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CN114410994A - Based on CaO-MgO-Al2O3Method for smelting nickel-based high-temperature alloy by using refractory material - Google Patents

Based on CaO-MgO-Al2O3Method for smelting nickel-based high-temperature alloy by using refractory material Download PDF

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CN114410994A
CN114410994A CN202111658192.1A CN202111658192A CN114410994A CN 114410994 A CN114410994 A CN 114410994A CN 202111658192 A CN202111658192 A CN 202111658192A CN 114410994 A CN114410994 A CN 114410994A
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侯新梅
刘云松
陈光耀
王恩会
杨树峰
赵飞
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University of Science and Technology Beijing USTB
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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。

Figure 202111658192

The invention provides a method for melting nickel-based superalloy based on CaO - MgO - Al 2 O 3 refractory material. The base superalloy raw material is put into the CaO-MgO-Al 2 O 3 refractory crucible and smelted in an induction melting device to obtain a nickel-based superalloy. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material provided by the invention can effectively prevent oxidation pollution of nickel-based superalloy melt, and smelt nickel-based superalloy with high metallurgical quality.

Figure 202111658192

Description

基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法Method for melting nickel-based superalloy based on CaO-MgO-Al2O3 refractory

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 nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory materials.

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 turbine disks and blades of aero-engines and gas turbines, and are also key materials for the manufacture of major equipment in petrochemical, thermal and 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 existing 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 a trace amount of oxygen is contained in the nickel-based alloy liquid. Oxide inclusions are usually the initiation sites and expansion channels of fatigue cracks, which affect the creep and endurance 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, the vacuum crucible induction melting technology is mostly used for the melting of superalloys. The most commonly used refractory crucibles for smelting are alumina crucibles, magnesia crucibles or calcium oxide crucibles. However, alumina refractory crucibles are used in nickel-based superalloy melts. The dissolution reaction easily occurs in the nickel-based alloy, resulting in the formation of inclusions and affecting the properties of nickel-based alloys. The magnesia refractory crucible is prone to decompose under vacuum conditions, supplying oxygen to the nickel-based alloy melt, and further polluting the nickel-based alloy melt. Although calcium oxide refractory crucible has good thermodynamic stability, it is difficult to be applied on an industrial scale due to 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 polluted alloys existing in the induction melting of refractory crucibles such as magnesium oxide, aluminum oxide or calcium oxide to prepare nickel-based superalloys.

发明内容SUMMARY 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 object 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, using CaO-MgO-Al 2 O 3 refractory materials as crucible materials for smelting, and in Vacuum melting is adopted in the induction melting equipment, the melting temperature and time are controlled and the protective atmosphere is used during melting, which can effectively prevent the oxidation pollution of the nickel-based superalloy melt.

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-mentioned technical problems, the present invention provides a method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material, 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 an induction melting device to obtain a 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 the raw material powder of the CaO-MgO-Al 2 O 3 refractory material with the 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 rammed or cold isostatically pressed into a crucible blank;

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 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.

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 dehydrated alcohol.

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 inside of the openable spherical furnace and the periphery of the crucible, the hollow copper coil is connected to a power supply 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;An asbestos cloth is arranged between the crucible and the hollow copper coil, the asbestos cloth wraps the bottom and the upper part of the crucible, alumina sand is filled between the asbestos cloth and the bottom of the crucible, and the asbestos cloth and the crucible are The upper part is filled with magnesia sand;

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 chamber 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 by the vacuum induction smelting 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 interior 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 operations 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 with a heating power of 5-8KW by the power supply in the power box, and the heated hollow copper coil heats the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible to melt;

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 box with a heating power of 3-5KW, and the heated hollow copper coil heats and refines the molten 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, the heating power is first increased at a rate of 1-2KW/h, and when the nickel-based superalloy raw material begins to melt, the vacuum pump is turned off, and the protective gas is filled, and at the same time Increase the heating power to 5-8KW at a speed of 5-10KW/h, and keep the temperature for 0.1-0.5h until the nickel-based superalloy raw materials are melted 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。The heating power is then reduced to 3-5KW at a speed of 2-5KW/h, and the molten nickel-based superalloy raw material is heated and refined for 0.5-1.5h of heat preservation.

