CN110423904A - A kind of electron-beam smelting homogenizes the method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy - Google Patents
A kind of electron-beam smelting homogenizes the method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy Download PDFInfo
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- CN110423904A CN110423904A CN201910706037.9A CN201910706037A CN110423904A CN 110423904 A CN110423904 A CN 110423904A CN 201910706037 A CN201910706037 A CN 201910706037A CN 110423904 A CN110423904 A CN 110423904A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
It homogenizes the method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy the invention discloses a kind of electron-beam smelting, there are following steps: weighing each raw material of Ni-Cr-Co-Fe-Mn high-entropy alloy: Ni, Cr, Co, Fe and Mn；Each raw material symmetrically obtained is cleaned, spare；Each raw material after cleaning up is placed in the water jacketed copper crucible of electron beam furnace；Vacuum is carried out to electron beam furnace to take out in advance, later, pumping high vacuum is carried out to electron beam furnace, reaches high vacuum standard；Electron-beam smelting is carried out to the raw material in water jacketed copper crucible and instantaneously drops beam later, is quickly solidified, the sample being cooled to room temperature；Turn-over remelting is carried out in water jacketed copper crucible to the sample being cooled to room temperature and instantaneously drops beam later, quickly solidifies, obtains Ni-Cr-Co-Fe-Mn high-entropy alloy.Purity is high, the uniform Ni-Cr-Co-Fe-Mn high-entropy alloy of ingredient can be efficiently prepared in the present invention, and ingot casting effectively controls ingot metallurgy quality without shrinkage cavity.
Description
Technical field
The present invention relates to a kind of preparation method of alloy, specifically a kind of electron-beam smelting homogenize High Purity preparation
The method of Ni-Cr-Co-Fe-Mn high-entropy alloy.
Background technique
Multi-principal high-entropy alloy intensity with higher, good wearability, high processing hardening, high temperature resistant softening, resistance to height
The combination of the excellent properties such as warm oxidation, corrosion-resistant and high resistivity or these excellent characteristics.Based on the above advantage, high-entropy alloy is
Through stiff dough, the high-frequency soft magnetic thin film in high speed cutting tool, the golf club head scope of attack, oil pressure atmospheric pressure pole, steel pipe and roll-in cylinder
Etc. be applied.
The preparation method of high-entropy alloy block materials generally has following several: vacuum arc melting, vacuum induction melting, powder
Last metallurgy method and mechanical alloying method.Wherein most of high-entropy alloy is prepared using the method for vacuum arc melting, should
Method can be with the most of alloys of melting, including some high-melting-point high-entropy alloys.But its disadvantage it is also obvious that for example, fusing point compared with
High element can generate serious segregation；Vacuum induction melting can not the dystectic alloy of melting, due to high-entropy alloy pivot member
Element can include generally one or more high-melting-point elements, so vacuum induction melting is of little use；The method of powder metallurgy is same only
The high temperature alloy of low-melting-point metal can be prepared；And the appearance of mechanical alloying method, then effectively overcome above-mentioned many disadvantages.Tool
Body is will to prepare the elemental powder of high-entropy alloy in proportion, and the mechanical mixture under high-energy ball milling effect, powder particle is through repeatedly
Cold welding, the process for being crushed and welding again, finally obtain high-entropy alloy powder.Finally alloyed powder is suppressed, is obtained by techniques such as HIP
To block materials.However, mechanical alloying is there are long flow path, the problems such as complex process, and need in alloying process tight
Lattice control condition avoids metal powder contaminated.
Summary of the invention
According to technical problem set forth above, and a kind of electron-beam smelting is provided and is homogenized High Purity preparation Ni-Cr-Co-
The method of Fe-Mn high-entropy alloy.Electron-beam smelting technology, has that power is controllable, the melting environment of high vacuum, and beam spot, which has, disturbs
Dynamic property, and the advantages that beam spot size position is controllable.In addition, water jacketed copper crucible can provide faster cooling rate.It is based on
This, electron-beam smelting technology have can homogenize, High Purity prepares the condition of high-entropy alloy.
