CN114410994B - Based on CaO-MgO-Al 2 O 3 Method for smelting nickel-base superalloy by refractory material - Google Patents
Based on CaO-MgO-Al 2 O 3 Method for smelting nickel-base superalloy by refractory material Download PDFInfo
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- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 95
- 229910018072 Al 2 O 3 Inorganic materials 0.000 title claims abstract description 56
- 238000003723 Smelting Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000011819 refractory material Substances 0.000 title claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 194
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 97
- 238000002844 melting Methods 0.000 claims abstract description 74
- 230000008018 melting Effects 0.000 claims abstract description 74
- 230000006698 induction Effects 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000000155 melt Substances 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 25
- 229910052802 copper Inorganic materials 0.000 claims description 25
- 239000010949 copper Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 23
- 230000001681 protective effect Effects 0.000 claims description 22
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 19
- 239000010425 asbestos Substances 0.000 claims description 17
- 239000004744 fabric Substances 0.000 claims description 17
- 229910052895 riebeckite Inorganic materials 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 239000006104 solid solution Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 229910020068 MgAl Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 15
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000000956 alloy Substances 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000010309 melting process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 238000010308 vacuum induction melting process Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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Abstract
本发明提供了一种基于CaO‑MgO‑Al2O3耐火材料熔炼镍基高温合金的方法，其步骤包括：将CaO‑MgO‑Al2O3耐火材料坩埚置于感应熔炼设备中，将镍基高温合金原料放入所述CaO‑MgO‑Al2O3耐火材料坩埚中在感应熔炼设备中熔炼得到镍基高温合金。本发明提供的基于CaO‑MgO‑Al2O3耐火材料熔炼镍基高温合金的方法，能够有效防止镍基高温合金熔体的氧化污染，熔炼出高冶金质量的镍基高温合金。
The invention provides a method for smelting a nickel-based superalloy based on a CaO-MgO-Al 2 O 3 refractory material. The steps include: placing a CaO-MgO-Al 2 O 3 refractory crucible in an induction melting device, putting a nickel-based superalloy raw material into the CaO-MgO-Al 2 O 3 refractory crucible, and melting in the induction melting device to obtain a nickel-based superalloy. The method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractories provided by the present invention can effectively prevent oxidation pollution of nickel-based superalloy melts and melt nickel-based superalloys with high metallurgical quality.
Description
技术领域technical field
本发明涉及镍基高温合金冶炼技术领域，特别涉及一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法。The invention relates to the technical field of nickel-based superalloy smelting, in particular to a method for smelting a nickel-based superalloy based on a CaO-MgO-Al 2 O 3 refractory material.
背景技术Background technique
镍基高温合金广泛应用于航空发动机和燃气轮机的涡轮盘和叶片，也是石油化工、火电核电、节能环保等多领域重大装备制造的关键材料。镍基高温合金中的微量元素可以分为有益元素和有害元素两大类，氧在镍基高温合金中是作为有害的微量杂质元素存在的，其存在形态为固溶态及氧化物夹杂。由于镍基高温合金通常含有铝等强氧化物形成元素，所以镍基合金液中即使含有微量氧，也会形成氧化铝等夹杂物。氧化物夹杂通常是疲劳裂纹的萌生地及扩展通道，影响镍基高温合金的蠕变、持久强度等性能，所以维持镍基高温合金中的低氧含量具有极为重要的意义。Nickel-based superalloys are widely used in the turbine disks and blades of aero-engines and gas turbines, and are also key materials for the manufacture of major equipment in many fields such as petrochemical, thermal power, nuclear power, energy conservation and environmental protection. Trace elements in nickel-based superalloys can be divided into two categories: beneficial elements and harmful elements. Oxygen exists as a harmful trace impurity element in nickel-based superalloys, and its existence forms are solid solution and oxide inclusions. Since nickel-based superalloys usually contain strong oxide-forming elements such as aluminum, inclusions such as alumina will be formed even if there is a trace amount of oxygen in the nickel-based alloy liquid. Oxide inclusions are usually the initiation site and propagation channel of fatigue cracks, which affect the creep and durability strength of nickel-based superalloys. Therefore, it is of great significance to maintain low oxygen content in nickel-based superalloys.
目前对于高温合金的熔炼大都采用真空坩埚式感应熔炼技术，其熔炼最常使用的耐火材料坩埚有氧化铝坩埚、氧化镁坩埚或氧化钙坩埚，然而氧化铝耐火材料坩埚在镍基高温合金熔体中容易发生溶解反应，导致夹杂物形成，影响镍基合金的性能。氧化镁耐火材料坩埚在真空度条件下易发生分解，向镍基合金熔体中供氧，进一步污染镍基合金熔体。氧化钙耐火材料坩埚虽具有较好的热力学稳定性，但由于其易水化，在工业化规模应用过程中难度较大。At present, vacuum crucible induction melting technology is mostly used for melting superalloys. The most commonly used refractory crucibles for melting are alumina crucibles, magnesia crucibles or calcium oxide crucibles. However, alumina refractory crucibles are prone to dissolution reactions in nickel-based superalloy melts, resulting in the formation of inclusions and affecting the performance of nickel-based alloys. The magnesia refractory crucible is easy to decompose under the condition of vacuum, supply oxygen to the nickel-based alloy melt, and further pollute the nickel-based alloy melt. Although calcium oxide refractory crucible has good thermodynamic stability, it is difficult to apply it on an industrial scale because of its easy hydration.
