CN117721334B - Preparation method of TiZrNb-series refractory multi-principal element alloy with uniform equiaxed fine grain structure - Google Patents
Preparation method of TiZrNb-series refractory multi-principal element alloy with uniform equiaxed fine grain structure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910001325 element alloy Inorganic materials 0.000 title claims 6
- 230000006698 induction Effects 0.000 claims abstract description 172
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 91
- 239000000956 alloy Substances 0.000 claims abstract description 91
- 239000000155 melt Substances 0.000 claims abstract description 75
- 238000003723 Smelting Methods 0.000 claims abstract description 33
- 238000005275 alloying Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 74
- 238000000034 method Methods 0.000 claims description 32
- 239000007789 gas Substances 0.000 claims description 12
- 230000001681 protective effect Effects 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 238000007711 solidification Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims 7
- 229910016285 MxNy Inorganic materials 0.000 claims 1
- 238000002844 melting Methods 0.000 description 36
- 230000008018 melting Effects 0.000 description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000000203 mixture Substances 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 7
- 230000000877 morphologic effect Effects 0.000 description 7
- 230000008023 solidification Effects 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 229910052758 niobium Inorganic materials 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005204 segregation Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
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- 230000006866 deterioration Effects 0.000 description 1
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- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法，属于合金技术领域。采用双线圈悬浮冷坩埚熔炼技术进行合金化熔炼，然后先将熔体温度降低至液相线与固相线之间，以此为基准将温度再升高至略高于液相线，随后先瞬时降低主感应线圈功率，待顶部熔体温度适当降低后再瞬时降低坩埚底部感应线圈功率，使合金整体在低过热度下快速凝固，避免了晶粒的过度生长，获得了细小的初始组织，改善铸锭的力学性能。The present invention relates to a preparation method of a TiZrNb-based refractory multi-principal alloy with uniform equiaxed fine-grained structure, and belongs to the technical field of alloys. The alloying smelting is performed by adopting a double-coil suspended cold crucible smelting technology, and then the melt temperature is first reduced to between the liquidus and the solidus, and based on this, the temperature is raised to slightly above the liquidus, and then the power of the main induction coil is instantaneously reduced, and after the top melt temperature is appropriately reduced, the power of the induction coil at the bottom of the crucible is instantaneously reduced, so that the alloy as a whole is rapidly solidified at a low superheat, the excessive growth of grains is avoided, a fine initial structure is obtained, and the mechanical properties of the ingot are improved.
Description
技术领域Technical Field
本发明涉及一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法，属于合金技术领域。The invention relates to a preparation method of a TiZrNb series refractory multi-principal alloy with uniform equiaxed fine-grained structure, belonging to the technical field of alloys.
背景技术Background technique
多主元合金是一种新提出的合金设计理念，极大的拓宽了金属材料的成分设计空间。TiZrNb系多主元合金是一种典型的难熔多主元合金体系，该类合金由不同配比的Ti、Zr、Nb以及Hf、Ta、Al等添加元素组合而成，元素种类多，熔点高且差异大（Nb熔点2477℃，Ti熔点1668℃），导致合金熔炼易出现成分偏析、组织粗大且不均匀等问题，严重制约了合金的制备生产。Multi-principal alloy is a newly proposed alloy design concept, which greatly broadens the composition design space of metal materials. TiZrNb multi-principal alloy is a typical refractory multi-principal alloy system. This type of alloy is composed of different proportions of Ti, Zr, Nb and Hf, Ta, Al and other additive elements. There are many types of elements, high melting points and large differences (Nb melting point 2477℃, Ti melting point 1668℃), which leads to problems such as composition segregation, coarse and uneven organization in alloy smelting, which seriously restricts the preparation and production of alloys.
常用的电弧熔炼技术制备难熔多主元合金，存在单次制备量小、熔体温度梯度大等问题。冷坩埚悬浮熔炼技术能够进行几公斤级制备，具有洁净、化学成分均匀等优势。中国专利申请CN115558814A公开了一种多元、高活、难熔高熵合金的冷坩埚感应熔炼方法，能够制备成分准确、无明显偏析的含能高熵合金。然而，由于合金熔体体积较大，凝固时间长，且熔体与坩埚冷壁接触，不同位置冷速差异大，导致合金初始组织粗大且晶粒尺寸分布不均匀，铸态力学性能恶化。The commonly used arc melting technology for preparing refractory multi-principal alloys has problems such as small single preparation amount and large melt temperature gradient. The cold crucible suspension melting technology can be used for preparation of several kilograms, and has the advantages of cleanliness and uniform chemical composition. Chinese patent application CN115558814A discloses a cold crucible induction melting method for multi-element, high-activity, refractory high-entropy alloys, which can prepare energetic high-entropy alloys with accurate composition and no obvious segregation. However, due to the large volume of the alloy melt, the long solidification time, and the contact between the melt and the cold wall of the crucible, the cooling rate at different positions varies greatly, resulting in a coarse initial structure of the alloy and an uneven grain size distribution, and deterioration of the cast mechanical properties.
发明内容Summary of the invention
有鉴于此，本发明的目的在于提供一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法。采用双线圈悬浮冷坩埚熔炼技术进行合金化熔炼，然后先将熔体温度降低至液相线与固相线之间，以此为基准将温度再升高至略高于液相线，随后先瞬时降低主感应线圈功率，待顶部熔体温度适当降低后再瞬时降低坩埚底部感应线圈功率，使合金整体在低过热度下快速凝固，避免了晶粒的过度生长，获得了细小的初始组织。所述方法可有效减少坩埚内熔体不同位置的温度差异，获得组织均匀、成分准确，无明显偏析的多主元合金，同时减小了合金凝固前的过热度，缩短合金熔体凝固时间，有效降低铸锭的晶粒尺寸，改善铸态合金的力学性能。In view of this, the object of the present invention is to provide a method for preparing a TiZrNb-based refractory multi-principal alloy with uniform equiaxed fine-grained structure. The alloying smelting is carried out by using a double-coil suspended cold crucible smelting technology, and then the melt temperature is first reduced to between the liquidus and the solidus, and the temperature is then raised to slightly above the liquidus based on this. Then, the power of the main induction coil is first reduced instantaneously, and after the top melt temperature is appropriately reduced, the power of the induction coil at the bottom of the crucible is reduced instantaneously, so that the alloy as a whole is rapidly solidified at a low superheat, avoiding excessive growth of grains, and obtaining a fine initial structure. The method can effectively reduce the temperature difference of the melt at different positions in the crucible, obtain a multi-principal alloy with uniform structure, accurate composition, and no obvious segregation, and at the same time reduce the superheat before the alloy solidifies, shorten the solidification time of the alloy melt, effectively reduce the grain size of the ingot, and improve the mechanical properties of the cast alloy.