The technological means that the present invention uses is as follows:
A kind of electron-beam smelting homogenizes the method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy, has following step
It is rapid:
S1, each raw material for weighing Ni-Cr-Co-Fe-Mn high-entropy alloy: Ni, Cr, Co, Fe and Mn；
S2, each raw material symmetrically obtained are cleaned, spare；
S3, will clean up after each raw material be placed in the water jacketed copper crucible of electron beam furnace；
S4, electron beam furnace progress vacuum is taken out in advance, later, pumping high vacuum is carried out to electron beam furnace, reaches high
Vacuum standard；
S5, beam is instantaneously dropped later to the raw material progress electron-beam smelting in water jacketed copper crucible, quickly solidifies, is cooled down
To the sample of room temperature；
S6, turn-over remelting is carried out in water jacketed copper crucible to the sample being cooled to room temperature, later, instantaneously drops beam, fast rapid hardening
Gu obtaining Ni-Cr-Co-Fe-Mn high-entropy alloy.
In the step S1, each raw material of Ni-Cr-Co-Fe-Mn high-entropy alloy is weighed by following mass parts:
Co:104~108 part
Cr:156~160 part
Ni:303~307 part
Fe:160~165 part
Mn:409~415 part；
Ni, Cr, Co, Fe and Mn are block or particle.
In the step S3, each raw material after cleaning up is placed in the sequence in the water jacketed copper crucible of electron beam furnace
Are as follows:
Be sequentially placed into Mn, Cr, Fe, Co and Ni from water jacketed copper crucible bottom to top, and with Ni, Co, Fe completely by Cr and
Mn covering.Mn and Cr causes element to be easy scaling loss, therefore, it is necessary to lean on because its saturated vapor pressure is higher or the more low reason of fusing point
It places nearly water jacketed copper crucible bottom.The addition of each raw material of Ni-Cr-Co-Fe-Mn high-entropy alloy must strictly realize Ni, Co, Fe
Three kinds of elements completely cover Cr and Mn element.
Specific step is as follows by the step S4:
It closes electron-beam smelting furnace door progress vacuum to take out in advance, as the working chamber of electron beam furnace vacuum degree≤10Pa
Afterwards, pumping high vacuum is carried out to electron beam furnace, so that working chamber's vacuum degree of electron beam furnace is less than 5 × 10-2Pa, electronics
Gun body vacuum degree is less than 5 × 10-3Pa reaches high vacuum standard.
Specific step is as follows by the step S5:
S51, after reaching high vacuum standard, start electron-beam smelting after the filament pre-heating of electron beam furnace；
S52, it is slowly increased line with 5~10mA/s to 6kW, keeps 7min, while controlling beam spot and uniformly scanning
Raw material surface carries out it primary melting in water jacketed copper crucible；
S53, it is slowly increased line with 5~10mA/s to 9kW, keeps 2min, while controlling beam spot and uniformly scanning
Primary melting raw material in water jacketed copper crucible sufficiently melts raw material, obtains molten alloy；
S54, it reduces rapidly power and is solidified to molten alloy and be in red heat state；
S55, line is slowly increased with 5~10mA/s to 9kW, after the alloy melting in red heat state, 9kW keeps 3min,
Above process control beam spot uniformly scans alloy surface in water jacketed copper crucible, and the above process refers to step S55.
S56, beam is instantaneously dropped, quickly solidified, the sample being cooled to room temperature.
Beam spot equably scans its surface in raw material fusion process, in the fusion process of step S5 power control need and
When, avoid top bath temperature is too high from causing bottom Mn and Cr scaling loss excessive.
Specific step is as follows by the step S6:
S61, turn-over is carried out to the sample that is cooled to room temperature, line is slowly increased to 6kW with 5~10mA/s, keeps 5min,
Controlling beam spot uniformly scans the sample surfaces after turn-over simultaneously；It can be suitably in 6kW or less to the sample surfaces after turn-over
It is preheated, sample starts to melt.In the fusion process, it should control the movement of beam spot to avoid stopping in region
Long, cause hot-spot and the burning of element is caused to be lost, sample surfaces of being subject to melt.
After sample melting after S62, turn-over, line is slowly increased to 12kW with 5~10mA/s, keeps 2min, same to time control
Beam spot processed uniformly scans the sample surfaces after the turn-over after fusing；
S63, beam is instantaneously dropped, quickly solidifies, obtains Ni-Cr-Co-Fe-Mn high-entropy alloy.