因此，目前亟需一种高冶金质量的镍基高温合金的熔炼方法，以解决氧化镁、氧化铝或氧化钙等耐火材料坩埚在感应熔炼制备镍基高温合金方面存在的污染合金的问题。Therefore, there is an urgent need for a high metallurgical quality nickel-based superalloy smelting method to solve the problem of contaminated alloys in the induction melting of refractory crucibles such as magnesium oxide, aluminum oxide or calcium oxide.
发明内容Contents of the invention
本发明的目的是提供一种基于CaO-MgO-Al2O3耐火材料熔炼高冶金质量的镍基高温合金的方法，使用CaO-MgO-Al2O3耐火材料作为熔炼用坩埚材料，并在感应熔炼设备中采用真空熔炼，控制熔炼温度和时间及熔炼时采用保护气氛保护，能够有效防止镍基高温合金熔体的氧化污染。The purpose of the present invention is to provide a method for smelting nickel-based superalloys with high metallurgical quality based on CaO-MgO-Al 2 O 3 refractory materials. CaO-MgO-Al 2 O 3 refractory materials are used as melting crucible materials, vacuum melting is adopted in induction melting equipment, melting temperature and time are controlled, and protective atmosphere protection is used during smelting, which can effectively prevent oxidation pollution of nickel-based superalloy melts.
为解决上述技术问题，本发明提供了一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，包括如下步骤：In order to solve the above technical problems, the present invention provides a method for melting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractories, comprising the following steps:
将CaO-MgO-Al2O3耐火材料坩埚置于感应熔炼设备中；Place the CaO-MgO-Al 2 O 3 refractory crucible in the induction melting equipment;
将镍基高温合金原料放入所述CaO-MgO-Al2O3耐火材料坩埚中在感应熔炼设备中熔炼得到镍基高温合金。The nickel-based superalloy raw material is put into the CaO-MgO-Al 2 O 3 refractory crucible and smelted in the induction melting equipment to obtain the nickel-based superalloy.
进一步地，所述CaO-MgO-Al2O3耐火材料坩埚由下述方法制备：Further, the CaO-MgO-Al 2 O 3 refractory crucible is prepared by the following method:
将CaO-MgO-Al2O3耐火材料的原料粉料与粘结剂混合得到混合料；mixing raw material powder of CaO-MgO-Al 2 O 3 refractory material with binder to obtain a mixture;
将混合料捣打成型或冷等静压压制成型为坩埚素坯；The mixture is formed by ramming or cold isostatic pressing into a crucible green body;
坩埚素坯经高温烘烤或高温烧结炉煅烧得到CaO-MgO-Al2O3耐火材料坩埚。The crucible blank is baked at high temperature or calcined in a high temperature sintering furnace to obtain a CaO-MgO-Al 2 O 3 refractory crucible.
进一步地，所述粘结剂为硼砂、石蜡、丙三醇、无水乙醇中的一种或几种。Further, the binder is one or more of borax, paraffin, glycerol, and absolute ethanol.
进一步地，所述感应熔炼设备为真空感应熔炼炉，所述真空感应熔炼炉包括：Further, the induction melting equipment is a vacuum induction melting furnace, and the vacuum induction melting furnace includes:
设置于可开式球形炉膛内的CaO-MgO-Al2O3耐火材料坩埚；A CaO-MgO-Al 2 O 3 refractory crucible arranged in an openable spherical furnace;
设置在所述可开式球形炉膛内部与所述坩埚外围之间的中空铜线圈，所述中空铜线圈连接电源箱，中空铜线圈内部设置循环水；A hollow copper coil arranged between the interior of the openable spherical furnace and the periphery of the crucible, the hollow copper coil is connected to a power box, and circulating water is arranged inside the hollow copper coil;
所述坩埚与中空铜线圈之间设置石棉布，所述石棉布将所述坩埚底部与上部包裹，所述石棉布与所述坩埚底部之间填充氧化铝砂，所述石棉布与所述坩埚上部之间填充氧化镁砂；Asbestos cloth is arranged between the crucible and the hollow copper coil, the asbestos cloth wraps the bottom and upper part of the crucible, alumina sand is filled between the asbestos cloth and the bottom of the crucible, and magnesia sand is filled between the asbestos cloth and the upper part of the crucible;
所述石棉布底部设置固定于所述可开式球形炉膛内部的托盘；The bottom of the asbestos cloth is provided with a tray fixed inside the openable spherical furnace;
所述可开式球形炉膛分别设置连通低真空泵的通孔和连通高真空泵的通孔；The openable spherical furnace is respectively provided with a through hole communicating with the low vacuum pump and a through hole communicating with the high vacuum pump;
所述可开式球形炉膛分别设置连接保护气体输入装置的进气口和连通大气的进气口。The openable spherical furnace is respectively provided with an air inlet connected to the protective gas input device and an air inlet connected to the atmosphere.
