CN109175315B - Preparation method of copper-iron immiscible alloy - Google Patents
Preparation method of copper-iron immiscible alloy Download PDFInfo
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- CN109175315B CN109175315B CN201811130508.8A CN201811130508A CN109175315B CN 109175315 B CN109175315 B CN 109175315B CN 201811130508 A CN201811130508 A CN 201811130508A CN 109175315 B CN109175315 B CN 109175315B
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- copper
- iron
- power supply
- frequency induction
- induction heating
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 26
- 239000000956 alloy Substances 0.000 title claims abstract description 26
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000006698 induction Effects 0.000 claims abstract description 16
- 229910052582 BN Inorganic materials 0.000 claims abstract description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052742 iron Inorganic materials 0.000 abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052802 copper Inorganic materials 0.000 abstract description 7
- 239000010949 copper Substances 0.000 abstract description 7
- 239000000155 melt Substances 0.000 abstract description 3
- 238000007711 solidification Methods 0.000 description 11
- 230000008023 solidification Effects 0.000 description 11
- 239000012071 phase Substances 0.000 description 8
- 229910000640 Fe alloy Inorganic materials 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 230000005486 microgravity Effects 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 238000004781 supercooling Methods 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/02—Use of electric or magnetic effects
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
一种铜铁难混溶合金的制备方法,属于难混溶合金技术领域，其特征在于实施步骤如下：一、将氮化硼坩锅放置在高频感应炉的真空箱体内，将质量比为85:15的铜铁样品件放入氮化硼坩埚内，氮化硼坩埚与钼电极连接；真空箱体抽真空至2×10‑4 Pa。开启高频感应加热电源，加热至1400℃，使铜铁样品件全部熔化，保温10min；二、对保温后的铜铁样品件施加电脉冲，作用时间为10min；三、关闭高频感应加热电源，进入随炉冷却过程，待铜铁样品件熔体完全凝固后，关闭脉冲电源。优点是本发明方法制备的难混溶合金可以获得组织均匀、晶粒细化的铜铁难混熔合金。
A method for preparing a copper-iron immiscible alloy belongs to the technical field of immiscible alloys, and is characterized in that the implementation steps are as follows: 1. Place a boron nitride crucible in a vacuum box of a high-frequency induction furnace, and set the mass ratio to be The copper-iron sample at 85:15 was placed in a boron nitride crucible, which was connected to the molybdenum electrode; the vacuum box was evacuated to 2×10 ‑4 Pa. Turn on the high-frequency induction heating power supply and heat it to 1400 ° C to melt all the copper and iron samples, and keep the heat for 10 minutes; 2. Apply electric pulses to the insulated copper and iron samples for 10 minutes; 3. Turn off the high-frequency induction heating power supply , enter the cooling process with the furnace, and turn off the pulse power supply after the melt of the copper-iron sample piece is completely solidified. The advantage is that the immiscible alloy prepared by the method of the invention can obtain the copper-iron immiscible alloy with uniform structure and refined grain.
Description
Technical Field
The invention belongs to the technical field of immiscible alloys, and particularly relates to a preparation method of a copper-iron immiscible alloy.
Background
The immiscible alloy is easy to have serious segregation and even structure delamination under the conventional casting condition, thereby losing the application value. Therefore, only the second phase is uniformly and dispersedly distributed in the matrix or the two phases in the intergrowth are orderly arranged in a fiber shape, and the excellent performance of the immiscible alloy can be embodied. Thus, the preparation of immiscible alloys is gaining attention.
Many researchers have conducted directional solidification studies on immiscible alloys under space microgravity conditions. Although the space microgravity method is an ideal method for researching the liquid phase separation mechanism of the immiscible alloy, the method cannot be widely applied due to the high cost investment.
However, the Stokes motion of the immiscible alloy in the liquid phase separation process can only be weakened to a certain extent by means of simulating the microgravity environment, the influence of the Stokes motion on the coarsening of second-phase liquid drops cannot be completely eliminated, and meanwhile, the Marangoni migration still plays a leading role in the coarsening process of the second-phase liquid drops, so that the traditional method still cannot obtain a fine immiscible alloy solidification structure.
The metallurgical powder method utilizes the small size of liquid drops obtained by atomization, thereby greatly weakening the component segregation generated in the rapid solidification process, and effectively preventing the occurrence of macrosegregation in finished products. Because the difference of the melting points of the two components in the alloy melt is large, the preparation process of the powder metallurgy method belongs to liquid phase sintering. The method has the main advantages that the volume fraction of the second phase is higher, the macrosegregation is smaller, and other alloy elements can be added; however, the disadvantages are also significant, such as high production cost and complicated process.