Above-mentioned each " while controlling beam spot and uniformly scanning " refers to the process for increasing line and keeps the process of power equal
Beam spot is controlled uniformly to scan.
The beam spot size is 10 × 10 (device parameters).
Each raw material symmetrically obtained under alcohol immersion, is cleaned, scavenging period 10min respectively with supersonic cleaning machine.
Purity is high, the uniform Ni-Cr-Co-Fe-Mn high-entropy alloy of ingredient can be efficiently prepared in the present invention, and casts
Ingot effectively controls ingot metallurgy quality without shrinkage cavity.
The present invention can be widely popularized in fields such as alloy preparations based on the above reasons.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with
It obtains other drawings based on these drawings.
Fig. 1 is each raw material placement order signal of Ni-Cr-Co-Fe-Mn high-entropy alloy in a specific embodiment of the invention
Figure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
A kind of electron-beam smelting homogenizes the method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy, has following step
It is rapid:
One, raw material preparation
1. weighing each raw material of Ni-Cr-Co-Fe-Mn high-entropy alloy by following quality
1 raw material proportioning of table
2. cleaning
Each raw material symmetrically obtained under alcohol immersion, is cleaned, scavenging period 10min respectively with supersonic cleaning machine；
3. charging
As shown in Figure 1, each raw material after cleaning up is placed in the sequence in the water jacketed copper crucible of electron beam furnace are as follows:
Be sequentially placed into Mn, Cr, Fe, Co and Ni from water jacketed copper crucible bottom to top, and with Ni, Co, Fe completely by Cr and
Mn covering.
Two, electron-beam smelting
1. after charging, closes electron-beam smelting furnace door progress vacuum and take out in advance, after working chamber's vacuum degree≤10Pa,
Pumping high vacuum, working chamber's vacuum degree is less than 5 × 10-2Pa, electron gun vacuum degree is less than 5 × 10-3Pa reaches high vacuum standard.
2. after reaching high vacuum standard, starting electron-beam smelting after the filament pre-heating of electron beam furnace；With 5~10mA/s
Line is slowly increased to 6kW, keeps 7min, while controlling beam spot and uniformly scanning in water jacketed copper crucible raw material surface to it
It carries out primary melting；Line is slowly increased with 5~10mA/s and keeps 2min to 9kW, while being controlled beam spot and uniformly being scanned
Primary melting raw material in water jacketed copper crucible sufficiently melts raw material, obtains molten alloy；Power is reduced rapidly to melting
Alloy graining and be in red heat state；Line is slowly increased to 9kW with 5~10mA/s, and after the alloy melting in red heat state, 9kW is protected
3min is held, above process control beam spot uniformly scans alloy surface in water jacketed copper crucible.In above procedure, the electronics
Beam spot size is 10 × 10 (device parameters).
3. instantaneously drop beam quickly solidifies, the sample being cooled to room temperature.
4. pair sample being cooled to room temperature carries out turn-over, line is slowly increased to 6kW with 5~10mA/s, keeps 5min, together
When control beam spot uniformly scan the sample surfaces after turn-over；After sample melting after turn-over, slowly increased with 5~10mA/s
Add line to 12kW, keep 2min, while controlling the sample surfaces after the turn-over after beam spot uniformly scans fusing；Instantaneously
Beam is dropped, quickly solidifies, obtains Ni-Cr-Co-Fe-Mn high-entropy alloy.In above procedure, the beam spot size is 10 × 10
(device parameter).XRF detect ingot casting (Ni-Cr-Co-Fe-Mn high-entropy alloy) ultimate constituent is shown in Table 2
2 ingot casting of table (Ni-Cr-Co-Fe-Mn high-entropy alloy) ingredient (wt.%)
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (8)
- A kind of method that High Purity prepares Ni-Cr-Co-Fe-Mn high-entropy alloy 1. electron-beam smelting homogenizes, it is characterised in that tool It has the following steps:S1, each raw material for weighing Ni-Cr-Co-Fe-Mn high-entropy alloy: Ni, Cr, Co, Fe and Mn；S2, each raw material symmetrically obtained are cleaned, spare；S3, will clean up after each raw material be placed in the water jacketed copper crucible of electron beam furnace；S4, electron beam furnace progress vacuum is taken out in advance, later, pumping high vacuum is carried out to electron beam furnace, reaches high vacuum Standard；S5, beam is instantaneously dropped later to the raw material progress electron-beam smelting in water jacketed copper crucible, quickly solidifies, obtains being cooled to room The sample of temperature；S6, it turn-over remelting is carried out in water jacketed copper crucible to the sample being cooled to room temperature instantaneously drops beam later, quickly solidify, obtain To Ni-Cr-Co-Fe-Mn high-entropy alloy.