进一步地，所述低真空泵为机械泵，所述高真空泵为分子泵。Further, the low vacuum pump is a mechanical pump, and the high vacuum pump is a molecular pump.
进一步地，所述真空感应熔炼炉对镍基高温合金原料的熔炼包括如下步骤：Further, the smelting of the nickel-based superalloy raw material in the vacuum induction melting furnace includes the following steps:
用所述机械泵将密闭的真空感应熔炼炉内部抽空至0～20Pa，然后通过所述保护气体输入装置充入保护气体至0.01～0.08Mpa；Use the mechanical pump to evacuate the inside of the closed vacuum induction melting furnace to 0-20Pa, and then fill the protective gas to 0.01-0.08Mpa through the protective gas input device;
重复上述抽空与充气操作2～5次；Repeat the above evacuation and inflation operation 2 to 5 times;
用所述高真空泵将真空感应熔炼炉内部抽空至0.0001～0.01Pa；Use the high vacuum pump to evacuate the interior of the vacuum induction melting furnace to 0.0001-0.01Pa;
通过所述电源箱内电源以5～8KW的加热功率对所述中空铜线圈加热，加热后的中空铜线圈将所述CaO-MgO-Al2O3耐火材料坩埚中的镍基高温合金原料加热至熔化；The hollow copper coil is heated by the power supply in the power supply box with a heating power of 5-8KW, and the heated hollow copper coil heats the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible until it is melted;
通过所述电源箱内电源以3～5KW的加热功率对所述中空铜线圈加热，加热后的中空铜线圈对熔化的镍基高温合金原料加热精炼。The hollow copper coil is heated by the power supply in the power supply box with a heating power of 3-5KW, and the heated hollow copper coil heats and refines the melted nickel-based superalloy raw material.
进一步地，所述镍基高温合金原料加热熔化过程中，先以1-2KW/h速度升高加热功率，在镍基高温合金原料开始熔化时，关闭所述真空泵，充入保护气体，同时以5-10KW/h速度升高加热功率至5～8KW，保温0.1-0.5h至镍基高温合金原料熔化成金属液；Further, during the heating and melting process of the nickel-based superalloy raw material, first increase the heating power at a rate of 1-2KW/h, and when the nickel-based superalloy raw material starts to melt, turn off the vacuum pump, fill in the protective gas, and increase the heating power at a rate of 5-10KW/h to 5-8KW, and keep warm for 0.1-0.5h until the nickel-based superalloy raw material melts into molten metal;
再以2-5KW/h速度降低加热功率至3～5KW，保温0.5-1.5h对熔化的镍基高温合金原料加热精炼。Then reduce the heating power to 3-5KW at a speed of 2-5KW/h, heat and refine the melted nickel-based superalloy raw material for 0.5-1.5h.
进一步地，所述真空感应熔炼炉对镍基高温合金原料熔炼过程中熔炼温度控制在1450～1750℃，熔炼时间为2～15h。Further, during the melting process of the nickel-based superalloy raw material in the vacuum induction melting furnace, the melting temperature is controlled at 1450-1750° C., and the melting time is 2-15 hours.
进一步地，所述真空感应熔炼炉内的熔炼温度通过红外测温仪观察确定。Further, the melting temperature in the vacuum induction melting furnace is determined by observing with an infrared thermometer.
进一步地，所述熔炼过程中保护气体的气压控制在1～9×104Pa。Further, the pressure of the protective gas during the smelting process is controlled at 1˜9×10 4 Pa.
本发明提供的一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，采用热力学稳定性良好的CaO-MgO-Al2O3耐火材料坩埚来熔化镍基高温合金，CaO-MgO-Al2O3耐火材料简称CMA材料，它是由磁铅石结构的CaAl12O19和立方结构的MgAl2O4在高温下固溶形成，包含了CaAl12O19和MgAl2O4的特点，具有熔点高、导热系数低、隔热保温性好、热稳定性好、耐热震性好及抗渣性能优异等特点，在还原气氛中(如在CO中)十分稳定，对于金属熔体(包括钢铁和镍基高温合金)和熔渣具有较低的润湿作用，因此CaO-MgO-Al2O3耐火材料作为镍基高温合金熔炼用坩埚，能有效减少熔炼过程中坩埚耐火材料对镍基高温合金熔体的污染。A kind of based on CaO-MgO-Al provided by the invention2o3A method for smelting nickel-based superalloys with refractory materials, using CaO-MgO-Al with good thermodynamic stability2o3Refractory crucibles for melting nickel-based superalloys, CaO-MgO-Al2o3The refractory material is referred to as CMA material, which is composed of CaAl with magnetoplumbite structure.12o19and cubic MgAl2o4Formed in solid solution at high temperature, including CaAl12o19and MgAl2o4It has the characteristics of high melting point, low thermal conductivity, good heat insulation, good thermal stability, good thermal shock resistance and excellent slag resistance. It is very stable in reducing atmosphere (such as in CO) and has low wetting effect on metal melts (including steel and nickel-based superalloys) and slag. Therefore, CaO-MgO-Al2o3The refractory material is used as a crucible for nickel-based superalloy melting, which can effectively reduce the pollution of the crucible refractory material to the nickel-based superalloy melt during the melting process.