Disclosure of Invention
The invention aims to provide a preparation method of a copper-iron alloy difficult to mix and melt, which can effectively overcome the defects in the prior art.
The invention is realized by the following steps:
the first step is as follows: placing a boron nitride crucible in a vacuum box body of a CW-30P type high-frequency induction heating furnace, then placing a copper-iron sample piece with the mass ratio of 85:15 into the boron nitride crucible, connecting the boron nitride crucible with a molybdenum electrode, and vacuumizing the vacuum box body of the GW-30P type high-frequency induction heating furnace to 2 multiplied by 10-4 And Pa, starting a high-frequency induction heating power supply, heating the copper and iron sample piece to 1400 ℃, completely melting the copper and iron sample piece, and preserving heat for 10 min.
And secondly, applying electric pulse to the copper and iron sample after heat preservation, wherein the action time is 10 min. Firstly, starting a pulse power supply; then the output voltage of the pulse power supply is adjusted to 60V, the pulse width is 10 mus, the frequency is 30Hz, and the pulse current is realized by adjusting the peak value displayed by the output voltage on an oscilloscope.
The third step: and (4) turning off the high-frequency induction heating power supply, entering a furnace cooling process, and turning off the pulse power supply after the melt is completely solidified.
The invention has the positive effects that: (1) the critical nucleation radius of the immiscible alloy with the liquid phase immiscible region is reduced by applying electric pulses, the nucleation barrier is reduced, the supercooling degree is increased, and the nucleation rate is improved.
(2) Because the method for applying the pulse current emphasizes the research of pulse parameters, the introduction of the pulse current can also enable the alloy melt to obtain the supercooling degree generated by electromagnetic force; moreover, the electric pulse reduces the activity of the alloy melt, when the melt passes through an immiscible region, the number of atomic groups separated by a second phase is obviously reduced, the solidification of the second phase is effectively inhibited, therefore, the structure of the monotectic alloy can be refined along with the increase of supercooling degree like other traditional alloys, and finally, the purpose of refining the solidification structure of the immiscible alloy can be achieved by applying pulse current.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
in the figure: 1-oscilloscope, 2-pulse power supply, 3-argon gas, 4-molybdenum electrode, 5-copper iron sample piece, 6-boron nitride crucible, 7-vacuum box, 8-induction coil, 9-infrared temperature measuring hole and 10-high frequency induction heating power supply;
FIG. 2 is a solidification structure of a Cu-15 wt.% Fe hypermonotectic alloy without the application of an electric pulse;
FIG. 3 is a solidification structure of a Cu-15 wt.% Fe alloy at 500A pulse current;
FIG. 4 is the solidification structure of a Cu-15 wt.% Fe alloy at 1000A pulse current.
The specific implementation mode is as follows:
as shown in FIG. 1, the preparation method for preparing the copper-iron refractory alloy comprises the following steps:
the first step is as follows: placing a boron nitride crucible 6 in a vacuum box body 7 of a CW-30P type high-frequency induction heating furnace, then placing a copper-iron sample piece 5 with the mass ratio of 85:15 into the boron nitride crucible 6, connecting the boron nitride crucible 6 with a molybdenum electrode 4, vacuumizing the vacuum box body 7 of the GW-30P type high-frequency induction heating furnace to 2 multiplied by 10-4 Pa, starting a high-frequency induction heating power supply 10, heating the copper and iron sample to 1400 ℃, completely melting the copper and iron sample 5, and keeping the temperature for 10 min;
secondly, applying electric pulse to the heat-insulated copper-iron sample piece 5 for 10min, starting the pulse power supply 2, adjusting the output voltage of the pulse power supply 2 to 60V, the pulse width to 10 mus and the frequency to 30Hz, wherein the pulse current is realized by adjusting the peak value displayed by the output voltage on the oscilloscope 1,
the third step: and (3) turning off the high-frequency induction heating power supply 10, entering a furnace cooling process, and turning off the pulse power supply 2 after the copper-iron sample piece 5 is completely solidified.
FIG. 2 is a solidification structure of a Cu-15 wt.% Fe hypermonotectic alloy without the application of an electric pulse;
FIG. 3 is a solidification structure of a Cu-15 wt.% Fe alloy at 500A pulse current;
FIG. 4 is the solidification structure of a Cu-15 wt.% Fe alloy at 1000A pulse current.
As can be seen, the iron-rich phase in FIG. 2 aggregates, resulting in severe tissue segregation;
FIG. 3 shows that the iron-rich balls in the solidification structure disappear, and the interior of the grains grow in a dendrite manner, so that a more uniform structure is obtained.