为实现上述目的，本发明的技术方案如下。To achieve the above objectives, the technical solution of the present invention is as follows.
一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法，方法步骤包括：A method for preparing a TiZrNb-based refractory multi-principal alloy having a uniform equiaxed fine-grained structure, the method comprising the following steps:
（1）将TiZrNb系难熔多主元合金原料置于真空悬浮熔炼炉的水冷铜坩埚内；对真空悬浮熔炼炉进行抽真空，并充入保护气体；(1) placing TiZrNb-based refractory multi-principal alloy raw materials in a water-cooled copper crucible of a vacuum suspension melting furnace; evacuating the vacuum suspension melting furnace and filling it with protective gas;
（2）先启动主感应线圈逐级提高功率并维持，然后启动坩埚底部感应线圈逐级提高功率并维持，进行合金化熔炼；(2) First, start the main induction coil and gradually increase the power and maintain it, then start the induction coil at the bottom of the crucible and gradually increase the power and maintain it to perform alloying smelting;
（3）待合金熔化后，降低主感应线圈和坩埚底部感应线圈的功率，使熔体温度降低至液相线与固相线之间，熔体处于半凝固状态，稳定1~2min；(3) After the alloy is melted, reduce the power of the main induction coil and the induction coil at the bottom of the crucible to reduce the melt temperature to between the liquidus and solidus. The melt is in a semi-solidified state and stabilizes for 1 to 2 minutes.
（4）提高主感应线圈和坩埚底部感应线圈的功率，使合金熔体温度达到液相线，熔体重新液化后，将主感应线圈和坩埚底部感应线圈的功率分别提高5~10kW，稳定1~2min；(4) Increase the power of the main induction coil and the induction coil at the bottom of the crucible to make the alloy melt temperature reach the liquidus. After the melt is re-liquefied, increase the power of the main induction coil and the induction coil at the bottom of the crucible by 5-10 kW respectively and stabilize for 1-2 minutes;
（5）5秒内关闭主感应线圈功率，保持坩埚底部感应线圈功率，待熔体上部凝固后，5秒内关闭坩埚底部感应线圈功率，冷却；(5) Turn off the power of the main induction coil within 5 seconds, maintain the power of the induction coil at the bottom of the crucible, and after the upper part of the melt solidifies, turn off the power of the induction coil at the bottom of the crucible within 5 seconds and cool it down;
（6）重复步骤（2）至（5），进行反复熔炼三次以上，熔炼结束后得到一种TiZrNb系难熔多主元合金铸锭；(6) Repeating steps (2) to (5) for repeated smelting three or more times, and obtaining a TiZrNb-based refractory multi-principal alloy ingot after the smelting is completed;
其中，所述TiZrNb系难熔多主元合金的化学式为TiaZrbNbcMxNy，M为Al、Cr、Mn、Fe、Cu、Ni、Mo、W中的一种以上，N为B、C、N、O、Si中的一种以上，10≤a≤60，5≤b≤60，15≤c≤75，0≤x≤10，0≤y≤5，且a+b+c+x+y=100。The chemical formula of the TiZrNb-based refractory multi-principal alloy is Ti a Zr b Nb c M x N y , where M is one or more of Al, Cr, Mn, Fe, Cu, Ni, Mo, and W, N is one or more of B, C, N, O, and Si, 10≤a≤60, 5≤b≤60, 15≤c≤75, 0≤x≤10, 0≤y≤5, and a+b+c+x+y=100.
优选的，15≤a≤30，5≤b≤60，15≤c≤75，0≤x≤10，0≤y≤5，且a+b+c+x+y=100。Preferably, 15≤a≤30, 5≤b≤60, 15≤c≤75, 0≤x≤10, 0≤y≤5, and a+b+c+x+y=100.
优选的，步骤（1）中，所述保护气体为惰性气体。Preferably, in step (1), the protective gas is an inert gas.
优选的，步骤（2）中，启动主感应线圈功率至100~120kW，稳定2~3min，提高至180~200kW，稳定2~3min，提高至300~400kW，稳定加热功率3~5min；启动坩埚底部感应线圈至20~30kW，稳定2~3min，提高至40~50kW，稳定2~3min，提高至70~80kW，稳定1~2min。Preferably, in step (2), the power of the main induction coil is started to 100-120 kW, stabilized for 2-3 min, increased to 180-200 kW, stabilized for 2-3 min, increased to 300-400 kW, and the heating power is stabilized for 3-5 min; the induction coil at the bottom of the crucible is started to 20-30 kW, stabilized for 2-3 min, increased to 40-50 kW, stabilized for 2-3 min, increased to 70-80 kW, and stabilized for 1-2 min.
优选的，步骤（3）中，将主感应线圈功率降低至200~250kW，将坩埚底部感应线圈功率降低至50~60kW。Preferably, in step (3), the power of the main induction coil is reduced to 200-250 kW, and the power of the induction coil at the bottom of the crucible is reduced to 50-60 kW.
优选的，步骤（4）中，将主感应线圈功率提高至250~300kW，将坩埚底部感应线圈功率提高至80~100kW。Preferably, in step (4), the power of the main induction coil is increased to 250-300 kW, and the power of the induction coil at the bottom of the crucible is increased to 80-100 kW.