并且，本发明提供的一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，将装有镍基高温合金的CaO-MgO-Al2O3耐火材料坩埚置于真空感应熔炼炉熔炼镍基高温合金中，采用真空感应熔炼工艺，通过控制真空条件，熔炼温度和熔炼时间，以及熔炼时采用保护气氛保护，严格控制保护气气压，可以防止高温合金熔体的氧化污染，能显著降低镍基高温合金中的氧污染量。In addition, the present invention provides a method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials. The CaO-MgO-Al 2 O 3 refractory crucible filled with nickel-based superalloys is placed in a vacuum induction melting furnace to melt nickel-based superalloys. The vacuum induction melting process is adopted. By controlling the vacuum conditions, melting temperature and melting time, and using protective atmosphere protection during smelting, the protective gas pressure can be strictly controlled to prevent oxidation pollution of the superalloy melt. Significantly reduces the amount of oxygen contamination in nickel-based superalloys.
同时，本发明提供的一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，熔炼工艺流程简单，工艺参数要求较低，能够降低能耗、减少污染，符合绿色冶金的要求，且具有较高的经济效益，值得推广应用。At the same time, the method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractories provided by the present invention has a simple smelting process flow, low requirements on process parameters, can reduce energy consumption and pollution, meet the requirements of green metallurgy, and has high economic benefits, and is worthy of popularization and application.
附图说明Description of drawings
图1为本发明实施例提供的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法流程图；Fig. 1 is the flow chart of the method for melting nickel-based superalloy based on CaO-MgO- Al2O3 refractory material provided by the embodiment of the present invention;
图2为本发明实施例提供的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法中真空感应熔炼炉内的坩埚和填充物放置顺序图；Fig. 2 is a diagram of the placement sequence of the crucible and the filler in the vacuum induction melting furnace in the method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials provided by the embodiment of the present invention;
图3为本发明实施例和对比例提供的使用氧化铝耐火材料坩埚、氧化镁耐火材料坩埚及CaO-MgO-Al2O3耐火材料坩埚熔炼镍基高温合金得到的镍基高温合金中夹杂物面积分布图；Fig. 3 is the area distribution diagram of inclusions in nickel-based superalloys obtained by melting nickel-based superalloys using alumina refractory crucibles, magnesia refractory crucibles and CaO-MgO-Al 2 O 3 refractory crucibles provided by the embodiments of the present invention and comparative examples;
图4为本发明实施例和对比例提供的使用氧化铝耐火材料坩埚、氧化镁耐火材料坩埚及CaO-MgO-Al2O3耐火材料坩埚熔炼镍基高温合金得到的镍基高温合金中夹杂物不同尺寸数量分布图。Fig. 4 is a distribution diagram of different sizes and quantities of inclusions in nickel-based superalloys obtained by melting nickel-based superalloys using alumina refractory crucibles, magnesia refractory crucibles, and CaO-MgO-Al 2 O 3 refractory crucibles provided in Examples and Comparative Examples of the present invention.
具体实施方式Detailed ways
参见图1，本发明实施例提供的一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，主要包括如下步骤：Referring to Fig. 1, a method for melting a nickel-based superalloy based on a CaO-MgO-Al 2 O 3 refractory material provided by an embodiment of the present invention mainly includes the following steps:
步骤1)将CaO-MgO-Al2O3耐火材料坩埚置于真空感应熔炼炉中。Step 1) Place the CaO-MgO-Al 2 O 3 refractory crucible in a vacuum induction melting furnace.
其中，CaO-MgO-Al2O3耐火材料坩埚的制备包括如下步骤：Wherein, the preparation of CaO-MgO-Al 2 O 3 refractory material crucible comprises the following steps:
(1)将CaO-MgO-Al2O3耐火材料的原料粉料与粘结剂混合得到混合料。(1) Mix raw material powder of CaO-MgO-Al 2 O 3 refractory material with binder to obtain a mixture.
具体地，先将CaO-MgO-Al2O3耐火材料原料、氧化锆磨球、无水乙醇，并按照原料：磨球：乙醇的质量比为2:3:0.8进行配置后加入球磨罐中，在行星球磨机上球磨8h。然后在120℃烘箱里烘干并筛分得到粉料，再将得到的粉料加入粘结剂搅拌均匀得到混合料。其中，所述粘结剂为硼砂、石蜡、丙三醇、无水乙醇中的一种或几种。作为本发明的一种具体实施方式，将得到的粉料与无水乙醇混合，搅拌均匀得到混合料。Specifically, CaO-MgO-Al 2 O 3 refractory raw materials, zirconia grinding balls, and absolute ethanol were prepared according to the mass ratio of raw materials: grinding balls: ethanol of 2:3:0.8, then added to the ball mill tank, and ball milled on a planetary ball mill for 8 hours. Then dry and sieve in an oven at 120°C to obtain a powder, then add the obtained powder to a binder and stir evenly to obtain a mixture. Wherein, the binder is one or more of borax, paraffin, glycerol and absolute ethanol. As a specific embodiment of the present invention, the obtained powder is mixed with absolute ethanol, and stirred evenly to obtain a mixture.