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, in the process of smelting the nickel-based superalloy raw material in the vacuum induction melting furnace, the smelting temperature is controlled at 1450-1750° C., and the smelting 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 observation 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 gas pressure of the protective gas in 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。The invention provides a method for melting nickel-based superalloy based on CaO - MgO -Al 2 O 3 refractory material. -MgO-Al 2 O 3 refractory material is referred to as CMA material, which is formed by solid solution of CaAl 12 O 19 of magnetoplumbite structure and MgAl 2 O 4 of cubic structure at high temperature, including CaAl 12 O 19 and MgAl 2 O 4 has the characteristics of high melting point, low thermal conductivity, good thermal insulation, good thermal stability, good thermal shock resistance and excellent slag resistance. It is very stable in a reducing atmosphere (such as in CO). Metal melt (including steel and nickel-based superalloy) and slag have low wetting effect, so CaO-MgO-Al 2 O 3 refractory is used as a crucible for nickel-based superalloy smelting, which can effectively reduce the number of crucibles in the smelting process. Refractory contamination of nickel-based superalloy melts.

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。Furthermore, the present invention provides a method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material. The CaO-MgO-Al 2 O 3 refractory crucible containing nickel-based superalloy is placed in a vacuum induction In the smelting of nickel-based superalloys in the melting furnace, the vacuum induction melting process is adopted. By controlling the vacuum conditions, melting temperature and melting time, and using protective atmosphere protection during smelting, and strictly controlling the protective gas pressure, the oxidation pollution of the superalloy melt can be prevented. Can significantly reduce 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 present invention provides a method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material, the smelting process is simple, the requirements for process parameters are low, energy consumption and pollution can be reduced, and the requirements of green metallurgy are met. It 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;1 is a flowchart of a method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials provided in an 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;2 is a sequence diagram of placing crucibles and fillers in a vacuum induction melting furnace in a method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials provided by an 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;3 shows the 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 and comparative examples of the present invention area distribution map;

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。4 shows the 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 and comparative examples of the present invention Quantity distribution map of different sizes.

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 smelting nickel-based superalloy based on 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 the CaO-MgO-Al 2 O 3 refractory crucible includes 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) The raw material powder of the CaO-MgO-Al 2 O 3 refractory material is mixed with a 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, the CaO-MgO-Al 2 O 3 refractory raw materials, zirconia grinding balls, and anhydrous ethanol are first prepared and added to the ball mill after the mass ratio of raw materials: grinding balls: ethanol is 2:3:0.8. , milled on a planetary ball mill for 8h. Then, it is dried and sieved in an oven at 120° C. to obtain powder, and then the obtained powder is added to the binder and stirred 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 anhydrous ethanol, and the mixture is uniformly stirred to obtain a mixed material.

(2)将混合料捣打成型或冷等静压压制成型为坩埚素坯。(2) Ramming the mixture or cold isostatic pressing to form 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 placed in a self-made crucible mold, and a pressure of 140 MPa is applied in a cold isostatic pressing device and the pressure is maintained for 5 minutes to obtain 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 CaO-MgO-Al 2 O 3 refractory crucible is obtained by calcining the crucible green body at a high temperature or in a high-temperature sintering furnace.