优选的，步骤（6）中，重复（2）至（5）时，启动主感应线圈功率至100~120kW，稳定1~2min；提高至300~400kW，稳定3~5min；启动坩埚底部感应线圈功率至70~80kW，稳定1~2min；待合金熔化后，将主感应线圈功率降低至200~250kW，将坩埚底部感应线圈功率降低至50~60kW，使熔体处于半凝固状态，稳定1~2min；将主感应线圈功率提高至250~300kW，将坩埚底部感应线圈功率提高至80~90kW，熔体重新液化后，将主感应线圈和坩埚底部感应线圈的功率分别提高5~10kW，稳定1~2min；5秒内关闭主感应线圈功率，保持坩埚底部感应线圈功率，待熔体上部凝固后，5秒内关闭坩埚底部感应线圈功率，冷却。Preferably, in step (6), when (2) to (5) are repeated, the power of the main induction coil is started to 100-120 kW and stabilized for 1-2 min; the power is increased to 300-400 kW and stabilized for 3-5 min; the power of the induction coil at the bottom of the crucible is started to 70-80 kW and stabilized for 1-2 min; after the alloy is melted, the power of the main induction coil is reduced to 200-250 kW, and the power of the induction coil at the bottom of the crucible is reduced to 50-60 kW, so that the melt is in a semi-solidified state, and stabilized for 1-2 min; the power of the main induction coil is increased to 250-300 kW, and the power of the induction coil at the bottom of the crucible is increased to 80-90 kW. After the melt is liquefied again, the power of the main induction coil and the power of the induction coil at the bottom of the crucible are respectively increased by 5-10 kW and stabilized for 1-2 min; the power of the main induction coil is turned off within 5 seconds, and the power of the induction coil at the bottom of the crucible is maintained. After the upper part of the melt solidifies, the power of the induction coil at the bottom of the crucible is turned off within 5 seconds, and the melt is cooled.
优选的，步骤（6）中，最后一次熔炼时，仅重复步骤（2）。Preferably, in step (6), during the last smelting, only step (2) is repeated.
优选的，步骤（6）中，反复熔炼三次到四次。Preferably, in step (6), smelting is repeated three to four times.
一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金，通过以上方法制备得到。A TiZrNb-based refractory multi-principal alloy with uniform equiaxed fine-grained structure is prepared by the above method.
有益效果Beneficial Effects
本发明提供了一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法，通过对两组感应线圈的功率进行匹配控制，有效缩短了合金熔体的凝固时间，并降低了坩埚内不同位置的温度差异，获得了组织均匀、晶粒细小、且成分准确无偏析的TiZrNb系难熔多主元合金锭，有效提高了铸态合金的力学性能，而且该方法工艺简单，操作安全性高，可实现大容量难熔多主元合金熔炼，生产效率高，适用于工业化生产。The present invention provides a method for preparing a TiZrNb-based refractory multi-principal component alloy with a uniform equiaxed fine-grained structure. By matching and controlling the power of two groups of induction coils, the solidification time of the alloy melt is effectively shortened, and the temperature difference at different positions in the crucible is reduced, so that a TiZrNb-based refractory multi-principal component alloy ingot with uniform structure, fine grains, accurate composition and no segregation is obtained, and the mechanical properties of the cast alloy are effectively improved. Moreover, the method has a simple process and high operational safety, can realize large-capacity refractory multi-principal component alloy smelting, has high production efficiency, and is suitable for industrial production.
本发明提供了一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法，先启动主感应线圈逐级提高功率并维持，然后启动坩埚底部感应线圈逐级提高功率并维持，使熔体下部完全脱离坩埚壁，避免熔体底部热量快速流失，使整个熔体温度场分布更加均匀。进一步，合金熔化后通过将主感应线圈和坩埚底部感应线圈降低，使熔体温度降低至液相线与固相线之间，并以此作为基准调控最终凝固前的过热度。并通过再次提高主感应线圈和坩埚底部感应线圈的功率，使熔体温度略高于液相线，保证熔体凝固前的过热度尽量低，且温度场均匀，有利于大量晶核在熔体中均匀产生，同时缩短熔体凝固时间，形成细小、均匀、等轴的铸态组织。最后，先瞬时降低主感应线圈功率，经过一定时间间隔后再瞬时降低坩埚底部感应线圈功率，避免了底部熔体与坩埚壁接触后快速冷却，保证了铸锭从顶部到底部的组织均一性。The present invention provides a preparation method of a TiZrNb-based refractory multi-principal alloy with uniform equiaxed fine-grained structure, first starting the main induction coil to increase the power step by step and maintain it, and then starting the induction coil at the bottom of the crucible to increase the power step by step and maintain it, so that the lower part of the melt is completely separated from the crucible wall, avoiding the rapid loss of heat at the bottom of the melt, and making the temperature field distribution of the entire melt more uniform. Further, after the alloy is melted, the main induction coil and the induction coil at the bottom of the crucible are lowered to reduce the melt temperature to between the liquidus and the solidus, and this is used as a reference to regulate the superheat before the final solidification. And by increasing the power of the main induction coil and the induction coil at the bottom of the crucible again, the melt temperature is slightly higher than the liquidus, ensuring that the superheat before the melt solidifies is as low as possible, and the temperature field is uniform, which is conducive to the uniform generation of a large number of crystal nuclei in the melt, while shortening the melt solidification time, forming a fine, uniform, equiaxed cast structure. Finally, the power of the main induction coil is first reduced instantaneously, and then the power of the induction coil at the bottom of the crucible is reduced instantaneously after a certain time interval, which avoids the rapid cooling of the bottom melt after contacting the crucible wall and ensures the uniformity of the structure of the ingot from top to bottom.
本发明提供了一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金，所述难熔多主元合金的成分均匀，为等轴组织且无树枝晶，铸锭不同位置组织均匀，晶粒细小，性能优异且一致性好。The present invention provides a TiZrNb-based refractory multi-principal alloy with uniform equiaxed fine-grained structure. The refractory multi-principal alloy has uniform composition, an equiaxed structure and no dendrites, uniform structure at different positions of the ingot, fine grains, excellent performance and good consistency.
具体实施方式Detailed ways
下面结合具体实施例对本发明作进一步详细的说明。The present invention is further described in detail below in conjunction with specific embodiments.