(2)将混合料捣打成型或冷等静压压制成型为坩埚素坯。(2) Forming the mixed material by ramming or cold isostatic pressing into a crucible green body.
作为本发明的一种具体实施方式，将得到的混合料装在自制的坩埚模具中，在冷等静压设备中施加140MPa压力并保压5min成型，得到坩埚素坯。As a specific embodiment of the present invention, the obtained mixture is packed in a self-made crucible mould, and a pressure of 140 MPa is applied in a cold isostatic pressing device, and the pressure is maintained for 5 minutes to form a crucible green body.
(3)坩埚素坯经高温烘烤或高温烧结炉煅烧得到CaO-MgO-Al2O3耐火材料坩埚。(3) The crucible green body is baked at high temperature or calcined in a high temperature sintering furnace to obtain a CaO-MgO-Al 2 O 3 refractory crucible.
作为本发明的一种具体实施方式，得到的坩埚素坯先在800℃下预烧结6h，然后在1400℃下烧结6h，再在1700℃下烧结6h，最后冷却至室温，即制得CaO-MgO-Al2O3耐火材料坩埚，其中，升降温过程中的升降温速率控制为100℃/h。As a specific embodiment of the present invention, the obtained crucible green body is pre-sintered at 800°C for 6 hours, then sintered at 1400°C for 6 hours, then sintered at 1700°C for 6 hours, and finally cooled to room temperature to obtain a CaO-MgO-Al 2 O 3 refractory crucible, wherein the heating and cooling rate during the heating and cooling process is controlled at 100 ℃/h.
步骤2)将镍基高温合金原料置于CaO-MgO-Al2O3耐火材料坩埚中在感应熔炼设备中熔炼得到镍基高温合金。Step 2) The nickel-based superalloy raw material is placed in a CaO-MgO-Al 2 O 3 refractory crucible and smelted in an induction melting device to obtain a nickel-based superalloy.
作为本发明的一种具体实施方式，感应熔炼设备为真空感应熔炼炉。As a specific embodiment of the present invention, the induction melting equipment is a vacuum induction melting furnace.
参见图2，真空感应熔炼炉包括设置于可开式球形炉膛(可开式球形炉膛图2未示出)内的CaO-MgO-Al2O3耐火材料坩埚7，设置在可开式球形炉膛内部与坩埚7外围之间的中空铜线圈3。其中，中空铜线圈3一端连接电源箱，通过控制电源箱内的电源可以一定的加热功率对中空铜线圈3进行加热，从而再通过加热后的中空铜线圈3对围在其内的坩埚7内的镍基高温合金加热。为了便于冷却，中空铜线圈3内部设置循环水。Referring to Fig. 2, the vacuum induction melting furnace includes a CaO-MgO- Al2O3 refractory crucible 7 arranged in an openable spherical furnace (the openable spherical furnace is not shown in Fig . 2), and a hollow copper coil 3 arranged between the inside of the openable spherical furnace and the periphery of the crucible 7. Wherein, one end of the hollow copper coil 3 is connected to the power supply box, and the hollow copper coil 3 can be heated with a certain heating power by controlling the power supply in the power supply box, so that the nickel-based superalloy in the crucible 7 surrounded by the heated hollow copper coil 3 can be heated. In order to facilitate cooling, circulating water is arranged inside the hollow copper coil 3 .
另外，在坩埚7与中空铜线圈3之间设置石棉布2，石棉布2将坩埚7的底部和上部包裹。其中，在石棉布2与坩埚7的底部之间填充氧化铝砂8，在石棉布2与坩埚7上部之间填充氧化镁砂5。In addition, an asbestos cloth 2 is arranged between the crucible 7 and the hollow copper coil 3 , and the asbestos cloth 2 wraps the bottom and the upper part of the crucible 7 . Among them, alumina sand 8 is filled between the asbestos cloth 2 and the bottom of the crucible 7 , and magnesia sand 5 is filled between the asbestos cloth 2 and the upper part of the crucible 7 .
石棉布2的底部设置固定于可开式球形炉膛内部的托盘1，托盘1将石棉布2底部托住，从而将包裹在石棉布2内的坩埚7固定。The bottom of the asbestos cloth 2 is provided with a tray 1 fixed inside the openable spherical furnace, and the tray 1 holds the bottom of the asbestos cloth 2 to fix the crucible 7 wrapped in the asbestos cloth 2 .
同时，可开式球形炉膛上分别设置连通低真空泵的通孔和连通高真空泵的通孔。通过低真空泵和高真空泵可对炉膛内抽真空。而且，可开式球形炉膛上还设置有连接保护气体输入装置的进气口和连通大气的进气口，通过保护气体输入装置可向炉膛内充入保护气体，同时也可通过连通大气的进气口将炉膛内的气体排出。Simultaneously, the through hole connected with the low vacuum pump and the through hole connected with the high vacuum pump are respectively arranged on the openable spherical furnace. The furnace can be evacuated by low vacuum pump and high vacuum pump. Moreover, the openable spherical furnace is also provided with an air inlet connected to the protective gas input device and an air inlet connected to the atmosphere. The protective gas can be filled into the furnace through the protective gas input device, and the gas in the furnace can also be discharged through the air inlet connected to the atmosphere.