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 china is first 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 CaO- The MgO-Al 2 O 3 refractory crucible, wherein the heating and cooling rate during the heating and cooling process is controlled to be 100°C/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) Place the nickel-based superalloy raw material in a CaO-MgO-Al 2 O 3 refractory crucible and smelt 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-Al 2 O 3 refractory crucible 7 arranged in an openable spherical furnace (the openable spherical furnace is not shown in FIG. 2 ), which is arranged in the openable spherical furnace The hollow copper coil 3 between the interior and the periphery of the crucible 7 . One end of the hollow copper coil 3 is connected to the power supply box, and the hollow copper coil 3 can be heated by a certain heating power by controlling the power supply in the power supply box, so that the heated hollow copper coil 3 can heat the crucible 7 enclosed within it. Heating of nickel-based superalloys. In order to facilitate cooling, circulating water is provided 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 provided between the crucible 7 and the hollow copper coil 3 , and the asbestos cloth 2 wraps the bottom and the upper portion 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. The tray 1 supports the bottom of the asbestos cloth 2, thereby fixing 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。At the same time, the openable spherical furnace chamber is respectively provided with a through hole communicating with the low vacuum pump and a through hole communicating with the high vacuum pump. The chamber can be evacuated by a low vacuum pump and a high vacuum pump. In addition, 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. The gas port exhausts the gas in the furnace.

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 gas as the protective gas, and at the same time, the gas flow rate is guaranteed to be 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:Smelting the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible 7 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) First use a mechanical pump to evacuate low vacuum, evacuate the inside of the closed vacuum induction melting furnace to 0-20Pa, and 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 inflating operations for 2 to 5 times to perform low-vacuum 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 number of low-vacuum scrubbing, turn on high-vacuum scrubbing, and use a molecular pump to evacuate the inside of the vacuum induction melting furnace. Repeat at least 1 to 3 times to evacuate the interior of the vacuum induction melting furnace to the maximum. Excellent vacuum degree 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 scrubbing reaches the optimum vacuum degree, the hollow copper coil 3 is heated by the power supply in the power box with a heating power of 5-8KW, and the heated hollow copper coil 3 will make the CaO-MgO-Al 2 O 3 refractory to CaO-MgO-Al 2 O 3 The nickel-based superalloy feedstock in the material crucible is heated to melt. Among them, in the process of heating and melting the nickel-based superalloy raw materials, the heating power is first increased at a speed of 1-2KW/h, and when the nickel-based superalloy raw materials start to melt, the molecular pump is closed and the protective gas is filled, as one of the present invention. In a specific embodiment, the gas pressure of the filled protective gas is controlled at 1˜9×10 4 Pa. At the same time, the heating power is increased to 5-8KW at a speed of 5-10KW/h, and the temperature is kept for 0.1-0.5h until the nickel-based superalloy raw materials are melted 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 box with a heating power of 3-5KW, and the heated hollow copper coil heats and refines the molten nickel-based superalloy raw material. Among them, in this process, the heating power when the nickel-based superalloy raw materials are first melted into molten metal is 5-8KW, and the heating power is reduced to 3-5KW at a speed of 2-5KW/h, and the temperature is kept for 0.5-1.5h. Alloy raw materials are heated and refined.

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 smelting temperature in the whole smelting process of the nickel-based superalloy raw material in the vacuum induction smelting furnace is controlled at 1450-1750 ℃, and the smelting time is 2-15 h. Among them, the melting temperature in the vacuum induction melting furnace is observed and determined by 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 melting stage, it is best to repeat the low-vacuum scrubbing of the furnace chamber of the vacuum induction melting furnace 3 times.

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 melting stage, it is best to repeat the high-vacuum scrubbing of the furnace chamber of the vacuum induction melting furnace twice. And the vacuum degree reached by high-vacuum scrubbing is 3×10 -3 Pa.

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 melting stage, the pressure in the furnace cavity of the melting furnace under high vacuum is 1-8 × 10 -3 Pa, and the pressure in the furnace cavity of the melting furnace under low vacuum is 1-30 Pa. good.