实施例1Example 1
一种具有均匀等轴细晶组织的Ti24Zr46Nb28Al2难熔多主元合金的制备方法，方法步骤包括：A method for preparing a Ti 24 Zr 46 Nb 28 Al 2 refractory multi-principal alloy having a uniform equiaxed fine-grained structure, the method comprising the following steps:
（1）按照原子百分比Ti:Zr:Nb:Al=24:46:28:2称量出总质量为(1500±0.1)g的原料，将洁净处理的单质元素Ti、Zr、Nb、Al均匀的放置于熔炼坩埚中，其中，低熔点的单质金属放于坩埚底部，熔点最高的单质金属置于坩埚中部区域，其余单质元素均匀的放置于坩埚中；(1) Weigh out a total mass of (1500±0.1) g of raw materials according to the atomic percentage of Ti:Zr:Nb:Al=24:46:28:2, and evenly place the cleaned single elements Ti, Zr, Nb, and Al in a melting crucible, wherein the single element metal with a low melting point is placed at the bottom of the crucible, the single element metal with the highest melting point is placed in the middle area of the crucible, and the remaining single elements are evenly placed in the crucible;
（2）对真空悬浮冷坩埚熔炼炉进行抽真空，待炉体内真空度达到高真空标准后，充入高纯氩气作为保护气体。采用感应熔炼炉进行合金化熔炼，熔炼时保护气体为氩气。熔炼室的真空度≤1×10-2Pa。(2) Evacuate the vacuum suspension cold crucible melting furnace, and after the vacuum degree in the furnace reaches the high vacuum standard, fill it with high-purity argon as the protective gas. Use an induction melting furnace for alloying smelting, and the protective gas during smelting is argon. The vacuum degree of the melting chamber is ≤1×10 -2 Pa.
（3）启动主感应线圈进行合金化熔炼，逐级提高功率，首先将加热功率加到120kW，稳定3min；其次提高加热功率至200Kw，稳定3min；最后提高加热功率至400kW，稳定加热功率5min。(3) Start the main induction coil for alloying smelting and increase the power step by step. First, increase the heating power to 120 kW and stabilize it for 3 minutes; then increase the heating power to 200 kW and stabilize it for 3 minutes; finally, increase the heating power to 400 kW and stabilize it for 5 minutes.
（4）启动坩埚底部感应线圈，逐级提高功率，首先将加热功率加到30kW，稳定3min；然后提高加热功率至50kW，稳定3min；最后提高加热功率至80kW，稳定2min，且合金熔体完全脱离坩埚壁。(4) Start the induction coil at the bottom of the crucible and increase the power step by step. First, increase the heating power to 30 kW and stabilize it for 3 minutes; then increase the heating power to 50 kW and stabilize it for 3 minutes; finally, increase the heating power to 80 kW and stabilize it for 2 minutes, and the alloy melt completely detaches from the crucible wall.
（5）待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体温度降低至液相线以下，熔体处于半凝固状态，稳定2min。(5) After the alloy is melted, reduce the power of the main induction coil to 250 kW and the power of the induction coil at the bottom of the crucible to 70 kW, so that the melt temperature drops below the liquidus line and the melt is in a semi-solidified state and stabilizes for 2 minutes.
（6）将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到100kW，使熔体温度达到液相线，熔体重新液化后，将加热功率再提升10kW，稳定2min。(6) Increase the power of the main induction coil to 300 kW and the power of the induction coil at the bottom of the crucible to 100 kW, so that the melt temperature reaches the liquidus. After the melt is reliquefied, increase the heating power by another 10 kW and stabilize for 2 minutes.
（7）先三秒内将主感应线圈功率降低至最低，待熔体上部凝固后，再三秒内将坩埚底部感应线圈功率降低至最低，随后关闭加热电源，得到冷却至室温的合金铸锭。(7) First, reduce the power of the main induction coil to the minimum within three seconds. After the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within another three seconds. Then, turn off the heating power to obtain an alloy ingot that is cooled to room temperature.
（8）重新对铸锭进行加热熔炼。首先将主感应线圈加热功率加到120kW，稳定2min；然后提高加热功率至400kW，稳定5min；启动坩埚底部感应线圈，加热功率加到80kW，稳定2min；待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后再增加10kW加热功率；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源。反复熔炼4次，得到一种Ti24Zr46Nb28Al2难熔多主元合金。(8) Reheat and melt the ingot. First, increase the heating power of the main induction coil to 120kW and stabilize for 2 minutes; then increase the heating power to 400kW and stabilize for 5 minutes; start the induction coil at the bottom of the crucible, increase the heating power to 80kW and stabilize for 2 minutes; after the alloy is melted, reduce the power of the main induction coil to 250kW and the power of the induction coil at the bottom of the crucible to 70kW to make the melt semi-solidified; increase the power of the main induction coil to 300kW and the power of the induction coil at the bottom of the crucible to 90kW, and increase the heating power by 10kW after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power. Repeat the melting four times to obtain a Ti 24 Zr 46 Nb 28 Al 2 refractory multi-principal alloy.
顶部和底部分别取样后进行形貌表征，Ti24Zr46Nb28Al2难熔多主元合金的成分均匀、准确，以等轴组织为主，组织均匀，晶粒细小，力学性能优异。具体地，顶部晶粒尺寸为345μm，底部晶粒尺寸为295μm。The top and bottom samples were taken for morphological characterization. The Ti 24 Zr 46 Nb 28 Al 2 refractory multi-principal alloy has uniform and accurate composition, mainly equiaxed structure, uniform structure, fine grains and excellent mechanical properties. Specifically, the top grain size is 345μm and the bottom grain size is 295μm.
实施例2Example 2
一种具有均匀等轴细晶组织的Ti24Zr58Nb18难熔多主元合金的制备方法，方法步骤包括：A method for preparing a Ti 24 Zr 58 Nb 18 refractory multi-principal alloy having a uniform equiaxed fine-grained structure, the method comprising the following steps:
（1）按照原子百分比Ti:Zr:Nb =24:58:18称量出总质量为(1500±0.1)g的原料，将洁净处理的单质元素Ti、Zr、Nb均匀的放置于熔炼坩埚中，其中，低熔点的单质金属放于坩埚底部，熔点最高的单质金属置于坩埚中部区域；(1) Weigh out a total mass of (1500±0.1) g of raw materials according to the atomic percentage of Ti:Zr:Nb =24:58:18, and evenly place the cleaned single elements Ti, Zr, and Nb in a melting crucible, wherein the single element metal with a low melting point is placed at the bottom of the crucible, and the single element metal with the highest melting point is placed in the middle area of the crucible;
（2）对真空悬浮冷坩埚熔炼炉进行抽真空，待炉体内真空度达到高真空标准后，充入高纯氩气作为保护气体。采用感应熔炼炉进行合金化熔炼，熔炼时保护气体为氩气。熔炼室的真空度≤1×10-2Pa。(2) Evacuate the vacuum suspension cold crucible melting furnace, and after the vacuum degree in the furnace reaches the high vacuum standard, fill it with high-purity argon as the protective gas. Use an induction melting furnace for alloying smelting, and the protective gas during smelting is argon. The vacuum degree of the melting chamber is ≤1×10 -2 Pa.