作为本发明的一种具体实施方式，保护气体输入装置内部的气罐里充装氩气作为保护气体，同时输出时保证气体流速平稳。As a specific embodiment of the present invention, the gas tank inside the protective gas input device is filled with argon as the protective gas, and at the same time, the gas flow rate is stable during output.
作为本发明的一种具体实施方式，低真空泵为机械泵，高真空泵为分子泵。As a specific embodiment of the present invention, the low vacuum pump is a mechanical pump, and the high vacuum pump is a molecular pump.
在利用真空感应熔炼炉对CaO-MgO-Al2O3耐火材料坩埚7中的镍基高温合金原料熔炼，包括如下步骤：Melting the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible 7 by using a vacuum induction melting furnace includes the following steps:
(1)先用机械泵进行抽低真空，将密闭的真空感应熔炼炉炉膛内部抽空至0～20Pa，达到最优真空度后通过保护气体输入装置向炉膛内充入保护气体至0.01～0.08Mpa。(1) Use a mechanical pump to evacuate first, and evacuate the interior of the closed vacuum induction melting furnace to 0-20Pa. After reaching the optimal vacuum degree, fill the furnace with protective gas to 0.01-0.08Mpa through the protective gas input device.
(2)然后重复上述抽真空与充气操作2～5次，进行低真空洗炉。(2) Then repeat the above-mentioned vacuuming and inflation operations for 2 to 5 times to perform low-vacuum furnace cleaning.
(3)达到低真空洗气最优次数后，开启高真空洗气，用分子泵对真空感应熔炼炉内部进行抽高真空，至少重复1～3次，将真空感应熔炼炉内部抽空至达到最优真空度0.0001～0.01Pa。(3) After reaching the optimal times of low-vacuum gas washing, turn on high-vacuum gas washing, and use a molecular pump to evacuate the interior of the vacuum induction melting furnace to a high degree of vacuum, repeat at least 1 to 3 times, and evacuate the interior of the vacuum induction melting furnace to reach the optimal vacuum degree of 0.0001-0.01Pa.
(4)高真空洗气达到最优真空度后，通过电源箱内电源以5～8KW的加热功率对中空铜线圈3加热，加热后的中空铜线圈3将CaO-MgO-Al2O3耐火材料坩埚中的镍基高温合金原料加热至熔化。其中，在镍基高温合金原料加热熔化过程中，先以1-2KW/h速度升高加热功率，在镍基高温合金原料开始熔化时，关闭分子泵，充入保护气体，作为本发明的一种具体实施方式，充入的保护气体的气压控制在1～9×104Pa。同时以5-10KW/h速度升高加热功率至5～8KW，保温0.1-0.5h至镍基高温合金原料熔化成金属液。(4) After the high-vacuum gas washing reaches the optimal vacuum degree, the hollow copper coil 3 is heated by the power supply in the power supply box with a heating power of 5-8KW, and the heated hollow copper coil 3 heats the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible until it is melted. Among them, during the heating and melting process of the nickel-based superalloy raw material, the heating power is first increased at a rate of 1-2KW/h. When the nickel-based superalloy raw material starts to melt, the molecular pump is turned off and the protective gas is charged. As a specific embodiment of the present invention, the pressure of the charged protective gas is controlled at 1-9×10 4 Pa. At the same time, increase the heating power to 5-8KW at a speed of 5-10KW/h, and keep warm for 0.1-0.5h until the nickel-based superalloy raw material melts into molten metal.
(5)再通过电源箱内电源以3～5KW的加热功率对中空铜线圈3加热，加热后的中空铜线圈对熔化的镍基高温合金原料加热精炼。其中，该过程中，先将镍基高温合金原料熔化成金属液时的加热功率5～8KW以2-5KW/h速度降低加热功率至3～5KW，保温0.5-1.5h对熔化的镍基高温合金原料加热精炼。(5) The hollow copper coil 3 is heated by the power supply in the power supply box with a heating power of 3-5KW, and the heated hollow copper coil heats and refines the melted nickel-based superalloy raw material. Among them, in this process, first melt the nickel-based superalloy raw material into molten metal with a heating power of 5-8KW, reduce the heating power to 3-5KW at a speed of 2-5KW/h, and heat and refine the melted nickel-based superalloy raw material for 0.5-1.5h.
其中，真空感应熔炼炉对镍基高温合金原料的整个熔炼过程中熔炼温度控制在1450～1750℃，熔炼时间为2～15h。其中，真空感应熔炼炉内的熔炼温度通过红外测温仪观察确定。Among them, the melting temperature of the vacuum induction melting furnace is controlled at 1450-1750° C. during the whole melting process of the nickel-based superalloy raw material, and the melting time is 2-15 hours. Wherein, the melting temperature in the vacuum induction melting furnace is determined by observing with an infrared thermometer.
作为本发明的一种具体实施方式，真空感应熔炼阶段，对真空感应熔炼炉炉膛进行低真空洗气时重复3次为最佳。As a specific embodiment of the present invention, in the vacuum induction smelting stage, it is best to repeat 3 times when performing low-vacuum scrubbing on the hearth of the vacuum induction smelting furnace.