In fig. 4, dendrites disappear, a more uniform structure is obtained, and grains are obviously refined.
Claims (1)
1. A preparation method of a copper-iron immiscible alloy is characterized by comprising the following implementation steps:
the first step is as follows: placing a boron nitride crucible (6) in a vacuum box body (7) of a CW-30P type high-frequency induction heating furnace, then placing a copper-iron sample piece (5) with the mass ratio of 85:15 into the boron nitride crucible (6), connecting the boron nitride crucible (6) with a molybdenum electrode (4), and vacuumizing the vacuum box body (7) of the GW-30P type high-frequency induction heating furnace to 2 multiplied by 10-4 Pa, starting a high-frequency induction heating power supply (10), heating the copper-iron sample to 1400 ℃, completely melting the copper-iron sample piece (5), and preserving heat for 10 min;
secondly, applying electric pulse to the copper-iron sample piece (5) after heat preservation for 10min, starting the pulse power supply (2), then adjusting the output voltage of the pulse power supply (2) to 60V, the pulse width to 10 mus, the frequency to 30Hz, the pulse current is realized by adjusting the peak value displayed by the output voltage on the oscilloscope (1),
the third step: and (3) turning off the high-frequency induction heating power supply (10), entering a furnace cooling process, and turning off the pulse power supply (2) after the copper-iron sample piece (5) is completely solidified.
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| CN201811130508.8A CN109175315B (en) | 2018-09-27 | 2018-09-27 | Preparation method of copper-iron immiscible alloy |
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| CN201811130508.8A CN109175315B (en) | 2018-09-27 | 2018-09-27 | Preparation method of copper-iron immiscible alloy |
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| Publication Number | Publication Date |
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| CN109175315B true CN109175315B (en) | 2021-01-19 |
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| CN110814305B (en) * | 2019-11-07 | 2021-06-15 | 中南大学 | A kind of Cu-Fe composite material double melt mixed casting equipment and technology |
| CN110724841B (en) * | 2019-11-07 | 2021-09-07 | 中南大学 | A kind of preparation method of immiscible alloy and continuous casting equipment |
| CN115261653B (en) * | 2022-08-12 | 2023-11-10 | 山西工程职业学院 | A preparation method of modified ZL102 aluminum alloy |
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| IL100136A (en) * | 1991-11-24 | 1994-12-29 | Ontec Ltd | Method and device for producing homogeneous alloys |
| JP2006098085A (en) * | 2004-09-28 | 2006-04-13 | Toyota Motor Corp | Prediction method for overlay layer structure |
| CN101100705A (en) * | 2007-07-25 | 2008-01-09 | 上海大学 | Pulse current liquid level disturbance solidification fine grain method |
| CN101885053A (en) * | 2010-06-24 | 2010-11-17 | 西北工业大学 | A method and device for directional solidification grain ultra-refinement by strong pulse current |
| CN102031399B (en) * | 2010-11-11 | 2012-02-29 | 东北大学 | A kind of preparation method of Cu-Fe alloy under the action of magnetic field |
| CN103540779A (en) * | 2012-07-12 | 2014-01-29 | 中国科学院兰州化学物理研究所 | Method for preparing copper and iron immiscible alloy |
| CN103212697B (en) * | 2013-04-12 | 2015-04-01 | 西北工业大学 | Casting mould method for improving casting aluminium alloy solidification structure by adopting variable-frequency low-voltage modulating pulse electric field |
| CN104630512B (en) * | 2013-11-06 | 2017-02-08 | 中国科学院金属研究所 | Dispersion type copper-bismuth-tin immiscible alloy composite wire rod and preparation method thereof |
| CN103817314B (en) * | 2014-03-20 | 2017-01-18 | 辽宁工业大学 | Electric pulse control method and device for iron-rich aluminum-silicon alloy iron phases |
| CN104131185B (en) * | 2014-07-21 | 2016-04-06 | 东北大学 | The method of immiscible alloy ingot casting is prepared in a kind of slag refining |
| CN104128592B (en) * | 2014-08-14 | 2017-02-01 | 昆明理工大学 | Device for refining metal solidification structure with electric current pulses |
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Effective date of registration: 20201225 Address after: 030024 No. 66 tile Road, Wan Berlin District, Shanxi, Taiyuan Applicant after: TAIYUAN University OF SCIENCE AND TECHNOLOGY Applicant after: Shanxi Engineering Vocational College Address before: 030024 No. 66 tile Road, Wan Berlin District, Shanxi, Taiyuan Applicant before: TAIYUAN University OF SCIENCE AND TECHNOLOGY |
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