（3）启动主感应线圈进行合金化熔炼，逐级提高功率，首先将加热功率加到100kW，稳定3min；其次提高加热功率至180Kw，稳定3min；最后提高加热功率至400kW，稳定加热功率5min。(3) Start the main induction coil for alloying smelting and increase the power step by step. First, increase the heating power to 100 kW and stabilize it for 3 minutes; secondly, increase the heating power to 180 kW and stabilize it for 3 minutes; finally, increase the heating power to 400 kW and stabilize it for 5 minutes.
（4）启动坩埚底部感应线圈，逐级提高功率，首先将加热功率加到20kW，稳定3min；然后提高加热功率至40kW，稳定3min；最后提高加热功率至70kW，稳定2min，且合金熔体完全脱离坩埚壁。(4) Start the induction coil at the bottom of the crucible and increase the power step by step. First, increase the heating power to 20 kW and stabilize it for 3 minutes; then increase the heating power to 40 kW and stabilize it for 3 minutes; finally, increase the heating power to 70 kW and stabilize it for 2 minutes, and the alloy melt completely detaches from the crucible wall.
（5）待合金熔化后，将主感应线圈功率降低至200kW，将坩埚底部感应线圈功率降低至50kW，使熔体温度降低至液相线以下，熔体处于半凝固状态，稳定2min。(5) After the alloy is melted, reduce the power of the main induction coil to 200 kW and the power of the induction coil at the bottom of the crucible to 50 kW, so that the melt temperature drops below the liquidus line and the melt is in a semi-solidified state and stabilizes for 2 minutes.
（6）将主感应线圈功率加到250kW，将坩埚底部感应线圈功率加到80kW，使熔体温度达到液相线，熔体重新液化后，将加热功率再提升5kW，稳定2min。(6) Increase the power of the main induction coil to 250 kW and the power of the induction coil at the bottom of the crucible to 80 kW so that the melt temperature reaches the liquidus. After the melt is reliquefied, increase the heating power by another 5 kW and stabilize for 2 minutes.
（7）先三秒内将主感应线圈功率降低至最低，待熔体上部凝固后，再三秒内将坩埚底部感应线圈功率降低至最低，随后关闭加热电源，得到冷却至室温的合金铸锭。(7) First, reduce the power of the main induction coil to the minimum within three seconds. After the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within another three seconds. Then, turn off the heating power to obtain an alloy ingot that is cooled to room temperature.
（8）重新对铸锭进行加热熔炼。首先将主感应线圈加热功率加到100kW，稳定2min；然后提高加热功率至300kW，稳定5min；启动坩埚底部感应线圈，加热功率加到70kW，稳定2min；待合金熔化后，将主感应线圈功率降低至200kW，将坩埚底部感应线圈功率降低至50kW，使熔体处于半凝固状态稳定1min；将主感应线圈功率加到250kW，将坩埚底部感应线圈功率加到80kW，使熔体温度达到液相线后再增加5kW加热功率，稳定1min；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源。反复熔炼4次，得到一种Ti24Zr58Nb18难熔多主元合金。(8) Reheat and melt the ingot. First, increase the heating power of the main induction coil to 100kW and stabilize for 2 minutes; then increase the heating power to 300kW and stabilize for 5 minutes; start the induction coil at the bottom of the crucible, increase the heating power to 70kW and stabilize for 2 minutes; after the alloy is melted, reduce the power of the main induction coil to 200kW and the power of the induction coil at the bottom of the crucible to 50kW, so that the melt is in a semi-solidified state and stabilize for 1 minute; increase the power of the main induction coil to 250kW and the power of the induction coil at the bottom of the crucible to 80kW, and increase the heating power by 5kW after the melt temperature reaches the liquidus line, and stabilize for 1 minute; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power. Repeat the melting four times to obtain a Ti 24 Zr 58 Nb 18 refractory multi-principal alloy.
顶部和底部分别取样后进行形貌表征，Ti24Zr58Nb18难熔多主元合金的成分均匀、准确，以等轴组织为主，组织均匀，晶粒细小，力学性能优异。具体地，顶部晶粒尺寸为334μm，底部晶粒尺寸为282μm。The top and bottom samples were taken for morphological characterization. The Ti 24 Zr 58 Nb 18 refractory multi-principal alloy has uniform and accurate composition, mainly equiaxed structure, uniform structure, fine grains and excellent mechanical properties. Specifically, the top grain size is 334μm and the bottom grain size is 282μm.
实施例3Example 3
一种具有均匀等轴细晶组织的Ti24Zr46Nb28O2难熔多主元合金的制备方法，方法步骤包括：A method for preparing a Ti 24 Zr 46 Nb 28 O 2 refractory multi-principal alloy having a uniform equiaxed fine-grained structure, the method comprising the following steps:
（1）按照原子百分比Ti:Zr:Nb:O=24:46:28:2称量出总质量为(1500±0.1)g的原料，将洁净处理的单质元素Ti、Zr、Nb、O均匀的放置于熔炼坩埚中，其中，低熔点的单质金属放于坩埚底部，熔点最高的单质金属置于坩埚中部区域，其余单质元素均匀的放置于坩埚中；(1) Weigh out a raw material with a total mass of (1500±0.1) g according to the atomic percentage of Ti:Zr:Nb:O=24:46:28:2, and evenly place the cleaned single elements Ti, Zr, Nb, and O in a melting crucible, wherein the single metal with a low melting point is placed at the bottom of the crucible, the single metal with the highest melting point is placed in the middle area of the crucible, and the remaining single elements are evenly placed in the crucible;
（2）对真空悬浮冷坩埚熔炼炉进行抽真空，待炉体内真空度达到高真空标准后，充入高纯氩气作为保护气体。采用感应熔炼炉进行合金化熔炼，熔炼时保护气体为氩气。熔炼室的真空度≤1×10-2Pa。(2) Evacuate the vacuum suspension cold crucible melting furnace, and after the vacuum degree in the furnace reaches the high vacuum standard, fill it with high-purity argon as the protective gas. Use an induction melting furnace for alloying smelting, and the protective gas during smelting is argon. The vacuum degree of the melting chamber is ≤1×10 -2 Pa.