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 nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material provided by the present invention will be further described in detail 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。Using nickel-based superalloy GH4169 as raw material. The nickel-based superalloy GH4169 was placed in a CaO-MgO-Al 2 O 3 refractory crucible, and then the crucible was placed in the hollow copper coil in the hearth of the vacuum induction melting furnace. Vacuum scrubbing, and then carry out 2 high vacuum scrubbing to make the vacuum degree in the furnace chamber of the vacuum induction melting furnace reach 3 × 10 -3 Pa, and then heat the hollow copper coil through the power supply in the power box, and then pass the hollow copper coil to the crucible. The inner nickel-based superalloy GH4169 is heated. During the heating and melting process, the heating power was first increased to 1.5KW at a rate of 1KW/h, and when the nickel-based superalloy GH4169 began to melt, a high vacuum of 3×10 -3 to 1×10 -1 Pa was maintained. 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 rate of 2.5KW/h to refine the molten nickel-based superalloy GH4169, keep it at a temperature of 1550 ° C for 0.5h and then cool it naturally, so that the nickel-based superalloy GH4169 solidifies inside the crucible, take out the crucible The solid obtained by internal solidification, the sample obtained at this time is designated 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。Using nickel-based superalloy GH4169 as raw material. The alloy ingot was placed in the Al 2 O 3 crucible of the inner coil of the vacuum induction furnace, and the power was applied under 3 times of low vacuum and 2 times of high vacuum to reach the vacuum degree of 3 × 10 -3 Pa, and the high vacuum was maintained at 3 × 10 - 3 to 1×10 -1 Pa state. After 6.7KW high-power rapid melting and 3-3.4KW medium-power refining, it was kept at 1550°C for 30min and then cooled inside the crucible, and 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。Using nickel-based superalloy GH4169 as raw material. The alloy ingot is placed in the MgO crucible of the inner coil of the vacuum induction furnace, and the power is applied under the vacuum degree of 3×10 -3 Pa after 3 times of low vacuum and 2 times of high vacuum, and the high vacuum is maintained at 3×10 -3 ~1 ×10 -1 Pa state. After 6.7KW high-power rapid melting and 3-3.4KW medium-power refining, it was kept at 1550°C for 30min and then cooled inside the crucible, and 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-based superalloy GH4169 samples obtained by smelting in the embodiment of the present invention and the comparative example 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 the embodiment and the comparative example, respectively. The test results are shown in Table 1. As can be seen from Table 1, Example 1 of the present invention uses a CaO-MgO-Al 2 O 3 refractory crucible to obtain the high-temperature nickel-based alloy sample A1 obtained by melting according to the shown smelting process, compared to Comparative Example 1 using Al 2 O 3 Crucibles and Comparative Examples 2 High-temperature nickel-based alloy samples A2 and A3 obtained by smelting MgO crucibles, the oxygen content in the alloys is low, thus illustrating the use of CaO-MgO-Al 2 O 3 refractory crucibles smelting in the embodiment of the present invention to obtain The nickel-based superalloys are of higher quality.

表1Table 1

Figure BDA0003446595680000101
Figure BDA0003446595680000101

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 using 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 alloy after smelting was compared with those of Comparative Examples 1 and 1. Comparative example 2 is cleaner. By dissecting the interface between the nickel-based superalloy and the crucible, it is found that the CaO-MgO-Al 2 O 3 refractory material shows obvious non-wetting, which further indicates that CaO-MgO-Al 2 O 3 refractory material crucible melting nickel-based superalloy shows better corrosion resistance to nickel-based alloy melt.

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 inclusions and the distribution of different sizes and numbers of inclusions in the nickel-based superalloys obtained by smelting Example 1, Comparative Example 1 and Comparative Example 2 of the present invention, it can be seen that the present invention The nickel-based superalloy prepared in Example 1 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 invention provides a method for preparing a high metallurgical quality nickel-based superalloy based on a CaO-MgO-Al 2 O 3 (CMA) refractory material. The CaO-MgO-Al 2 O 3 refractory material is used as the crucible material for melting, and the The control of vacuum smelting process flow, smelting temperature, smelting time and protective gas pressure during smelting can effectively prevent oxidation pollution of nickel-based superalloy melt, and can smelt to obtain nickel-based superalloy with high metallurgical quality.

