop, at the same molten drop because
The effect of its surface tension and there is nodularization, and final rapid solidification forms spherical TiTa alloy powders；The high-purity argon gas
Bulk purity is 99.99%, and the feed speed of the final alloy bar is 1.0mm/min~1.4mm/min.
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