（3）启动主感应线圈进行合金化熔炼，逐级提高功率，首先将加热功率加到120kW，稳定2min；其次提高加热功率至200Kw，稳定2min；最后提高加热功率至400kW，稳定加热功率3min。(3) Start the main induction coil for alloying smelting and increase the power step by step. First, increase the heating power to 120 kW and stabilize it for 2 minutes; then increase the heating power to 200 kW and stabilize it for 2 minutes; finally, increase the heating power to 400 kW and stabilize it for 3 minutes.
（4）启动坩埚底部感应线圈，逐级提高功率，首先将加热功率加到30kW，稳定2min；然后提高加热功率至50kW，稳定2min；最后提高加热功率至80kW，稳定1min，且合金熔体完全脱离坩埚壁。(4) Start the induction coil at the bottom of the crucible and increase the power step by step. First, increase the heating power to 30 kW and stabilize it for 2 minutes; then increase the heating power to 50 kW and stabilize it for 2 minutes; finally, increase the heating power to 80 kW and stabilize it for 1 minute, and the alloy melt is completely separated from the crucible wall.
（5）待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体温度降低至液相线以下，熔体处于半凝固状态维持1min。(5) After the alloy is melted, reduce the power of the main induction coil to 250 kW and the power of the induction coil at the bottom of the crucible to 70 kW, so that the melt temperature drops below the liquidus line and the melt is kept in a semi-solidified state for 1 min.
（6）将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到100kW，使熔体温度达到液相线，熔体重新液化后，将加热功率再提升10kW，维持1min。(6) Increase the power of the main induction coil to 300 kW and the power of the induction coil at the bottom of the crucible to 100 kW, so that the melt temperature reaches the liquidus. After the melt is reliquefied, increase the heating power by another 10 kW and maintain it for 1 min.
（7）先三秒内将主感应线圈功率降低至最低，待熔体上部凝固后，再三秒内将坩埚底部感应线圈功率降低至最低，随后关闭加热电源，得到冷却至室温的合金铸锭。(7) First, reduce the power of the main induction coil to the minimum within three seconds. After the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within another three seconds. Then, turn off the heating power to obtain an alloy ingot that is cooled to room temperature.
（8）重新对铸锭进行加热熔炼。首先将主感应线圈加热功率加到120kW，稳定1min；然后提高加热功率至400kW，稳定3min；启动坩埚底部感应线圈，加热功率加到80kW，稳定1min；待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态，维持1min；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后再增加10kW加热功率；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源。反复熔炼4次，得到一种Ti24Zr46Nb28O2难熔多主元合金。(8) Reheat and melt the ingot. First, increase the heating power of the main induction coil to 120kW and stabilize for 1 minute; then increase the heating power to 400kW and stabilize for 3 minutes; start the induction coil at the bottom of the crucible, increase the heating power to 80kW and stabilize for 1 minute; after the alloy is melted, reduce the power of the main induction coil to 250kW and the power of the induction coil at the bottom of the crucible to 70kW, so that the melt is in a semi-solidified state and maintain for 1 minute; increase the power of the main induction coil to 300kW and the power of the induction coil at the bottom of the crucible to 90kW, and increase the heating power by 10kW after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power. Repeat the melting four times to obtain a Ti 24 Zr 46 Nb 28 O 2 refractory multi-principal alloy.
顶部和底部分别取样后进行形貌表征，Ti24Zr46Nb28O2难熔多主元合金的成分均匀、准确，以等轴组织为主，组织均匀，晶粒细小，力学性能优异。具体地，顶部晶粒尺寸为352μm，底部晶粒尺寸为298μm。实施例4The top and bottom were sampled and characterized for morphology. The Ti 24 Zr 46 Nb 28 O 2 refractory multi-principal alloy had uniform and accurate composition, mainly equiaxed structure, uniform structure, fine grains, and excellent mechanical properties. Specifically, the top grain size was 352 μm, and the bottom grain size was 298 μm. Example 4
一种具有均匀等轴细晶组织的Ti30Zr55Nb15难熔多主元合金的制备方法，方法步骤包括：A method for preparing a Ti 30 Zr 55 Nb 15 refractory multi-principal alloy having a uniform equiaxed fine-grained structure, the method comprising the following steps:
（1）按照原子百分比Ti:Zr:Nb=30:55:15称量出总质量为(1500±0.1)g的原料，将洁净处理的单质元素Ti、Zr、Nb、Al均匀的放置于熔炼坩埚中，其中，低熔点的单质金属放于坩埚底部，熔点最高的单质金属置于坩埚中部区域，其余单质元素均匀的放置于坩埚中；(1) Weigh out a total mass of (1500±0.1) g of raw materials according to the atomic percentage of Ti:Zr:Nb=30:55:15, and evenly place the cleaned single elements Ti, Zr, Nb, and Al in a melting crucible, wherein the single element metal with a low melting point is placed at the bottom of the crucible, the single element metal with the highest melting point is placed in the middle area of the crucible, and the remaining single elements are evenly placed in the crucible;
（2）对真空悬浮冷坩埚熔炼炉进行抽真空，待炉体内真空度达到高真空标准后，充入高纯氩气作为保护气体。采用感应熔炼炉进行合金化熔炼，熔炼时保护气体为氩气。熔炼室的真空度≤1×10-2Pa。(2) Evacuate the vacuum suspension cold crucible melting furnace, and after the vacuum degree in the furnace reaches the high vacuum standard, fill it with high-purity argon as the protective gas. Use an induction melting furnace for alloying smelting, and the protective gas during smelting is argon. The vacuum degree of the melting chamber is ≤1×10 -2 Pa.
（3）启动主感应线圈进行合金化熔炼，逐级提高功率，首先将加热功率加到100kW，稳定2min；其次提高加热功率至180Kw，稳定2min；最后提高加热功率至300kW，稳定加热功率3min。(3) Start the main induction coil for alloying smelting and increase the power step by step. First, increase the heating power to 100 kW and stabilize it for 2 minutes; secondly, increase the heating power to 180 kW and stabilize it for 2 minutes; finally, increase the heating power to 300 kW and stabilize it for 3 minutes.