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 and not to limit them. 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 Modifications or equivalent substitutions without departing from the spirit and scope of the technical solutions of the present invention should be included in the scope of the claims of the present invention.

Claims (10)

1.一种基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于,包括如下步骤:1. a method based on CaO-MgO-Al 2 O 3 refractory smelting nickel-based superalloy, is characterized in that, comprises the 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 an induction melting device to obtain a nickel-based superalloy. 2.根据权利要求1所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于,所述CaO-MgO-Al2O3耐火材料坩埚由下述方法制备:2. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 1, wherein the CaO-MgO-Al 2 O 3 refractory material 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 the raw material powder of the CaO-MgO-Al 2 O 3 refractory material with the 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 rammed or cold isostatically pressed into a crucible blank; 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 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. 3.根据权利要求2所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于:所述粘结剂为硼砂、石蜡、丙三醇、无水乙醇中的一种或几种。3. the method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 2, is characterized in that: described binder is borax, paraffin, glycerol, dehydrated alcohol one or more of them. 4.根据权利要求1所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于,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:4. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 1, wherein the induction melting equipment is a vacuum induction melting furnace, and the vacuum induction melting furnace comprises : 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 inside of the openable spherical furnace and the periphery of the crucible, the hollow copper coil is connected to a power supply 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;An asbestos cloth is arranged between the crucible and the hollow copper coil, the asbestos cloth wraps the bottom and the upper part of the crucible, alumina sand is filled between the asbestos cloth and the bottom of the crucible, and the asbestos cloth and the crucible are The upper part is filled with magnesia sand; 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 chamber 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. 5.根据权利要求4所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于:所述低真空泵为机械泵,所述高真空泵为分子泵。5 . The method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials according to claim 4 , wherein the low vacuum pump is a mechanical pump, and the high vacuum pump is a molecular pump. 6 . 6.根据权利要求5所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于,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:6. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 5, characterized in that, the smelting of nickel-based superalloy raw materials in the vacuum induction melting furnace comprises 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 interior 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 operations 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 with a heating power of 5-8KW by the power supply in the power box, and the heated hollow copper coil heats the nickel-based superalloy raw material in the CaO-MgO-Al 2 O 3 refractory crucible to melt; 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 box with a heating power of 3-5KW, and the heated hollow copper coil heats and refines the molten nickel-based superalloy raw material. 7.根据权利要求6所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于:7. the method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 6, is characterized in that: 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;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, and when the nickel-based superalloy raw material begins to melt, the vacuum pump is turned off, and the protective gas is filled, while the heating power is 5-10KW. The heating power is increased to 5-8KW at the speed of /h, and the temperature is kept for 0.1-0.5h until the nickel-based superalloy raw materials are melted 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。The heating power is then reduced to 3-5KW at a speed of 2-5KW/h, and the molten nickel-based superalloy raw material is heated and refined for 0.5-1.5h of heat preservation. 8.根据权利要求7所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于: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。8. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 7, wherein the vacuum induction melting furnace controls the smelting temperature in the smelting process of nickel-based superalloy raw materials At 1450~1750℃, the smelting time is 2~15h. 9.根据权利要求8所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于: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。9 . The method for smelting nickel-based superalloys based on CaO-MgO-Al 2 O 3 refractory materials according to claim 8 , wherein the smelting temperature in the vacuum induction melting furnace is observed and determined by an infrared thermometer. 10 . 10.根据权利要求7所述的基于CaO-MgO-Al2O3耐火材料熔炼镍基高温合金的方法,其特征在于:所述熔炼过程中保护气体的气压控制在1~9×104Pa。10. The method for smelting nickel-based superalloy based on CaO-MgO-Al 2 O 3 refractory material according to claim 7, characterized in that: the gas pressure of the protective gas in the smelting process is controlled at 1~9×10 4 Pa .
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