作为本发明的一种具体实施方式，真空感应熔炼阶段，对真空感应熔炼炉炉膛进行高真空洗气时重复2次为最佳。且高真空洗气达到的真空度为3×10-3Pa最佳。As a specific embodiment of the present invention, in the vacuum induction smelting stage, it is best to repeat twice when performing high vacuum scrubbing on the hearth of the vacuum induction smelting furnace. And the vacuum achieved by high-vacuum washing is 3×10 -3 Pa, which is the best.
作为本发明的一种具体实施方式，真空感应熔炼阶段，高真空下熔炼炉炉腔内压力为1～8×10-3Pa最佳，低真空下熔炼炉炉腔内压力为1～30Pa最佳。As a specific embodiment of the present invention, in the vacuum induction smelting stage, the best pressure in the furnace chamber of the melting furnace under high vacuum is 1-8×10 -3 Pa, and the best pressure inside the furnace chamber of the melting furnace under low vacuum is 1-30 Pa.
下面以实施例和对比例对本发明提供的一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法，做进一步具体说明。A method for smelting a nickel-based superalloy based on the CaO-MgO-Al 2 O 3 refractory material provided by the present invention will be further specifically described below with examples and comparative examples.
实施例1Example 1
以镍基高温合金GH4169为原料。将镍基高温合金GH4169置于CaO-MgO-Al2O3耐火材料坩埚中，然后将该坩埚放入真空感应熔炼炉炉膛内的中空铜线圈中，对真空感应熔炼炉炉膛先进行3次低真空洗气，再进行2次高真空洗气，使真空感应熔炼炉炉膛内真空度达到3×10-3Pa，然后通过电源箱内的电源对中空铜线圈加热，再通过中空铜线圈对坩埚内的镍基高温合金GH4169进行加热。该加热熔炼过程中，先以1KW/h速度升高加热功率至1.5KW，在镍基高温合金GH4169开始熔化时，保持高真空3×10-3～1×10-1Pa状态。同时以5.5KW/h速度升高加热功率至6.5KW，迅速将镍基高温合金GH4169熔化成金属液。然后以2.5KW/h速度降低加热功率至3.5KW对熔化的镍基高温合金GH4169进行精炼，在1550℃的温度下保温0.5h后自然冷却，使镍基高温合金GH4169凝固在坩埚内部，取出坩埚内部凝固得到的固体，此时得到的样品标记为A1。The nickel base superalloy GH4169 is used as the raw material. Put the nickel-based superalloy GH4169 in a CaO-MgO-Al 2 O 3 refractory crucible, and then put the crucible into the hollow copper coil in the hearth of the vacuum induction melting furnace. The hearth of the vacuum induction melting furnace is firstly washed with low vacuum for 3 times, and then with high vacuum for 2 times, so that the vacuum degree in the hearth of the vacuum induction melting furnace reaches 3×10 -3 Pa. The nickel-based superalloy GH4169 in the crucible is heated. During the heating and smelting process, the heating power is increased to 1.5KW at a rate of 1KW/h, and a high vacuum of 3×10 -3 ~ 1×10 -1 Pa is maintained when the nickel-based superalloy GH4169 starts to melt. At the same time, the heating power is increased to 6.5KW at a speed of 5.5KW/h, and the nickel-based superalloy GH4169 is rapidly melted into molten metal. Then reduce the heating power to 3.5KW at a speed of 2.5KW/h to refine the melted nickel-based superalloy GH4169, keep it at a temperature of 1550°C for 0.5h, and then cool it naturally to solidify the nickel-based superalloy GH4169 inside the crucible, take out the solid obtained by solidification inside the crucible, and the sample obtained at this time is marked as A1.
对比例1Comparative example 1
以镍基高温合金GH4169为原料。将合金锭置于真空式感应炉膛内部线圈的Al2O3坩埚中，经历3次低真空、2次高真空达到3×10-3pa的真空度下加功率，保持高真空3×10-3～1×10-1Pa状态。经历6.7KW的大功率快速熔化、3～3.4KW的中功率精炼，在1550℃保温30min后冷却在坩埚内部，标记样品为A2。The nickel base superalloy GH4169 is used as the raw material. The alloy ingot was placed in the Al 2 O 3 crucible of the inner coil of the vacuum induction furnace, experienced 3 times of low vacuum and 2 times of high vacuum to reach a vacuum degree of 3×10 -3 Pa, and then applied power to maintain a state of high vacuum of 3×10 -3 ~ 1×10 -1 Pa. After undergoing high-power rapid melting of 6.7KW and medium-power refining of 3-3.4KW, it was kept at 1550°C for 30 minutes and then cooled inside the crucible. The sample was marked as A2.