（4）启动坩埚底部感应线圈，逐级提高功率，首先将加热功率加到20kW，稳定2min；然后提高加热功率至40kW，稳定2min；最后提高加热功率至70kW，稳定1min，且合金熔体完全脱离坩埚壁。(4) Start the induction coil at the bottom of the crucible and increase the power step by step. First, increase the heating power to 20 kW and stabilize it for 2 minutes; then increase the heating power to 40 kW and stabilize it for 2 minutes; finally, increase the heating power to 70 kW and stabilize it for 1 minute, and the alloy melt completely detaches from the crucible wall.
（5）待合金熔化后，将主感应线圈功率降低至200kW，将坩埚底部感应线圈功率降低至50kW，使熔体温度降低至液相线以下，熔体处于半凝固状态，维持1min。(5) After the alloy is melted, reduce the power of the main induction coil to 200 kW and the power of the induction coil at the bottom of the crucible to 50 kW, so that the melt temperature drops below the liquidus line and the melt is in a semi-solidified state for 1 min.
（6）将主感应线圈功率加到250kW，将坩埚底部感应线圈功率加到80kW，使熔体温度达到液相线，熔体重新液化后，将加热功率再提升5kW，维持1min。(6) Increase the power of the main induction coil to 250 kW and the power of the induction coil at the bottom of the crucible to 80 kW so that the melt temperature reaches the liquidus. After the melt is reliquefied, increase the heating power by another 5 kW and maintain for 1 min.
（7）先三秒内将主感应线圈功率降低至最低，待熔体上部凝固后，再三秒内将坩埚底部感应线圈功率降低至最低，随后关闭加热电源，得到冷却至室温的合金铸锭。(7) First, reduce the power of the main induction coil to the minimum within three seconds. After the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within another three seconds. Then, turn off the heating power to obtain an alloy ingot that is cooled to room temperature.
（8）重新对铸锭进行加热熔炼。首先将主感应线圈加热功率加到100kW，稳定1min；然后提高加热功率至300kW，稳定3min；启动坩埚底部感应线圈，加热功率加到70kW，稳定1min；待合金熔化后，将主感应线圈功率降低至200kW，将坩埚底部感应线圈功率降低至50kW，使熔体处于半凝固状态；将主感应线圈功率加到250kW，将坩埚底部感应线圈功率加到80kW，使熔体温度达到液相线后再增加5kW加热功率；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源。反复熔炼4次，得到一种Ti30Zr55Nb15难熔多主元合金。(8) Reheat and melt the ingot. First, increase the heating power of the main induction coil to 100kW and stabilize for 1 minute; then increase the heating power to 300kW and stabilize for 3 minutes; start the induction coil at the bottom of the crucible, increase the heating power to 70kW and stabilize for 1 minute; after the alloy is melted, reduce the power of the main induction coil to 200kW and the power of the induction coil at the bottom of the crucible to 50kW to make the melt semi-solidified; increase the power of the main induction coil to 250kW and the power of the induction coil at the bottom of the crucible to 80kW, and increase the heating power by 5kW after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power. Repeat the melting four times to obtain a Ti 30 Zr 55 Nb 15 refractory multi-principal alloy.
顶部和底部分别取样后进行形貌表征，Ti30Zr55Nb15难熔多主元合金的成分均匀、准确，以等轴组织为主，组织均匀，晶粒细小，力学性能优异。具体地，顶部晶粒尺寸为363μm，底部晶粒尺寸为311μm。The top and bottom samples were taken for morphological characterization. The Ti 30 Zr 55 Nb 15 refractory multi-principal alloy has uniform and accurate composition, mainly equiaxed structure, uniform structure, fine grains and excellent mechanical properties. Specifically, the top grain size is 363μm and the bottom grain size is 311μm.
对比例1Comparative Example 1
在实施例1的基础上，将最后一次熔炼的工艺改为：首先将主感应线圈加热功率加到120kW，稳定2min；然后提高加热功率至400kW，稳定5min；启动坩埚底部感应线圈，加热功率加到80kW，稳定2min；待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后再增加30kW加热功率；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源，得到多主元合金铸锭。On the basis of Example 1, the process of the last smelting is changed to: first, the heating power of the main induction coil is increased to 120kW, and stabilized for 2 minutes; then the heating power is increased to 400kW, and stabilized for 5 minutes; the induction coil at the bottom of the crucible is started, and the heating power is increased to 80kW, and stabilized for 2 minutes; after the alloy is melted, the power of the main induction coil is reduced to 250kW, and the power of the induction coil at the bottom of the crucible is reduced to 70kW, so that the melt is in a semi-solidified state; the power of the main induction coil is increased to 300kW, and the power of the induction coil at the bottom of the crucible is increased to 90kW, and the heating power is increased by 30kW after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power to obtain a multi-principal alloy ingot.
经过形貌表征可知，合金呈等轴晶组织，晶粒尺寸粗大。具体地，顶部晶粒尺寸为534μm，底部晶粒尺寸为463μm。The morphological characterization shows that the alloy presents an equiaxed crystal structure with coarse grain size. Specifically, the top grain size is 534 μm and the bottom grain size is 463 μm.
对比例2Comparative Example 2
在实施例1的基础上，将最后一次熔炼的工艺改为：首先将主感应线圈加热功率加到120kW，稳定2min；然后提高加热功率至400kW，稳定5min；启动坩埚底部感应线圈，加热功率加到80kW，稳定2min；待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后维持加热功率不变；先三秒内降低主感应线圈功率至最低，待熔体上部凝固后，再三秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源，得到多主元合金铸锭。On the basis of Example 1, the process of the last smelting is changed to: first, the heating power of the main induction coil is increased to 120kW, and stabilized for 2 minutes; then the heating power is increased to 400kW, and stabilized for 5 minutes; the induction coil at the bottom of the crucible is started, and the heating power is increased to 80kW, and stabilized for 2 minutes; after the alloy is melted, the power of the main induction coil is reduced to 250kW, and the power of the induction coil at the bottom of the crucible is reduced to 70kW, so that the melt is in a semi-solidified state; the power of the main induction coil is increased to 300kW, and the power of the induction coil at the bottom of the crucible is increased to 90kW, so that the heating power is maintained unchanged after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within three seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within three seconds, and then turn off the heating power to obtain a multi-principal alloy ingot.