- 2. according to the method described in claim 1, it is characterized by: in the step S1, Ni-Cr-Co-Fe-Mn high-entropy alloy Each raw material weighed by following mass parts:Co:104~108 partCr:156~160 partNi:303~307 partFe:160~165 partMn:409~415 part；Ni, Cr, Co, Fe and Mn are block or particle.
- 3. according to the method described in claim 1, it is characterized by: each raw material after cleaning up is set in the step S3 Sequence in the water jacketed copper crucible of electron beam furnace are as follows:It is sequentially placed into Mn, Cr, Fe, Co and Ni from water jacketed copper crucible bottom to top, and is completely covered Cr and Mn with Ni, Co, Fe Lid.
- 4. according to the method described in claim 1, it is characterized by: the step S4 specific step is as follows:Electron-beam smelting furnace door progress vacuum is closed to take out in advance, it is right after the working chamber of electron beam furnace vacuum degree≤10Pa Electron beam furnace carries out pumping high vacuum, so that working chamber's vacuum degree of electron beam furnace is less than 5 × 10-2Pa, electron gun Vacuum degree is less than 5 × 10-3Pa reaches high vacuum standard.
- 5. according to the method described in claim 1, it is characterized by: the step S5 specific step is as follows:S51, after reaching high vacuum standard, start electron-beam smelting after the filament pre-heating of electron beam furnace；S52, it is slowly increased line with 5~10mA/s to 6kW, keeps 7min, while controlling beam spot and uniformly scanning water cooling Raw material surface carries out it primary melting in copper crucible；S53, it is slowly increased line with 5~10mA/s to 9kW, keeps 2min, while controlling beam spot and uniformly scanning water cooling Primary melting raw material in copper crucible sufficiently melts raw material, obtains molten alloy；S54, it reduces rapidly power and is solidified to molten alloy and be in red heat state；S55, line is slowly increased with 5~10mA/s to 9kW, after the alloy melting in red heat state, 9kW keeps 3min, above-mentioned Process control beam spot uniformly scans alloy surface in water jacketed copper crucible；S56, beam is instantaneously dropped, quickly solidified, the sample being cooled to room temperature.
- 6. according to the method described in claim 1, it is characterized by: the step S6 specific step is as follows:S61, turn-over is carried out to the sample being cooled to room temperature, line is slowly increased to 6kW with 5~10mA/s, keeps 5min, simultaneously Control beam spot uniformly scans the sample surfaces after turn-over；After sample melting after S62, turn-over, line is slowly increased with 5~10mA/s and keeps 2min to 12kW, while controlling electricity Beamlet spot uniformly scans the sample surfaces after the turn-over after fusing；S63, beam is instantaneously dropped, quickly solidifies, obtains Ni-Cr-Co-Fe-Mn high-entropy alloy.
- 7. method according to claim 5 or 6, it is characterised in that: the beam spot size is 10 × 10.
- 8. according to the method described in claim 1, it is characterized by: the cleaning refers in the step S2: symmetrical to obtain Each raw material arrived under alcohol immersion, is cleaned, scavenging period 10min respectively with supersonic cleaning machine.
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Cited By (3)
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| CN112048624A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Method for improving component uniformity of nickel-based high-temperature alloy through electron beam circulating overtemperature treatment |
| CN112095018A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for controlling components in process of refining high-temperature alloy by electron beam |
| CN116607028A (en) * | 2023-07-11 | 2023-08-18 | 北京中辰至刚科技有限公司 | Smelting method of refractory high-entropy alloy |
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