对比例2Comparative example 2
以镍基高温合金GH4169为原料。将合金锭置于真空式感应炉膛内部线圈的MgO坩埚中，经历3次低真空、2次高真空达到3×10-3Pa的真空度下加功率，保持高真空3×10-3～1×10-1Pa状态。经历6.7KW的大功率快速熔化、3～3.4KW的中功率精炼，在1550℃保温30min后冷却在坩埚内部，标记样品为A3。The nickel base superalloy GH4169 is used as the raw material. The alloy ingot was placed in the MgO crucible of the inner coil of the vacuum induction furnace, experienced three times of low vacuum and two times of high vacuum to reach a vacuum degree of 3×10 -3 Pa, and then applied power to maintain a state of high vacuum of 3×10 -3 ~ 1×10 -1 Pa. After undergoing high-power rapid melting of 6.7KW and medium-power refining of 3-3.4KW, it was kept at 1550°C for 30 minutes and then cooled inside the crucible. The sample was marked as A3.
对本发明实施例和对比例熔炼得到的镍基高温合金GH4169样品进行性质检测。The properties of the nickel-base superalloy GH4169 samples obtained by smelting in the examples and comparative examples of the present invention were tested.
采用氧/氮分析仪对实施例和对比例熔炼得到的三个样品分别进行氧含量的检测，测试结果如表1所示。从表1中可以看出，本发明实施例1使用CaO-MgO-Al2O3耐火材料坩埚按照所示的熔炼工艺熔炼得到的高温镍基合金样品A1，相比对比例1使用Al2O3坩埚和对比例2使用MgO坩埚熔炼得到的高温镍基合金样品A2和A3，合金中的氧含量要低，由此说明本发明实施例使用CaO-MgO-Al2O3耐火材料坩埚熔炼得到的镍基高温合金质量更高。An oxygen/nitrogen analyzer was used to detect the oxygen content of the three samples smelted in Examples and Comparative Examples respectively, and the test results are shown in Table 1. It can be seen from Table 1 that the high-temperature nickel-based alloy sample A1 obtained by melting the CaO-MgO-Al 2 O 3 refractory crucible according to the shown smelting process in Example 1 of the present invention is compared with the high-temperature nickel-based alloy samples A2 and A3 obtained by melting the Al 2 O 3 crucible in Comparative Example 1 and the MgO crucible in Comparative Example 2. The nickel-based superalloy obtained by smelting is of higher quality.
表1Table 1
在熔炼过程中，本发明实施例1使用CaO-MgO-Al2O3耐火材料坩埚熔炼得到的镍基高温合金呈现出良好的纯净度，熔炼后的合金表面形貌相比于对比例1和对比例2更为干净，通过解剖镍基高温合金和坩埚界面，发现相比于对镍基高温合金呈现明显润湿性的氧化铝耐火材料和氧化镁耐火材料来说，CaO-MgO-Al2O3耐火材料呈现明显的不润湿性，这进一步说了CaO-MgO-Al2O3耐火材料坩埚熔炼镍基高温合金对镍基合金熔体呈现较好的抗侵蚀性。During the smelting process, the nickel-based superalloy obtained by melting the CaO-MgO-Al 2 O 3 refractory crucible in Example 1 of the present invention showed good purity, and the surface morphology of the smelted alloy was cleaner than that of Comparative Example 1 and Comparative Example 2. By dissecting the interface between the nickel-based superalloy and the crucible, it was found that the CaO-MgO-Al 2 O 3 refractory exhibited obvious wettability to the nickel-based superalloy. The obvious non-wetting property further shows that the CaO-MgO-Al 2 O 3 refractory crucible for melting nickel-based superalloys has better corrosion resistance to nickel-based alloy melts.
参见图3和图4，通过对比本发明实施例1、对比例1和对比例2熔炼得到的镍基高温合金中夹杂物的面积分别情况和夹杂物不同尺寸数量分布情况，可以看出本发明实施例1制得的镍基高温合金明显优于对比例1和对比例2制得的镍基高温合金。Referring to Fig. 3 and Fig. 4, by comparing the area of the inclusions in the nickel-based superalloy obtained by smelting in Example 1, Comparative Example 1 and Comparative Example 2 of the present invention and the distribution of different sizes and quantities of the inclusions, it can be seen that the nickel-based superalloy prepared in Example 1 of the present invention is significantly better than the nickel-based superalloy prepared in Comparative Example 1 and Comparative Example 2.
本发明提供的一种基于CaO-MgO-Al2O3(CMA)耐火材料的高冶金质量镍基高温合金制备方法，使用CaO-MgO-Al2O3耐火材料作为熔炼用坩埚材料，并通过对真空熔炼工艺流程、熔炼温度、熔炼时间及熔炼时的保护气体气压的控制，能够有效防止镍基高温合金熔体的氧化污染，能够熔炼得到高冶金质量的镍基高温合金。The present invention provides a high metallurgical quality nickel-based superalloy preparation method based on CaO-MgO-Al 2 O 3 (CMA) refractory material. CaO-MgO-Al 2 O 3 refractory material is used as the crucible material for smelting, and through the control of vacuum melting process flow, melting temperature, smelting time and protective gas pressure during smelting, oxidation pollution of nickel-based superalloy melt can be effectively prevented, and nickel-based superalloy with high metallurgical quality can be smelted.
最后所应说明的是，以上具体实施方式仅用以说明本发明的技术方案而非限制，尽管参照实例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to examples, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
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