经过形貌表征可知，合金呈等轴晶组织，但由于坩埚底部悬浮力不够，熔体贴壁热量快速流失，导致铸锭底部晶粒尺寸明显小于铸锭顶部，组织不均匀。具体地，顶部晶粒尺寸为437μm，底部晶粒尺寸为280μm。The morphological characterization shows that the alloy presents an equiaxed crystal structure, but due to the insufficient suspension force at the bottom of the crucible, the heat of the melt adheres to the wall and is lost quickly, resulting in the grain size at the bottom of the ingot being significantly smaller than that at the top of the ingot, and the structure is uneven. Specifically, the grain size at the top is 437μm, and the grain size at the bottom is 280μm.
对比例3Comparative Example 3
在实施例1的基础上，将最后一次熔炼的工艺改为：首先将主感应线圈加热功率加到120kW，稳定2min；然后提高加热功率至400kW，稳定5min；启动坩埚底部感应线圈，加热功率加到80kW，稳定2min；待合金熔化后，将主感应线圈功率降低至200~250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后再增加10kW加热功率；三秒内同时降低主感应线圈和坩埚底部感应线圈功率至最低，待随后关闭加热电源，得到多主元合金铸锭。On the basis of Example 1, the process of the last smelting is changed to: first, the heating power of the main induction coil is increased to 120kW, and stabilized for 2 minutes; then the heating power is increased to 400kW, and stabilized for 5 minutes; the induction coil at the bottom of the crucible is started, and the heating power is increased to 80kW, and stabilized for 2 minutes; after the alloy is melted, the power of the main induction coil is reduced to 200-250kW, and the power of the induction coil at the bottom of the crucible is reduced to 70kW, so that the melt is in a semi-solidified state; the power of the main induction coil is increased to 300kW, and the power of the induction coil at the bottom of the crucible is increased to 90kW, and the heating power is increased by 10kW after the melt temperature reaches the liquidus; within three seconds, the power of the main induction coil and the induction coil at the bottom of the crucible are simultaneously reduced to the minimum, and then the heating power is turned off to obtain a multi-principal alloy ingot.
经过形貌表征可知，合金呈等轴晶组织，但由于坩埚底部熔体贴壁面积大，热量流失更快，导致铸锭底部晶粒尺寸明显小于铸锭顶部，组织不均匀。具体地，顶部晶粒尺寸为496μm，底部晶粒尺寸为350μm。The morphological characterization shows that the alloy presents an equiaxed crystal structure, but due to the large area of the melt adhering to the wall at the bottom of the crucible, the heat loss is faster, resulting in the grain size at the bottom of the ingot being significantly smaller than that at the top of the ingot, and the structure is uneven. Specifically, the grain size at the top is 496μm, and the grain size at the bottom is 350μm.
对比例4Comparative Example 4
在实施例1的基础上，对实施例1中最后一次熔炼的工艺改为：首先将主感应线圈加热功率加到120kW，稳定2min；然后提高加热功率至400kW，稳定5min；启动坩埚底部感应线圈，加热功率加到80kW，稳定2min；待合金熔化后，将主感应线圈功率降低至250kW，将坩埚底部感应线圈功率降低至70kW，使熔体处于半凝固状态；将主感应线圈功率加到300kW，将坩埚底部感应线圈功率加到90kW，使熔体温度达到液相线后再增加10kW加热功率；先十五秒内降低主感应线圈功率至最低，待熔体上部凝固后，再十五秒内降低坩埚底部感应线圈功率至最低，随后关闭加热电源，得到多主元合金铸锭。On the basis of Example 1, the process of the last smelting in Example 1 is changed to: first, the heating power of the main induction coil is increased to 120kW, and stabilized for 2 minutes; then the heating power is increased to 400kW, and stabilized for 5 minutes; the induction coil at the bottom of the crucible is started, and the heating power is increased to 80kW, and stabilized for 2 minutes; after the alloy is melted, the power of the main induction coil is reduced to 250kW, and the power of the induction coil at the bottom of the crucible is reduced to 70kW, so that the melt is in a semi-solidified state; the power of the main induction coil is increased to 300kW, and the power of the induction coil at the bottom of the crucible is increased to 90kW, and the heating power is increased by 10kW after the melt temperature reaches the liquidus; first reduce the power of the main induction coil to the minimum within fifteen seconds, and after the upper part of the melt solidifies, reduce the power of the induction coil at the bottom of the crucible to the minimum within fifteen seconds, and then turn off the heating power to obtain a multi-principal alloy ingot.
经过形貌表征可知，合金呈等轴晶组织，但由于凝固时过热度缓慢降低，晶粒快速长大，导致所得合金晶粒尺寸粗大。具体地，顶部晶粒尺寸为510μm，底部晶粒尺寸为498μm。The morphological characterization shows that the alloy presents an equiaxed crystal structure, but due to the slow decrease of superheat during solidification, the grains grow rapidly, resulting in a coarse grain size of the obtained alloy. Specifically, the top grain size is 510 μm and the bottom grain size is 498 μm.
由此可知，本发明所述方法通过主感应线圈和坩埚底部感应线圈的功率匹配，确保坩埚底部熔体获得足够的热量和悬浮力，避免熔体与坩埚壁接触导致热量流失过快，减小了熔体整体的温度梯度，提高了熔体内温度分布的均匀性，保证了铸锭不同位置的组织均匀。It can be seen that the method of the present invention ensures that the melt at the bottom of the crucible obtains sufficient heat and suspension force by matching the power of the main induction coil and the induction coil at the bottom of the crucible, avoids excessive heat loss caused by contact between the melt and the crucible wall, reduces the overall temperature gradient of the melt, improves the uniformity of temperature distribution in the melt, and ensures uniform organization of different positions of the ingot.
综上所述，发明包括但不限于以上实施例，凡是在本发明的精神和原则之下进行的任何等同替换或局部改进，都将视为在本发明的保护范围之内。In summary, the invention includes but is not limited to the above embodiments. Any equivalent substitution or partial improvement made under the spirit and principle of the invention shall be deemed to be within the protection scope of the invention.
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